monthly monitoring report july 2015 · 317 e. main street ventura, ca 93001 tel: (805) 585-2110...

317 E. Main Street Ventura, CA 93001

Tel: (805) 585-2110 Fax: (805) 585-2111

MONTHLY MONITORING REPORT JULY 2015 Date: September 9, 2015

Prepared For: Rose Marie Caraway, Remedial Project Manager/Environmental Scientist U.S. Environmental Protection Agency, Region 9 75 Hawthorne Street, SFD 7-2 San Francisco, California 94105

Prepared By:

Max Ramos, E.I.T., Staff Environmental Engineer, OTIE Lindsey Larsen, Staff Environmental Scientist, OTIE John Wingate, P.E., Project Manager, OTIE

Re: July 2015 Plant Influent and Effluent Sampling Results for the Pemaco Superfund Site Treatment Plant, Maywood, California

1.0 INTRODUCTION The United States Environmental Protection Agency (EPA) is currently implementing the Long-Term Response Action (LTRA) at the Pemaco Superfund Site. Oneida Total Integrated Enterprises, LLC. (OTIE) performed monthly monitoring work for the EPA under contract by the United States Army Corps of Engineers, Los Angeles District Contract Number W912PL 13-D-0017, Task Order 0002.

OTIE prepared this Report to summarize the results of monthly plant influent and effluent sampling performed on July 23, 2015 at the Pemaco Superfund Site Treatment Plant (Plant).

The influent and effluent water samples (SP-201 and SP-209, respectively), and influent and effluent vapor samples (SP-104 and SP-108, respectively) were analyzed for volatile organic compounds (VOCs) and 1,4-dioxane. Samples were analyzed in accordance with the Draft Final Sampling and Analysis Plan, (Field Sampling Plan and Quality Assurance Project Plan), Long-Term Response Action for the Pemaco Remedial Action (OTIE 2015a).

Monthly water and vapor sampling is performed to demonstrate compliance with Los Angeles County Sanitation District (LACSD) limits and South Coast Air Quality Management District (SCAQMD) guidance; confirm liquid phase granular activated carbon (LGAC) and vapor phase granular activated carbon (VGAC) effectiveness; and summarize data trends necessary for evaluation of remedial progress. The metric for “mass removal” is evaluated in the Quarterly Operations and Maintenance Report.

The groundwater treatment system (GTS) and vapor treatment system (VTS) were not in operation during the beginning of July to accommodate the well redevelopment task. The GTS operated July 21 – 31 and the VTS operated July 22 – 31. Prior to the July 2015 sampling event, the GTS and VTS were operated minimally in June 2015 (84.5 hours and 12 hours, respectively) to accommodate the June 2015 Semiannual Groundwater Monitoring Event, pump repair, and well redevelopment tasks. Please refer to the Second Quarter 2015 Operation and Maintenance Report (OTIE 2015b) and the most recent Operations Summary located on the Pemaco SharePoint website for additional operations details.

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SEMS-RM DOCID # 1163850

Monthly Monitoring Report July 2015 Plant Influent and Effluent Sampling Results Pemaco Superfund Site, Maywood, California

2.0 PLANT WATER SAMPLING RESULTS Influent and effluent water grab samples were collected on July 23, 2015 and the detected analytical results are summarized in Table 1. The laboratory analysis was performed by Eurofins CalScience, Inc. The laboratory report containing the full list of analytes is provided in Attachment 1. The influent sample results represent a composite of flow from the following active wells screened in the Perched and Exposition Zones:

• Perched Zone (dual-phase extraction [DPE]): PB-01, PB-02, PB-03, PB-05, PC-06, PD-04, PD-05, and PD-06.

• Exposition Zones (groundwater only): DA-01, DA-04, DA-07, DB-01, DB-03, DB-04, DB-05, DB-07, DB-09, and DAB-08.

Table 1 – Monthly Summary of Detected VOCs in Influent/Effluent Water Samples

Analyte Name Method

Sample Location Sample ID

Sample Date

SP-201 (Influent) SP-201-20150723

7/23/2015

SP-209 (Effluent) SP-209-20150723

7/23/2015

SSRL Unit Result Result

1,2,4-Trimethylbenzene SW8260B 5 μg/L 7.7 <0.36

1,4-Dioxane (P-Dioxane) SW8270C 1* μg/L 8.3 12**

cis-1,2-Dichloroethene SW8260B 6 μg/L 9.1 <0.48

Ethylbenzene SW8260B 300 μg/L 1.9 <0.14

Naphthalene SW8260B NC μg/L 19 <2.5

N-Butylbenzene SW8260B NC μg/L 2.2 <0.23

Sec-Butylbenzene SW8260B NC μg/L 1.3 <0.25

Trichloroethene SW8260B 5 μg/L 92 <0.37 Notes: 1. * - Indicates value is a "California Notification Level" which is less than the SSRL of 3.0, listed in the ROD (EPA 2005). 2. ** - Indicates effluent concentration was higher than influent concentration. The difference in the influent concentration

and the effluent concentration of 1,4- dioxane is a result of the desorption properties of 1,4-dioxane and does not indicate breakthrough conditions.

3. Bold indicates a sample detection. 4. μg/L = micrograms per liter; ID = identification; SSRL = site-specific remediation level; NC = no criteria established for this

analyte; < = indicates compound was not detected above the method detection limits. 5. Effluent water quality satisfied the LACSD permit limit of 1,000 μg/L.

2.1. PROCESS WATER INFLUENT (SP-201) DISCUSSION The following VOCs are associated with groundwater plumes being monitored as part of the semi-annual groundwater monitoring program and are therefore pertinent for discussion:

• Cis-1,2-dichloroethene (cis-1,2-DCE) was detected at a concentration of 9.1 μg/L, slightly lower than the previous month (13 μg/L). The cis-1,2-DCE concentration in process water influent samples from the previous 24 months shows a generally decreasing trend (Figure 1).

• Trichloroethene (TCE) was detected at a concentration of 92 μg/L, lower than the previous month (180 μg/L). The TCE concentration in process water influent samples from the previous

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24 months shows relatively large variations between monthly samples, with no apparent concentration trend. (Figure 2).

• 1,4-Dioxane was detected at a concentration of 8.3 µg/L, slightly lower than the previous month (14 μg/L). (Figure 3). The 1,4–dioxane concentration in process water influent from the previous 24 months shows relatively large variations between monthly samples, with a generally increasing trend.

Figure 1 – Historical Concentrations of cis-1,2-Dichloroethene in Influent Water

Notes for Figures 1: 1. Data collected over a 24 month period beginning in August 2013. Concentration values reflected on the figure represent

samples collected during monthly monitoring events. 2. Values that were below the laboratory detection limit are expressed as concentrations of zero.

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Monthly Monitoring Report July 2015 Plant Influent and Effluent Sampling Results Pemaco Superfund Site, Maywood, California Figure 2 – Historical Concentrations of Trichloroethene in Influent Water

Figure 3 – Historical Concentrations of 1,4-Dioxane in Influent Water

Notes for Figures 2 and 3: 1. Data collected over a 24 month period beginning in August 2013. Concentration values reflected on the figure represent

samples collected during monthly monitoring events. 2. Values that were below the laboratory detection limit are expressed as concentrations of zero.

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Monthly Monitoring Report July 2015 Plant Influent and Effluent Sampling Results Pemaco Superfund Site, Maywood, California 2.2. PROCESS WATER EFFLUENT (SP-209) DISCUSSION The water effluent quality satisfied the LACSD permit limit for total VOCs of 1,000 μg/L. VOCs detected in the influent were removed from the effluent with the exception of 1,4-dioxane, which has a low adsorptive capacity. Based on the results shown in Table 1, the LGAC demonstrated satisfactory VOC removal.

3.0 PLANT VAPOR SAMPLING RESULTS The influent and effluent vapor samples were collected in 1-liter SUMMA® canisters on July 23, 2015. The analytical results for this event are summarized in Table 2. The laboratory analysis was performed by ALS Environmental and the laboratory report is provided as Attachment 2. The July 2015 influent vapor sample represents a composite of concentrations from active DPE wells (PB-01, PB-02, PB-03, PB-05, PC-06, PD-04, PD-05 and PD-06), all screened in the Perched Zone.

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Monthly Monitoring Report July 2015 Plant Influent and Effluent Sampling Results Pemaco Superfund Site, Maywood, California Table 2 – Summary of Detected VOCs in Influent and Effluent Vapor Samples

Analyte Name

Sample Location Sample ID

Sample Date

SP-104 (Influent) SP-104-20150723

7/23/2015

SP-108 (Effluent) SP-108-20150723

7/23/2015 Method Unit Result Result

1,1-Dichloroethane TO15 μg/m3 <11 8.6* 1,1-Dichloroethene TO15 μg/m3 58 55 1,1,1-Trichloroethane TO15 μg/m3 <11 4.3* 1,2,4-Trimethylbenzene TO15 μg/m3 630 1.2 J 1,3,5-Trimethylbenzene TO15 μg/m3 20 J <0.52 2-Butanone TO15 μg/m3 <14 5.5 J* 2-Hexanone TO15 μg/m3 <11 0.95 J* Acetone TO15 μg/m3 <52 69** Benzene TO15 μg/m3 17 J <0.52 Carbon Disulfide TO15 μg/m3 <10 0.81 J* Chloroform TO15 μg/m3 <11 5.2* cis-1,2-Dichloroethene TO15 μg/m3 18 J 160** Cumene TO15 μg/m3 82 <0.49 Cyclohexane TO15 μg/m3 580 450 Dichlorodifluoromethane TO15 μg/m3 <11 0.74 J* Ethanol TO15 μg/m3 <54 4.8 J* Ethylbenzene TO15 μg/m3 980 <0.52 Isopropylbenzene TO15 μg/m3 82 <0.49 Naphthalene TO15 μg/m3 490 1.2 J N-Heptane TO15 μg/m3 200 <0.55 N-Hexane TO15 μg/m3 3500 160 N-Propylbenzene TO15 μg/m3 260 <0.52 Tetrachloroethene TO15 μg/m3 890 <0.46 Tetrahydrofuran TO15 μg/m3 14 J 14 trans-1,2-Dichloroethene TO15 μg/m3 <13 5* Trichloroethene TO15 μg/m3 39 <0.46 Vinyl chloride TO15 μg/m3 <11 0.56 J* Notes: * - Indicates a compound detected in effluent sample and not in influent sample as a result of higher detection limits for influent analysis. Significantly higher concentrations of VOCs in the influent sample resulted in higher detection limits for the influent sample than the effluent sample. ** - Indicates effluent sample concentration was higher than influent sample concentration as a result of preferential desorption. A complete listing of analytes is found in the laboratory report (Attachment 3). 3. Bold indicates sample detection. μg/m3 = micrograms per cubic meter; ID = identification; J = estimated value; < = indicates compound was not detected above the method detection limits.

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Monthly Monitoring Report July 2015 Plant Influent and Effluent Sampling Results Pemaco Superfund Site, Maywood, California 3.1. PROCESS VAPOR INFLUENT (SP-204) DISCUSSION Influent vapor concentrations over the past 23 months are presented in Figure 4.

Figure 4 – Historical Influent VOC Concentrations in Vapor

Notes: 1. Monthly data collected over a 23 month period beginning in September 2013. Concentration values reflected on the figure

represent samples collected during monthly monitoring events.

The sum of VOCs detected in plant vapor influent shows an increasing trend, as seen on Figure 4. The trend is biased by the high VOC concentrations observed during the months of January and February 2015. This concentration spike is attributed to the shutdown of the VTS system from December 4, 2014 to January 16, 2015 for the Flameless Thermal Oxidizer (FTO) removal work. The July 2015 influent vapor VOC concentration (7860 μg/m3) is consistent with influent vapor VOC concentrations prior to the VTS shutdown.

3.2. PROCESS VAPOR EFFLUENT (SP-208) DISCUSSION Destruction removal efficiency (DRE) is calculated to evaluate the performance of the VGAC. The DRE equals the mass difference between the influent and effluent divided by the total mass in the influent. The sum of VOCs detected in the influent is 7860 μg/m3; the sum of VOCs detected in the effluent is 947 μg/m3. The resulting DRE was 88% for July 2015.

The Pemaco Treatment Plant air effluent is not formally permitted but does comply with the SCAQMD permit guidance for health risk. Using SCAQMD protocols, a Tier 2 Air Screening Risk Assessment (Attachment 3) was performed for the purpose of calculating the maximum incremental cancer risk

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Monthly Monitoring Report July 2015 Plant Influent and Effluent Sampling Results Pemaco Superfund Site, Maywood, California (MICR), the chronic hazard index (HIc), and acute hazard index (HIa) (SCAQMD 2005). A summary of the results from the Tier 2 Air Screening Risk Assessment is presented in Table 3.

Table 3 – Summary of Tier 2 Air Screening Risk Assessment for Toxic Air Contaminants (TACs) to Nearest Receptor (75 Meters from Stack)

Maximum Individual Cancer Risk1 (MICR)

Chronic Hazard Index1 (HIc)

Acute Hazard Index1 (HIa)

Toxic Air Contaminants2 (including carcinogens and non-carcinogens) 1.66E-09 1.59E-05 1.31E-10

Notes: 1. Cancer Risk and Chronic and Acute Hazard Index to nearest receptor at approximately 75 meters from stack. 2. Refer to California Health and Safety Code 39655. "Toxic Air Contaminant" means an air pollutant which may cause or

contribute to an increase in mortality or in serious illness, or which may pose a present or potential hazard to human health. A substance that is listed as a hazardous air pollutant pursuant to subsection (b) of Section 112 of the federal act (42 U.S.C. Sec. 7412 [b]) is a toxic air contaminant.

As shown in Table 3, the risk associated with potential exposure to the toxic air contaminants (TACs) at a distance of 75 meters from the stack are roughly three orders of magnitude less than “one-in-a-million” (1 x 10-6). Also, both acute and chronic hazardous indexes from potential exposure to TACs are less than 1, indicating that emissions comply with the SCAQMD permit regulations.

4.0 CONCLUSIONS VTS and GTS shutdowns occurred during early July to accommodate the well redevelopment event, plant maintenance, and repairs which will be reported in the 2015 Third Quarter Operations and Maintenance Report. The VTS and GTS resumed normal operation on July 22, 2015 and July 21, 2015, respectively.

Results of the July 2015 plant water and vapor sampling demonstrated compliance with LACSD permit limits and SCAQMD permit guidance. LGAC and VGAC both demonstrated satisfactory VOC removal for plant water and plant vapor, respectively.

The cis-1,2-DCE concentration in process water influent samples from the previous 24 months shows a generally decreasing trend. The TCE concentration in process water influent samples from the previous 24 months shows relatively large variations between monthly samples, with no apparent concentration trend over time. The 1,4–dioxane concentration in process water influent samples from the previous 24 months shows relatively large variations between monthly samples, with a generally increasing trend.

Further investigation of VOCs in groundwater upgradient of the Pemaco Site is being planned to determine if offsite sources may be contributing to the treatment plant influent.

The July 2015 influent vapor VOC concentration is consistent with influent vapor VOC concentrations prior to the VTS shutdown.

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5.0 REFERENCES Oneida Total Integrated Enterprises (OTIE). 2015a. Draft-Final Sampling and Analysis Plan (Field

Sampling Plan and Quality Assurance Project Plan), Long-Term Response Action for the Pemaco Remedial Action. February.

_____. 2015b. 2015 Second Quarter Operation and Maintenance Report (April – June), Pemaco Superfund Site, 5973 District Boulevard, Maywood, California. August.

South Coast Air Quality Management District. 2005. Risk Assessment Procedures for Rules 1401 and 212 Version 7.0, Permit Application Package “L” Rules 1401 and 212 Version 7.0. July 1.

ATTACHMENTS Attachment 1 Lab Report from Eurofins CalScience, Inc.

Attachment 2 Lab Report from ALS Environmental

Attachment 3 Tier 2 Air Screening Risk Assessment for VOCs to Nearest Receptor, Approximately 75 Meters from Stack, Pemaco Superfund Site, Maywood, California

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ATTACHMENT 1

Lab Report from Eurofins CalScience, Inc.

WORK ORDER NUMBER: 15-07-1506

Analytical Report ForClient: OTIE

Client Project Name: Pemaco - MonthlyAttention: Orval Osbourne

317 East Main StreetVentura, CA 93001-2624

Approved for release on by:Virendra PatelProject Manager

AIR SOIL WATER MARINE CHEMISTRY

Eurofins Calscience, Inc. (Calscience) certifies that the test results provided in this report meet all NELAC requirements for parameters for which accreditation isrequired or available. Any exceptions to NELAC requirements are noted in the case narrative. The original report of subcontracted analyses, if any, is attached tothis report. The results in this report are limited to the sample(s) tested and any reproduction thereof must be made in its entirety. The client or recipient of thisreport is specifically prohibited from making material changes to said report and, to the extent that such changes are made, Calscience is not responsible, legally orotherwise. The client or recipient agrees to indemnify Calscience for any defense to any litigation which may arise.

07/30/2015

Page 1 of 20

mailto:[email protected]

https://www.calscience.com/clientwebaccess/login.aspx

Contents

7440 Lincoln Way, Garden Grove, CA 92841-1427 • TEL: (714) 895-5494 • FAX: (714) 894-7501

Client Project Name: Pemaco - Monthly

Work Order Number: 15-07-1506

1 Work Order Narrative. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3

2 Sample Summary. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4

3 Detections Summary. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

4 Client Sample Data. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 64.1 1,4-Dioxane by EPA 8270C (M) Isotope Dilution (Aqueous). . . . . . . . . . . . . . . . . . . 64.2 EPA 8260B Volatile Organics (Aqueous). . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

5 Quality Control Sample Data. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 135.1 MS/MSD. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 135.2 LCS/LCSD. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

6 Sample Analysis Summary. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17

7 Glossary of Terms and Qualifiers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18

8 Chain-of-Custody/Sample Receipt Form. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19

Page 2 of 20

Condition Upon Receipt: Samples were received under Chain-of-Custody (COC) on 07/23/15. They were assigned to Work Order 15-07-1506. Unless otherwise noted on the Sample Receiving forms all samples were received in good condition and within the

recommended EPA temperature criteria for the methods noted on the COC. The COC and Sample Receiving Documents are

integral elements of the analytical report and are presented at the back of the report. Holding Times: All samples were analyzed within prescribed holding times (HT) and/or in accordance with the Calscience Sample Acceptance

Policy unless otherwise noted in the analytical report and/or comprehensive case narrative, if required. Any parameter identified in 40CFR Part 136.3 Table II that is designated as "analyze immediately" with a holding time of <= 15

minutes (40CFR-136.3 Table II, footnote 4), is considered a "field" test and the reported results will be qualified as being

received outside of the stated holding time unless received at the laboratory within 15 minutes of the collection time. Quality Control: All quality control parameters (QC) were within established control limits except where noted in the QC summary forms or

described further within this report. Subcontractor Information: Unless otherwise noted below (or on the subcontract form), no samples were subcontracted. Additional Comments: Air - Sorbent-extracted air methods (EPA TO-4A, EPA TO-10, EPA TO-13A, EPA TO-17): Analytical results are converted from

mass/sample basis to mass/volume basis using client-supplied air volumes. Solid - Unless otherwise indicated, solid sample data is reported on a wet weight basis, not corrected for % moisture. All QC

results are always reported on a wet weight basis.

Work Order Narrative


Work Order: 15-07-1506 Page 1 of 1

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Sample Identification Lab Number Collection Date and Time Number ofContainers

Matrix

SP-201-20150723 15-07-1506-1 07/23/15 08:15 4 Aqueous

SP-209-20150723 15-07-1506-2 07/23/15 08:00 4 Aqueous

Sample Summary


Client: OTIE

317 East Main Street

Ventura, CA 93001-2624

Work Order: 15-07-1506

Project Name: Pemaco - Monthly

PO Number: 2014166

Date/TimeReceived:

07/23/15 14:10

Number ofContainers:

8

Attn: Orval Osbourne

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Subcontracted analyses, if any, are not included in this summary.

SP-201-20150723 (15-07-1506-1)

n-Butylbenzene 2.2 1.0 ug/L EPA 8260B EPA 5030C

sec-Butylbenzene 1.3 1.0 ug/L EPA 8260B EPA 5030C

c-1,2-Dichloroethene 9.1 1.0 ug/L EPA 8260B EPA 5030C

Ethylbenzene 1.9 1.0 ug/L EPA 8260B EPA 5030C

Naphthalene 19 10 ug/L EPA 8260B EPA 5030C

Trichloroethene 92 1.0 ug/L EPA 8260B EPA 5030C

1,2,4-Trimethylbenzene 7.7 1.0 ug/L EPA 8260B EPA 5030C

1,4-Dioxane 8.3 1.0 ug/L EPA 8270C (M) IsotopeDilution

EPA 3510C

SP-209-20150723 (15-07-1506-2)

1,4-Dioxane 12 1.0 ug/L EPA 8270C (M) IsotopeDilution

EPA 3510C

Detections Summary


Client: OTIE




Project Name: Pemaco - Monthly

Received: 07/23/15

Attn: Orval Osbourne Page 1 of 1

Client SampleID

Analyte Result Qualifiers RL Units Method Extraction

* MDL is shown

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Client Sample Number Lab SampleNumber

Date/TimeCollected

Matrix Instrument DatePrepared

Date/TimeAnalyzed

QC Batch ID

SP-201-20150723 15-07-1506-1-F 07/23/1508:15

Aqueous GC/MS DDD 07/24/15 07/24/1517:57

150724L08

Parameter Result RL DF Qualifiers

1,4-Dioxane 8.3 1.0 1.00

Surrogate Rec. (%) Control Limits Qualifiers

Nitrobenzene-d5 66 56-123

1,4-Dioxane-d8(IDS-IS) 38 30-120

SP-209-20150723 15-07-1506-2-F 07/23/1508:00

Aqueous GC/MS DDD 07/24/15 07/24/1518:13

150724L08


1,4-Dioxane 12 1.0 1.00




Method Blank 099-16-216-510 N/A Aqueous GC/MS DDD 07/24/15 07/24/1516:53

150724L08


1,4-Dioxane ND 1.0 1.00




Analytical Report


OTIE



Date Received: 07/23/15


Preparation: EPA 3510C

Method: EPA 8270C (M) Isotope Dilution

Units: ug/L

Project: Pemaco - Monthly Page 1 of 1

RL: Reporting Limit. DF: Dilution Factor. MDL: Method Detection Limit.

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Date/TimeCollected


Date/TimeAnalyzed

QC Batch ID

SP-201-20150723 15-07-1506-1-A 07/23/1508:15

Aqueous GC/MS R 07/23/15 07/24/1504:51

150723L030


Acetone ND 20 1.00

Benzene ND 0.50 1.00

Bromobenzene ND 1.0 1.00

Bromochloromethane ND 1.0 1.00

Bromodichloromethane ND 1.0 1.00

Bromoform ND 1.0 1.00

Bromomethane ND 10 1.00

2-Butanone ND 10 1.00

n-Butylbenzene 2.2 1.0 1.00

sec-Butylbenzene 1.3 1.0 1.00

tert-Butylbenzene ND 1.0 1.00

Carbon Disulfide ND 10 1.00

Carbon Tetrachloride ND 0.50 1.00

Chlorobenzene ND 1.0 1.00

Chloroethane ND 5.0 1.00

Chloroform ND 1.0 1.00

Chloromethane ND 10 1.00

2-Chlorotoluene ND 1.0 1.00


Dibromochloromethane ND 1.0 1.00

1,2-Dibromo-3-Chloropropane ND 5.0 1.00

1,2-Dibromoethane ND 1.0 1.00

Dibromomethane ND 1.0 1.00

1,2-Dichlorobenzene ND 1.0 1.00



Dichlorodifluoromethane ND 1.0 1.00

1,1-Dichloroethane ND 1.0 1.00


1,1-Dichloroethene ND 1.0 1.00

c-1,2-Dichloroethene 9.1 1.0 1.00

t-1,2-Dichloroethene ND 1.0 1.00

1,2-Dichloropropane ND 1.0 1.00



Analytical Report


OTIE






Method: EPA 8260B

Units: ug/L



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1,1-Dichloropropene ND 1.0 1.00

c-1,3-Dichloropropene ND 0.50 1.00

t-1,3-Dichloropropene ND 0.50 1.00

Ethylbenzene 1.9 1.0 1.00

2-Hexanone ND 10 1.00

Isopropylbenzene ND 1.0 1.00

p-Isopropyltoluene ND 1.0 1.00

Methylene Chloride ND 10 1.00

4-Methyl-2-Pentanone ND 10 1.00

Naphthalene 19 10 1.00

n-Propylbenzene ND 1.0 1.00

Styrene ND 1.0 1.00

1,1,1,2-Tetrachloroethane ND 1.0 1.00


Tetrachloroethene ND 1.0 1.00

Toluene ND 1.0 1.00

1,2,3-Trichlorobenzene ND 1.0 1.00


1,1,1-Trichloroethane ND 1.0 1.00

1,1,2-Trichloro-1,2,2-Trifluoroethane ND 10 1.00


Trichloroethene 92 1.0 1.00

Trichlorofluoromethane ND 10 1.00

1,2,3-Trichloropropane ND 5.0 1.00

1,2,4-Trimethylbenzene 7.7 1.0 1.00

1,3,5-Trimethylbenzene ND 1.0 1.00

Vinyl Acetate ND 10 1.00

Vinyl Chloride ND 0.50 1.00

p/m-Xylene ND 1.0 1.00

o-Xylene ND 1.0 1.00

Methyl-t-Butyl Ether (MTBE) ND 1.0 1.00


1,4-Bromofluorobenzene 95 80-120

Dibromofluoromethane 103 78-126

1,2-Dichloroethane-d4 102 75-135

Toluene-d8 106 80-120

Analytical Report


OTIE






Method: EPA 8260B

Units: ug/L



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Date/TimeCollected


Date/TimeAnalyzed

QC Batch ID

SP-209-20150723 15-07-1506-2-A 07/23/1508:00

Aqueous GC/MS R 07/23/15 07/24/1505:18

150723L030


Acetone ND 20 1.00








n-Butylbenzene ND 1.0 1.00

sec-Butylbenzene ND 1.0 1.00





















c-1,2-Dichloroethene ND 1.0 1.00





Analytical Report


OTIE






Method: EPA 8260B

Units: ug/L



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Ethylbenzene ND 1.0 1.00






Naphthalene ND 10 1.00


Styrene ND 1.0 1.00




Toluene ND 1.0 1.00






Trichloroethene ND 1.0 1.00














Toluene-d8 106 80-120

Analytical Report


OTIE






Method: EPA 8260B

Units: ug/L



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Date/TimeCollected


Date/TimeAnalyzed

QC Batch ID

Method Blank 099-14-001-17747 N/A Aqueous GC/MS R 07/23/15 07/24/1503:03

150723L030


Acetone ND 20 1.00








n-Butylbenzene ND 1.0 1.00

sec-Butylbenzene ND 1.0 1.00





















c-1,2-Dichloroethene ND 1.0 1.00





Analytical Report


OTIE






Method: EPA 8260B

Units: ug/L



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Ethylbenzene ND 1.0 1.00






Naphthalene ND 10 1.00


Styrene ND 1.0 1.00




Toluene ND 1.0 1.00






Trichloroethene ND 1.0 1.00














Toluene-d8 105 80-120

Analytical Report


OTIE






Method: EPA 8260B

Units: ug/L



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Quality Control Sample ID Type Matrix Instrument Date Prepared Date Analyzed MS/MSD Batch Number

SP-201-20150723 Sample Aqueous GC/MS DDD 07/24/15 07/24/15 17:57 150724S08

SP-201-20150723 Matrix Spike Aqueous GC/MS DDD 07/24/15 07/24/15 17:25 150724S08

SP-201-20150723 Matrix Spike Duplicate Aqueous GC/MS DDD 07/24/15 07/24/15 17:41 150724S08

Parameter SampleConc.

SpikeAdded

MSConc.

MS%Rec.

MSDConc.

MSD%Rec.

%Rec. CL RPD RPD CL Qualifiers

1,4-Dioxane 8.328 20.00 27.09 94 26.87 93 50-130 1 0-20

Quality Control - Spike/Spike Duplicate


OTIE








RPD: Relative Percent Difference. CL: Control Limits

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Quality Control Sample ID Type Matrix Instrument Date Prepared Date Analyzed MS/MSD Batch Number

SP-201-20150723 Sample Aqueous GC/MS R 07/23/15 07/24/15 04:51 150723S011

SP-201-20150723 Matrix Spike Aqueous GC/MS R 07/23/15 07/24/15 01:16 150723S011

SP-201-20150723 Matrix Spike Duplicate Aqueous GC/MS R 07/23/15 07/24/15 01:43 150723S011

Parameter SampleConc.

SpikeAdded

MSConc.

MS%Rec.

MSDConc.

MSD%Rec.

%Rec. CL RPD RPD CL Qualifiers

Benzene ND 50.00 50.75 101 52.10 104 74-122 3 0-21

Carbon Tetrachloride ND 50.00 51.48 103 51.52 103 60-144 0 0-21

Chlorobenzene ND 50.00 48.66 97 48.84 98 73-120 0 0-22

1,2-Dibromoethane ND 50.00 52.59 105 53.68 107 80-122 2 0-20

1,2-Dichlorobenzene ND 50.00 47.07 94 46.84 94 70-120 0 0-26

1,2-Dichloroethane ND 50.00 53.10 106 54.30 109 64-142 2 0-20

1,1-Dichloroethene ND 50.00 48.21 96 49.30 99 52-136 2 0-21

Ethylbenzene 1.903 50.00 52.77 102 53.90 104 77-125 2 0-24

Toluene ND 50.00 49.67 99 51.19 102 72-126 3 0-23

Trichloroethene 91.53 50.00 136.6 90 135.8 89 74-128 1 0-22

Vinyl Chloride ND 50.00 55.94 112 57.81 116 67-133 3 0-20

p/m-Xylene ND 100.0 96.17 96 97.69 98 63-129 2 0-25

o-Xylene ND 50.00 46.59 93 47.27 95 62-128 1 0-24

Methyl-t-Butyl Ether (MTBE) ND 50.00 43.91 88 47.94 96 68-134 9 0-21

Quality Control - Spike/Spike Duplicate


OTIE






Method: EPA 8260B



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Quality Control Sample ID Type Matrix Instrument Date Prepared Date Analyzed LCS Batch Number

099-16-216-510 LCS Aqueous GC/MS DDD 07/24/15 07/24/15 17:09 150724L08

Parameter Spike Added Conc. Recovered LCS %Rec. %Rec. CL Qualifiers

1,4-Dioxane 20.00 18.21 91 50-130

Quality Control - LCS


OTIE









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Total number of LCS compounds: 14

Total number of ME compounds: 0

Total number of ME compounds allowed: 1

LCS ME CL validation result: Pass

Quality Control Sample ID Type Matrix Instrument Date Prepared Date Analyzed LCS Batch Number

099-14-001-17747 LCS Aqueous GC/MS R 07/23/15 07/24/15 00:49 150723L030

Parameter Spike Added Conc. Recovered LCS %Rec. %Rec. CL ME CL Qualifiers

Benzene 50.00 48.47 97 80-120 73-127

Carbon Tetrachloride 50.00 47.23 94 67-139 55-151

Chlorobenzene 50.00 47.40 95 78-120 71-127

1,2-Dibromoethane 50.00 52.15 104 80-120 73-127

1,2-Dichlorobenzene 50.00 47.37 95 63-129 52-140

1,2-Dichloroethane 50.00 52.30 105 70-130 60-140

1,1-Dichloroethene 50.00 45.31 91 66-126 56-136

Ethylbenzene 50.00 49.52 99 80-123 73-130

Toluene 50.00 47.83 96 80-120 73-127

Trichloroethene 50.00 49.48 99 80-122 73-129

Vinyl Chloride 50.00 52.11 104 70-130 60-140

p/m-Xylene 100.0 93.41 93 75-123 67-131

o-Xylene 50.00 45.22 90 74-122 66-130

Methyl-t-Butyl Ether (MTBE) 50.00 45.87 92 69-129 59-139

Quality Control - LCS


OTIE






Method: EPA 8260B



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Method Extraction Chemist ID Instrument Analytical Location

EPA 8260B EPA 5030C 927 GC/MS R 2

EPA 8270C (M) Isotope Dilution EPA 3510C 928 GC/MS DDD 1

Sample Analysis Summary Report



Location 1: 7440 Lincoln Way, Garden Grove, CA 92841

Location 2: 7445 Lampson Avenue, Garden Grove, CA 92841

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Qualifiers Definition

* See applicable analysis comment.

< Less than the indicated value.

> Greater than the indicated value.

1 Surrogate compound recovery was out of control due to a required sample dilution. Therefore, the sample data was reported without furtherclarification.

2 Surrogate compound recovery was out of control due to matrix interference. The associated method blank surrogate spike compound wasin control and, therefore, the sample data was reported without further clarification.

3 Recovery of the Matrix Spike (MS) or Matrix Spike Duplicate (MSD) compound was out of control due to suspected matrix interference. Theassociated LCS recovery was in control.

4 The MS/MSD RPD was out of control due to suspected matrix interference.

5 The PDS/PDSD or PES/PESD associated with this batch of samples was out of control due to suspected matrix interference.

6 Surrogate recovery below the acceptance limit.

7 Surrogate recovery above the acceptance limit.

B Analyte was present in the associated method blank.

BU Sample analyzed after holding time expired.

BV Sample received after holding time expired.

CI See case narrative.

E Concentration exceeds the calibration range.

ET Sample was extracted past end of recommended max. holding time.

HD The chromatographic pattern was inconsistent with the profile of the reference fuel standard.

HDH The sample chromatographic pattern for TPH matches the chromatographic pattern of the specified standard but heavier hydrocarbonswere also present (or detected).

HDL The sample chromatographic pattern for TPH matches the chromatographic pattern of the specified standard but lighter hydrocarbons werealso present (or detected).

J Analyte was detected at a concentration below the reporting limit and above the laboratory method detection limit. Reported value isestimated.

JA Analyte positively identified but quantitation is an estimate.

ME LCS Recovery Percentage is within Marginal Exceedance (ME) Control Limit range (+/- 4 SD from the mean).

ND Parameter not detected at the indicated reporting limit.

Q Spike recovery and RPD control limits do not apply resulting from the parameter concentration in the sample exceeding the spikeconcentration by a factor of four or greater.

SG The sample extract was subjected to Silica Gel treatment prior to analysis.

X % Recovery and/or RPD out-of-range.

Z Analyte presence was not confirmed by second column or GC/MS analysis.

Solid - Unless otherwise indicated, solid sample data is reported on a wet weight basis, not corrected for % moisture. All QC results arereported on a wet weight basis.

Any parameter identified in 40CFR Part 136.3 Table II that is designated as "analyze immediately" with a holding time of <= 15 minutes(40CFR-136.3 Table II, footnote 4), is considered a "field" test and the reported results will be qualified as being received outside of thestated holding time unless received at the laboratory within 15 minutes of the collection time.

A calculated total result (Example: Total Pesticides) is the summation of each component concentration and/or, if "J" flags are reported,estimated concentration. Component concentrations showing not detected (ND) are summed into the calculated total result as zeroconcentrations.

Glossary of Terms and Qualifiers



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Return to Contents

Page 19 of 20

Chain of Custody

:.·OTIE • Oneida Tow.I lnteorated Enterpris~s

~ OTIE 317 East Main Street Ventura. CA 93001 Phone: (805) 585-211 O Fax: (805) 585-2111

Sampler Name: Brian Hendron

Report To:

Contact: Orval Osborne Company: OTI E Address: 317 East Main Street Ventura, CA 93001 Phone: (805) 585-4313 Fax: (805) 585-2111 E-Mail: [email protected]

Project Name: Pemaco - Monthly Project Number: 2014166

Project Location: 5973 S. District Date Requested 0 ood CA 0270 Blvd Ma

Lab PM: Virendra Patel, Ca1Science 714-895-5494

MS Client MSD Sample !D

SP-201-20150723

SP-209-20150723

atrix Key WN ~ Wastewater SE = Sediment

w =Water SO= Solid s = Soil DS = Drum Solid SL ~ Sludge DL = Drum Liquid MS ~ Miscellaneous L = Leachate OL ~ Oil Wl=Wipe

A =Air 0 =

r (D

X a N

b e 0 0 >

Sampling Date Time

7/23/15 0815 w X X X

7/23/15 0800 w X X X

DATE J l 7,2.'$ /5 DATE

'?

Container Key

f l.t' Preservative Key

1. Plastic 1, HCI, Cool to 4• 2. VOA Vial 2. H2S04, Cool to 4° 3. Sterile Plastic 3. HN03, Cool to 4• 4. Amber Glass 4. NaOH, Cool to 4• 5. Widemouth Glass 5. NaOH/Zn Acetate, Cool to 4 ' 6. Other 6. Cool to 4'

7. None

Bill To:

Contact -------------

Company: -------------

Address· ~15~.0~1-1~5....,00--Phone:--------------

Fax: --------------

PO#: _____ _ Quote: _____ _

COMPANY

COMMENTS: OTIE-specific EDDs needed 1 ,4-Dioxane: 1 uq/L RL

..

Shaded Areas For Internal Use Only _ 1 _ of 1 _

Lab Lot# Pa9k~~~ ~f3~1E;id > .· · ,y¢s\ :.N9 0') _·····

· ; ·.,:." . ;

•.: rteceive&dH:ice < · : :}J¥°%§\°1NgY

Additional Analyses I Remarks

Field grab pH reading at 0800 = 7.32

TIME I/ Z!("

DATE TIME

"1 /J.ol \S \I.Fm .

Date Received

Courier: Hand DelivereQ

Bill of Lading:

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Page 20 of 20.. ' .

~:: eurofi ns WORK ORDER NUMBER: 15-07- I 60-6 Calscience

SAMPLE RECEIPT CHECKLIST

CLIENT: ----"--C!J-· T._l=E=------'----"---------

COOLER~ OF _I_

DATE: 07 / 'Z-.Z / 2015

TEMPERATURE: (Criteria: 0.0°C- 6.0°C, not frozen except sediment/tissue)

Thermometer ID: SC5 (CF:-0.2°C); Temperature (w/o CF): 2 • .f °C (w/ CF): l.. • ? D Sample(s) outside temperature criteria (PM/APM contacted by: )

°C;.el Blank D Sarilple

D Sample(s) outside temperature criteria.but received on ice/chilled on same day of sampling

D Sample(s) received at ambient temperature; placed on ice for transport by courier

Ambient Temperature: D Air D Filter Checked by:, ~

CUSTODY SEAL:

Cooler D Present and Intact D Present but Not Intact ..0"Not Present

Sample(s) D Present and Intact D Present but Not Intact ..6' Not Present

D N/A

D N/A

Checked by:I 'iri>7 Checked by:! £f'b-f

SAMPLE CONDITION: Yes Noi

Chain-ofsCustody (COC) document(s) received with samples ......... .. ..................................... . .. J1 D

COC document(s) received complete ................................................................................. fo D

D Sampling date D Sampling time D Matrix D Number of containers

D No analysis requested D Not relinquished D No relinquished date D No relinquished time

Sampler's name indicated on COC ........ . ........... . .. . .. .. .. ... . ... ... .. ...... ...... .. ..... .. .... .. .. . ... .. ... . .. .

Sample container label(s) consistent with COC .. ... .... . .. .... .. .... .. ........ .. .. .................... . .. . ........ .

Sample container(s) intact and in good condition ...... .. ..... .. ... ... .... .. .. . .. . ............... . .. . ..... .. ...... .

Proper containers for analyses requested ......... .. . ... .. . ... .. .... .. . .... .. .... .. ........ . ..... . .. .. .. .. . .. ...... .

Sufficient volume/mass for analyses requested .. ... .... .. .... .. .... . ...... .. ............. .. .. . ... ......... .. .... .. .

Samples received within holding time ......... . ......................... . .. .. .. . .. ... ..... . .. ......... . ......... .. . .. .

Aqueous samples for certain analyses received within 15-minute holding time

D pH D Residual Chlorine D Dissolved Sulfide D Dissolved Oxygen .. .... .. .. .. ... ............ . ..

Proper preservation chemical(s) noted on COC and/or sample container . .. . .... . .. . .. . .. .. .. ...... . .. . .. . . .

Unpreserved aqueous sample(s) received for certain analyses

D Volatile Organics D Total Metals D Dissolved Metals

~·

£1.

Ef

)21 0 El'

D z(

Container(s) for certain analysis free of headspace .. .. .. . ..... . ................................................ .. .zf ¢'Volatile Organics D Dissolved Gases (RSK-175) D Dissolved Oxygen (SM 4500)

D Carbon Dioxide (SM 4500) · D Ferrous Iron (SM 3500) D Hydrogen Sulfide (Hach)

Tedlar™ bag(s) free of condensation . .. ... .. . .. . ... ... ... ... .. . ... .. .... .. . ... ... .. . .. . ... ... ... ... ... .. . ... ... ... ... D

D

D

D

D :

D

D

D

D

D

D

N/A

D

D

D

D

D

D

D

D

i6 D

D

z CONTAINER TYPE: S (Trip Blank Lot Number: ___ __... ___ ,)

Aqueous: D VOA JZl'VOAh D VOAna2 D 100PJ D 100PJna2 D 125AGB D 125AGBh D 125AGBp D 125P~

D 125PB:znna D 250AGB D 250CGB D 250CGBs D 250PB D 250PBn efsoOAGB D 500AGJ D 500AGJs I

D 500PB D 1AGB D 1AGBna2 D 1AGBs D 1PB D 1PBna D D D D __ _

Solid: D 4ozCGJ D 8ozCGJ D 16ozCGJ D Sleeve l___) D Encores® (__J D TerraCores® (_. __ ) D --,---

Air: D Tedlar™ D Canister D Sorbent Tube D PUF D Other Matrix ( ): D q __ _

Container: A= Amber, B = Bottle, C ::: Clear, E = Envelope, G = Glass, J = Jar, P = Plastic, and Z = Ziploc/Resealable Bag

Preservative: b = buffered, f::: filtered, h = HCI, n = HN0 3, na = NaOH, na2 = Na2S203, p = H3PQ4, Labeled/Checked by: Cf'7!' s = H2S04, u = ultra-pure, znna = Zn(CH3C02)2 + NaOH Reviewed byJ fir:b

t

2015-04-10 Revision

ATTACHMENT 2

Lab Report from ALS Environmental

2655 Park Center Dr., Suite A Simi Valley, CA 93065 T: +1 805 526 7161 F: +1 805 526 7270 www.alsglobal.com

R I G H T S O L U T I O N S | R I G H T P A R T N E R

LABORATORY REPORT August 13, 2015 Orval Osborne Oneida Total Integrated Enterprises (OTIE) 317 E. Main St. Ventura, CA 93001 RE: Pemaco Plant Vapor Monitoring Dear Orval: Enclosed are the results of the samples submitted to our laboratory on July 24, 2015. For your reference, these analyses have been assigned our service request number P1503012. All analyses were performed according to our laboratory’s NELAP and DoD-ELAP-approved quality assurance program. The test results meet requirements of the current NELAP and DoD-ELAP standards, where applicable, and except as noted in the laboratory case narrative provided. For a specific list of NELAP and DoD-ELAP-accredited analytes, refer to the certifications section at www.alsglobal.com. Results are intended to be considered in their entirety and apply only to the samples analyzed and reported herein. If you have any questions, please call me at (805) 526-7161. Respectfully submitted, ALS | Environmental Kelly Horiuchi Laboratory Director

1 of 128

http://www.alsglobal.com/


Kelly.Horiuchi

Kelly



Client: Oneida Total Integrated Enterprises (OTIE) Service Request No: P1503012 Project: Pemaco Plant Vapor Monitoring _______________________________________________________________________________

CASE NARRATIVE

The samples were received intact under chain of custody on July 24, 2015 and were stored in accordance with the analytical method requirements. Please refer to the sample acceptance check form for additional information. The results reported herein are applicable only to the condition of the samples at the time of sample receipt. Volatile Organic Compound Analysis The samples were analyzed for volatile organic compounds in accordance with EPA Method TO-15 from the Compendium of Methods for the Determination of Toxic Organic Compounds in Ambient Air, Second Edition (EPA/625/R-96/010b), January, 1999. This procedure is described in laboratory SOP VOA-TO15. The analytical system was comprised of a gas chromatograph / mass spectrometer (GC/MS) interfaced to a whole-air preconcentrator. This method is included on the laboratory’s NELAP and DoD-ELAP scope of accreditation, however it is not part of the AIHA-LAP accreditation. Any analytes flagged with an X are not included on the NELAP or DoD-ELAP accreditation. The canisters were cleaned, prior to sampling, down to the method reporting limit (MRL) reported for this project. Please note, projects which require reporting below the MRL could have results between the MRL and method detection limit (MDL) that are biased high. ______________________________________________________________________________________ The results of analyses are given in the attached laboratory report. All results are intended to be considered in their entirety, and ALS Environmental (ALS) is not responsible for utilization of less than the complete report. Use of ALS Environmental (ALS)’s Name. Client shall not use ALS’s name or trademark in any marketing or reporting materials, press releases or in any other manner (“Materials”) whatsoever and shall not attribute to ALS any test result, tolerance or specification derived from ALS’s data (“Attribution”) without ALS’s prior written consent, which may be withheld by ALS for any reason in its sole discretion. To request ALS’s consent, Client shall provide copies of the proposed Materials or Attribution and describe in writing Client’s proposed use of such Materials or Attribution. If ALS has not provided written approval of the Materials or Attribution within ten (10) days of receipt from Client, Client’s request to use ALS’s name or trademark in any Materials or Attribution shall be deemed denied. ALS may, in its discretion, reasonably charge Client for its time in reviewing Materials or Attribution requests. Client acknowledges and agrees that the unauthorized use of ALS’s name or trademark may cause ALS to incur irreparable harm for which the recovery of money damages will be inadequate. Accordingly, Client acknowledges and agrees that a violation shall justify preliminary injunctive relief. For questions contact the laboratory.

2 of 128




ALS Environmental – Simi Valley

CERTIFICATIONS, ACCREDITATIONS, AND REGISTRATIONS

Agency Web Site Number

AIHA http://www.aihaaccreditedlabs.org 101661

Arizona DHS http://www.azdhs.gov/lab/license/env.htm AZ0694

DoD ELAP http://www.pjlabs.com/search-accredited-labs L14-2

Florida DOH (NELAP)

http://www.doh.state.fl.us/lab/EnvLabCert/WaterCert.htm E871020

Maine DHHS http://www.maine.gov/dhhs/mecdc/environmental-health/water/dwp-services/labcert/labcert.htm

2014025

Minnesota DOH (NELAP)

http://www.health.state.mn.us/accreditation 876241

New Jersey DEP (NELAP)

http://www.nj.gov/dep/oqa/ CA009

New York DOH (NELAP)

http://www.wadsworth.org/labcert/elap/elap.html 11221

Oregon PHD (NELAP)

http://public.health.oregon.gov/LaboratoryServices/EnvironmentalLaboratoryAccreditation/Pages/index.aspx

4068-001

Pennsylvania DEP http://www.depweb.state.pa.us/labs 68-03307

(Registration) Texas CEQ (NELAP)

http://www.tceq.texas.gov/field/qa/env_lab_accreditation.html T104704413-

15-6 Utah DOH (NELAP)

http://www.health.utah.gov/lab/labimp/certification/index.html CA01627201

5-5

Washington DOE http://www.ecy.wa.gov/programs/eap/labs/lab-accreditation.html C946

Analyses were performed according to our laboratory’s NELAP and DoD-ELAP approved quality assurance program. A complete listing of specific NELAP and DoD-ELAP certified analytes can be found in the certifications section at www.alsglobal.com, or at the accreditation body’s website. Each of the certifications listed above have an explicit Scope of Accreditation that applies to specific matrices/methods/analytes; therefore, please contact the laboratory for information corresponding to a particular certification.

3 of 128


http://www.aihaaccreditedlabs.org/

http://www.azdhs.gov/lab/license/env.htm

http://www.pjlabs.com/search-accredited-labs

http://www.doh.state.fl.us/lab/EnvLabCert/WaterCert.htm

http://www.maine.gov/dhhs/mecdc/environmental-health/water/dwp-services/labcert/labcert.htm

http://www.maine.gov/dhhs/mecdc/environmental-health/water/dwp-services/labcert/labcert.htm

http://www.health.state.mn.us/accreditation

http://www.nj.gov/dep/oqa/

http://www.wadsworth.org/labcert/elap/elap.html



http://www.depweb.state.pa.us/labs

http://www.tceq.texas.gov/field/qa/env_lab_accreditation.html

http://www.health.utah.gov/lab/labimp/certification/index.html

http://www.ecy.wa.gov/programs/eap/labs/lab-accreditation.html


P1503012_Detail Summary_1508071446_RG.xls - DETAIL SUMMARY

Client: Oneida Total Integrated Enterprises (OTIE) Service Request: P1503012Project ID: Pemaco Plant Vapor Monitoring

Date Received: 7/24/2015Time Received: 15:00

Client Sample ID Lab Code MatrixDate

CollectedTime

CollectedContainer

IDPi1

(psig)Pf1

(psig)

SP-108-20150723 P1503012-001 Air 7/23/2015 14:00 1BV04202 -0.19 -5.20 XSP-104-20150723 P1503012-002 Air 7/23/2015 14:30 1BV04204 -0.04 5.10 X

ALS ENVIRONMENTAL

DETAIL SUMMARY REPORT

TO-1

5 - V

OC

Can

s

4 of 128

5 o

f 12

8

ALS Environmental .2666 Park CGnt0r Ortve, Sult& A

Simi Valley, CA 9306$

TEL: (805) 5;2S,7181. FJ{J(: (SOSI 526·7220

l.A.eCRATORYCllEhT.

OTIE J.O:JRE33:

317 E. Main Street Ventura CA 93001 ·

'TE~: "AX: E-IJAI~

'

'

CHAJN OF CUSTODY RECORD DATE: 7/23/2015

PAOia: ___ .:_ __ OF __ _:1c_ __

,. . P.O. NO:

Pemaco. Plant Vacor Monitorina 2014166 1•'1~,H:'.CI CCN1N..:1: LAS USE ONLY

Orval Osborne >.,~ DD-DODD ~IF1..":~~). ($<";1,V..TV~E: COEL T LOG CODE COOLER RECEIPT

Rl'IA" Mt:i,nl'll'l'ln 806.686.4313 805.585.2111 oosbome""otie.com, DODD Temp= °C

..... o sAMe DAY o 24 HR n 48HR D 72 HR D S DAYS [i] 10 DAYS REQUESTED ANALYSIS srec:A:.. REQUIR::'h1EN-s (r,CQTil)l>.I.".'· COST'Sf\\o\Y ArPL y~

D D D .. l'IPFO.r.;. IN8ffU.CTICi-,.3 . Please report EDDs in both ppmv ancl mg/m3 ., SP-108 started at-29.71 and ended at -0.44 ...

0

SP-104 started at -29.81 and ended at -0.24 ,_ :&' - SAMPLING ,..u.ur ll

;

us~ SAMPLE ID f'lq!d Point Nam& MATRIX co,r. ,' ONLY DATE TIME 0 CONTAINER TYPE >

SP-108-.20150723 Vapor sample Pon 108 07/23/15 14:00 air 1 X ' Bottle 1 BV04202 ..

SP-104-20150723 Vapor umpli> Port 104 07/23/15 14:30 air . .,

1 X Bottle 1 BV04204

,

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,-.

8/13/15 4:10 PMP1503012_Oneida Total Integrated Enterprises (OTIE)_Pemaco Plant Vapor Monitoring.xls - Page 1 of 1

ALS EnvironmentalSample Acceptance Check Form

Client: Oneida Total Integrated Enterprises (OTIE) Work order: P1503012Project: Pemaco Plant Vapor MonitoringSample(s) received on: 7/24/15 Date opened: 7/24/15 by: KKELPE

Note: This form is used for all samples received by ALS. The use of this form for custody seals is strictly meant to indicate presence/absence and not as an indication of

compliance or nonconformity. Thermal preservation and pH will only be evaluated either at the request of the client and/or as required by the method/SOP.Yes No N/A

1 Were sample containers properly marked with client sample ID? 2 Container(s) supplied by ALS? 3 Did sample containers arrive in good condition? 4 Were chain-of-custody papers used and filled out? 5 Did sample container labels and/or tags agree with custody papers? 6 Was sample volume received adequate for analysis? 7 Are samples within specified holding times? 8 Was proper temperature (thermal preservation) of cooler at receipt adhered to?

9 Was a trip blank received?

10 Were custody seals on outside of cooler/Box? Location of seal(s)? Sealing Lid?

Were signature and date included? Were seals intact? Were custody seals on outside of sample container?

Location of seal(s)? Sealing Lid? Were signature and date included? Were seals intact?

11 Is there a client indication that the submitted samples are pH preserved? Were VOA vials checked for presence/absence of air bubbles?

12 Tubes: Are the tubes capped and intact?

Do they contain moisture? 13 Badges: Are the badges properly capped and intact?

Are dual bed badges separated and individually capped and intact?

Lab Sample ID Container Required Received Adjusted VOA HeadspaceDescription pH * pH pH (Presence/Absence) Comments

1.0 L Bottle-Vac™1.0 L Bottle-Vac™

RSK - MEEPP, HCL (pH<2); RSK - CO2, (pH 5-8); Sulfur (pH>4)

Do containers have appropriate preservation, according to method/SOP or Client specified information?

Does the client/method/SOP require that the analyst check the sample pH and if necessary alter it?

Receipt / Preservation

P1503012-001.01P1503012-002.01

Explain any discrepancies: (include lab sample ID numbers):

6 of 128

TO15SCAN.XLS - 75 Compounds - PageNo.:P1503012_TO15_1508070913_SC.xls - Sample

ALS ENVIRONMENTAL

RESULTS OF ANALYSISPage 1 of 3

Client: Oneida Total Integrated Enterprises (OTIE)SP-108-20150723 ALS Project ID: P1503012Pemaco Plant Vapor Monitoring ALS Sample ID: P1503012-001

Test Code: EPA TO-15 Date Collected: 7/23/15Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date Received: 7/24/15Analyst: Simon Cao Date Analyzed: 8/5/15Sample Type: 1.0 L Bottle-Vac™ Volume(s) Analyzed: 0.20 Liter(s)Test Notes: Container ID: 1BV04202

Initial Pressure (psig): -0.19 Final Pressure (psig): -5.20

Canister Dilution Factor: 0.65

CAS # Compound MRL MDL MRL MDL Dataµg/m³ µg/m³ ppbV ppbV Qualifier

115-07-1 Propene ND 1.6 0.46 ND 0.94 0.2675-71-8 Dichlorodifluoromethane (CFC 12) 0.74 1.6 0.55 0.15 0.33 0.11 J74-87-3 Chloromethane ND 1.6 0.49 ND 0.79 0.24

76-14-2 1,2-Dichloro-1,1,2,2-tetrafluoroethane (CFC 114) ND 1.6 0.62 ND 0.23 0.088

75-01-4 Vinyl Chloride 0.56 1.6 0.55 0.22 0.64 0.22 J106-99-0 1,3-Butadiene ND 1.6 0.72 ND 0.73 0.3274-83-9 Bromomethane ND 1.6 0.62 ND 0.42 0.1675-00-3 Chloroethane ND 1.6 0.55 ND 0.62 0.2164-17-5 Ethanol 4.8 16 2.6 2.6 8.6 1.4 J75-05-8 Acetonitrile ND 1.6 0.59 ND 0.97 0.35107-02-8 Acrolein ND 6.5 0.55 ND 2.8 0.2467-64-1 Acetone 69 16 2.5 29 6.8 1.1 B75-69-4 Trichlorofluoromethane ND 1.6 0.55 ND 0.29 0.09867-63-0 2-Propanol (Isopropyl Alcohol) ND 16 1.4 ND 6.6 0.56107-13-1 Acrylonitrile ND 1.6 0.55 ND 0.75 0.2575-35-4 1,1-Dichloroethene 55 1.6 0.55 14 0.41 0.1475-09-2 Methylene Chloride ND 1.6 0.55 ND 0.47 0.16107-05-1 3-Chloro-1-propene (Allyl Chloride) ND 1.6 0.52 ND 0.52 0.1776-13-1 Trichlorotrifluoroethane ND 1.6 0.55 ND 0.21 0.07275-15-0 Carbon Disulfide 0.81 16 0.49 0.26 5.2 0.16 J156-60-5 trans-1,2-Dichloroethene 5.0 1.6 0.62 1.3 0.41 0.1675-34-3 1,1-Dichloroethane 8.6 1.6 0.52 2.1 0.40 0.131634-04-4 Methyl tert-Butyl Ether ND 1.6 0.55 ND 0.45 0.15108-05-4 Vinyl Acetate ND 16 2.1 ND 4.6 0.6078-93-3 2-Butanone (MEK) 5.5 16 0.68 1.9 5.5 0.23 J

ND = Compound was analyzed for, but not detected above the laboratory detection limit.MRL = Method Reporting Limit - The minimum quantity of a target analyte that can be confidently determined by the referenced method.J = The result is an estimated concentration that is less than the MRL but greater than or equal to the MDL.B = Analyte detected in both the sample and associated method blank.

Client Sample ID:Client Project ID:

ResultppbV

Resultµg/m³

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ALS ENVIRONMENTAL







156-59-2 cis-1,2-Dichloroethene 160 1.6 0.52 39 0.41 0.13141-78-6 Ethyl Acetate ND 3.3 1.1 ND 0.90 0.32110-54-3 n-Hexane 160 1.6 0.49 44 0.46 0.1467-66-3 Chloroform 5.2 1.6 0.55 1.1 0.33 0.11109-99-9 Tetrahydrofuran (THF) 14 1.6 0.65 4.9 0.55 0.22107-06-2 1,2-Dichloroethane ND 1.6 0.52 ND 0.40 0.1371-55-6 1,1,1-Trichloroethane 4.3 1.6 0.55 0.79 0.30 0.1071-43-2 Benzene ND 1.6 0.52 ND 0.51 0.1656-23-5 Carbon Tetrachloride ND 1.6 0.49 ND 0.26 0.078110-82-7 Cyclohexane 450 3.3 0.94 130 0.94 0.2778-87-5 1,2-Dichloropropane ND 1.6 0.52 ND 0.35 0.1175-27-4 Bromodichloromethane ND 1.6 0.49 ND 0.24 0.07379-01-6 Trichloroethene ND 1.6 0.46 ND 0.30 0.085123-91-1 1,4-Dioxane ND 1.6 0.52 ND 0.45 0.1480-62-6 Methyl Methacrylate ND 3.3 1.0 ND 0.79 0.25142-82-5 n-Heptane ND 1.6 0.55 ND 0.40 0.1310061-01-5 cis-1,3-Dichloropropene ND 1.6 0.46 ND 0.36 0.10108-10-1 4-Methyl-2-pentanone ND 1.6 0.52 ND 0.40 0.1310061-02-6 trans-1,3-Dichloropropene ND 1.6 0.52 ND 0.36 0.1179-00-5 1,1,2-Trichloroethane ND 1.6 0.52 ND 0.30 0.095108-88-3 Toluene ND 1.6 0.55 ND 0.43 0.15591-78-6 2-Hexanone 0.95 1.6 0.52 0.23 0.40 0.13 J124-48-1 Dibromochloromethane ND 1.6 0.52 ND 0.19 0.061106-93-4 1,2-Dibromoethane ND 1.6 0.52 ND 0.21 0.068123-86-4 n-Butyl Acetate ND 1.6 0.52 ND 0.34 0.11

ND = Compound was analyzed for, but not detected above the laboratory detection limit.MRL = Method Reporting Limit - The minimum quantity of a target analyte that can be confidently determined by the referenced method.J = The result is an estimated concentration that is less than the MRL but greater than or equal to the MDL.


ppbVResultµg/m³

Result

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MRL MDL MRL MDL Data CAS # Compound µg/m³ µg/m³ ppbV ppbV Qualifier

111-65-9 n-Octane ND 1.6 0.59 ND 0.35 0.13127-18-4 Tetrachloroethene ND 1.6 0.46 ND 0.24 0.067108-90-7 Chlorobenzene ND 1.6 0.52 ND 0.35 0.11100-41-4 Ethylbenzene ND 1.6 0.52 ND 0.37 0.12179601-23-1 m,p-Xylenes ND 3.3 0.98 ND 0.75 0.2275-25-2 Bromoform ND 1.6 0.49 ND 0.16 0.047100-42-5 Styrene ND 1.6 0.49 ND 0.38 0.1195-47-6 o-Xylene ND 1.6 0.49 ND 0.37 0.11111-84-2 n-Nonane ND 1.6 0.49 ND 0.31 0.09379-34-5 1,1,2,2-Tetrachloroethane ND 1.6 0.49 ND 0.24 0.07198-82-8 Cumene ND 1.6 0.49 ND 0.33 0.09980-56-8 alpha-Pinene ND 1.6 0.46 ND 0.29 0.082103-65-1 n-Propylbenzene ND 1.6 0.52 ND 0.33 0.11622-96-8 4-Ethyltoluene ND 1.6 0.52 ND 0.33 0.11108-67-8 1,3,5-Trimethylbenzene ND 1.6 0.52 ND 0.33 0.1195-63-6 1,2,4-Trimethylbenzene 1.2 1.6 0.49 0.24 0.33 0.099 J100-44-7 Benzyl Chloride ND 1.6 0.36 ND 0.31 0.069541-73-1 1,3-Dichlorobenzene ND 1.6 0.49 ND 0.27 0.081106-46-7 1,4-Dichlorobenzene ND 1.6 0.46 ND 0.27 0.07695-50-1 1,2-Dichlorobenzene ND 1.6 0.49 ND 0.27 0.0815989-27-5 d-Limonene ND 1.6 0.46 ND 0.29 0.08296-12-8 1,2-Dibromo-3-chloropropane ND 1.6 0.32 ND 0.17 0.033120-82-1 1,2,4-Trichlorobenzene ND 1.6 0.52 ND 0.22 0.07091-20-3 Naphthalene 1.2 1.6 0.59 0.24 0.31 0.11 J87-68-3 Hexachlorobutadiene ND 1.6 0.46 ND 0.15 0.043


ResultResultµg/m³


ppbV

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ALS ENVIRONMENTAL




Initial Pressure (psig): -0.04 Final Pressure (psig): 5.10



115-07-1 Propene ND 34 9.5 ND 20 5.575-71-8 Dichlorodifluoromethane (CFC 12) ND 34 11 ND 6.8 2.374-87-3 Chloromethane ND 34 10 ND 16 4.9

76-14-2 1,2-Dichloro-1,1,2,2-tetrafluoroethane (CFC 114) ND 34 13 ND 4.8 1.8

75-01-4 Vinyl Chloride ND 34 11 ND 13 4.5106-99-0 1,3-Butadiene ND 34 15 ND 15 6.774-83-9 Bromomethane ND 34 13 ND 8.7 3.375-00-3 Chloroethane ND 34 11 ND 13 4.464-17-5 Ethanol ND 340 54 ND 180 2975-05-8 Acetonitrile ND 34 12 ND 20 7.2107-02-8 Acrolein ND 140 11 ND 59 5.067-64-1 Acetone ND 340 52 ND 140 2275-69-4 Trichlorofluoromethane ND 34 11 ND 6.0 2.067-63-0 2-Propanol (Isopropyl Alcohol) ND 340 28 ND 140 12107-13-1 Acrylonitrile ND 34 11 ND 16 5.375-35-4 1,1-Dichloroethene 58 34 11 15 8.5 2.975-09-2 Methylene Chloride ND 34 11 ND 9.7 3.3107-05-1 3-Chloro-1-propene (Allyl Chloride) ND 34 11 ND 11 3.576-13-1 Trichlorotrifluoroethane ND 34 11 ND 4.4 1.575-15-0 Carbon Disulfide ND 340 10 ND 110 3.3156-60-5 trans-1,2-Dichloroethene ND 34 13 ND 8.5 3.275-34-3 1,1-Dichloroethane ND 34 11 ND 8.3 2.71634-04-4 Methyl tert-Butyl Ether ND 34 11 ND 9.4 3.2108-05-4 Vinyl Acetate ND 340 44 ND 96 1278-93-3 2-Butanone (MEK) ND 340 14 ND 110 4.8

ND = Compound was analyzed for, but not detected above the laboratory detection limit.MRL = Method Reporting Limit - The minimum quantity of a target analyte that can be confidently determined by the referenced method.


Result Resultµg/m³ ppbV

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ALS ENVIRONMENTAL







156-59-2 cis-1,2-Dichloroethene 18 34 11 4.6 8.5 2.7 J141-78-6 Ethyl Acetate ND 68 24 ND 19 6.6110-54-3 n-Hexane 3,500 34 10 990 9.6 2.967-66-3 Chloroform ND 34 11 ND 6.9 2.4109-99-9 Tetrahydrofuran (THF) 14 34 14 4.6 11 4.6 J107-06-2 1,2-Dichloroethane ND 34 11 ND 8.3 2.771-55-6 1,1,1-Trichloroethane ND 34 11 ND 6.2 2.171-43-2 Benzene 17 34 11 5.2 11 3.4 J56-23-5 Carbon Tetrachloride ND 34 10 ND 5.4 1.6110-82-7 Cyclohexane 580 68 20 170 20 5.778-87-5 1,2-Dichloropropane ND 34 11 ND 7.3 2.375-27-4 Bromodichloromethane ND 34 10 ND 5.0 1.579-01-6 Trichloroethene 39 34 9.5 7.3 6.3 1.8123-91-1 1,4-Dioxane ND 34 11 ND 9.4 3.080-62-6 Methyl Methacrylate ND 68 21 ND 16 5.1142-82-5 n-Heptane 200 34 11 50 8.2 2.810061-01-5 cis-1,3-Dichloropropene ND 34 9.5 ND 7.4 2.1108-10-1 4-Methyl-2-pentanone ND 34 11 ND 8.2 2.610061-02-6 trans-1,3-Dichloropropene ND 34 11 ND 7.4 2.479-00-5 1,1,2-Trichloroethane ND 34 11 ND 6.2 2.0108-88-3 Toluene ND 34 11 ND 9.0 3.0591-78-6 2-Hexanone ND 34 11 ND 8.2 2.6124-48-1 Dibromochloromethane ND 34 11 ND 4.0 1.3106-93-4 1,2-Dibromoethane ND 34 11 ND 4.4 1.4123-86-4 n-Butyl Acetate ND 34 11 ND 7.1 2.3




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ALS ENVIRONMENTAL







111-65-9 n-Octane ND 34 12 ND 7.2 2.6127-18-4 Tetrachloroethene 890 34 9.5 130 5.0 1.4108-90-7 Chlorobenzene ND 34 11 ND 7.3 2.3100-41-4 Ethylbenzene 980 34 11 230 7.8 2.5179601-23-1 m,p-Xylenes ND 68 20 ND 16 4.775-25-2 Bromoform ND 34 10 ND 3.3 0.98100-42-5 Styrene ND 34 10 ND 7.9 2.495-47-6 o-Xylene ND 34 10 ND 7.8 2.3111-84-2 n-Nonane ND 34 10 ND 6.4 1.979-34-5 1,1,2,2-Tetrachloroethane ND 34 10 ND 4.9 1.598-82-8 Cumene 82 34 10 17 6.9 2.180-56-8 alpha-Pinene ND 34 9.5 ND 6.1 1.7103-65-1 n-Propylbenzene 260 34 11 53 6.9 2.2622-96-8 4-Ethyltoluene ND 34 11 ND 6.9 2.2108-67-8 1,3,5-Trimethylbenzene 20 34 11 4.1 6.9 2.2 J95-63-6 1,2,4-Trimethylbenzene 630 34 10 130 6.9 2.1100-44-7 Benzyl Chloride ND 34 7.4 ND 6.5 1.4541-73-1 1,3-Dichlorobenzene ND 34 10 ND 5.6 1.7106-46-7 1,4-Dichlorobenzene ND 34 9.5 ND 5.6 1.695-50-1 1,2-Dichlorobenzene ND 34 10 ND 5.6 1.75989-27-5 d-Limonene ND 34 9.5 ND 6.1 1.796-12-8 1,2-Dibromo-3-chloropropane ND 34 6.7 ND 3.5 0.69120-82-1 1,2,4-Trichlorobenzene ND 34 11 ND 4.5 1.591-20-3 Naphthalene 490 34 12 94 6.4 2.387-68-3 Hexachlorobutadiene ND 34 9.5 ND 3.2 0.89




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Client: Oneida Total Integrated Enterprises (OTIE)Method Blank ALS Project ID: P1503012Pemaco Plant Vapor Monitoring ALS Sample ID: P150804-MB

Test Code: EPA TO-15 Date Collected: NAInstrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date Received: NAAnalyst: Simon Cao Date Analyzed: 8/4/15Sample Type: 1.0 L Bottle-Vac™ Volume(s) Analyzed: 1.00 Liter(s)Test Notes:



115-07-1 Propene ND 0.50 0.14 ND 0.29 0.08175-71-8 Dichlorodifluoromethane (CFC 12) ND 0.50 0.17 ND 0.10 0.03474-87-3 Chloromethane ND 0.50 0.15 ND 0.24 0.073


75-01-4 Vinyl Chloride ND 0.50 0.17 ND 0.20 0.067106-99-0 1,3-Butadiene ND 0.50 0.22 ND 0.23 0.09974-83-9 Bromomethane ND 0.50 0.19 ND 0.13 0.04975-00-3 Chloroethane ND 0.50 0.17 ND 0.19 0.06464-17-5 Ethanol ND 5.0 0.80 ND 2.7 0.4275-05-8 Acetonitrile ND 0.50 0.18 ND 0.30 0.11107-02-8 Acrolein ND 2.0 0.17 ND 0.87 0.07467-64-1 Acetone ND 5.0 0.77 ND 2.1 0.3275-69-4 Trichlorofluoromethane ND 0.50 0.17 ND 0.089 0.03067-63-0 2-Propanol (Isopropyl Alcohol) ND 5.0 0.42 ND 2.0 0.17107-13-1 Acrylonitrile ND 0.50 0.17 ND 0.23 0.07875-35-4 1,1-Dichloroethene ND 0.50 0.17 ND 0.13 0.04375-09-2 Methylene Chloride ND 0.50 0.17 ND 0.14 0.049107-05-1 3-Chloro-1-propene (Allyl Chloride) ND 0.50 0.16 ND 0.16 0.05176-13-1 Trichlorotrifluoroethane ND 0.50 0.17 ND 0.065 0.02275-15-0 Carbon Disulfide ND 5.0 0.15 ND 1.6 0.048156-60-5 trans-1,2-Dichloroethene ND 0.50 0.19 ND 0.13 0.04875-34-3 1,1-Dichloroethane ND 0.50 0.16 ND 0.12 0.0401634-04-4 Methyl tert-Butyl Ether ND 0.50 0.17 ND 0.14 0.047108-05-4 Vinyl Acetate ND 5.0 0.65 ND 1.4 0.1878-93-3 2-Butanone (MEK) ND 5.0 0.21 ND 1.7 0.071



ResultppbV

Resultµg/m³

13 of 128


ALS ENVIRONMENTAL






156-59-2 cis-1,2-Dichloroethene ND 0.50 0.16 ND 0.13 0.040141-78-6 Ethyl Acetate ND 1.0 0.35 ND 0.28 0.097110-54-3 n-Hexane ND 0.50 0.15 ND 0.14 0.04367-66-3 Chloroform ND 0.50 0.17 ND 0.10 0.035109-99-9 Tetrahydrofuran (THF) ND 0.50 0.20 ND 0.17 0.068107-06-2 1,2-Dichloroethane ND 0.50 0.16 ND 0.12 0.04071-55-6 1,1,1-Trichloroethane ND 0.50 0.17 ND 0.092 0.03171-43-2 Benzene ND 0.50 0.16 ND 0.16 0.05056-23-5 Carbon Tetrachloride ND 0.50 0.15 ND 0.080 0.024110-82-7 Cyclohexane ND 1.0 0.29 ND 0.29 0.08478-87-5 1,2-Dichloropropane ND 0.50 0.16 ND 0.11 0.03575-27-4 Bromodichloromethane ND 0.50 0.15 ND 0.075 0.02279-01-6 Trichloroethene ND 0.50 0.14 ND 0.093 0.026123-91-1 1,4-Dioxane ND 0.50 0.16 ND 0.14 0.04480-62-6 Methyl Methacrylate ND 1.0 0.31 ND 0.24 0.076142-82-5 n-Heptane ND 0.50 0.17 ND 0.12 0.04110061-01-5 cis-1,3-Dichloropropene ND 0.50 0.14 ND 0.11 0.031108-10-1 4-Methyl-2-pentanone ND 0.50 0.16 ND 0.12 0.03910061-02-6 trans-1,3-Dichloropropene ND 0.50 0.16 ND 0.11 0.03579-00-5 1,1,2-Trichloroethane ND 0.50 0.16 ND 0.092 0.029108-88-3 Toluene ND 0.50 0.17 ND 0.13 0.045591-78-6 2-Hexanone ND 0.50 0.16 ND 0.12 0.039124-48-1 Dibromochloromethane ND 0.50 0.16 ND 0.059 0.019106-93-4 1,2-Dibromoethane ND 0.50 0.16 ND 0.065 0.021123-86-4 n-Butyl Acetate ND 0.50 0.16 ND 0.11 0.034



Resultµg/m³

ResultppbV

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ALS ENVIRONMENTAL






111-65-9 n-Octane ND 0.50 0.18 ND 0.11 0.039127-18-4 Tetrachloroethene ND 0.50 0.14 ND 0.074 0.021108-90-7 Chlorobenzene ND 0.50 0.16 ND 0.11 0.035100-41-4 Ethylbenzene ND 0.50 0.16 ND 0.12 0.037179601-23-1 m,p-Xylenes ND 1.0 0.30 ND 0.23 0.06975-25-2 Bromoform ND 0.50 0.15 ND 0.048 0.015100-42-5 Styrene ND 0.50 0.15 ND 0.12 0.03595-47-6 o-Xylene ND 0.50 0.15 ND 0.12 0.035111-84-2 n-Nonane ND 0.50 0.15 ND 0.095 0.02979-34-5 1,1,2,2-Tetrachloroethane ND 0.50 0.15 ND 0.073 0.02298-82-8 Cumene ND 0.50 0.15 ND 0.10 0.03180-56-8 alpha-Pinene ND 0.50 0.14 ND 0.090 0.025103-65-1 n-Propylbenzene ND 0.50 0.16 ND 0.10 0.033622-96-8 4-Ethyltoluene ND 0.50 0.16 ND 0.10 0.033108-67-8 1,3,5-Trimethylbenzene ND 0.50 0.16 ND 0.10 0.03395-63-6 1,2,4-Trimethylbenzene ND 0.50 0.15 ND 0.10 0.031100-44-7 Benzyl Chloride ND 0.50 0.11 ND 0.097 0.021541-73-1 1,3-Dichlorobenzene ND 0.50 0.15 ND 0.083 0.025106-46-7 1,4-Dichlorobenzene ND 0.50 0.14 ND 0.083 0.02395-50-1 1,2-Dichlorobenzene ND 0.50 0.15 ND 0.083 0.0255989-27-5 d-Limonene ND 0.50 0.14 ND 0.090 0.02596-12-8 1,2-Dibromo-3-chloropropane ND 0.50 0.099 ND 0.052 0.010120-82-1 1,2,4-Trichlorobenzene ND 0.50 0.16 ND 0.067 0.02291-20-3 Naphthalene ND 0.50 0.18 ND 0.095 0.03487-68-3 Hexachlorobutadiene ND 0.50 0.14 ND 0.047 0.013


ResultppbV

Resultµg/m³


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115-07-1 Propene ND 0.50 0.14 ND 0.29 0.08175-71-8 Dichlorodifluoromethane (CFC 12) ND 0.50 0.17 ND 0.10 0.03474-87-3 Chloromethane ND 0.50 0.15 ND 0.24 0.073


75-01-4 Vinyl Chloride ND 0.50 0.17 ND 0.20 0.067106-99-0 1,3-Butadiene ND 0.50 0.22 ND 0.23 0.09974-83-9 Bromomethane ND 0.50 0.19 ND 0.13 0.04975-00-3 Chloroethane ND 0.50 0.17 ND 0.19 0.06464-17-5 Ethanol ND 5.0 0.80 ND 2.7 0.4275-05-8 Acetonitrile ND 0.50 0.18 ND 0.30 0.11107-02-8 Acrolein ND 2.0 0.17 ND 0.87 0.07467-64-1 Acetone 0.85 5.0 0.77 0.36 2.1 0.32 J75-69-4 Trichlorofluoromethane ND 0.50 0.17 ND 0.089 0.03067-63-0 2-Propanol (Isopropyl Alcohol) ND 5.0 0.42 ND 2.0 0.17107-13-1 Acrylonitrile ND 0.50 0.17 ND 0.23 0.07875-35-4 1,1-Dichloroethene ND 0.50 0.17 ND 0.13 0.04375-09-2 Methylene Chloride ND 0.50 0.17 ND 0.14 0.049107-05-1 3-Chloro-1-propene (Allyl Chloride) ND 0.50 0.16 ND 0.16 0.05176-13-1 Trichlorotrifluoroethane ND 0.50 0.17 ND 0.065 0.02275-15-0 Carbon Disulfide ND 5.0 0.15 ND 1.6 0.048156-60-5 trans-1,2-Dichloroethene ND 0.50 0.19 ND 0.13 0.04875-34-3 1,1-Dichloroethane ND 0.50 0.16 ND 0.12 0.0401634-04-4 Methyl tert-Butyl Ether ND 0.50 0.17 ND 0.14 0.047108-05-4 Vinyl Acetate ND 5.0 0.65 ND 1.4 0.1878-93-3 2-Butanone (MEK) ND 5.0 0.21 ND 1.7 0.071




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156-59-2 cis-1,2-Dichloroethene ND 0.50 0.16 ND 0.13 0.040141-78-6 Ethyl Acetate ND 1.0 0.35 ND 0.28 0.097110-54-3 n-Hexane ND 0.50 0.15 ND 0.14 0.04367-66-3 Chloroform ND 0.50 0.17 ND 0.10 0.035109-99-9 Tetrahydrofuran (THF) ND 0.50 0.20 ND 0.17 0.068107-06-2 1,2-Dichloroethane ND 0.50 0.16 ND 0.12 0.04071-55-6 1,1,1-Trichloroethane ND 0.50 0.17 ND 0.092 0.03171-43-2 Benzene ND 0.50 0.16 ND 0.16 0.05056-23-5 Carbon Tetrachloride ND 0.50 0.15 ND 0.080 0.024110-82-7 Cyclohexane ND 1.0 0.29 ND 0.29 0.08478-87-5 1,2-Dichloropropane ND 0.50 0.16 ND 0.11 0.03575-27-4 Bromodichloromethane ND 0.50 0.15 ND 0.075 0.02279-01-6 Trichloroethene ND 0.50 0.14 ND 0.093 0.026123-91-1 1,4-Dioxane ND 0.50 0.16 ND 0.14 0.04480-62-6 Methyl Methacrylate ND 1.0 0.31 ND 0.24 0.076142-82-5 n-Heptane ND 0.50 0.17 ND 0.12 0.04110061-01-5 cis-1,3-Dichloropropene ND 0.50 0.14 ND 0.11 0.031108-10-1 4-Methyl-2-pentanone ND 0.50 0.16 ND 0.12 0.03910061-02-6 trans-1,3-Dichloropropene ND 0.50 0.16 ND 0.11 0.03579-00-5 1,1,2-Trichloroethane ND 0.50 0.16 ND 0.092 0.029108-88-3 Toluene ND 0.50 0.17 ND 0.13 0.045591-78-6 2-Hexanone ND 0.50 0.16 ND 0.12 0.039124-48-1 Dibromochloromethane ND 0.50 0.16 ND 0.059 0.019106-93-4 1,2-Dibromoethane ND 0.50 0.16 ND 0.065 0.021123-86-4 n-Butyl Acetate ND 0.50 0.16 ND 0.11 0.034




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111-65-9 n-Octane ND 0.50 0.18 ND 0.11 0.039127-18-4 Tetrachloroethene ND 0.50 0.14 ND 0.074 0.021108-90-7 Chlorobenzene ND 0.50 0.16 ND 0.11 0.035100-41-4 Ethylbenzene ND 0.50 0.16 ND 0.12 0.037179601-23-1 m,p-Xylenes ND 1.0 0.30 ND 0.23 0.06975-25-2 Bromoform ND 0.50 0.15 ND 0.048 0.015100-42-5 Styrene ND 0.50 0.15 ND 0.12 0.03595-47-6 o-Xylene ND 0.50 0.15 ND 0.12 0.035111-84-2 n-Nonane ND 0.50 0.15 ND 0.095 0.02979-34-5 1,1,2,2-Tetrachloroethane ND 0.50 0.15 ND 0.073 0.02298-82-8 Cumene ND 0.50 0.15 ND 0.10 0.03180-56-8 alpha-Pinene ND 0.50 0.14 ND 0.090 0.025103-65-1 n-Propylbenzene ND 0.50 0.16 ND 0.10 0.033622-96-8 4-Ethyltoluene ND 0.50 0.16 ND 0.10 0.033108-67-8 1,3,5-Trimethylbenzene ND 0.50 0.16 ND 0.10 0.03395-63-6 1,2,4-Trimethylbenzene ND 0.50 0.15 ND 0.10 0.031100-44-7 Benzyl Chloride ND 0.50 0.11 ND 0.097 0.021541-73-1 1,3-Dichlorobenzene ND 0.50 0.15 ND 0.083 0.025106-46-7 1,4-Dichlorobenzene ND 0.50 0.14 ND 0.083 0.02395-50-1 1,2-Dichlorobenzene ND 0.50 0.15 ND 0.083 0.0255989-27-5 d-Limonene ND 0.50 0.14 ND 0.090 0.02596-12-8 1,2-Dibromo-3-chloropropane ND 0.50 0.099 ND 0.052 0.010120-82-1 1,2,4-Trichlorobenzene ND 0.50 0.16 ND 0.067 0.02291-20-3 Naphthalene ND 0.50 0.18 ND 0.095 0.03487-68-3 Hexachlorobutadiene ND 0.50 0.14 ND 0.047 0.013




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TO15SCAN.XLS - 75 Compounds - PageNo.:P1503012_TO15_1508070913_SC.xls - Surrogates

ALS ENVIRONMENTAL

SURROGATE SPIKE RECOVERY RESULTSPage 1 of 1

Client: Oneida Total Integrated Enterprises (OTIE)Pemaco Plant Vapor Monitoring ALS Project ID: P1503012

Test Code: EPA TO-15Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Date(s) Collected: 7/23/15Analyst: Simon Cao Date(s) Received: 7/24/15Sample Type: 1.0 L Bottle-Vac™(s) Date(s) Analyzed: 8/4 - 8/5/15Test Notes:

Client Sample ID ALS Sample ID Acceptance DataLimits Qualifier

P150804-MB 70-130 P150805-MB 70-130 P150804-LCS 70-130 P150805-LCS 70-130 P1503012-001 70-130 P1503012-002 70-130

Surrogate percent recovery is verified and accepted based on the on-column result.Reported results are shown in concentration units and as a result of the calculation, may vary slightly from the on-column percent recovery.

106

105 110113108105

98

Recovered106105

Percent

8791

8481

81 104Lab Control Sample

SP-104-20150723

Recovered

Method Blank

SP-108-20150723

Method Blank 82

Lab Control Sample

Client Project ID:

112

Percent PercentRecovered

BromofluorobenzeneToluene-d81,2-Dichloroethane-d4

109

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ALS ENVIRONMENTAL

LABORATORY CONTROL SAMPLE SUMMARYPage 1 of 3

Client: Oneida Total Integrated Enterprises (OTIE)Lab Control Sample ALS Project ID: P1503012Pemaco Plant Vapor Monitoring ALS Sample ID: P150804-LCS


CAS # Compound Data Qualifier

115-07-1 Propene 69 50-12875-71-8 Dichlorodifluoromethane (CFC 12) 81 66-11774-87-3 Chloromethane 73 51-133

76-14-2 1,2-Dichloro-1,1,2,2-tetrafluoroethane (CFC 114) 90 65-117

75-01-4 Vinyl Chloride 80 61-127106-99-0 1,3-Butadiene 80 65-13274-83-9 Bromomethane 95 62-11475-00-3 Chloroethane 86 64-12264-17-5 Ethanol 73 57-13175-05-8 Acetonitrile 67 52-135107-02-8 Acrolein 73 64-12467-64-1 Acetone 75 60-11375-69-4 Trichlorofluoromethane 74 64-11267-63-0 2-Propanol (Isopropyl Alcohol) 77 62-129107-13-1 Acrylonitrile 82 69-13375-35-4 1,1-Dichloroethene 88 70-11475-09-2 Methylene Chloride 76 63-103107-05-1 3-Chloro-1-propene (Allyl Chloride) 76 57-13576-13-1 Trichlorotrifluoroethane 92 69-11675-15-0 Carbon Disulfide 74 66-118156-60-5 trans-1,2-Dichloroethene 83 69-12375-34-3 1,1-Dichloroethane 81 65-1181634-04-4 Methyl tert-Butyl Ether 84 57-125108-05-4 Vinyl Acetate 86 69-13178-93-3 2-Butanone (MEK) 81 63-121

Laboratory Control Sample percent recovery is verified and accepted based on the on-column result.Reported results are shown in concentration units and as a result of the calculation, may vary slightly.

166202155175

212216

171

178220

Resultµg/m³

169

160164

813

173

142

184

189

214 1571,080216418

160323

212

191200998

171729

ALSAcceptanceSpike Amount

206

135152

% RecoveryLimitsµg/m³

146

220

222


200

202

204200

196188

212216

210210

218

1828951,040

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ALS ENVIRONMENTAL





156-59-2 cis-1,2-Dichloroethene 81 69-119141-78-6 Ethyl Acetate 80 65-129110-54-3 n-Hexane 80 55-11667-66-3 Chloroform 82 68-111109-99-9 Tetrahydrofuran (THF) 78 69-120107-06-2 1,2-Dichloroethane 78 67-11771-55-6 1,1,1-Trichloroethane 87 74-11671-43-2 Benzene 81 61-10956-23-5 Carbon Tetrachloride 83 76-120110-82-7 Cyclohexane 90 72-11578-87-5 1,2-Dichloropropane 84 67-11975-27-4 Bromodichloromethane 88 78-12479-01-6 Trichloroethene 91 69-115123-91-1 1,4-Dioxane 91 69-12780-62-6 Methyl Methacrylate 94 76-128142-82-5 n-Heptane 88 66-11810061-01-5 cis-1,3-Dichloropropene 93 77-124108-10-1 4-Methyl-2-pentanone 81 66-13410061-02-6 trans-1,3-Dichloropropene 87 80-13079-00-5 1,1,2-Trichloroethane 91 75-119108-88-3 Toluene 94 68-114591-78-6 2-Hexanone 84 60-136124-48-1 Dibromochloromethane 106 75-132106-93-4 1,2-Dibromoethane 103 72-122123-86-4 n-Butyl Acetate 85 60-137


µg/m³177

216

210

170

214 167

192

192218

216210

224

Client Sample ID:

218

Client Project ID:

µg/m³

212

Spike Amount

428 342

230381

182

ALS

183

AcceptanceLimits

% RecoveryResult

185234

182

197

226

191

196

220220

190193

206218

218

179220

210

216422 395

208

226

220224

182

183

424216

172

192

21 of 128


ALS ENVIRONMENTAL




CAS # Compound DataQualifier

111-65-9 n-Octane 91 66-120127-18-4 Tetrachloroethene 103 67-120108-90-7 Chlorobenzene 100 69-114100-41-4 Ethylbenzene 97 71-117179601-23-1 m,p-Xylenes 96 71-11875-25-2 Bromoform 96 76-149100-42-5 Styrene 102 71-12895-47-6 o-Xylene 95 72-118111-84-2 n-Nonane 86 63-12379-34-5 1,1,2,2-Tetrachloroethane 95 73-12498-82-8 Cumene 97 71-11880-56-8 alpha-Pinene 100 71-123103-65-1 n-Propylbenzene 96 71-120622-96-8 4-Ethyltoluene 100 71-121108-67-8 1,3,5-Trimethylbenzene 98 72-12195-63-6 1,2,4-Trimethylbenzene 98 71-122100-44-7 Benzyl Chloride 99 79-143541-73-1 1,3-Dichlorobenzene 99 67-121106-46-7 1,4-Dichlorobenzene 103 68-12195-50-1 1,2-Dichlorobenzene 99 68-1215989-27-5 d-Limonene 98 69-13796-12-8 1,2-Dibromo-3-chloropropane 95 73-145120-82-1 1,2,4-Trichlorobenzene 84 60-13591-20-3 Naphthalene 80 63-14287-68-3 Hexachlorobutadiene 82 65-127


174

225215

205207

189

194

217

214209

217213

220228

218

208

208

204

211

199175199

210

196

214

230

230

218

220210218

214

228222 227

212 213

210204

219

202

410

208202

428

192

219218

ALSAcceptance

Limits% RecoveryResult

µg/m³µg/m³Spike Amount

Client Project ID:

220

210

Client Sample ID:

22 of 128

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ALS ENVIRONMENTAL





115-07-1 Propene 66 50-12875-71-8 Dichlorodifluoromethane (CFC 12) 77 66-11774-87-3 Chloromethane 68 51-133

76-14-2 1,2-Dichloro-1,1,2,2-tetrafluoroethane (CFC 114) 89 65-117

75-01-4 Vinyl Chloride 78 61-127106-99-0 1,3-Butadiene 75 65-13274-83-9 Bromomethane 93 62-11475-00-3 Chloroethane 83 64-12264-17-5 Ethanol 70 57-13175-05-8 Acetonitrile 64 52-135107-02-8 Acrolein 71 64-12467-64-1 Acetone 73 60-11375-69-4 Trichlorofluoromethane 72 64-11267-63-0 2-Propanol (Isopropyl Alcohol) 73 62-129107-13-1 Acrylonitrile 79 69-13375-35-4 1,1-Dichloroethene 86 70-11475-09-2 Methylene Chloride 75 63-103107-05-1 3-Chloro-1-propene (Allyl Chloride) 72 57-13576-13-1 Trichlorotrifluoroethane 91 69-11675-15-0 Carbon Disulfide 71 66-118156-60-5 trans-1,2-Dichloroethene 80 69-12375-34-3 1,1-Dichloroethane 78 65-1181634-04-4 Methyl tert-Butyl Ether 81 57-125108-05-4 Vinyl Acetate 84 69-13178-93-3 2-Butanone (MEK) 79 63-121


1,040 875220 173

210 169212 165216 176

218 158220 201210 150

212 167216 186222 166

1,080 786216 156418 307

998 696212 136214 153

206 155202 188200 165

200 135

204 181200 155

µg/m³ µg/m³ Limits196 129188 145


ALSSpike Amount Result % Recovery Acceptance

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ALS ENVIRONMENTAL





156-59-2 cis-1,2-Dichloroethene 78 69-119141-78-6 Ethyl Acetate 77 65-129110-54-3 n-Hexane 77 55-11667-66-3 Chloroform 79 68-111109-99-9 Tetrahydrofuran (THF) 76 69-120107-06-2 1,2-Dichloroethane 74 67-11771-55-6 1,1,1-Trichloroethane 84 74-11671-43-2 Benzene 80 61-10956-23-5 Carbon Tetrachloride 81 76-120110-82-7 Cyclohexane 88 72-11578-87-5 1,2-Dichloropropane 82 67-11975-27-4 Bromodichloromethane 85 78-12479-01-6 Trichloroethene 90 69-115123-91-1 1,4-Dioxane 90 69-12780-62-6 Methyl Methacrylate 92 76-128142-82-5 n-Heptane 86 66-11810061-01-5 cis-1,3-Dichloropropene 90 77-124108-10-1 4-Methyl-2-pentanone 78 66-13410061-02-6 trans-1,3-Dichloropropene 84 80-13079-00-5 1,1,2-Trichloroethane 89 75-119108-88-3 Toluene 92 68-114591-78-6 2-Hexanone 80 60-136124-48-1 Dibromochloromethane 104 75-132106-93-4 1,2-Dibromoethane 100 72-122123-86-4 n-Butyl Acetate 80 60-137


218 217226 181

218 200220 176220 228

220 172210 176216 193

422 389216 185208 188

218 186216 195210 188

230 186424 374216 177

214 159210 177226 180

212 163224 177220 168

µg/m³ µg/m³ Limits218 171428 330

Client Project ID:


Client Sample ID:

24 of 128


ALS ENVIRONMENTAL




CAS # Compound DataQualifier

111-65-9 n-Octane 88 66-120127-18-4 Tetrachloroethene 101 67-120108-90-7 Chlorobenzene 97 69-114100-41-4 Ethylbenzene 94 71-117179601-23-1 m,p-Xylenes 93 71-11875-25-2 Bromoform 93 76-149100-42-5 Styrene 100 71-12895-47-6 o-Xylene 92 72-118111-84-2 n-Nonane 81 63-12379-34-5 1,1,2,2-Tetrachloroethane 91 73-12498-82-8 Cumene 94 71-11880-56-8 alpha-Pinene 97 71-123103-65-1 n-Propylbenzene 93 71-120622-96-8 4-Ethyltoluene 96 71-121108-67-8 1,3,5-Trimethylbenzene 94 72-12195-63-6 1,2,4-Trimethylbenzene 94 71-122100-44-7 Benzyl Chloride 95 79-143541-73-1 1,3-Dichlorobenzene 96 67-121106-46-7 1,4-Dichlorobenzene 100 68-12195-50-1 1,2-Dichlorobenzene 96 68-1215989-27-5 d-Limonene 93 69-13796-12-8 1,2-Dibromo-3-chloropropane 92 73-145120-82-1 1,2,4-Trichlorobenzene 82 60-13591-20-3 Naphthalene 77 63-14287-68-3 Hexachlorobutadiene 80 65-127


218 168230 184

210 195218 200230 189

228 219208 208220 211

214 202218 206220 209

212 206204 189214 206

204 166210 192208 196

228 213222 221210 193

220 213218 204428 396

µg/m³ µg/m³ Limits210 184202 205

Client Project ID:


Client Sample ID:

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TO15SCAN.XLS - 75 Compounds - PageNo.:P1503012_TO15_1508070913_SC.xls - ISS

ALS ENVIRONMENTAL


Client: Oneida Total Integrated Enterprises (OTIE) ALS Project ID: P1503012Pemaco Plant Vapor Monitoring

Internal Standard Area and RT Summary

Test Code: EPA TO-15Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Lab File ID: 08041502.DAnalyst: Simon Cao Date Analyzed: 8/4/15Sample Type: 1.0 L Bottle-Vac™(s) Time Analyzed: 06:14

Test Notes:

IS1 (BCM) IS2 (DFB) IS3 (CBZ)AREA # RT # AREA # RT # AREA # RT #

24 Hour Standard 149787 9.00 769681 10.97 327176 15.31 Upper Limit 209702 9.33 1077553 11.30 458046 15.64 Lower Limit 89872 8.67 461809 10.64 196306 14.98

Client Sample ID01 Method Blank 150501 8.98 775372 10.96 318022 15.3102 Lab Control Sample 150972 9.00 772259 10.97 324392 15.3203 SP-104-20150723 137737 8.98 716236 10.97 325769 15.310405060708091011121314151617181920

IS1 (BCM) = BromochloromethaneIS2 (DFB) = 1,4-DifluorobenzeneIS3 (CBZ) = Chlorobenzene-d5

AREA UPPER LIMIT = 140% of internal standard areaAREA LOWER LIMIT = 60% of internal standard areaRT UPPER LIMIT = 0.33 minutes of internal standard RTRT LOWER LIMIT = 0.33 minutes of internal standard RT

# Column used to flag values outside QC limits with an I.I = Internal standard not within the specified limits.

Client Project ID:

26 of 128

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ALS ENVIRONMENTAL


Client: Oneida Total Integrated Enterprises (OTIE) ALS Project ID: P1503012Pemaco Plant Vapor Monitoring

Internal Standard Area and RT Summary

Test Code: EPA TO-15Instrument ID: Tekmar AUTOCAN/Agilent 5973inert/6890N/MS9 Lab File ID: 08051502.DAnalyst: Simon Cao Date Analyzed: 8/5/15Sample Type: 1.0 L Bottle-Vac™(s) Time Analyzed: 04:14

Test Notes:

IS1 (BCM) IS2 (DFB) IS3 (CBZ)AREA # RT # AREA # RT # AREA # RT #

24 Hour Standard 160733 9.00 821657 10.97 348336 15.31 Upper Limit 225026 9.33 1150320 11.30 487670 15.64 Lower Limit 96440 8.67 492994 10.64 209002 14.98

Client Sample ID01 Method Blank 159572 8.98 821162 10.96 340840 15.3102 Lab Control Sample 159933 8.99 814393 10.97 345321 15.3103 SP-108-20150723 148578 9.00 771890 10.97 321116 15.310405060708091011121314151617181920

IS1 (BCM) = BromochloromethaneIS2 (DFB) = 1,4-DifluorobenzeneIS3 (CBZ) = Chlorobenzene-d5

AREA UPPER LIMIT = 140% of internal standard areaAREA LOWER LIMIT = 60% of internal standard areaRT UPPER LIMIT = 0.33 minutes of internal standard RTRT LOWER LIMIT = 0.33 minutes of internal standard RT

# Column used to flag values outside QC limits with an I.I = Internal standard not within the specified limits.

Client Project ID:

27 of 128

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_08\05\08051516.D Acq On : 5 Aug 2015 12:08 Operator: SC Sample : P1503012-001 (200mL) Misc : S29-07071501 ALS Vial : 13 Sample Multiplier: 1 Quant Time: Aug 05 12:53:29 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 1) Bromochloromethane (IS1) 9.00 130 148578 12.500 ng -0.02 37) 1,4-Difluorobenzene (IS2) 10.97 114 771890 12.500 ng 0.00 56) Chlorobenzene-d5 (IS3) 15.31 82 321116 12.500 ng 0.00 System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.78 65 258791 10.833 ng -0.01 Spiked Amount 12.500 Recovery = 86.64% 57) Toluene-d8 (SS2) 13.41 98 767238 13.154 ng 0.00 Spiked Amount 12.500 Recovery = 105.20% 73) Bromofluorobenzene (SS3) 16.92 174 250863 13.530 ng 0.00 Spiked Amount 12.500 Recovery = 108.24% Target Compounds Qvalue 2) Propene 0.00 42 0 N.D. d 3) Dichlorodifluoromethan... 3.88 85 9059 0.229 ng # 97 4) Chloromethane 4.07 50 3576 0.108 ng 92 5) 1,2-Dichloro-1,1,2,2-t... 0.00 135 0 N.D. 6) Vinyl Chloride 4.35 62 4757 0.173 ng 96 7) 1,3-Butadiene 4.48 54 698 N.D. 8) Bromomethane 0.00 94 0 N.D. 9) Chloroethane 0.00 64 0 N.D. 10) Ethanol 5.22 45 24450 1.481 ng 90 11) Acetonitrile 5.45 41 3115 N.D. 12) Acrolein 5.57 56 1579 0.124 ng 80 13) Acetone 5.70 58 319937m 21.220 ng 14) Trichlorofluoromethane 5.91 101 1221 N.D. 15) 2-Propanol (Isopropanol) 6.02 45 5901 0.111 ng 87 16) Acrylonitrile 6.21 53 1497 N.D. 17) 1,1-Dichloroethene 6.59 96 272855 16.820 ng 88 18) 2-Methyl-2-Propanol (t... 0.00 59 0 N.D. d 19) Methylene Chloride 6.72 84 2300 0.119 ng 86 20) 3-Chloro-1-propene (Al... 0.00 41 0 N.D. d 21) Trichlorotrifluoroethane 0.00 151 0 N.D. 22) Carbon Disulfide 7.02 76 18292 0.250 ng 95 23) trans-1,2-Dichloroethene 7.75 61 41570 1.535 ng 93 24) 1,1-Dichloroethane 7.96 63 92490 2.637 ng 98 25) Methyl tert-Butyl Ether 7.98 73 808 N.D. 26) Vinyl Acetate 0.00 86 0 N.D. d 27) 2-Butanone (MEK) 8.38 72 21406 1.696 ng # 81 28) cis-1,2-Dichloroethene 8.83 61 1249444 47.761 ng 93 29) Diisopropyl Ether 0.00 87 0 N.D. d 30) Ethyl Acetate 0.00 61 0 N.D. d 31) n-Hexane 9.11 57 1578846 47.721 ng 99 32) Chloroform 9.14 83 49128 1.606 ng 83 34) Tetrahydrofuran (THF) 9.54 72 56618 4.413 ng # 91 35) Ethyl tert-Butyl Ether 0.00 87 0 N.D. 36) 1,2-Dichloroethane 0.00 62 0 N.D. d 38) 1,1,1-Trichloroethane 10.17 97 34935 1.325 ng 98 39) Isopropyl Acetate 0.00 61 0 N.D. 40) 1-Butanol 0.00 56 0 N.D. d 41) Benzene 10.62 78 2971 N.D. 42) Carbon Tetrachloride 10.78 117 2794 0.126 ng 87 43) Cyclohexane 10.91 84 3655637 139.031 ng 91 44) tert-Amyl Methyl Ether 0.00 73 0 N.D. 45) 1,2-Dichloropropane 11.28 63 1093 N.D. 46) Bromodichloromethane 11.64 83 1472 N.D. 47) Trichloroethene 0.00 130 0 N.D. 48) 1,4-Dioxane 0.00 88 0 N.D. 49) 2,2,4-Trimethylpentane... 11.74 57 3054 N.D.

R9071315.M Wed Aug 05 12:54:28 2015 Page: 1

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simon.cao

Simon

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_08\05\08051516.D Acq On : 5 Aug 2015 12:08 Operator: SC Sample : P1503012-001 (200mL) Misc : S29-07071501 ALS Vial : 13 Sample Multiplier: 1 Quant Time: Aug 05 12:53:29 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 50) Methyl Methacrylate 0.00 100 0 N.D. 51) n-Heptane 0.00 71 0 N.D. 52) cis-1,3-Dichloropropene 0.00 75 0 N.D. 53) 4-Methyl-2-pentanone 12.32 58 621 N.D. 54) trans-1,3-Dichloropropene 0.00 75 0 N.D. 55) 1,1,2-Trichloroethane 0.00 97 0 N.D. 58) Toluene 13.51 91 10345 0.159 ng 100 59) 2-Hexanone 13.76 43 12555 0.291 ng 99 60) Dibromochloromethane 0.00 129 0 N.D. 61) 1,2-Dibromoethane 0.00 107 0 N.D. 62) n-Butyl Acetate 14.41 43 540 N.D. 63) n-Octane 14.53 57 609 N.D. 64) Tetrachloroethene 0.00 166 0 N.D. 65) Chlorobenzene 0.00 112 0 N.D. 66) Ethylbenzene 15.76 91 8250 0.114 ng 97 67) m- & p-Xylenes 15.95 91 5226 N.D. 68) Bromoform 0.00 173 0 N.D. 69) Styrene 16.33 104 509 N.D. 70) o-Xylene 16.45 91 2411 N.D. 71) n-Nonane 16.69 43 1748 N.D. 72) 1,1,2,2-Tetrachloroethane 16.51 83 1971 N.D. 74) Cumene 17.07 105 1992 N.D. 75) alpha-Pinene 0.00 93 0 N.D. 76) n-Propylbenzene 17.60 91 9746 0.104 ng # 39 77) 3-Ethyltoluene 17.71 105 1517 N.D. 78) 4-Ethyltoluene 17.76 105 943 N.D. 79) 1,3,5-Trimethylbenzene 17.84 105 1276 N.D. 80) alpha-Methylstyrene 0.00 118 0 N.D. 81) 2-Ethyltoluene 18.04 105 1208 N.D. 82) 1,2,4-Trimethylbenzene 18.26 105 21588 0.359 ng 93 83) n-Decane 0.00 57 0 N.D. d 84) Benzyl Chloride 18.42 91 606 N.D. 85) 1,3-Dichlorobenzene 0.00 146 0 N.D. 86) 1,4-Dichlorobenzene 0.00 146 0 N.D. 87) sec-Butylbenzene 0.00 105 0 N.D. d 88) 4-Isopropyltoluene (p-... 18.72 119 2238 N.D. 89) 1,2,3-Trimethylbenzene 18.72 105 2089 N.D. 90) 1,2-Dichlorobenzene 0.00 146 0 N.D. 91) d-Limonene 0.00 68 0 N.D. d 92) 1,2-Dibromo-3-Chloropr... 0.00 157 0 N.D. 93) n-Undecane 0.00 57 0 N.D. d 94) 1,2,4-Trichlorobenzene 0.00 180 0 N.D. 95) Naphthalene 20.78 128 33932 0.384 ng 77 96) n-Dodecane 0.00 57 0 N.D. d 97) Hexachlorobutadiene 0.00 225 0 N.D. 98) Cyclohexanone 0.00 55 0 N.D. d 99) tert-Butylbenzene 18.26 119 3807 N.D. 100) n-Butylbenzene 0.00 91 0 N.D. d -------------------------------------------------------------------------- (#) = qualifier out of range (m) = manual integration (+) = signals summed

R9071315.M Wed Aug 05 12:54:28 2015 Page: 2

29 of 128

Quantitation Report (QT Reviewed)

Data File: I:\MS09\Data\2015_08\05\08051516.D Acq On : 5 Aug 2015 12:08 Operator: SC Sample : P1503012-001 (200mL) Misc : S29-07071501 ALS Vial : 13 Sample Multiplier: 1

Quant Time: Aug 05 12:53:29 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M

4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.000

1000000

2000000

3000000

4000000

5000000

6000000

7000000

8000000

9000000

1e+07

1.1e+07

1.2e+07

1.3e+07

1.4e+07

1.5e+07

1.6e+07

1.7e+07

1.8e+07

1.9e+07

2e+07

2.1e+07

2.2e+07

2.3e+07

2.4e+07

Time-->

Abundance TIC: 08051516.D\data.ms

Nap

htha

lene

,T

1,2,

4-Tr

imet

hylb

enze

ne,T

n-Pr

opyl

benz

ene,

T

Brom

oflu

orob

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ne (S

S3),S

Ethy

lben

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,T

Chl

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ne-d

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3),IR

2-H

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TTo

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(SS2

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Difl

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benz

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(IS2)

,IRC

yclo

hexa

ne,T

Car

bon

Tetra

chlo

ride,

T

1,1,

1-Tr

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than

e,T

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S1),S

Tetra

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HF)

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n-H

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Brom

ochl

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ne (I

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Rci

s-1,

2-D

ichl

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then

e,T

2-Bu

tano

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Dic

hlor

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ane,

Ttra

ns-1

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ichl

oroe

then

e,T

Car

bon

Dis

ulfid

e,T

Met

hyle

ne C

hlor

ide,

T1,

1-D

ichl

oroe

then

e,T

2-Pr

opan

ol (I

sopr

opan

ol),T

Acet

one,

TAc

role

in,T

Etha

nol,T

Viny

l Chl

orid

e,T

Chl

orom

etha

ne,T

Dic

hlor

odifl

uoro

met

hane

(CFC

12)

,T

R9071315.M Wed Aug 05 12:54:29 2015 Page: 3

30 of 128

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_08\05\08051516.D Acq On : 5 Aug 2015 12:08 Operator: SC Sample : P1503012-001 (200mL) Misc : S29-07071501 ALS Vial : 13 Sample Multiplier: 1 Quant Time: Aug 05 12:53:29 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 1) Bromochloromethane (IS1) 9.00 130 148578 12.500 ng -0.02 37) 1,4-Difluorobenzene (IS2) 10.97 114 771890 12.500 ng 0.00 56) Chlorobenzene-d5 (IS3) 15.31 82 321116 12.500 ng 0.00 System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.78 65 258791 10.833 ng -0.01 Spiked Amount 12.500 Recovery = 86.64% 57) Toluene-d8 (SS2) 13.41 98 767238 13.154 ng 0.00 Spiked Amount 12.500 Recovery = 105.20% 73) Bromofluorobenzene (SS3) 16.92 174 250863 13.530 ng 0.00 Spiked Amount 12.500 Recovery = 108.24% Target Compounds Qvalue 3) Dichlorodifluoromethan... 3.88 85 9059 0.229 ng # 97 4) Chloromethane 4.07 50 3576 0.108 ng 92 6) Vinyl Chloride 4.35 62 4757 0.173 ng 96 10) Ethanol 5.22 45 24450 1.481 ng 90 12) Acrolein 5.57 56 1579 0.124 ng 80 13) Acetone 5.70 58 319937m 21.220 ng 15) 2-Propanol (Isopropanol) 6.02 45 5901 0.111 ng 87 17) 1,1-Dichloroethene 6.59 96 272855 16.820 ng 88 19) Methylene Chloride 6.72 84 2300 0.119 ng 86 22) Carbon Disulfide 7.02 76 18292 0.250 ng 95 23) trans-1,2-Dichloroethene 7.75 61 41570 1.535 ng 93 24) 1,1-Dichloroethane 7.96 63 92490 2.637 ng 98 27) 2-Butanone (MEK) 8.38 72 21406 1.696 ng # 81 28) cis-1,2-Dichloroethene 8.83 61 1249444 47.761 ng 93 31) n-Hexane 9.11 57 1578846 47.721 ng 99 32) Chloroform 9.14 83 49128 1.606 ng 83 34) Tetrahydrofuran (THF) 9.54 72 56618 4.413 ng # 91 38) 1,1,1-Trichloroethane 10.17 97 34935 1.325 ng 98 42) Carbon Tetrachloride 10.78 117 2794 0.126 ng 87 43) Cyclohexane 10.91 84 3655637 139.031 ng 91 58) Toluene 13.51 91 10345 0.159 ng 100 59) 2-Hexanone 13.76 43 12555 0.291 ng 99 66) Ethylbenzene 15.76 91 8250 0.114 ng 97 76) n-Propylbenzene 17.60 91 9746 0.104 ng # 39 82) 1,2,4-Trimethylbenzene 18.26 105 21588 0.359 ng 93 95) Naphthalene 20.78 128 33932 0.384 ng 77 -------------------------------------------------------------------------- (#) = qualifier out of range (m) = manual integration (+) = signals summed

R9071315.M Wed Aug 05 12:53:43 2015 Page: 1

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simon.cao

Simon




4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.000

1000000

2000000

3000000

4000000

5000000

6000000

7000000

8000000

9000000

1e+07

1.1e+07

1.2e+07

1.3e+07

1.4e+07

1.5e+07

1.6e+07

1.7e+07

1.8e+07

1.9e+07

2e+07

2.1e+07

2.2e+07

2.3e+07

2.4e+07

Time-->


Nap

htha

lene

,T

1,2,

4-Tr

imet

hylb

enze

ne,T

n-Pr

opyl

benz

ene,

T

Brom

oflu

orob

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ne (S

S3),S

Ethy

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Chl

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5 (IS

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2-H

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one,

TTo

luen

e,TTo

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(SS2

),S

1,4-

Difl

uoro

benz

ene

(IS2)

,IRC

yclo

hexa

ne,T

Car

bon

Tetra

chlo

ride,

T

1,1,

1-Tr

ichl

oroe

than

e,T

1,2-

Dic

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ane-

d4(S

S1),S

Tetra

hydr

ofur

an (T

HF)

,TC

hlor

ofor

m,T

n-H

exan

e,T

Brom

ochl

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etha

ne (I

S1),I

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s-1,

2-D

ichl

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then

e,T

2-Bu

tano

ne (M

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Ttra

ns-1

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ichl

oroe

then

e,T

Car

bon

Dis

ulfid

e,T

Met

hyle

ne C

hlor

ide,

T1,

1-D

ichl

oroe

then

e,T

2-Pr

opan

ol (I

sopr

opan

ol),T

Acet

one,

TAc

role

in,T

Etha

nol,T

Viny

l Chl

orid

e,T

Chl

orom

etha

ne,T

Dic

hlor

odifl

uoro

met

hane

(CFC

12)

,T

R9071315.M Wed Aug 05 12:53:43 2015 Page: 2

32 of 128

#3Dichlorodifluoromethane (CFC 12)Concen: 0.23 ng RT: 3.88 min Scan# 91Delta R.T. 0.020 minLab File: 08051516.DAcq: 5 Aug 2015 12:08

Tgt Ion: 85 Resp: 9059Ion Ratio Lower Upper 85 100 87 33.4 12.4 52.4 101 9.1 0.0 28.8 103 0.0 0.0 25.7

Ref

Raw

Sub

20 30 40 50 60 70 80 90 100 110 1200

50

m/z-->

Abundance Scan 88 (3.856 min): 07131519.D\data.ms (-79) (-)85

50 10135 66 1227442

20 30 40 50 60 70 80 90 100 110 1200

50

m/z-->

Abundance Scan 91 (3.881 min): 08051516.D\data.ms29

4485

37 10164

20 30 40 50 60 70 80 90 100 110 1200

50

m/z-->


4385

10151 64

3.85 3.900

1000

2000

3000

4000

5000

Time-->

Abundance 3.881

#4ChloromethaneConcen: 0.11 ng RT: 4.07 min Scan# 126Delta R.T. 0.012 minLab File: 08051516.DAcq: 5 Aug 2015 12:08

Tgt Ion: 50 Resp: 3576Ion Ratio Lower Upper 50 100 52 27.9 12.3 52.3

Ref

Raw

Sub

20 25 30 35 40 45 50 55 60 65 700

50

m/z-->


4735 38 44 53

20 25 30 35 40 45 50 55 60 65 700

50

m/z-->


3229

4440 654736

20 25 30 35 40 45 50 55 60 65 700

50

m/z-->


32

6547

4.00 4.05 4.10 4.150

500

1000

1500

Time-->

Abundance 4.073

08051516.D R9071315.M Wed Aug 05 12:53:44 2015 Page 3

33 of 128

#6Vinyl ChlorideConcen: 0.17 ng RT: 4.35 min Scan# 177Delta R.T. 0.017 minLab File: 08051516.DAcq: 5 Aug 2015 12:08


Ref

Raw

Sub

20 25 30 35 40 45 50 55 60 65 700

50

m/z-->


35 47 59 655038

20 25 30 35 40 45 50 55 60 65 700

50

m/z-->


3243

6239 57

20 25 30 35 40 45 50 55 60 65 700

50

m/z-->


32 43

6239 57

4.30 4.35 4.400

500

1000

1500

2000

2500

Time-->

Abundance 4.353

#10EthanolConcen: 1.48 ng RT: 5.22 min Scan# 427Delta R.T. -0.069 minLab File: 08051516.DAcq: 5 Aug 2015 12:08


Ref

Raw

Sub

26 28 30 32 34 36 38 40 42 44 46 48 50 52 54 560

50

m/z-->


4341 4736

26 28 30 32 34 36 38 40 42 44 46 48 50 52 54 560

50

m/z-->


4340

26 28 30 32 34 36 38 40 42 44 46 48 50 52 54 560

50

m/z-->


4340

5.20 5.400

2000

4000

6000

8000

Time-->

Abundance 5.221

08051516.D R9071315.M Wed Aug 05 12:53:44 2015 Page 4

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#12AcroleinConcen: 0.12 ng RT: 5.57 min Scan# 550Delta R.T. -0.003 minLab File: 08051516.DAcq: 5 Aug 2015 12:08


Ref

Raw

Sub

30 35 40 45 50 55 60 650

50

m/z-->


37 5339 42 44 58

30 35 40 45 50 55 60 650

50

m/z-->


4440 58

42

30 35 40 45 50 55 60 650

50

m/z-->


4258

5.55 5.600

200

400

600

800

Time-->

Abundance 5.573

#13AcetoneConcen: 21.22 ng mRT: 5.70 min Scan# 594Delta R.T. -0.033 minLab File: 08051516.DAcq: 5 Aug 2015 12:08


Ref

Raw

Sub

30 35 40 45 50 55 60 650

50

m/z-->


58

394137 5645 605254

30 35 40 45 50 55 60 650

50

m/z-->


58

3937 41 6045 52 55

30 35 40 45 50 55 60 650

50

m/z-->


58

3937 41 6045 52 55

5.60 5.65 5.70 5.750

100000

200000

300000

400000

Time-->

Abundance

5.699

08051516.D R9071315.M Wed Aug 05 12:53:44 2015 Page 5

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#152-Propanol (Isopropanol)Concen: 0.11 ng RT: 6.02 min Scan# 706Delta R.T. -0.047 minLab File: 08051516.DAcq: 5 Aug 2015 12:08


Ref

Raw

Sub

30 35 40 45 50 55 60 65 70 750

50

m/z-->


41 5938 5552

30 35 40 45 50 55 60 65 70 750

50

m/z-->


42 5855 70

30 35 40 45 50 55 60 65 70 750

50

m/z-->


70

6.00 6.100

500

1000

1500

2000

Time-->

Abundance 6.020

#171,1-DichloroetheneConcen: 16.82 ng RT: 6.59 min Scan# 906Delta R.T. 0.013 minLab File: 08051516.DAcq: 5 Aug 2015 12:08


Ref

Raw

Sub

30 40 50 60 70 80 90 1000

50

m/z-->


96

35 47 827041 53

30 40 50 60 70 80 90 1000

50

m/z-->


96

35 47 75 8241

30 40 50 60 70 80 90 1000

50

m/z-->


96

35 47 75 82

6.50 6.60 6.700

50000

100000

150000

Time-->

Abundance

6.592

08051516.D R9071315.M Wed Aug 05 12:53:45 2015 Page 6

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#19Methylene ChlorideConcen: 0.12 ng RT: 6.72 min Scan# 951Delta R.T. -0.020 minLab File: 08051516.DAcq: 5 Aug 2015 12:08


Ref

Raw

Sub

25 30 35 40 45 50 55 60 65 70 75 80 85 90 950

50

m/z-->


84

35 887073

25 30 35 40 45 50 55 60 65 70 75 80 85 90 950

50

m/z-->


43

49 8439 7455

25 30 35 40 45 50 55 60 65 70 75 80 85 90 950

50

m/z-->


4349 84

7456

6.65 6.70 6.750

500

1000

Time-->

Abundance

6.721

#22Carbon DisulfideConcen: 0.25 ng RT: 7.02 min Scan# 1057Delta R.T. 0.020 minLab File: 08051516.DAcq: 5 Aug 2015 12:08


Ref

Raw

Sub

40 60 80 100 120 140 1600

50

m/z-->


44101 1518764 113 132 16934

40 60 80 100 120 140 1600

50

m/z-->


44

40 60 80 100 120 140 1600

50

m/z-->


44

6.95 7.00 7.05 7.100

2000

4000

6000

Time-->

Abundance 7.025

08051516.D R9071315.M Wed Aug 05 12:53:45 2015 Page 7

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#23trans-1,2-DichloroetheneConcen: 1.53 ng RT: 7.75 min Scan# 1311Delta R.T. -0.002 minLab File: 08051516.DAcq: 5 Aug 2015 12:08


Ref

Raw

Sub

30 40 50 60 70 80 90 1000

50

m/z-->


96

4735 70 82

30 40 50 60 70 80 90 1000

50

m/z-->


96

4735 67 7941

30 40 50 60 70 80 90 1000

50

m/z-->


96

4935 6741

7.70 7.800

5000

10000

15000

Time-->

Abundance 7.752

#241,1-DichloroethaneConcen: 2.64 ng RT: 7.96 min Scan# 1385Delta R.T. -0.012 minLab File: 08051516.DAcq: 5 Aug 2015 12:08


Ref

Raw

Sub

30 40 50 60 70 80 90 1000

50

m/z-->


839835 47 7041

30 40 50 60 70 80 90 1000

50

m/z-->

Abundance Scan 1385 (7.964 min): 08051516.D\data.ms63 75

45 839835

30 40 50 60 70 80 90 1000

50

m/z-->

Abundance Scan 1385 (7.964 min): 08051516.D\data.ms (-1302) (-)63 75

834535 100

7.85 7.90 7.95 8.00 8.050

10000

20000

30000

Time-->

Abundance 7.964

08051516.D R9071315.M Wed Aug 05 12:53:45 2015 Page 8

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#272-Butanone (MEK)Concen: 1.70 ng RT: 8.38 min Scan# 1530Delta R.T. -0.012 minLab File: 08051516.DAcq: 5 Aug 2015 12:08

Tgt Ion: 72 Resp: 21406Ion Ratio Lower Upper 72 100 43 419.0 449.8 489.8#

Ref

Raw

Sub

30 35 40 45 50 55 60 65 70 75 800

50

m/z-->


725746 53 69

30 35 40 45 50 55 60 65 70 75 800

50

m/z-->


725739 50 53

30 35 40 45 50 55 60 65 70 75 800

50

m/z-->


45

8.30 8.40 8.500

10000

20000

30000

40000

Time-->

Abundance

8.379

#28cis-1,2-DichloroetheneConcen: 47.76 ng RT: 8.83 min Scan# 1689Delta R.T. -0.015 minLab File: 08051516.DAcq: 5 Aug 2015 12:08


Ref

Raw

Sub

40 60 80 100 120 140 160 180 2000

50

m/z-->


96

35 48 74

40 60 80 100 120 140 160 180 2000

50

m/z-->


96

35 47 20774

40 60 80 100 120 140 160 180 2000

50

m/z-->


96

35 47 20774

8.80 9.000

100000

200000

300000

400000

500000

Time-->

Abundance 8.834

08051516.D R9071315.M Wed Aug 05 12:53:46 2015 Page 9

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#31n-HexaneConcen: 47.72 ng RT: 9.11 min Scan# 1785Delta R.T. 0.028 minLab File: 08051516.DAcq: 5 Aug 2015 12:08

Tgt Ion: 57 Resp: 1578846Ion Ratio Lower Upper 57 100 56 51.5 40.6 61.0 86 13.7 10.1 15.1

Ref

Raw

Sub

40 60 80 100 120 140 160 180 2000

50

m/z-->


578770 101

40 60 80 100 120 140 160 180 2000

50

m/z-->


41

8671 130 207

40 60 80 100 120 140 160 180 2000

50

m/z-->


41

8671 128 207

9.00 9.10 9.200

200000

400000

600000

Time-->

Abundance 9.109

#32ChloroformConcen: 1.61 ng RT: 9.14 min Scan# 1797Delta R.T. -0.018 minLab File: 08051516.DAcq: 5 Aug 2015 12:08


Ref

Raw

Sub

40 60 80 100 120 140 160 180 2000

50

m/z-->


4735

11859 207

40 60 80 100 120 140 160 180 2000

50

m/z-->


4183

71 117

40 60 80 100 120 140 160 180 2000

50

m/z-->


4183

71 117

9.05 9.10 9.15 9.200

5000

10000

15000

20000

Time-->

Abundance 9.144

08051516.D R9071315.M Wed Aug 05 12:53:46 2015 Page 10

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#34Tetrahydrofuran (THF)Concen: 4.41 ng RT: 9.54 min Scan# 1934Delta R.T. 0.007 minLab File: 08051516.DAcq: 5 Aug 2015 12:08

Tgt Ion: 72 Resp: 56618Ion Ratio Lower Upper 72 100 71 96.8 77.5 117.5 42 250.6 251.9 291.9#

Ref

Raw

Sub

25 30 35 40 45 50 55 60 65 70 75 80 85 900

50

m/z-->


7239

505335 57 6846

25 30 35 40 45 50 55 60 65 70 75 80 85 900

50

m/z-->


72

3955 6945 8450

25 30 35 40 45 50 55 60 65 70 75 80 85 900

50

m/z-->


72

395545 50 67

9.50 9.600

20000

40000

Time-->

Abundance

9.536

#381,1,1-TrichloroethaneConcen: 1.32 ng RT: 10.17 min Scan# 2155Delta R.T. 0.004 minLab File: 08051516.DAcq: 5 Aug 2015 12:08


Ref

Raw

Sub

40 60 80 100 120 140 160 180 2000

50

m/z-->


61

11735 47 82

40 60 80 100 120 140 160 180 2000

50

m/z-->


61

41 11785 207

40 60 80 100 120 140 160 180 2000

50

m/z-->


61 11735 47

10.10 10.15 10.20 10.250

5000

10000

15000

Time-->

Abundance10.169

08051516.D R9071315.M Wed Aug 05 12:53:46 2015 Page 11

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#42Carbon TetrachlorideConcen: 0.13 ng RT: 10.78 min Scan# 2367Delta R.T. 0.002 minLab File: 08051516.DAcq: 5 Aug 2015 12:08

Tgt Ion:117 Resp: 2794Ion Ratio Lower Upper117 100119 108.5 75.4 115.4

Ref

Raw

Sub

40 60 80 100 120 140 160 180 2000

50

m/z-->


824735

59

40 60 80 100 120 140 160 180 2000

50

m/z-->


85 11755207

40 60 80 100 120 140 160 180 2000

50

m/z-->


85 11755

10.75 10.800

500

1000

1500

Time-->

Abundance10.776

#43CyclohexaneConcen: 139.03 ng RT: 10.91 min Scan# 2415Delta R.T. 0.010 minLab File: 08051516.DAcq: 5 Aug 2015 12:08


Ref

Raw

Sub

25 30 35 40 45 50 55 60 65 70 75 80 85 900

50

m/z-->


8441

69

535038 7763 7344 806033 66

25 30 35 40 45 50 55 60 65 70 75 80 85 900

50

m/z-->


41

69

5338 50 7763 73 80604433 66

25 30 35 40 45 50 55 60 65 70 75 80 85 900

50

m/z-->


41

69

51 7763 73 806036 4844 66

10.80 10.90 11.000

500000

1000000

1500000

Time-->

Abundance

10.913

08051516.D R9071315.M Wed Aug 05 12:53:47 2015 Page 12

42 of 128

#58TolueneConcen: 0.16 ng RT: 13.51 min Scan# 3321Delta R.T. -0.006 minLab File: 08051516.DAcq: 5 Aug 2015 12:08


Ref

Raw

Sub

30 40 50 60 70 80 90 1000

50

m/z-->


6539 5145 8574

30 40 50 60 70 80 90 1000

50

m/z-->


39 6551 987745

30 40 50 60 70 80 90 1000

50

m/z-->


6539 51 987745

13.45 13.50 13.550

1000

2000

3000

4000

Time-->

Abundance13.507

#592-HexanoneConcen: 0.29 ng RT: 13.76 min Scan# 3410Delta R.T. 0.001 minLab File: 08051516.DAcq: 5 Aug 2015 12:08


Ref

Raw

Sub

30 40 50 60 70 80 90 1000

50

m/z-->


58

100857150 776437

30 40 50 60 70 80 90 1000

50

m/z-->


58

1008571

30 40 50 60 70 80 90 1000

50

m/z-->


58

8571 100

13.70 13.800

1000

2000

3000

4000

5000

Time-->

Abundance13.762

08051516.D R9071315.M Wed Aug 05 12:53:47 2015 Page 13

43 of 128

#66EthylbenzeneConcen: 0.11 ng RT: 15.76 min Scan# 4108Delta R.T. -0.007 minLab File: 08051516.DAcq: 5 Aug 2015 12:08

Tgt Ion: 91 Resp: 8250Ion Ratio Lower Upper 91 100106 28.2 10.0 50.0

Ref

Raw

Sub

30 40 50 60 70 80 90 100 1100

50

m/z-->


106

51 65 7739 83 97

30 40 50 60 70 80 90 100 1100

50

m/z-->


1066543 51 7871

30 40 50 60 70 80 90 100 1100

50

m/z-->


1066551 787139

15.70 15.75 15.800

1000

2000

3000

4000

Time-->

Abundance15.761

#76n-PropylbenzeneConcen: 0.10 ng RT: 17.60 min Scan# 4750Delta R.T. -0.007 minLab File: 08051516.DAcq: 5 Aug 2015 12:08

Tgt Ion: 91 Resp: 9746Ion Ratio Lower Upper 91 100120 21.6 1.3 41.3 65 78.6 0.0 30.6#

Ref

Raw

Sub

30 40 50 60 70 80 90 100 110 1200

50

m/z-->


12065 7839 51 10557 98 113

30 40 50 60 70 80 90 100 110 1200

50

m/z-->


55 6539120

83 1117347

30 40 50 60 70 80 90 100 110 1200

50

m/z-->


65120

38 51 77 105

17.55 17.60 17.650

1000

2000

3000

4000

5000

Time-->

Abundance17.599

08051516.D R9071315.M Wed Aug 05 12:53:47 2015 Page 14

44 of 128

#821,2,4-TrimethylbenzeneConcen: 0.36 ng RT: 18.26 min Scan# 4982Delta R.T. -0.012 minLab File: 08051516.DAcq: 5 Aug 2015 12:08


Ref

Raw

Sub

40 60 80 100 120 140 160 1800

50

m/z-->


91

77 13441 6553

40 60 80 100 120 140 160 1800

50

m/z-->


41 6912083

140193

40 60 80 100 120 140 160 1800

50

m/z-->


41 69 12083140

193

18.20 18.25 18.300

5000

10000

Time-->

Abundance18.263

#95NaphthaleneConcen: 0.38 ng RT: 20.78 min Scan# 5860Delta R.T. -0.005 minLab File: 08051516.DAcq: 5 Aug 2015 12:08


Ref

Raw

Sub

40 60 80 100 120 140 160 180 2000

50

m/z-->


10251 64 7739 89 207114

40 60 80 100 120 140 160 180 2000

50

m/z-->


55 819541 69

109 151 166207

40 60 80 100 120 140 160 180 2000

50

m/z-->


81 9555 67 151 16641 109 207

20.75 20.800

5000

10000

15000

20000

Time-->

Abundance20.777

08051516.D R9071315.M Wed Aug 05 12:53:48 2015 Page 15

45 of 128

Quantitation Report (Qedit)



5.15 5.20 5.25 5.30 5.35 5.40 5.45 5.50 5.55 5.60 5.65 5.70 5.75 5.80 5.85 5.90 5.95 6.00 6.05 6.10 6.15 6.20 6.25 6.30 6.35 6.40 6.45

0

20000

40000

60000

80000

100000

Time-->

Abundance Ion 58.00 (57.70 to 58.70): 08051516.D\data.ms 5.699

|

| |

|

|

|

|

|

Ion 43.00 (42.70 to 43.70): 08051516.D\data.ms

26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69

200000

400000

m/z-->


58

4239 44413837 595740 5336 5545 52 6056

26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 690

5000

m/z-->


58

4239 44413837 59574036 53 5545 52 6054 5646

TIC: 08051516.D\data.ms

0.00 0.00 0.00

0.00 0.00 0.00

43.00 332.20 265.50#

58.00 100 100

Ion Exp% Act%

response 365215

5.699min (-0.033) 24.22ng

(13) Acetone (T)

R9071315.M Wed Aug 05 12:50:23 2015 Page: 1

46 of 128

Quantitation Report (Qedit)



5.15 5.20 5.25 5.30 5.35 5.40 5.45 5.50 5.55 5.60 5.65 5.70 5.75 5.80 5.85 5.90 5.95 6.00 6.05 6.10 6.15 6.20 6.25 6.30 6.35 6.40 6.45

0

20000

40000

60000

80000

100000

Time-->

Abundance Ion 58.00 (57.70 to 58.70): 08051516.D\data.ms 5.699

|

| |

|

|

|

|

|

Ion 43.00 (42.70 to 43.70): 08051516.D\data.ms

26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69

200000

400000

m/z-->


58

4239 44413837 595740 5336 5545 52 6056

26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 690

5000

m/z-->


58

4239 44413837 59574036 53 5545 52 6054 5646

TIC: 08051516.D\data.ms

0.00 0.00 0.00

0.00 0.00 0.00

43.00 332.20 303.08

58.00 100 100

Ion Exp% Act%

response 319937

5.699min (-0.033) 21.22ng m

(13) Acetone (T)

R9071315.M Wed Aug 05 12:50:38 2015 Page: 1

47 of 128

simon.cao

IPC

simon.cao

Simon

chris.parnell

Chris

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_08\04\08041526.D Acq On : 4 Aug 2015 20:24 Operator: SC Sample : P1503012-002 (20mL) Misc : S29-07071501 ALS Vial : 14 Sample Multiplier: 1 Quant Time: Aug 05 09:48:24 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 1) Bromochloromethane (IS1) 8.98 130 137737 12.500 ng -0.03 37) 1,4-Difluorobenzene (IS2) 10.97 114 716236 12.500 ng -0.01 56) Chlorobenzene-d5 (IS3) 15.31 82 325769 12.500 ng 0.00 System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.77 65 252923 11.420 ng -0.02 Spiked Amount 12.500 Recovery = 91.36% 57) Toluene-d8 (SS2) 13.40 98 726291 12.274 ng 0.00 Spiked Amount 12.500 Recovery = 98.16% 73) Bromofluorobenzene (SS3) 16.92 174 250122 13.297 ng 0.00 Spiked Amount 12.500 Recovery = 106.40% Target Compounds Qvalue 2) Propene 0.00 42 0 N.D. d 3) Dichlorodifluoromethan... 3.86 85 1222 N.D. 4) Chloromethane 0.00 50 0 N.D. 5) 1,2-Dichloro-1,1,2,2-t... 0.00 135 0 N.D. 6) Vinyl Chloride 4.35 62 588 N.D. 7) 1,3-Butadiene 0.00 54 0 N.D. d 8) Bromomethane 0.00 94 0 N.D. 9) Chloroethane 0.00 64 0 N.D. 10) Ethanol 5.28 45 77 N.D. 11) Acetonitrile 5.46 41 30 N.D. 12) Acrolein 0.00 56 0 N.D. 13) Acetone 0.00 58 0 N.D. d 14) Trichlorofluoromethane 0.00 101 0 N.D. 15) 2-Propanol (Isopropanol) 6.05 45 792 N.D. 16) Acrylonitrile 0.00 53 0 N.D. d 17) 1,1-Dichloroethene 6.58 96 12938 0.860 ng 91 18) 2-Methyl-2-Propanol (t... 6.71 59 1121 N.D. 19) Methylene Chloride 6.73 84 1744 0.098 ng 92 20) 3-Chloro-1-propene (Al... 0.00 41 0 N.D. d 21) Trichlorotrifluoroethane 0.00 151 0 N.D. 22) Carbon Disulfide 7.02 76 998 N.D. 23) trans-1,2-Dichloroethene 0.00 61 0 N.D. 24) 1,1-Dichloroethane 7.95 63 2585 N.D. 25) Methyl tert-Butyl Ether 8.05 73 709 N.D. 26) Vinyl Acetate 0.00 86 0 N.D. d 27) 2-Butanone (MEK) 8.39 72 1970 0.168 ng # 65 28) cis-1,2-Dichloroethene 8.82 61 6488 0.268 ng 96 29) Diisopropyl Ether 0.00 87 0 N.D. d 30) Ethyl Acetate 0.00 61 0 N.D. d 31) n-Hexane 9.09 57 1589240 51.816 ng 99 32) Chloroform 0.00 83 0 N.D. d 34) Tetrahydrofuran (THF) 9.57 72 2414 0.203 ng 93 35) Ethyl tert-Butyl Ether 0.00 87 0 N.D. 36) 1,2-Dichloroethane 0.00 62 0 N.D. d 38) 1,1,1-Trichloroethane 10.16 97 513 N.D. 39) Isopropyl Acetate 0.00 61 0 N.D. 40) 1-Butanol 0.00 56 0 N.D. d 41) Benzene 10.61 78 16215 0.246 ng 98 42) Carbon Tetrachloride 0.00 117 0 N.D. 43) Cyclohexane 10.90 84 210818 8.641 ng 93 44) tert-Amyl Methyl Ether 0.00 73 0 N.D. 45) 1,2-Dichloropropane 0.00 63 0 N.D. d 46) Bromodichloromethane 0.00 83 0 N.D. d 47) Trichloroethene 11.67 130 9394 0.583 ng 97 48) 1,4-Dioxane 0.00 88 0 N.D. 49) 2,2,4-Trimethylpentane... 0.00 57 0 N.D. d

R9071315.M Wed Aug 05 09:49:50 2015 Page: 1

48 of 128

simon.cao

Simon

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_08\04\08041526.D Acq On : 4 Aug 2015 20:24 Operator: SC Sample : P1503012-002 (20mL) Misc : S29-07071501 ALS Vial : 14 Sample Multiplier: 1 Quant Time: Aug 05 09:48:24 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 50) Methyl Methacrylate 0.00 100 0 N.D. d 51) n-Heptane 11.99 71 50674 3.024 ng 97 52) cis-1,3-Dichloropropene 12.65 75 670 N.D. 53) 4-Methyl-2-pentanone 0.00 58 0 N.D. d 54) trans-1,3-Dichloropropene 0.00 75 0 N.D. 55) 1,1,2-Trichloroethane 0.00 97 0 N.D. d 58) Toluene 13.50 91 3047 N.D. 59) 2-Hexanone 0.00 43 0 N.D. d 60) Dibromochloromethane 0.00 129 0 N.D. 61) 1,2-Dibromoethane 0.00 107 0 N.D. 62) n-Butyl Acetate 0.00 43 0 N.D. d 63) n-Octane 14.53 57 1032 N.D. 64) Tetrachloroethene 14.66 166 216618 13.174 ng 100 65) Chlorobenzene 0.00 112 0 N.D. d 66) Ethylbenzene 15.76 91 1059053 14.474 ng 98 67) m- & p-Xylenes 15.95 91 2284 N.D. 68) Bromoform 0.00 173 0 N.D. 69) Styrene 0.00 104 0 N.D. 70) o-Xylene 16.46 91 3329 N.D. 71) n-Nonane 0.00 43 0 N.D. d 72) 1,1,2,2-Tetrachloroethane 0.00 83 0 N.D. d 74) Cumene 17.07 105 90698 1.218 ng 100 75) alpha-Pinene 0.00 93 0 N.D. d 76) n-Propylbenzene 17.60 91 369432 3.874 ng 98 77) 3-Ethyltoluene 17.72 105 1132 N.D. 78) 4-Ethyltoluene 17.75 105 3434 N.D. 79) 1,3,5-Trimethylbenzene 17.84 105 17974 0.302 ng 98 80) alpha-Methylstyrene 0.00 118 0 N.D. d 81) 2-Ethyltoluene 0.00 105 0 N.D. d 82) 1,2,4-Trimethylbenzene 18.27 105 565873 9.270 ng 90 83) n-Decane 0.00 57 0 N.D. d 84) Benzyl Chloride 0.00 91 0 N.D. d 85) 1,3-Dichlorobenzene 0.00 146 0 N.D. 86) 1,4-Dichlorobenzene 0.00 146 0 N.D. 87) sec-Butylbenzene 0.00 105 0 N.D. d 88) 4-Isopropyltoluene (p-... 0.00 119 0 N.D. d 89) 1,2,3-Trimethylbenzene 0.00 105 0 N.D. d 90) 1,2-Dichlorobenzene 0.00 146 0 N.D. 91) d-Limonene 0.00 68 0 N.D. d 92) 1,2-Dibromo-3-Chloropr... 0.00 157 0 N.D. 93) n-Undecane 0.00 57 0 N.D. d 94) 1,2,4-Trichlorobenzene 20.67 180 1939 N.D. 95) Naphthalene 20.78 128 653375 7.285 ng 54 96) n-Dodecane 0.00 57 0 N.D. d 97) Hexachlorobutadiene 0.00 225 0 N.D. 98) Cyclohexanone 0.00 55 0 N.D. d 99) tert-Butylbenzene 0.00 119 0 N.D. d 100) n-Butylbenzene 0.00 91 0 N.D. d -------------------------------------------------------------------------- (#) = qualifier out of range (m) = manual integration (+) = signals summed

R9071315.M Wed Aug 05 09:49:50 2015 Page: 2

49 of 128




4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.000

500000

1000000

1500000

2000000

2500000

3000000

3500000

4000000

4500000

5000000

5500000

6000000

6500000

7000000

7500000

8000000

8500000

9000000

9500000

1e+07

1.05e+07

1.1e+07

1.15e+07

1.2e+07

1.25e+07

1.3e+07

1.35e+07

1.4e+07

1.45e+07

Time-->


Nap

htha

lene

,T

1,2,

4-Tr

imet

hylb

enze

ne,T

1,3,

5-Tr

imet

hylb

enze

ne,T

n-Pr

opyl

benz

ene,

T

Cum

ene,

TBr

omof

luor

oben

zene

(SS3

),S

Ethy

lben

zene

,T

Chl

orob

enze

ne-d

5 (IS

3),IR

Tetra

chlo

roet

hene

,T

Tolu

ene-

d8 (S

S2),S

n-H

epta

ne,T

Tric

hlor

oeth

ene,

T

1,4-

Difl

uoro

benz

ene

(IS2)

,IRC

yclo

hexa

ne,T

Benz

ene,

T

1,2-

Dic

hlor

oeth

ane-

d4(S

S1),S

Tetra

hydr

ofur

an (T

HF)

,T

n-H

exan

e,T

Brom

ochl

orom

etha

ne (I

S1),I

Rci

s-1,

2-D

ichl

oroe

then

e,T

2-Bu

tano

ne (M

EK),T

Met

hyle

ne C

hlor

ide,

T1,

1-D

ichl

oroe

then

e,T

R9071315.M Wed Aug 05 09:49:50 2015 Page: 3

50 of 128

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_08\04\08041526.D Acq On : 4 Aug 2015 20:24 Operator: SC Sample : P1503012-002 (20mL) Misc : S29-07071501 ALS Vial : 14 Sample Multiplier: 1 Quant Time: Aug 05 09:48:24 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 1) Bromochloromethane (IS1) 8.98 130 137737 12.500 ng -0.03 37) 1,4-Difluorobenzene (IS2) 10.97 114 716236 12.500 ng -0.01 56) Chlorobenzene-d5 (IS3) 15.31 82 325769 12.500 ng 0.00 System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.77 65 252923 11.420 ng -0.02 Spiked Amount 12.500 Recovery = 91.36% 57) Toluene-d8 (SS2) 13.40 98 726291 12.274 ng 0.00 Spiked Amount 12.500 Recovery = 98.16% 73) Bromofluorobenzene (SS3) 16.92 174 250122 13.297 ng 0.00 Spiked Amount 12.500 Recovery = 106.40% Target Compounds Qvalue 17) 1,1-Dichloroethene 6.58 96 12938 0.860 ng 91 19) Methylene Chloride 6.73 84 1744 0.098 ng 92 27) 2-Butanone (MEK) 8.39 72 1970 0.168 ng # 65 28) cis-1,2-Dichloroethene 8.82 61 6488 0.268 ng 96 31) n-Hexane 9.09 57 1589240 51.816 ng 99 34) Tetrahydrofuran (THF) 9.57 72 2414 0.203 ng 93 41) Benzene 10.61 78 16215 0.246 ng 98 43) Cyclohexane 10.90 84 210818 8.641 ng 93 47) Trichloroethene 11.67 130 9394 0.583 ng 97 51) n-Heptane 11.99 71 50674 3.024 ng 97 64) Tetrachloroethene 14.66 166 216618 13.174 ng 100 66) Ethylbenzene 15.76 91 1059053 14.474 ng 98 74) Cumene 17.07 105 90698 1.218 ng 100 76) n-Propylbenzene 17.60 91 369432 3.874 ng 98 79) 1,3,5-Trimethylbenzene 17.84 105 17974 0.302 ng 98 82) 1,2,4-Trimethylbenzene 18.27 105 565873 9.270 ng 90 95) Naphthalene 20.78 128 653375 7.285 ng 54 -------------------------------------------------------------------------- (#) = qualifier out of range (m) = manual integration (+) = signals summed

R9071315.M Wed Aug 05 09:48:38 2015 Page: 1

51 of 128

simon.cao

Simon




4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.000

500000

1000000

1500000

2000000

2500000

3000000

3500000

4000000

4500000

5000000

5500000

6000000

6500000

7000000

7500000

8000000

8500000

9000000

9500000

1e+07

1.05e+07

1.1e+07

1.15e+07

1.2e+07

1.25e+07

1.3e+07

1.35e+07

1.4e+07

1.45e+07

Time-->


Nap

htha

lene

,T

1,2,

4-Tr

imet

hylb

enze

ne,T

1,3,

5-Tr

imet

hylb

enze

ne,T

n-Pr

opyl

benz

ene,

T

Cum

ene,

TBr

omof

luor

oben

zene

(SS3

),S

Ethy

lben

zene

,T

Chl

orob

enze

ne-d

5 (IS

3),IR

Tetra

chlo

roet

hene

,T

Tolu

ene-

d8 (S

S2),S

n-H

epta

ne,T

Tric

hlor

oeth

ene,

T

1,4-

Difl

uoro

benz

ene

(IS2)

,IRC

yclo

hexa

ne,T

Benz

ene,

T

1,2-

Dic

hlor

oeth

ane-

d4(S

S1),S

Tetra

hydr

ofur

an (T

HF)

,T

n-H

exan

e,T

Brom

ochl

orom

etha

ne (I

S1),I

Rci

s-1,

2-D

ichl

oroe

then

e,T

2-Bu

tano

ne (M

EK),T

Met

hyle

ne C

hlor

ide,

T1,

1-D

ichl

oroe

then

e,T

R9071315.M Wed Aug 05 09:48:38 2015 Page: 2

52 of 128

#171,1-DichloroetheneConcen: 0.86 ng RT: 6.58 min Scan# 901Delta R.T. -0.001 minLab File: 08041526.DAcq: 4 Aug 2015 20:24


Ref

Raw

Sub

30 40 50 60 70 80 90 1000

50

m/z-->


96

35 47 827041 53

30 40 50 60 70 80 90 1000

50

m/z-->


96

35 47

30 40 50 60 70 80 90 1000

50

m/z-->


96

35 47

6.50 6.55 6.60 6.650

2000

4000

6000

8000

Time-->

Abundance

6.578

#19Methylene ChlorideConcen: 0.10 ng RT: 6.73 min Scan# 953Delta R.T. -0.014 minLab File: 08041526.DAcq: 4 Aug 2015 20:24


Ref

Raw

Sub

25 30 35 40 45 50 55 60 65 70 75 80 85 90 950

50

m/z-->


84

35 887073

25 30 35 40 45 50 55 60 65 70 75 80 85 90 950

50

m/z-->


4359

25 30 35 40 45 50 55 60 65 70 75 80 85 90 950

50

m/z-->


4359

6.70 6.750

500

1000

Time-->

Abundance

6.727

08041526.D R9071315.M Wed Aug 05 09:48:39 2015 Page 3

53 of 128

#272-Butanone (MEK)Concen: 0.17 ng RT: 8.39 min Scan# 1535Delta R.T. 0.002 minLab File: 08041526.DAcq: 4 Aug 2015 20:24

Tgt Ion: 72 Resp: 1970Ion Ratio Lower Upper 72 100 43 562.6 449.8 489.8#

Ref

Raw

Sub

30 35 40 45 50 55 60 65 70 75 800

50

m/z-->


725746 53 69

30 35 40 45 50 55 60 65 70 75 800

50

m/z-->


7240 57

30 35 40 45 50 55 60 65 70 75 800

50

m/z-->


8.35 8.40 8.450

1000

2000

3000

Time-->

Abundance

8.393

#28cis-1,2-DichloroetheneConcen: 0.27 ng RT: 8.82 min Scan# 1685Delta R.T. -0.026 minLab File: 08041526.DAcq: 4 Aug 2015 20:24


Ref

Raw

Sub

30 40 50 60 70 80 90 1000

50

m/z-->


96

35 48 70 82

30 40 50 60 70 80 90 1000

50

m/z-->


96

4048

30 40 50 60 70 80 90 1000

50

m/z-->


6140

8.75 8.80 8.85 8.900

500

1000

1500

2000

2500

Time-->

Abundance 8.823

08041526.D R9071315.M Wed Aug 05 09:48:39 2015 Page 4

54 of 128

#31n-HexaneConcen: 51.82 ng RT: 9.09 min Scan# 1780Delta R.T. 0.014 minLab File: 08041526.DAcq: 4 Aug 2015 20:24


Ref

Raw

Sub

30 40 50 60 70 80 90 100 110 120 1300

50

m/z-->


578770 77 10150

30 40 50 60 70 80 90 100 110 120 1300

50

m/z-->


41

867150 79 95 128

30 40 50 60 70 80 90 100 110 120 1300

50

m/z-->


41

867150 12879 95

9.00 9.10 9.20 9.300

200000

400000

600000

Time-->

Abundance 9.095

#34Tetrahydrofuran (THF)Concen: 0.20 ng RT: 9.57 min Scan# 1945Delta R.T. 0.038 minLab File: 08041526.DAcq: 4 Aug 2015 20:24


Ref

Raw

Sub

25 30 35 40 45 50 55 60 65 70 75 800

50

m/z-->


7239

45 50 5335 57 68

25 30 35 40 45 50 55 60 65 70 75 800

50

m/z-->


72

39

25 30 35 40 45 50 55 60 65 70 75 800

50

m/z-->


72

9.55 9.600

1000

2000

Time-->

Abundance

9.567

08041526.D R9071315.M Wed Aug 05 09:48:39 2015 Page 5

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#41BenzeneConcen: 0.25 ng RT: 10.61 min Scan# 2310Delta R.T. -0.011 minLab File: 08041526.DAcq: 4 Aug 2015 20:24


Ref

Raw

Sub

30 35 40 45 50 55 60 65 70 75 80 850

50

m/z-->


52746337 49

30 35 40 45 50 55 60 65 70 75 80 850

50

m/z-->


5139 56 7443 63 69

30 35 40 45 50 55 60 65 70 75 80 850

50

m/z-->


5139 746343 55 69

10.55 10.60 10.650

2000

4000

6000

Time-->

Abundance10.612

#43CyclohexaneConcen: 8.64 ng RT: 10.90 min Scan# 2411Delta R.T. -0.002 minLab File: 08041526.DAcq: 4 Aug 2015 20:24


Ref

Raw

Sub

25 30 35 40 45 50 55 60 65 70 75 80 85 900

50

m/z-->


8441

69

535038 7763 7344 806033 66

25 30 35 40 45 50 55 60 65 70 75 80 85 900

50

m/z-->


41

69

535038 6366 7774 80

25 30 35 40 45 50 55 60 65 70 75 80 85 900

50

m/z-->


41

69

535038 6366 7774 80

10.80 10.90 11.000

50000

100000

Time-->

Abundance

10.902

08041526.D R9071315.M Wed Aug 05 09:48:40 2015 Page 6

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#47TrichloroetheneConcen: 0.58 ng RT: 11.67 min Scan# 2678Delta R.T. -0.009 minLab File: 08041526.DAcq: 4 Aug 2015 20:24


Ref

Raw

Sub

30 40 50 60 70 80 90 100 110 120 130 1400

50

m/z-->


60

4735 8268

30 40 50 60 70 80 90 100 110 120 130 1400

50

m/z-->


41

83

95 132

30 40 50 60 70 80 90 100 110 120 130 1400

50

m/z-->


41

8395 132

11.60 11.65 11.700

1000

2000

3000

4000

Time-->

Abundance11.666

#51n-HeptaneConcen: 3.02 ng RT: 11.99 min Scan# 2791Delta R.T. -0.003 minLab File: 08041526.DAcq: 4 Aug 2015 20:24


Ref

Raw

Sub

30 40 50 60 70 80 90 1000

50

m/z-->


7157

1008550 7837 63

30 40 50 60 70 80 90 1000

50

m/z-->


7157

1008150 65

30 40 50 60 70 80 90 1000

50

m/z-->


71

10085

11.90 11.95 12.00 12.050

5000

10000

15000

20000

25000

Time-->

Abundance11.990

08041526.D R9071315.M Wed Aug 05 09:48:40 2015 Page 7

57 of 128

#64TetrachloroetheneConcen: 13.17 ng RT: 14.66 min Scan# 3724Delta R.T. -0.006 minLab File: 08041526.DAcq: 4 Aug 2015 20:24


Ref

Raw

Sub

40 60 80 100 120 140 1600

50

m/z-->


129

94

4759 8235

11770

40 60 80 100 120 140 1600

50

m/z-->


129

94846947 5935

111

40 60 80 100 120 140 1600

50

m/z-->


129

94

47 84695935111

14.60 14.700

20000

40000

60000

80000

100000

Time-->

Abundance14.661

#66EthylbenzeneConcen: 14.47 ng RT: 15.76 min Scan# 4108Delta R.T. -0.007 minLab File: 08041526.DAcq: 4 Aug 2015 20:24

Tgt Ion: 91 Resp: 1059053Ion Ratio Lower Upper 91 100106 31.0 10.0 50.0

Ref

Raw

Sub

30 40 50 60 70 80 90 100 110 120 1300

50

m/z-->


106

51 65 7739 84 98

30 40 50 60 70 80 90 100 110 120 1300

50

m/z-->


106

51 65 7739 84 98 12658

30 40 50 60 70 80 90 100 110 120 1300

50

m/z-->


106

51 65 77 84 9838 126

15.70 15.800

100000

200000

300000

400000

500000

Time-->

Abundance15.761

08041526.D R9071315.M Wed Aug 05 09:48:40 2015 Page 8

58 of 128

#74CumeneConcen: 1.22 ng RT: 17.07 min Scan# 4565Delta R.T. -0.009 minLab File: 08041526.DAcq: 4 Aug 2015 20:24


Ref

Raw

Sub

40 60 80 100 120 140 160 1800

50

m/z-->


1207751 9139 63

40 60 80 100 120 140 160 1800

50

m/z-->


43

70 85 105120 142 17695

40 60 80 100 120 140 160 1800

50

m/z-->


43

71 85 105120 142 176

17.00 17.05 17.10 17.150

10000

20000

30000

40000

50000

Time-->

Abundance17.069

#76n-PropylbenzeneConcen: 3.87 ng RT: 17.60 min Scan# 4751Delta R.T. -0.005 minLab File: 08041526.DAcq: 4 Aug 2015 20:24

Tgt Ion: 91 Resp: 369432Ion Ratio Lower Upper 91 100120 21.4 1.3 41.3 65 12.9 0.0 30.6

Ref

Raw

Sub

30 40 50 60 70 80 90 100 110 120 130 1400

50

m/z-->


12065 7839 51 105

30 40 50 60 70 80 90 100 110 120 130 1400

50

m/z-->


556941 120

83 111 14099

30 40 50 60 70 80 90 100 110 120 130 1400

50

m/z-->


12065 1117851 14010337

17.50 17.60 17.700

50000

100000

150000

200000

Time-->

Abundance17.602

08041526.D R9071315.M Wed Aug 05 09:48:41 2015 Page 9

59 of 128



Ref

Raw

Sub

30 40 50 60 70 80 90 100 110 120 130 140 150 1600

50

m/z-->


120

77 9139 51 65

30 40 50 60 70 80 90 100 110 120 130 140 150 1600

50

m/z-->


5541

12583 11197 140154

30 40 50 60 70 80 90 100 110 120 130 140 150 1600

50

m/z-->


12557

111 140834395

154

17.80 17.85 17.900

2000

4000

6000

8000

10000

Time-->

Abundance17.837



Ref

Raw

Sub

30 40 50 60 70 80 90 100 110 120 130 140 150 1600

50

m/z-->


91

77 13441 51 65

30 40 50 60 70 80 90 100 110 120 130 140 150 1600

50

m/z-->


694112083

140111154

30 40 50 60 70 80 90 100 110 120 130 140 150 1600

50

m/z-->


694112083

140111154

18.20 18.25 18.30 18.350

100000

200000

300000

Time-->

Abundance18.266

08041526.D R9071315.M Wed Aug 05 09:48:41 2015 Page 10

60 of 128

#95NaphthaleneConcen: 7.28 ng RT: 20.78 min Scan# 5861Delta R.T. -0.002 minLab File: 08041526.DAcq: 4 Aug 2015 20:24


Ref

Raw

Sub

40 60 80 100 120 140 160 180 2000

50

m/z-->


10251 64 7739 89 207114

40 60 80 100 120 140 160 180 2000

50

m/z-->


6741

151109 166

182 207

40 60 80 100 120 140 160 180 2000

50

m/z-->


81 95

67 151 16655 109

41180 207

20.70 20.75 20.80 20.850

100000

200000

300000

Time-->

Abundance20.780

08041526.D R9071315.M Wed Aug 05 09:48:41 2015 Page 11

61 of 128

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_08\04\08041504.D Acq On : 4 Aug 2015 7:22 Operator: SC Sample : MB R9080415_1000mL Misc : S29-07071501 ALS Vial : 2 Sample Multiplier: 1 Quant Time: Aug 04 09:17:24 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 1) Bromochloromethane (IS1) 8.98 130 150501 12.500 ng -0.04 37) 1,4-Difluorobenzene (IS2) 10.96 114 775372 12.500 ng -0.02 56) Chlorobenzene-d5 (IS3) 15.31 82 318022 12.500 ng 0.00 System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.76 65 248352 10.263 ng -0.03 Spiked Amount 12.500 Recovery = 82.08% 57) Toluene-d8 (SS2) 13.40 98 768256 13.299 ng 0.00 Spiked Amount 12.500 Recovery = 106.40% 73) Bromofluorobenzene (SS3) 16.92 174 250385 13.635 ng 0.00 Spiked Amount 12.500 Recovery = 109.12% Target Compounds Qvalue 2) Propene 3.80 42 1343 N.D. 3) Dichlorodifluoromethan... 0.00 85 0 N.D. 4) Chloromethane 0.00 50 0 N.D. 5) 1,2-Dichloro-1,1,2,2-t... 0.00 135 0 N.D. 6) Vinyl Chloride 0.00 62 0 N.D. 7) 1,3-Butadiene 0.00 54 0 N.D. 8) Bromomethane 0.00 94 0 N.D. 9) Chloroethane 0.00 64 0 N.D. 10) Ethanol 5.25 45 1476 N.D. 11) Acetonitrile 5.47 41 882 N.D. 12) Acrolein 5.57 56 27 N.D. 13) Acetone 5.74 58 11542 0.756 ng # 56 14) Trichlorofluoromethane 0.00 101 0 N.D. 15) 2-Propanol (Isopropanol) 6.07 45 866 N.D. 16) Acrylonitrile 0.00 53 0 N.D. 17) 1,1-Dichloroethene 0.00 96 0 N.D. 18) 2-Methyl-2-Propanol (t... 6.75 59 32 N.D. 19) Methylene Chloride 6.72 84 1948 0.100 ng 81 20) 3-Chloro-1-propene (Al... 0.00 41 0 N.D. 21) Trichlorotrifluoroethane 0.00 151 0 N.D. 22) Carbon Disulfide 7.02 76 1361 N.D. 23) trans-1,2-Dichloroethene 0.00 61 0 N.D. 24) 1,1-Dichloroethane 0.00 63 0 N.D. 25) Methyl tert-Butyl Ether 0.00 73 0 N.D. 26) Vinyl Acetate 8.12 86 913 0.208 ng # 5 27) 2-Butanone (MEK) 8.41 72 1073 N.D. 28) cis-1,2-Dichloroethene 0.00 61 0 N.D. 29) Diisopropyl Ether 0.00 87 0 N.D. 30) Ethyl Acetate 0.00 61 0 N.D. 31) n-Hexane 0.00 57 0 N.D. 32) Chloroform 0.00 83 0 N.D. 34) Tetrahydrofuran (THF) 0.00 72 0 N.D. 35) Ethyl tert-Butyl Ether 0.00 87 0 N.D. 36) 1,2-Dichloroethane 0.00 62 0 N.D. 38) 1,1,1-Trichloroethane 0.00 97 0 N.D. 39) Isopropyl Acetate 0.00 61 0 N.D. 40) 1-Butanol 10.61 56 849 N.D. 41) Benzene 10.60 78 2307 N.D. 42) Carbon Tetrachloride 0.00 117 0 N.D. 43) Cyclohexane 0.00 84 0 N.D. 44) tert-Amyl Methyl Ether 0.00 73 0 N.D. 45) 1,2-Dichloropropane 0.00 63 0 N.D. 46) Bromodichloromethane 0.00 83 0 N.D. 47) Trichloroethene 0.00 130 0 N.D. 48) 1,4-Dioxane 0.00 88 0 N.D. 49) 2,2,4-Trimethylpentane... 0.00 57 0 N.D.

R9071315.M Tue Aug 04 09:17:48 2015 Page: 1

62 of 128

simon.cao

Simon

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_08\04\08041504.D Acq On : 4 Aug 2015 7:22 Operator: SC Sample : MB R9080415_1000mL Misc : S29-07071501 ALS Vial : 2 Sample Multiplier: 1 Quant Time: Aug 04 09:17:24 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 50) Methyl Methacrylate 0.00 100 0 N.D. 51) n-Heptane 0.00 71 0 N.D. 52) cis-1,3-Dichloropropene 0.00 75 0 N.D. 53) 4-Methyl-2-pentanone 0.00 58 0 N.D. 54) trans-1,3-Dichloropropene 0.00 75 0 N.D. 55) 1,1,2-Trichloroethane 0.00 97 0 N.D. 58) Toluene 13.50 91 1178 N.D. 59) 2-Hexanone 0.00 43 0 N.D. 60) Dibromochloromethane 0.00 129 0 N.D. 61) 1,2-Dibromoethane 0.00 107 0 N.D. 62) n-Butyl Acetate 0.00 43 0 N.D. 63) n-Octane 0.00 57 0 N.D. 64) Tetrachloroethene 0.00 166 0 N.D. 65) Chlorobenzene 0.00 112 0 N.D. 66) Ethylbenzene 0.00 91 0 N.D. 67) m- & p-Xylenes 0.00 91 0 N.D. 68) Bromoform 0.00 173 0 N.D. 69) Styrene 0.00 104 0 N.D. 70) o-Xylene 0.00 91 0 N.D. 71) n-Nonane 0.00 43 0 N.D. 72) 1,1,2,2-Tetrachloroethane 0.00 83 0 N.D. 74) Cumene 0.00 105 0 N.D. 75) alpha-Pinene 0.00 93 0 N.D. 76) n-Propylbenzene 0.00 91 0 N.D. 77) 3-Ethyltoluene 17.49 105 547 N.D. 78) 4-Ethyltoluene 0.00 105 0 N.D. 79) 1,3,5-Trimethylbenzene 0.00 105 0 N.D. 80) alpha-Methylstyrene 0.00 118 0 N.D. 81) 2-Ethyltoluene 0.00 105 0 N.D. 82) 1,2,4-Trimethylbenzene 0.00 105 0 N.D. 83) n-Decane 0.00 57 0 N.D. 84) Benzyl Chloride 0.00 91 0 N.D. 85) 1,3-Dichlorobenzene 0.00 146 0 N.D. 86) 1,4-Dichlorobenzene 0.00 146 0 N.D. 87) sec-Butylbenzene 0.00 105 0 N.D. 88) 4-Isopropyltoluene (p-... 0.00 119 0 N.D. 89) 1,2,3-Trimethylbenzene 0.00 105 0 N.D. 90) 1,2-Dichlorobenzene 0.00 146 0 N.D. 91) d-Limonene 0.00 68 0 N.D. 92) 1,2-Dibromo-3-Chloropr... 0.00 157 0 N.D. 93) n-Undecane 0.00 57 0 N.D. 94) 1,2,4-Trichlorobenzene 0.00 180 0 N.D. 95) Naphthalene 20.81 128 1527 N.D. 96) n-Dodecane 0.00 57 0 N.D. 97) Hexachlorobutadiene 0.00 225 0 N.D. 98) Cyclohexanone 0.00 55 0 N.D. 99) tert-Butylbenzene 0.00 119 0 N.D. 100) n-Butylbenzene 0.00 91 0 N.D. -------------------------------------------------------------------------- (#) = qualifier out of range (m) = manual integration (+) = signals summed

R9071315.M Tue Aug 04 09:17:48 2015 Page: 2

63 of 128


Data File: I:\MS09\Data\2015_08\04\08041504.D Acq On : 4 Aug 2015 7:22 Operator: SC Sample : MB R9080415_1000mL Misc : S29-07071501 ALS Vial : 2 Sample Multiplier: 1


4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.000

50000

100000

150000

200000

250000

300000

350000

400000

450000

500000

550000

600000

650000

700000

750000

800000

850000

900000

950000

1000000

1050000

1100000

1150000

Time-->


Brom

oflu

orob

enze

ne (S

S3),S

Chl

orob

enze

ne-d

5 (IS

3),IR

Tolu

ene-

d8 (S

S2),S

1,4-

Difl

uoro

benz

ene

(IS2)

,IR

1,2-

Dic

hlor

oeth

ane-

d4(S

S1),S

Brom

ochl

orom

etha

ne (I

S1),I

R

Viny

l Ace

tate

,T

Met

hyle

ne C

hlor

ide,

T

Acet

one,

T

R9071315.M Tue Aug 04 09:17:49 2015 Page: 3

64 of 128

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_08\05\08051504.D Acq On : 5 Aug 2015 5:22 Operator: SC Sample : MB R9080515_1000mL Misc : S29-07071501 ALS Vial : 2 Sample Multiplier: 1 Quant Time: Aug 05 09:16:58 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 1) Bromochloromethane (IS1) 8.98 130 159572 12.500 ng -0.04 37) 1,4-Difluorobenzene (IS2) 10.96 114 821162 12.500 ng -0.02 56) Chlorobenzene-d5 (IS3) 15.31 82 340840 12.500 ng 0.00 System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.76 65 258249 10.065 ng -0.03 Spiked Amount 12.500 Recovery = 80.56% 57) Toluene-d8 (SS2) 13.40 98 815353 13.170 ng 0.00 Spiked Amount 12.500 Recovery = 105.36% 73) Bromofluorobenzene (SS3) 16.92 174 274955 13.971 ng 0.00 Spiked Amount 12.500 Recovery = 111.76% Target Compounds Qvalue 2) Propene 3.80 42 1496 N.D. 3) Dichlorodifluoromethan... 0.00 85 0 N.D. 4) Chloromethane 0.00 50 0 N.D. 5) 1,2-Dichloro-1,1,2,2-t... 0.00 135 0 N.D. 6) Vinyl Chloride 0.00 62 0 N.D. 7) 1,3-Butadiene 0.00 54 0 N.D. 8) Bromomethane 0.00 94 0 N.D. 9) Chloroethane 0.00 64 0 N.D. 10) Ethanol 5.25 45 1593 N.D. 11) Acetonitrile 5.48 41 894 N.D. 12) Acrolein 5.60 56 1003 N.D. 13) Acetone 5.73 58 13810 0.853 ng # 51 14) Trichlorofluoromethane 0.00 101 0 N.D. 15) 2-Propanol (Isopropanol) 6.07 45 893 N.D. 16) Acrylonitrile 0.00 53 0 N.D. 17) 1,1-Dichloroethene 0.00 96 0 N.D. 18) 2-Methyl-2-Propanol (t... 6.74 59 61 N.D. 19) Methylene Chloride 6.72 84 1891 0.091 ng 87 20) 3-Chloro-1-propene (Al... 0.00 41 0 N.D. 21) Trichlorotrifluoroethane 0.00 151 0 N.D. 22) Carbon Disulfide 7.02 76 713 N.D. 23) trans-1,2-Dichloroethene 0.00 61 0 N.D. 24) 1,1-Dichloroethane 0.00 63 0 N.D. 25) Methyl tert-Butyl Ether 0.00 73 0 N.D. 26) Vinyl Acetate 0.00 86 0 N.D. d 27) 2-Butanone (MEK) 8.41 72 1232 0.091 ng # 83 28) cis-1,2-Dichloroethene 0.00 61 0 N.D. 29) Diisopropyl Ether 0.00 87 0 N.D. 30) Ethyl Acetate 0.00 61 0 N.D. 31) n-Hexane 0.00 57 0 N.D. 32) Chloroform 0.00 83 0 N.D. 34) Tetrahydrofuran (THF) 0.00 72 0 N.D. 35) Ethyl tert-Butyl Ether 0.00 87 0 N.D. 36) 1,2-Dichloroethane 0.00 62 0 N.D. 38) 1,1,1-Trichloroethane 0.00 97 0 N.D. 39) Isopropyl Acetate 0.00 61 0 N.D. 40) 1-Butanol 10.62 56 977 N.D. 41) Benzene 10.60 78 1979 N.D. 42) Carbon Tetrachloride 0.00 117 0 N.D. 43) Cyclohexane 0.00 84 0 N.D. 44) tert-Amyl Methyl Ether 0.00 73 0 N.D. 45) 1,2-Dichloropropane 0.00 63 0 N.D. 46) Bromodichloromethane 0.00 83 0 N.D. 47) Trichloroethene 0.00 130 0 N.D. 48) 1,4-Dioxane 0.00 88 0 N.D. 49) 2,2,4-Trimethylpentane... 0.00 57 0 N.D.

R9071315.M Wed Aug 05 09:17:13 2015 Page: 1

65 of 128

simon.cao

Simon

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_08\05\08051504.D Acq On : 5 Aug 2015 5:22 Operator: SC Sample : MB R9080515_1000mL Misc : S29-07071501 ALS Vial : 2 Sample Multiplier: 1 Quant Time: Aug 05 09:16:58 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 50) Methyl Methacrylate 0.00 100 0 N.D. 51) n-Heptane 0.00 71 0 N.D. 52) cis-1,3-Dichloropropene 0.00 75 0 N.D. 53) 4-Methyl-2-pentanone 0.00 58 0 N.D. 54) trans-1,3-Dichloropropene 0.00 75 0 N.D. 55) 1,1,2-Trichloroethane 0.00 97 0 N.D. 58) Toluene 13.51 91 1315 N.D. 59) 2-Hexanone 0.00 43 0 N.D. 60) Dibromochloromethane 0.00 129 0 N.D. 61) 1,2-Dibromoethane 0.00 107 0 N.D. 62) n-Butyl Acetate 0.00 43 0 N.D. 63) n-Octane 0.00 57 0 N.D. 64) Tetrachloroethene 0.00 166 0 N.D. 65) Chlorobenzene 0.00 112 0 N.D. 66) Ethylbenzene 0.00 91 0 N.D. 67) m- & p-Xylenes 0.00 91 0 N.D. 68) Bromoform 0.00 173 0 N.D. 69) Styrene 0.00 104 0 N.D. 70) o-Xylene 0.00 91 0 N.D. 71) n-Nonane 0.00 43 0 N.D. 72) 1,1,2,2-Tetrachloroethane 0.00 83 0 N.D. 74) Cumene 0.00 105 0 N.D. 75) alpha-Pinene 0.00 93 0 N.D. 76) n-Propylbenzene 0.00 91 0 N.D. 77) 3-Ethyltoluene 0.00 105 0 N.D. 78) 4-Ethyltoluene 0.00 105 0 N.D. 79) 1,3,5-Trimethylbenzene 0.00 105 0 N.D. 80) alpha-Methylstyrene 0.00 118 0 N.D. 81) 2-Ethyltoluene 0.00 105 0 N.D. 82) 1,2,4-Trimethylbenzene 0.00 105 0 N.D. 83) n-Decane 18.62 57 744 N.D. 84) Benzyl Chloride 0.00 91 0 N.D. 85) 1,3-Dichlorobenzene 0.00 146 0 N.D. 86) 1,4-Dichlorobenzene 0.00 146 0 N.D. 87) sec-Butylbenzene 0.00 105 0 N.D. 88) 4-Isopropyltoluene (p-... 0.00 119 0 N.D. 89) 1,2,3-Trimethylbenzene 0.00 105 0 N.D. 90) 1,2-Dichlorobenzene 0.00 146 0 N.D. 91) d-Limonene 0.00 68 0 N.D. 92) 1,2-Dibromo-3-Chloropr... 0.00 157 0 N.D. 93) n-Undecane 0.00 57 0 N.D. 94) 1,2,4-Trichlorobenzene 0.00 180 0 N.D. 95) Naphthalene 20.81 128 2070 N.D. 96) n-Dodecane 0.00 57 0 N.D. 97) Hexachlorobutadiene 0.00 225 0 N.D. 98) Cyclohexanone 0.00 55 0 N.D. 99) tert-Butylbenzene 0.00 119 0 N.D. 100) n-Butylbenzene 0.00 91 0 N.D. -------------------------------------------------------------------------- (#) = qualifier out of range (m) = manual integration (+) = signals summed

R9071315.M Wed Aug 05 09:17:13 2015 Page: 2

66 of 128


Data File: I:\MS09\Data\2015_08\05\08051504.D Acq On : 5 Aug 2015 5:22 Operator: SC Sample : MB R9080515_1000mL Misc : S29-07071501 ALS Vial : 2 Sample Multiplier: 1


4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.000

50000

100000

150000

200000

250000

300000

350000

400000

450000

500000

550000

600000

650000

700000

750000

800000

850000

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950000

1000000

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1100000

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1200000

1250000

Time-->


Brom

oflu

orob

enze

ne (S

S3),S

Chl

orob

enze

ne-d

5 (IS

3),IR

Tolu

ene-

d8 (S

S2),S

1,4-

Difl

uoro

benz

ene

(IS2)

,IR

1,2-

Dic

hlor

oeth

ane-

d4(S

S1),S

Brom

ochl

orom

etha

ne (I

S1),I

R

2-Bu

tano

ne (M

EK),T

Met

hyle

ne C

hlor

ide,

T

Acet

one,

T

R9071315.M Wed Aug 05 09:17:14 2015 Page: 3

67 of 128

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_08\04\08041505.D Acq On : 4 Aug 2015 7:55 Operator: SC Sample : LCS R9080415_25ng Misc : S29-07071501/S29-07141502 (8/12) ALS Vial : 16 Sample Multiplier: 1 Quant Time: Aug 04 09:19:04 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 1) Bromochloromethane (IS1) 9.00 130 150972 12.500 ng -0.01 37) 1,4-Difluorobenzene (IS2) 10.97 114 772259 12.500 ng 0.00 56) Chlorobenzene-d5 (IS3) 15.32 82 324392 12.500 ng 0.00 System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.78 65 253787 10.455 ng -0.01 Spiked Amount 12.500 Recovery = 83.60% 57) Toluene-d8 (SS2) 13.41 98 771109 13.087 ng 0.00 Spiked Amount 12.500 Recovery = 104.72% 73) Bromofluorobenzene (SS3) 16.92 174 258216 13.786 ng 0.00 Spiked Amount 12.500 Recovery = 110.32% Target Compounds Qvalue 2) Propene 3.75 42 424048 16.911 ng 97 3) Dichlorodifluoromethan... 3.85 85 762092 18.989 ng 100 4) Chloromethane 4.06 50 612379 18.269 ng 99 5) 1,2-Dichloro-1,1,2,2-t... 4.22 135 389210 22.964 ng 100 6) Vinyl Chloride 4.33 62 561650 20.058 ng 99 7) 1,3-Butadiene 4.51 54 443043 20.540 ng 93 8) Bromomethane 4.81 94 386572 23.854 ng 99 9) Chloroethane 5.02 64 309016 21.405 ng 99 10) Ethanol 5.25 45 1528810 91.151 ng 98 11) Acetonitrile 5.44 41 775743 17.738 ng 99 12) Acrolein 5.56 56 254929 19.674 ng 99 13) Acetone 5.70 58 1556796 101.618 ng # 82 14) Trichlorofluoromethane 5.89 101 646594 20.035 ng 99 15) 2-Propanol (Isopropanol) 6.03 45 2193747 40.429 ng 100 16) Acrylonitrile 6.23 53 569550 21.571 ng 99 17) 1,1-Dichloroethene 6.57 96 389474 23.628 ng 87 18) 2-Methyl-2-Propanol (t... 6.67 59 2101650 43.008 ng 97 19) Methylene Chloride 6.72 84 412971 21.089 ng 85 20) 3-Chloro-1-propene (Al... 6.85 41 643154 20.798 ng 90 21) Trichlorotrifluoroethane 7.03 151 328995 25.216 ng 92 22) Carbon Disulfide 7.00 76 1434093 19.320 ng 100 23) trans-1,2-Dichloroethene 7.74 61 602158 21.876 ng 92 24) 1,1-Dichloroethane 7.96 63 762802 21.403 ng 99 25) Methyl tert-Butyl Ether 8.02 73 1233658 22.738 ng 97 26) Vinyl Acetate 8.14 86 493702 111.903 ng # 56 27) 2-Butanone (MEK) 8.37 72 285002 22.224 ng # 76 28) cis-1,2-Dichloroethene 8.84 61 587727 22.110 ng 91 29) Diisopropyl Ether 9.07 87 334147 20.851 ng # 62 30) Ethyl Acetate 9.07 61 325416 42.811 ng 94 31) n-Hexane 9.08 57 712893 21.206 ng 99 32) Chloroform 9.14 83 711814 22.900 ng 99 34) Tetrahydrofuran (THF) 9.52 72 280809 21.540 ng # 87 35) Ethyl tert-Butyl Ether 9.62 87 491886 24.189 ng # 88 36) 1,2-Dichloroethane 9.89 62 514297 20.867 ng 100 38) 1,1,1-Trichloroethane 10.15 97 601049 22.783 ng 98 39) Isopropyl Acetate 10.52 61 556329 47.475 ng # 80 40) 1-Butanol 10.54 56 919508 42.293 ng 92 41) Benzene 10.61 78 1626252 22.901 ng 99 42) Carbon Tetrachloride 10.76 117 531200 24.000 ng 99 43) Cyclohexane 10.89 84 1253751 47.660 ng 92 44) tert-Amyl Methyl Ether 11.21 73 1200682 23.387 ng 95 45) 1,2-Dichloropropane 11.43 63 449656 22.748 ng 100 46) Bromodichloromethane 11.61 83 570489 23.885 ng 100 47) Trichloroethene 11.67 130 428365 24.654 ng 100 48) 1,4-Dioxane 11.63 88 347987 23.952 ng 93 49) 2,2,4-Trimethylpentane... 11.73 57 1845152 21.899 ng 95

R9071315.M Tue Aug 04 09:19:59 2015 Page: 1

68 of 128

simon.cao

Simon

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_08\04\08041505.D Acq On : 4 Aug 2015 7:55 Operator: SC Sample : LCS R9080415_25ng Misc : S29-07071501/S29-07141502 (8/12) ALS Vial : 16 Sample Multiplier: 1 Quant Time: Aug 04 09:19:04 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 50) Methyl Methacrylate 11.86 100 328291 49.360 ng # 88 51) n-Heptane 11.99 71 428967 23.746 ng 95 52) cis-1,3-Dichloropropene 12.52 75 675401 24.149 ng 100 53) 4-Methyl-2-pentanone 12.55 58 419613 22.325 ng 89 54) trans-1,3-Dichloropropene 13.03 75 616192 22.713 ng 99 55) 1,1,2-Trichloroethane 13.21 97 407392 24.532 ng 98 58) Toluene 13.51 91 1695866 25.796 ng 99 59) 2-Hexanone 13.75 43 1008304 23.132 ng 94 60) Dibromochloromethane 13.92 129 472266 29.244 ng 100 61) 1,2-Dibromoethane 14.17 107 474497 28.011 ng 99 62) n-Butyl Acetate 14.39 43 1145840 23.990 ng 95 63) n-Octane 14.53 57 375750 23.958 ng 93 64) Tetrachloroethene 14.66 166 426627 26.057 ng 100 65) Chlorobenzene 15.36 112 1108987 27.344 ng 100 66) Ethylbenzene 15.76 91 1922785 26.391 ng 98 67) m- & p-Xylenes 15.96 91 3026151 51.249 ng 96 68) Bromoform 16.02 173 391048 27.342 ng 100 69) Styrene 16.33 104 1165731 28.409 ng 97 70) o-Xylene 16.45 91 1509198 24.933 ng 97 71) n-Nonane 16.69 43 887059 21.876 ng 94 72) 1,1,2,2-Tetrachloroethane 16.42 83 765787 24.897 ng 99 74) Cumene 17.07 105 1873653 25.272 ng 98 75) alpha-Pinene 17.48 93 980808 26.640 ng 97 76) n-Propylbenzene 17.60 91 2328366 24.518 ng 98 77) 3-Ethyltoluene 17.71 105 1866622 26.236 ng 98 78) 4-Ethyltoluene 17.76 105 1838998 26.721 ng 99 79) 1,3,5-Trimethylbenzene 17.84 105 1549466 26.109 ng 98 80) alpha-Methylstyrene 17.99 118 808667 27.125 ng 98 81) 2-Ethyltoluene 18.03 105 1810554 25.736 ng 99 82) 1,2,4-Trimethylbenzene 18.27 105 1620745 26.664 ng 99 83) n-Decane 18.39 57 932969 23.550 ng 97 84) Benzyl Chloride 18.40 91 1492055 27.171 ng 98 85) 1,3-Dichlorobenzene 18.42 146 897197 28.187 ng 100 86) 1,4-Dichlorobenzene 18.49 146 886559 26.817 ng 100 87) sec-Butylbenzene 18.55 105 2108373 26.203 ng 99 88) 4-Isopropyltoluene (p-... 18.72 119 1938204 24.426 ng 97 89) 1,2,3-Trimethylbenzene 18.71 105 1674601 25.927 ng 98 90) 1,2-Dichlorobenzene 18.85 146 859950 27.161 ng 100 91) d-Limonene 18.87 68 647233 25.599 ng 96 92) 1,2-Dibromo-3-Chloropr... 19.31 157 323122 25.893 ng 87 93) n-Undecane 19.72 57 965133 23.303 ng 97 94) 1,2,4-Trichlorobenzene 20.66 180 588563 24.278 ng 99 95) Naphthalene 20.78 128 1941525 21.738 ng 100 96) n-Dodecane 20.81 57 913263 21.713 ng 98 97) Hexachlorobutadiene 21.15 225 343376 23.637 ng 100 98) Cyclohexanone 16.10 55 619259 23.150 ng 94 99) tert-Butylbenzene 18.27 119 1539027 26.789 ng 99 100) n-Butylbenzene 19.16 91 1760902 25.922 ng 98 -------------------------------------------------------------------------- (#) = qualifier out of range (m) = manual integration (+) = signals summed

R9071315.M Tue Aug 04 09:19:59 2015 Page: 2

69 of 128


Data File: I:\MS09\Data\2015_08\04\08041505.D Acq On : 4 Aug 2015 7:55 Operator: SC Sample : LCS R9080415_25ng Misc : S29-07071501/S29-07141502 (8/12) ALS Vial : 16 Sample Multiplier: 1


4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.000

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R9071315.M Tue Aug 04 09:20:01 2015 Page: 3

70 of 128

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_08\05\08051505.D Acq On : 5 Aug 2015 5:56 Operator: SC Sample : LCS R9080515_25ng Misc : S29-07071501/S29-07141502 (8/12) ALS Vial : 16 Sample Multiplier: 1 Quant Time: Aug 05 09:18:25 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 1) Bromochloromethane (IS1) 8.99 130 159933 12.500 ng -0.02 37) 1,4-Difluorobenzene (IS2) 10.97 114 814393 12.500 ng 0.00 56) Chlorobenzene-d5 (IS3) 15.31 82 345321 12.500 ng 0.00 System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.78 65 260472 10.129 ng -0.01 Spiked Amount 12.500 Recovery = 81.04% 57) Toluene-d8 (SS2) 13.40 98 815491 13.001 ng 0.00 Spiked Amount 12.500 Recovery = 104.00% 73) Bromofluorobenzene (SS3) 16.92 174 280623 14.074 ng 0.00 Spiked Amount 12.500 Recovery = 112.56% Target Compounds Qvalue 2) Propene 3.74 42 427474 16.092 ng 97 3) Dichlorodifluoromethan... 3.85 85 773188 18.186 ng 100 4) Chloromethane 4.05 50 598050 16.841 ng 99 5) 1,2-Dichloro-1,1,2,2-t... 4.21 135 405269 22.572 ng 100 6) Vinyl Chloride 4.32 62 576235 19.426 ng 99 7) 1,3-Butadiene 4.50 54 442025 19.345 ng 94 8) Bromomethane 4.80 94 402649 23.454 ng 99 9) Chloroethane 5.01 64 315719 20.644 ng 100 10) Ethanol 5.24 45 1546820 87.058 ng 98 11) Acetonitrile 5.43 41 788014 17.009 ng 98 12) Acrolein 5.55 56 262251 19.105 ng 100 13) Acetone 5.70 58 1593555 98.189 ng # 80 14) Trichlorofluoromethane 5.88 101 664750 19.443 ng 99 15) 2-Propanol (Isopropanol) 6.02 45 2205839 38.374 ng 99 16) Acrylonitrile 6.23 53 582241 20.816 ng 99 17) 1,1-Dichloroethene 6.57 96 405007 23.194 ng # 84 18) 2-Methyl-2-Propanol (t... 6.66 59 2112778 40.813 ng 97 19) Methylene Chloride 6.72 84 430786 20.766 ng 83 20) 3-Chloro-1-propene (Al... 6.84 41 647271 19.759 ng 89 21) Trichlorotrifluoroethane 7.03 151 346712 25.085 ng 90 22) Carbon Disulfide 6.99 76 1476046 18.771 ng 100 23) trans-1,2-Dichloroethene 7.74 61 616859 21.155 ng 91 24) 1,1-Dichloroethane 7.96 63 776866 20.577 ng 99 25) Methyl tert-Butyl Ether 8.02 73 1267419 22.052 ng 97 26) Vinyl Acetate 8.14 86 511029 109.341 ng # 49 27) 2-Butanone (MEK) 8.36 72 293848 21.630 ng # 73 28) cis-1,2-Dichloroethene 8.83 61 600438 21.323 ng 90 29) Diisopropyl Ether 9.07 87 345827 20.371 ng # 57 30) Ethyl Acetate 9.07 61 332574 41.301 ng 94 31) n-Hexane 9.07 57 727140 20.418 ng 99 32) Chloroform 9.14 83 727687 22.099 ng 99 34) Tetrahydrofuran (THF) 9.52 72 289666 20.974 ng # 85 35) Ethyl tert-Butyl Ether 9.62 87 504277 23.409 ng # 87 36) 1,2-Dichloroethane 9.89 62 518924 19.875 ng 100 38) 1,1,1-Trichloroethane 10.15 97 616614 22.164 ng 97 39) Isopropyl Acetate 10.52 61 571016 46.208 ng # 77 40) 1-Butanol 10.53 56 935580 40.806 ng 90 41) Benzene 10.61 78 1682645 22.469 ng 99 42) Carbon Tetrachloride 10.76 117 542899 23.259 ng 99 43) Cyclohexane 10.89 84 1295260 46.690 ng 91 44) tert-Amyl Methyl Ether 11.21 73 1231313 22.743 ng 95 45) 1,2-Dichloropropane 11.43 63 461675 22.148 ng 100 46) Bromodichloromethane 11.61 83 586028 23.266 ng 100 47) Trichloroethene 11.66 130 446254 24.354 ng 100 48) 1,4-Dioxane 11.63 88 360687 23.541 ng 92 49) 2,2,4-Trimethylpentane... 11.73 57 1882959 21.192 ng 94

R9071315.M Wed Aug 05 09:19:58 2015 Page: 1

71 of 128

simon.cao

Simon

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_08\05\08051505.D Acq On : 5 Aug 2015 5:56 Operator: SC Sample : LCS R9080515_25ng Misc : S29-07071501/S29-07141502 (8/12) ALS Vial : 16 Sample Multiplier: 1 Quant Time: Aug 05 09:18:25 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 50) Methyl Methacrylate 11.85 100 340799 48.589 ng # 86 51) n-Heptane 11.98 71 440457 23.120 ng 95 52) cis-1,3-Dichloropropene 12.51 75 693242 23.504 ng 99 53) 4-Methyl-2-pentanone 12.55 58 427231 21.554 ng 88 54) trans-1,3-Dichloropropene 13.03 75 630255 22.030 ng 99 55) 1,1,2-Trichloroethane 13.21 97 422117 24.103 ng 97 58) Toluene 13.51 91 1750415 25.012 ng 99 59) 2-Hexanone 13.75 43 1019729 21.976 ng 93 60) Dibromochloromethane 13.91 129 489266 28.460 ng 100 61) 1,2-Dibromoethane 14.17 107 489974 27.171 ng 99 62) n-Butyl Acetate 14.39 43 1153209 22.681 ng 94 63) n-Octane 14.53 57 384741 23.045 ng 92 64) Tetrachloroethene 14.66 166 446889 25.640 ng 100 65) Chlorobenzene 15.36 112 1149853 26.633 ng 100 66) Ethylbenzene 15.76 91 1973032 25.439 ng 97 67) m- & p-Xylenes 15.96 91 3113002 49.524 ng 96 68) Bromoform 16.02 173 405225 26.616 ng 99 69) Styrene 16.33 104 1207914 27.652 ng 97 70) o-Xylene 16.45 91 1552976 24.101 ng 96 71) n-Nonane 16.69 43 896029 20.758 ng 93 72) 1,1,2,2-Tetrachloroethane 16.42 83 787524 24.052 ng 99 74) Cumene 17.07 105 1929245 24.445 ng 98 75) alpha-Pinene 17.48 93 1008394 25.729 ng 97 76) n-Propylbenzene 17.60 91 2389552 23.637 ng 97 77) 3-Ethyltoluene 17.71 105 1937947 25.587 ng 98 78) 4-Ethyltoluene 17.75 105 1885458 25.735 ng 98 79) 1,3,5-Trimethylbenzene 17.83 105 1592482 25.207 ng 97 80) alpha-Methylstyrene 17.99 118 834916 26.308 ng 99 81) 2-Ethyltoluene 18.03 105 1863006 24.877 ng 99 82) 1,2,4-Trimethylbenzene 18.26 105 1662890 25.699 ng 98 83) n-Decane 18.38 57 947385 22.465 ng 97 84) Benzyl Chloride 18.40 91 1528561 26.149 ng 97 85) 1,3-Dichlorobenzene 18.42 146 928191 27.393 ng 100 86) 1,4-Dichlorobenzene 18.49 146 916799 26.051 ng 100 87) sec-Butylbenzene 18.55 105 2164478 25.270 ng 98 88) 4-Isopropyltoluene (p-... 18.72 119 1993059 23.595 ng 97 89) 1,2,3-Trimethylbenzene 18.71 105 1710082 24.872 ng 97 90) 1,2-Dichlorobenzene 18.85 146 889206 26.383 ng 99 91) d-Limonene 18.87 68 656660 24.398 ng 96 92) 1,2-Dibromo-3-Chloropr... 19.31 157 331562 24.959 ng 86 93) n-Undecane 19.72 57 978139 22.186 ng 97 94) 1,2,4-Trichlorobenzene 20.66 180 608557 23.581 ng 100 95) Naphthalene 20.78 128 1993818 20.971 ng 100 96) n-Dodecane 20.81 57 925386 20.668 ng 97 97) Hexachlorobutadiene 21.15 225 356645 23.062 ng 100 98) Cyclohexanone 16.10 55 628821 22.082 ng 94 99) tert-Butylbenzene 18.26 119 1579779 25.832 ng 99 100) n-Butylbenzene 19.16 91 1797862 24.862 ng 98 -------------------------------------------------------------------------- (#) = qualifier out of range (m) = manual integration (+) = signals summed

R9071315.M Wed Aug 05 09:19:58 2015 Page: 2

72 of 128


Data File: I:\MS09\Data\2015_08\05\08051505.D Acq On : 5 Aug 2015 5:56 Operator: SC Sample : LCS R9080515_25ng Misc : S29-07071501/S29-07141502 (8/12) ALS Vial : 16 Sample Multiplier: 1


4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.000

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Time-->


Hex

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R9071315.M Wed Aug 05 09:19:59 2015 Page: 3

73 of 128

Response Factor Report MS09

Method Path : I:\MS09\Methods\ Method File : R9071315.M Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) Last Update : Tue Jul 14 10:53:11 2015 Response Via : Initial Calibration

Calibration Files 0.08=07131513.D 0.10=07131514.D 0.20=07131515.D 0.40=07131516.D 1.0 =07131517.D 5.0 =07131518.D 25 =07131519.D 50 =07131520.D 100 =07131521.D

Compound 0.08 0.10 0.20 0.40 1.0 5.0 25 50 100 Avg %RSD --------------------------------------------------------------------------------------------

1) IR Bromochloromethane... ----------------ISTD--------------------- 2) T Propene 1.851 2.356 2.226 2.204 2.231 2.022 2.204 1.860 1.731 2.076 10.45 3) T Dichlorodifluo... 2.223 3.293 3.725 3.584 3.781 3.460 3.723 3.203 2.915 3.323 15.09 4) T Chloromethane 1.815 2.819 3.181 3.071 3.199 2.804 3.212 2.672 2.206 2.775 17.47 5) T 1,2-Dichloro-1... 0.857 1.475 1.520 1.397 1.491 1.388 1.574 1.504 1.424 1.403 15.21 6) T Vinyl Chloride 1.499 2.161 2.517 2.427 2.574 2.384 2.643 2.405 2.255 2.318 14.74 7) T 1,3-Butadiene 1.066 1.687 1.876 1.844 1.958 1.822 2.115 1.942 1.762 1.786 16.62 8) T Bromomethane 0.966 1.412 1.510 1.316 1.505 1.257 1.406 1.377 1.327 1.342 12.19 9) T Chloroethane 0.775 1.260 1.337 1.273 1.381 1.051 1.355 1.267 1.058 1.195 16.49 10) T Ethanol 0.949 1.386 1.610 1.495 1.570 1.406 1.541 1.355 1.187 1.389 15.10 11) T Acetonitrile 2.572 3.789 4.118 3.936 4.063 3.673 3.894 3.435 3.109 3.621 13.96 12) T Acrolein 0.770 1.085 1.200 1.085 1.143 1.084 1.192 1.091 1.006 1.073 11.97 13) T Acetone 1.005 1.423 1.441 1.308 1.393 1.253 1.328 1.205 1.061 1.268 12.19 14) T Trichlorofluor... 1.711 2.703 2.982 2.816 2.979 2.699 2.900 2.705 2.554 2.672 14.52 15) T 2-Propanol (Is... 2.816 4.342 4.924 4.989 5.103 4.731 5.155 4.515 3.860 4.493 16.76 16) T Acrylonitrile 1.272 1.892 2.375 2.261 2.520 2.347 2.539 2.318 2.149 2.186 18.03 17) T 1,1-Dichloroet... 0.896 1.313 1.462 1.455 1.498 1.352 1.492 1.437 1.378 1.365 13.70 18) T 2-Methyl-2-Pro... 2.468 3.891 4.506 4.377 4.530 4.239 4.678 4.245 3.480 4.046 17.18 19) T Methylene Chlo... 1.892 1.818 1.479 1.585 1.514 1.439 1.621 11.64 20) T 3-Chloro-1-pro... 1.626 2.579 2.738 2.704 2.854 2.675 2.912 2.586 2.369 2.560 15.04 21) T Trichlorotrifl... 0.650 1.068 1.138 1.157 1.192 1.047 1.166 1.163 1.142 1.080 15.56 22) T Carbon Disulfide 4.252 6.118 6.569 6.164 6.796 6.312 6.716 6.365 6.020 6.146 12.35 23) T trans-1,2-Dich... 1.283 2.136 2.314 2.422 2.619 2.391 2.627 2.437 2.283 2.279 17.74 24) T 1,1-Dichloroet... 1.902 2.902 3.201 3.172 3.297 3.011 3.255 3.005 2.813 2.951 14.44 25) T Methyl tert-Bu... 2.725 4.444 4.898 4.740 4.921 4.607 4.964 4.683 4.448 4.492 15.36 26) T Vinyl Acetate 0.322 0.360 0.367 0.402 0.382 0.359 0.365 7.28 27) T 2-Butanone (MEK) 1.074 1.043 1.047 1.098 1.028 1.134 1.066 1.005 1.062 3.83 28) T cis-1,2-Dichlo... 1.449 2.130 2.342 2.289 2.472 2.247 2.484 2.270 2.126 2.201 14.04 29) T Diisopropyl Ether 1.276 1.518 1.468 1.575 1.151 1.270 1.215 1.141 1.327 12.78 30) T Ethyl Acetate 0.585 0.638 0.640 0.662 0.620 0.697 0.641 0.553 0.629 7.08 31) T n-Hexane 1.853 2.950 3.126 2.957 3.166 2.760 3.048 2.800 2.391 2.783 15.09 32) T Chloroform 1.729 2.494 2.807 2.800 2.803 2.584 2.839 2.630 2.478 2.574 13.47 33) S 1,2-Dichloroet... 1.964 2.013 2.073 2.091 2.095 2.125 2.045 1.893 1.790 2.010 5.46 34) T Tetrahydrofura... 1.095 1.114 1.113 1.154 1.014 1.110 1.043 0.992 1.079 5.23 35) T Ethyl tert-But... 1.005 1.490 1.856 1.759 1.868 1.704 1.894 1.820 1.757 1.684 16.76 36) T 1,2-Dichloroet... 1.319 2.013 2.229 2.147 2.304 2.115 2.294 2.055 1.889 2.041 14.80

37) IR 1,4-Difluorobenzen... ----------------ISTD---------------------38) T 1,1,1-Trichlor... 0.262 0.425 0.449 0.445 0.477 0.430 0.478 0.447 0.430 0.427 15.14 39) T Isopropyl Acetate 0.105 0.180 0.202 0.201 0.213 0.195 0.218 0.204 0.188 0.190 17.75 40) T 1-Butanol 0.326 0.365 0.370 0.351 0.350 0.339 0.383 0.354 0.329 0.352 5.34 41) T Benzene 0.851 1.359 1.233 1.205 1.217 1.083 1.194 1.126 1.077 1.149 12.30 42) T Carbon Tetrach... 0.214 0.326 0.383 0.366 0.395 0.363 0.411 0.388 0.378 0.358 16.55

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Method Path : I:\MS09\Methods\ Method File : R9071315.M Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS)43) T Cyclohexane 0.267 0.397 0.460 0.454 0.465 0.420 0.476 0.455 0.437 0.426 15.08 44) T tert-Amyl Meth... 0.529 0.811 0.865 0.857 0.895 0.851 0.938 0.883 0.849 0.831 14.26 45) T 1,2-Dichloropr... 0.215 0.308 0.349 0.337 0.359 0.315 0.356 0.329 0.312 0.320 13.63 46) T Bromodichlorom... 0.232 0.341 0.405 0.398 0.431 0.396 0.452 0.421 0.403 0.387 16.92 47) T Trichloroethene 0.176 0.262 0.316 0.290 0.305 0.267 0.310 0.303 0.302 0.281 15.48 48) T 1,4-Dioxane 0.183 0.258 0.250 0.235 0.240 0.221 0.251 0.241 0.237 0.235 9.48 49) T 2,2,4-Trimethy... 0.889 1.338 1.454 1.459 1.511 1.376 1.533 1.402 1.312 1.364 14.15 50) T Methyl Methacr... 0.080 0.108 0.101 0.104 0.113 0.106 0.122 0.118 0.116 0.108 11.53 51) T n-Heptane 0.191 0.267 0.313 0.303 0.329 0.291 0.331 0.310 0.297 0.292 14.59 52) T cis-1,3-Dichlo... 0.254 0.398 0.441 0.452 0.494 0.477 0.551 0.513 0.493 0.453 19.13 53) T 4-Methyl-2-pen... 0.229 0.301 0.321 0.317 0.329 0.298 0.339 0.311 0.293 0.304 10.52 54) T trans-1,3-Dich... 0.368 0.401 0.437 0.440 0.507 0.470 0.451 0.439 10.26 55) T 1,1,2-Trichlor... 0.154 0.250 0.280 0.277 0.301 0.273 0.310 0.292 0.283 0.269 17.31

56) IR Chlorobenzene-d5 (... ----------------ISTD---------------------57) S Toluene-d8 (SS2) 2.343 2.314 2.279 2.253 2.256 2.239 2.196 2.256 2.298 2.271 1.93 58) T Toluene 1.810 2.609 2.750 2.557 2.701 2.408 2.695 2.639 2.630 2.533 11.39 59) T 2-Hexanone 1.296 1.691 1.805 1.709 1.821 1.724 1.827 1.676 1.568 1.680 9.87 60) T Dibromochlorom... 0.318 0.565 0.628 0.603 0.672 0.634 0.726 0.720 0.734 0.622 20.61 61) T 1,2-Dibromoethane 0.367 0.595 0.668 0.677 0.705 0.658 0.739 0.730 0.735 0.653 17.86 62) T n-Butyl Acetate 1.359 1.771 2.002 1.892 1.966 1.887 2.050 1.882 1.756 1.841 11.14 63) T n-Octane 0.375 0.582 0.623 0.641 0.685 0.601 0.672 0.640 0.621 0.604 15.19 64) T Tetrachloroethene 0.360 0.650 0.660 0.637 0.676 0.594 0.681 0.692 0.729 0.631 17.17 65) T Chlorobenzene 1.062 1.554 1.649 1.574 1.657 1.497 1.692 1.680 1.699 1.563 12.80 66) T Ethylbenzene 1.722 2.731 2.933 2.843 3.052 2.783 3.145 3.040 3.019 2.807 15.29 67) T m- & p-Xylenes 1.492 2.159 2.313 2.277 2.469 2.245 2.565 2.485 2.473 2.275 14.19 68) T Bromoform 0.478 0.459 0.525 0.509 0.618 0.623 0.645 0.551 13.84 69) T Styrene 0.935 1.386 1.529 1.525 1.692 1.610 1.887 1.831 1.837 1.581 18.66 70) T o-Xylene 1.491 2.233 2.345 2.340 2.543 2.342 2.643 2.533 2.524 2.332 14.66 71) T n-Nonane 0.975 1.500 1.716 1.613 1.788 1.640 1.793 1.593 1.445 1.563 16.00 72) T 1,1,2,2-Tetrac... 0.687 1.080 1.174 1.205 1.304 1.232 1.374 1.311 1.300 1.185 17.42 73) S Bromofluoroben... 0.696 0.695 0.691 0.701 0.706 0.727 0.753 0.756 0.771 0.722 4.29 74) T Cumene 1.890 2.637 2.950 2.856 3.087 2.842 3.243 3.114 3.094 2.857 14.20 75) T alpha-Pinene 0.807 1.291 1.465 1.433 1.472 1.426 1.662 1.604 1.609 1.419 18.06 76) T n-Propylbenzene 2.201 3.406 3.812 3.666 4.060 3.756 4.219 3.972 3.843 3.659 16.25 77) T 3-Ethyltoluene 1.685 2.482 2.744 2.697 2.958 2.806 3.120 3.090 3.093 2.742 16.44 78) T 4-Ethyltoluene 1.608 2.498 2.702 2.655 2.854 2.673 3.135 2.898 2.846 2.652 16.27 79) T 1,3,5-Trimethy... 1.425 2.218 2.318 2.285 2.423 2.287 2.609 2.510 2.506 2.287 15.22 80) T alpha-Methylst... 0.648 0.901 1.141 1.101 1.149 1.119 1.452 1.407 1.421 1.149 22.79 81) T 2-Ethyltoluene 1.731 2.523 2.783 2.669 2.923 2.776 3.102 2.959 2.930 2.711 14.95 82) T 1,2,4-Trimethy... 1.439 2.129 2.289 2.223 2.486 2.416 2.802 2.711 2.586 2.342 17.29 83) T n-Decane 0.942 1.422 1.600 1.560 1.715 1.606 1.810 1.641 1.442 1.527 16.40 84) T Benzyl Chloride 1.562 1.609 1.938 2.205 2.590 2.487 2.420 2.116 19.85 85) T 1,3-Dichlorobe... 0.714 1.158 1.211 1.164 1.317 1.248 1.430 1.382 1.414 1.227 17.80 86) T 1,4-Dichlorobe... 0.850 1.133 1.219 1.237 1.377 1.298 1.486 1.419 1.446 1.274 15.47 87) T sec-Butylbenzene 2.000 2.849 3.120 3.073 3.382 3.210 3.589 3.390 3.292 3.101 14.98 88) T 4-Isopropyltol... 2.824 3.054 2.933 2.765 3.081 2.944 3.505 3.335 3.079 3.058 7.72 89) T 1,2,3-Trimethy... 1.744 2.387 2.369 2.298 2.590 2.533 2.960 2.838 2.680 2.489 14.26 90) T 1,2-Dichlorobe... 0.749 1.113 1.223 1.156 1.311 1.247 1.435 1.369 1.379 1.220 16.90 91) T d-Limonene 0.498 0.860 0.965 0.989 0.988 0.977 1.239 1.159 1.093 0.974 21.73 92) T 1,2-Dibromo-3-... 0.366 0.378 0.473 0.488 0.570 0.544 0.546 0.481 17.00 93) T n-Undecane 0.933 1.367 1.599 1.606 1.750 1.754 1.968 1.773 1.613 1.596 18.67 94) T 1,2,4-Trichlor... 0.713 0.711 0.906 0.950 1.109 1.067 1.083 0.934 18.02

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Method Path : I:\MS09\Methods\ Method File : R9071315.M Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS)95) T Naphthalene 3.152 3.164 2.809 2.568 3.589 3.761 4.191 3.953 3.788 3.442 15.89 96) T n-Dodecane 1.072 1.303 1.559 1.554 1.799 1.832 2.008 1.817 1.642 1.621 17.94 97) T Hexachlorobuta... 0.507 0.471 0.529 0.528 0.630 0.614 0.640 0.560 11.96 98) T Cyclohexanone 0.896 1.007 1.100 1.026 1.069 1.008 1.113 1.046 1.011 1.031 6.24 99) T tert-Butylbenzene 1.440 2.036 2.164 2.174 2.319 2.231 2.621 2.532 2.406 2.214 15.56 100) T n-Butylbenzene 1.801 2.406 2.476 2.509 2.885 2.785 3.102 2.866 2.730 2.618 14.50 ----------------------------------------------------------------------------(#) = Out of Range

R9071315.M Tue Jul 14 11:08:59 2015 Page: 3

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1ng/L Std. ID: S29-07111510

4ng/L Std. ID: S29-0711150620ng/L Std. ID: S29-07111505

200ng/L Std. ID: S29-07081503Dilution Factors: 5 50 250 1000 1 1 4 4 20 20 200 200 200

Source Std. Injection (L): 0.080 0.100 0.050 0.100 0.050 0.25 0.125 0.25 0.50Compounds mg/m3 200ng/L 20ng/L 4ng/L 1ng/L ICAL Points: 0.08ng 0.1ng 0.2ng 0.4ng 1ng 5ng 25ng 50ng 100ngPropene 1.00 200 20.0 4.00 1.00 0.0800 0.100 0.200 0.400 1.00 5.00 25.00 50.0 100Dichlorodifluoromethane 1.02 204 20.4 4.08 1.02 0.0816 0.102 0.204 0.408 1.02 5.10 25.50 51.0 102Chloromethane 0.99 198 19.8 3.96 0.99 0.0792 0.099 0.198 0.396 0.99 4.95 24.75 49.5 99Freon-114 1.03 206 20.6 4.12 1.03 0.0824 0.103 0.206 0.412 1.03 5.15 25.75 51.5 103Vinyl Chloride 1.01 202 20.2 4.04 1.01 0.0808 0.101 0.202 0.404 1.01 5.05 25.25 50.5 1011,3-Butadiene 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107Bromomethane 1.01 202 20.2 4.04 1.01 0.0808 0.101 0.202 0.404 1.01 5.05 25.25 50.5 101Chloroethane 1.01 202 20.2 4.04 1.01 0.0808 0.101 0.202 0.404 1.01 5.05 25.25 50.5 101Ethanol 5.09 1018 101.8 20.36 5.09 0.4072 0.509 1.018 2.036 5.09 25.45 127.25 254.5 509Acetonitrile 1.02 204 20.4 4.08 1.02 0.0816 0.102 0.204 0.408 1.02 5.10 25.50 51.0 102Acrolein 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107Acetone 5.40 1080 108.0 21.60 5.40 0.4320 0.540 1.080 2.160 5.40 27.00 135.00 270.0 540Trichlorofluoromethane 0.99 198 19.8 3.96 0.99 0.0792 0.099 0.198 0.396 0.99 4.95 24.75 49.5 99Isopropanol 2.10 420 42.0 8.40 2.10 0.1680 0.210 0.420 0.840 2.10 10.50 52.50 105.0 210Acrylonitrile 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 1041,1-Dichloroethene 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107tert-Butanol 2.11 422 42.2 8.44 2.11 0.1688 0.211 0.422 0.844 2.11 10.55 52.75 105.5 211Methylene Chloride 1.08 216 21.6 4.32 1.08 0.0864 0.108 0.216 0.432 1.08 5.40 27.00 54.0 108Allyl Chloride 1.09 218 21.8 4.36 1.09 0.0872 0.109 0.218 0.436 1.09 5.45 27.25 54.5 109Trichlorotrifluoroethane 1.08 216 21.6 4.32 1.08 0.0864 0.108 0.216 0.432 1.08 5.40 27.00 54.0 108Carbon Disulfide 0.98 196 19.6 3.92 0.98 0.0784 0.098 0.196 0.392 0.98 4.90 24.50 49.0 98trans-1,2-Dichloroethene 1.06 212 21.2 4.24 1.06 0.0848 0.106 0.212 0.424 1.06 5.30 26.50 53.0 1061,1-Dichloroethane 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 104Methyl tert-Butyl Ether 1.06 212 21.2 4.24 1.06 0.0848 0.106 0.212 0.424 1.06 5.30 26.50 53.0 106Vinyl Acetate 5.12 1024 102.4 20.48 5.12 0.4096 0.512 1.024 2.048 5.12 25.60 128.00 256.0 5122-Butanone 1.08 216 21.6 4.32 1.08 0.0864 0.108 0.216 0.432 1.08 5.40 27.00 54.0 108cis-1,2-Dichloroethene 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107Diisopropyl Ether 1.09 218 21.8 4.36 1.09 0.0872 0.109 0.218 0.436 1.09 5.45 27.25 54.5 109Ethyl Acetate 2.14 428 42.8 8.56 2.14 0.1712 0.214 0.428 0.856 2.14 10.70 53.50 107.0 214n-Hexane 1.05 210 21.0 4.20 1.05 0.0840 0.105 0.210 0.420 1.05 5.25 26.25 52.5 105Chloroform 1.08 216 21.6 4.32 1.08 0.0864 0.108 0.216 0.432 1.08 5.40 27.00 54.0 108Tetrahydrofuran 1.03 206 20.6 4.12 1.03 0.0824 0.103 0.206 0.412 1.03 5.15 25.75 51.5 103Ethyl tert-Butyl Ether 1.06 212 21.2 4.24 1.06 0.0848 0.106 0.212 0.424 1.06 5.30 26.50 53.0 1061,2-Dichloroethane 1.05 210 21.0 4.20 1.05 0.0840 0.105 0.210 0.420 1.05 5.25 26.25 52.5 1051,1,1-Trichloroethane 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 104Isopropyl Acetate 2.18 436 43.6 8.72 2.18 0.1744 0.218 0.436 0.872 2.18 10.90 54.50 109.0 2181-Butanol 2.23 446 44.6 8.92 2.23 0.1784 0.223 0.446 0.892 2.23 11.15 55.75 111.5 223Benzene 1.10 220 22.0 4.40 1.10 0.0880 0.110 0.220 0.440 1.10 5.50 27.50 55.0 110Carbon Tetrachloride 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107Cyclohexane 2.11 422 42.2 8.44 2.11 0.1688 0.211 0.422 0.844 2.11 10.55 52.75 105.5 211tert-Amyl Methyl Ether 1.05 210 21.0 4.20 1.05 0.0840 0.105 0.210 0.420 1.05 5.25 26.25 52.5 1051,2-Dichloropropane 1.06 212 21.2 4.24 1.06 0.0848 0.106 0.212 0.424 1.06 5.30 26.50 53.0 106Bromodichloromethane 1.08 216 21.6 4.32 1.08 0.0864 0.108 0.216 0.432 1.08 5.40 27.00 54.0 108Trichloroethene 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 1041,4-Dioxane 1.09 218 21.8 4.36 1.09 0.0872 0.109 0.218 0.436 1.09 5.45 27.25 54.5 109Isooctane 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 104Methyl Methacrylate 2.10 420 42.0 8.40 2.10 0.1680 0.210 0.420 0.840 2.10 10.50 52.50 105.0 210n-Heptane 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107

Primary Source Standards Concentrations (Working & Initial Calibration)

Working STD Conc.(ng/L):

Primary Working Standards

Q:\TO15 Std. Concentrations\MS16 Std. Conc\2015\R9071315\ICAL Conc. (Primary Source)

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1ng/L Std. ID: S29-07111510



Source Std. Injection (L): 0.080 0.100 0.050 0.100 0.050 0.25 0.125 0.25 0.50Compounds mg/m3 200ng/L 20ng/L 4ng/L 1ng/L ICAL Points: 0.08ng 0.1ng 0.2ng 0.4ng 1ng 5ng 25ng 50ng 100ng




cis-1,3-Dichloropropene 1.13 226 22.6 4.52 1.13 0.0904 0.113 0.226 0.452 1.13 5.65 28.25 56.5 113



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1ng/L Std. ID: S29-07111510



Source Std. Injection (L): 0.080 0.100 0.050 0.100 0.050 0.25 0.125 0.25 0.50Compounds mg/m3 200ng/L 20ng/L 4ng/L 1ng/L ICAL Points: 0.08ng 0.1ng 0.2ng 0.4ng 1ng 5ng 25ng 50ng 100ng




4-Methyl-2-pentanone 1.09 218 21.8 4.36 1.09 0.0872 0.109 0.218 0.436 1.09 5.45 27.25 54.5 109trans-1,3-Dichloropropene 1.08 216 21.6 4.32 1.08 0.0864 0.108 0.216 0.432 1.08 5.40 27.00 54.0 1081,1,2-Trichloroethane 1.06 212 21.2 4.24 1.06 0.0848 0.106 0.212 0.424 1.06 5.30 26.50 53.0 106Toluene 1.06 212 21.2 4.24 1.06 0.0848 0.106 0.212 0.424 1.06 5.30 26.50 53.0 1062-Hexanone 1.11 222 22.2 4.44 1.11 0.0888 0.111 0.222 0.444 1.11 5.55 27.75 55.5 111Dibromochloromethane 1.10 220 22.0 4.40 1.10 0.0880 0.110 0.220 0.440 1.10 5.50 27.50 55.0 1101,2-Dibromoethane 1.08 216 21.6 4.32 1.08 0.0864 0.108 0.216 0.432 1.08 5.40 27.00 54.0 108n-Butyl Acetate 1.12 224 22.4 4.48 1.12 0.0896 0.112 0.224 0.448 1.12 5.60 28.00 56.0 112n-Octane 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 104Tetrachloroethene 0.99 198 19.8 3.96 0.99 0.0792 0.099 0.198 0.396 0.99 4.95 24.75 49.5 99Chlorobenzene 1.08 216 21.6 4.32 1.08 0.0864 0.108 0.216 0.432 1.08 5.40 27.00 54.0 108Ethylbenzene 1.06 212 21.2 4.24 1.06 0.0848 0.106 0.212 0.424 1.06 5.30 26.50 53.0 106m-&p-Xylene 2.10 420 42.0 8.40 2.10 0.1680 0.210 0.420 0.840 2.10 10.50 52.50 105.0 210Bromoform 1.08 216 21.6 4.32 1.08 0.0864 0.108 0.216 0.432 1.08 5.40 27.00 54.0 108Styrene 1.09 218 21.8 4.36 1.09 0.0872 0.109 0.218 0.436 1.09 5.45 27.25 54.5 109o-Xylene 1.03 206 20.6 4.12 1.03 0.0824 0.103 0.206 0.412 1.03 5.15 25.75 51.5 103n-Nonane 1.02 204 20.4 4.08 1.02 0.0816 0.102 0.204 0.408 1.02 5.10 25.50 51.0 1021,1,2,2-Tetrachloroethane 1.01 202 20.2 4.04 1.01 0.0808 0.101 0.202 0.404 1.01 5.05 25.25 50.5 101Cumene 1.02 204 20.4 4.08 1.02 0.0816 0.102 0.204 0.408 1.02 5.10 25.50 51.0 102alpha-Pinene 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 104n-Propylbenzene 1.01 202 20.2 4.04 1.01 0.0808 0.101 0.202 0.404 1.01 5.05 25.25 50.5 1013-Ethyltoluene 1.06 212 21.2 4.24 1.06 0.0848 0.106 0.212 0.424 1.06 5.30 26.50 53.0 1064-Ethyltoluene 1.06 212 21.2 4.24 1.06 0.0848 0.106 0.212 0.424 1.06 5.30 26.50 53.0 1061,3,5-Trimethylbenzene 1.06 212 21.2 4.24 1.06 0.0848 0.106 0.212 0.424 1.06 5.30 26.50 53.0 106alpha-Methylstyrene 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 1042-Ethyltoluene 1.05 210 21.0 4.20 1.05 0.0840 0.105 0.210 0.420 1.05 5.25 26.25 52.5 1051,2,4-Trimethylbenzene 1.05 210 21.0 4.20 1.05 0.0840 0.105 0.210 0.420 1.05 5.25 26.25 52.5 105n-Decane 1.03 206 20.6 4.12 1.03 0.0824 0.103 0.206 0.412 1.03 5.15 25.75 51.5 103Benzyl Chloride 1.09 218 21.8 4.36 1.09 0.0872 0.109 0.218 0.436 1.09 5.45 27.25 54.5 1091,3-Dichlorobenzene 1.09 218 21.8 4.36 1.09 0.0872 0.109 0.218 0.436 1.09 5.45 27.25 54.5 1091,4-Dichlorobenzene 1.06 212 21.2 4.24 1.06 0.0848 0.106 0.212 0.424 1.06 5.30 26.50 53.0 106sec-Butylbenzene 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107p-Isopropyltoluene 1.01 202 20.2 4.04 1.01 0.0808 0.101 0.202 0.404 1.01 5.05 25.25 50.5 1011,2,3-Trimethylbenzene 1.05 210 21.0 4.20 1.05 0.0840 0.105 0.210 0.420 1.05 5.25 26.25 52.5 1051,2-Dichlorobenzene 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107d-Limonene 1.05 210 21.0 4.20 1.05 0.0840 0.105 0.210 0.420 1.05 5.25 26.25 52.5 1051,2-Dibromo-3-chloropropane 1.03 206 20.6 4.12 1.03 0.0824 0.103 0.206 0.412 1.03 5.15 25.75 51.5 103n-Undecane 1.01 202 20.2 4.04 1.01 0.0808 0.101 0.202 0.404 1.01 5.05 25.25 50.5 1011,2,4-Trichlorobenzene 1.05 210 21.0 4.20 1.05 0.0840 0.105 0.210 0.420 1.05 5.25 26.25 52.5 105Naphthalene 0.98 196 19.6 3.92 0.98 0.0784 0.098 0.196 0.392 0.98 4.90 24.50 49.0 98n-Dodecane 1.01 202 20.2 4.04 1.01 0.0808 0.101 0.202 0.404 1.01 5.05 25.25 50.5 101Hexachloro-1,3-butadiene 1.07 214 21.4 4.28 1.07 0.0856 0.107 0.214 0.428 1.07 5.35 26.75 53.5 107Methacrylonitrile 1.04 208 20.8 4.16 1.04 0.0832 0.104 0.208 0.416 1.04 5.20 26.00 52.0 104Cyclohexanone 1.11 222 22.2 4.44 1.11 0.0888 0.111 0.222 0.444 1.11 5.55 27.75 55.5 111tert-Butylbenzene 1.06 212 21.2 4.24 1.06 0.0848 0.106 0.212 0.424 1.06 5.30 26.50 53.0 106n-Butylbenzene 1.09 218 21.8 4.36 1.09 0.0872 0.109 0.218 0.436 1.09 5.45 27.25 54.5 109



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Calibration Status Report MS09

Method : I:\MS09\Methods\R9071315.M (RTE Integrator) Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) Last Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration

# ID Conc ISTD Path\File Conc -- ---- ---- ---- ------------------------------------------------- 1 0.08 0 13 I:\MS09\Data\2015_07\13\07131513.D 2 0.10 0 13 I:\MS09\Data\2015_07\13\07131514.D 3 0.20 0 13 I:\MS09\Data\2015_07\13\07131515.D 4 0.40 0 13 I:\MS09\Data\2015_07\13\07131516.D 5 1.0 1 13 I:\MS09\Data\2015_07\13\07131517.D 6 5.0 5 13 I:\MS09\Data\2015_07\13\07131518.D 7 25 25 13 I:\MS09\Data\2015_07\13\07131519.D 8 50 50 13 I:\MS09\Data\2015_07\13\07131520.D 9 100 100 13 I:\MS09\Data\2015_07\13\07131521.D

# ID Update Time Quant Time Acquisition Time -- -- -------------------- ----------------- --------------------- 1 0.08 Jul 14 10:50 2015 Jul 14 10:43 2015 13 Jul 2015 18:41 2 0.10 Jul 14 10:51 2015 Jul 14 10:41 2015 13 Jul 2015 19:15 3 0.20 Jul 14 10:51 2015 Jul 14 10:40 2015 13 Jul 2015 19:49 4 0.40 Jul 14 10:51 2015 Jul 14 10:39 2015 13 Jul 2015 20:23 5 1.0 Jul 14 10:51 2015 Jul 14 10:37 2015 13 Jul 2015 20:58 6 5.0 Jul 14 10:52 2015 Jul 14 10:35 2015 13 Jul 2015 21:32 7 25 Jul 14 10:52 2015 Jul 14 10:24 2015 13 Jul 2015 22:06 8 50 Jul 14 10:52 2015 Jul 14 10:47 2015 13 Jul 2015 22:40 9 100 Jul 14 10:53 2015 Jul 14 10:48 2015 13 Jul 2015 23:14

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Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_07\13\07131513.D Acq On : 13 Jul 2015 18:41 Operator: SC Sample : 0.08ng TO-15 ICAL STD Misc : S29-07071501/S29-07111510 (8/9) ALS Vial : 3 Sample Multiplier: 1 Quant Time: Jul 14 10:43:33 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:34:59 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 1) Bromochloromethane (IS1) 8.98 130 140866 12.500 ng -0.02 37) 1,4-Difluorobenzene (IS2) 10.96 114 738546 12.500 ng -0.02 56) Chlorobenzene-d5 (IS3) 15.31 82 318263 12.500 ng 0.00 System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.76 65 276723 15.509 ng -0.02 Spiked Amount 12.500 Recovery = 124.08% 57) Toluene-d8 (SS2) 13.40 98 745783 12.798 ng 0.00 Spiked Amount 12.500 Recovery = 102.40% 73) Bromofluorobenzene (SS3) 16.92 174 221366 9.346 ng 0.00 Spiked Amount 12.500 Recovery = 74.80% Target Compounds Qvalue 2) Propene 3.80 42 1669 0.114 ng 94 3) Dichlorodifluoromethan... 3.90 85 2044 0.069 ng # 85 4) Chloromethane 4.10 50 1620 0.078 ng # 42 5) 1,2-Dichloro-1,1,2,2-t... 4.24 135 796 0.053 ng # 43 6) Vinyl Chloride 4.37 62 1365 0.070 ng # 43 7) 1,3-Butadiene 4.54 54 1028 0.071 ng 91 8) Bromomethane 4.84 94 880 0.068 ng 99 9) Chloroethane 5.05 64 706 0.069 ng # 43 10) Ethanol 5.24 45 4354 0.441 ng 97 11) Acetonitrile 5.47 41 2365 0.084 ng 78 12) Acrolein 5.60 56 743 0.078 ng # 15 13) Acetone 5.73 58 4892 0.472 ng 97 14) Trichlorofluoromethane 5.90 101 1527 0.060 ng 95 15) 2-Propanol (Isopropanol) 6.06 45 5331 0.157 ng 94 16) Acrylonitrile 6.26 53 1193 0.068 ng 97 17) 1,1-Dichloroethene 6.58 96 864 0.066 ng 90 18) 2-Methyl-2-Propanol (t... 6.72 59 4694 0.144 ng # 92 19) Methylene Chloride 6.71 84 2773 0.191 ng 99 20) 3-Chloro-1-propene (Al... 6.85 41 1598 0.088 ng # 44 21) Trichlorotrifluoroethane 7.04 151 633 0.052 ng 85 22) Carbon Disulfide 7.02 76 3757 0.063 ng # 74 23) trans-1,2-Dichloroethene 7.74 61 1226 0.065 ng 95 24) 1,1-Dichloroethane 7.94 63 1783 0.071 ng 95 25) Methyl tert-Butyl Ether 8.07 73 2604 0.069 ng 92 26) Vinyl Acetate 8.14 86 555 0.190 ng # 3 27) 2-Butanone (MEK) 8.41 72 691 0.080 ng # 37 28) cis-1,2-Dichloroethene 8.81 61 1398 0.076 ng 100 29) Diisopropyl Ether 9.10 87 984 0.087 ng # 72 30) Ethyl Acetate 9.10 61 881 0.199 ng 96 31) n-Hexane 9.08 57 1754 0.083 ng # 92 32) Chloroform 9.11 83 1683 0.071 ng 91 34) Tetrahydrofuran (THF) 9.58 72 690 0.078 ng # 72 35) Ethyl tert-Butyl Ether 9.64 87 960 0.066 ng 93 36) 1,2-Dichloroethane 9.87 62 1249 0.074 ng # 42 38) 1,1,1-Trichloroethane 10.14 97 1290 0.060 ng 93 39) Isopropyl Acetate 10.54 61 1086 0.130 ng # 54 40) 1-Butanol 10.58 56 3439 0.255 ng 93 41) Benzene 10.60 78 4424 0.079 ng 98 42) Carbon Tetrachloride 10.76 117 1080 0.058 ng 96 43) Cyclohexane 10.88 84 2667 0.127 ng 96 44) tert-Amyl Methyl Ether 11.24 73 2626 0.068 ng # 85 45) 1,2-Dichloropropane 11.42 63 1079 0.075 ng 81 46) Bromodichloromethane 11.61 83 1185 0.064 ng 99 47) Trichloroethene 11.66 130 866 0.055 ng 97 48) 1,4-Dioxane 11.68 88 942 0.076 ng 77 49) 2,2,4-Trimethylpentane... 11.72 57 4370 0.073 ng 95

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Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_07\13\07131513.D Acq On : 13 Jul 2015 18:41 Operator: SC Sample : 0.08ng TO-15 ICAL STD Misc : S29-07071501/S29-07111510 (8/9) ALS Vial : 3 Sample Multiplier: 1 Quant Time: Jul 14 10:43:33 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:34:59 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 50) Methyl Methacrylate 11.86 100 798 0.152 ng # 88 51) n-Heptane 11.97 71 968 0.074 ng # 86 52) cis-1,3-Dichloropropene 12.52 75 1356 0.064 ng # 43 53) 4-Methyl-2-pentanone 12.58 58 1178 0.098 ng # 63 54) trans-1,3-Dichloropropene 13.04 75 875 0.042 ng # 43 55) 1,1,2-Trichloroethane 13.21 97 770 0.055 ng 97 58) Toluene 13.50 91 3909 0.062 ng 93 59) 2-Hexanone 13.78 43 2930 0.101 ng 92 60) Dibromochloromethane 13.91 129 713 0.044 ng 95 61) 1,2-Dibromoethane 14.17 107 808 0.051 ng 91 62) n-Butyl Acetate 14.41 43 3100 0.093 ng # 87 63) n-Octane 14.52 57 794 0.064 ng 97 64) Tetrachloroethene 14.66 166 726 0.039 ng 94 65) Chlorobenzene 15.36 112 2337 0.057 ng 91 66) Ethylbenzene 15.76 91 3717 0.054 ng 100 67) m- & p-Xylenes 15.96 91 6381 0.116 ng 99 68) Bromoform 16.02 173 451m 0.031 ng 69) Styrene 16.33 104 2075 0.051 ng 98 70) o-Xylene 16.45 91 3129 0.056 ng 95 71) n-Nonane 16.69 43 2025 0.071 ng 96 72) 1,1,2,2-Tetrachloroethane 16.43 83 1413 0.050 ng 99 74) Cumene 17.07 105 3926 0.054 ng 91 75) alpha-Pinene 17.48 93 1710 0.050 ng # 17 76) n-Propylbenzene 17.60 91 4528 0.052 ng 98 77) 3-Ethyltoluene 17.71 105 3637 0.054 ng 97 78) 4-Ethyltoluene 17.76 105 3471 0.053 ng 92 79) 1,3,5-Trimethylbenzene 17.83 105 3077 0.054 ng 87 80) alpha-Methylstyrene 17.99 118 1372 0.047 ng 87 81) 2-Ethyltoluene 18.03 105 3703 0.054 ng 92 82) 1,2,4-Trimethylbenzene 18.26 105 3077 0.054 ng 99 83) n-Decane 18.38 57 1977 0.063 ng # 73 84) Benzyl Chloride 18.40 91 1904 0.041 ng # 57 85) 1,3-Dichlorobenzene 18.42 146 1585 0.047 ng 98 86) 1,4-Dichlorobenzene 18.49 146 1836 0.051 ng 91 87) sec-Butylbenzene 18.55 105 4358 0.058 ng 97 88) 4-Isopropyltoluene (p-... 18.72 119 5810 0.082 ng 96 89) 1,2,3-Trimethylbenzene 18.71 105 3731 0.063 ng 99 90) 1,2-Dichlorobenzene 18.85 146 1632 0.050 ng 92 91) d-Limonene 18.87 68 1065 0.050 ng 95 92) 1,2-Dibromo-3-Chloropr... 0.00 157 0 N.D. 93) n-Undecane 19.72 57 1920 0.058 ng # 80 94) 1,2,4-Trichlorobenzene 20.67 180 954 0.039 ng # 83 95) Naphthalene 20.78 128 6291 0.075 ng # 71 96) n-Dodecane 20.81 57 2205 0.070 ng 93 97) Hexachlorobutadiene 21.14 225 659 0.039 ng # 18 98) Cyclohexanone 16.12 55 2025 0.098 ng 94 99) tert-Butylbenzene 18.26 119 3110 0.056 ng 99 100) n-Butylbenzene 19.16 91 3998 0.067 ng 96 -------------------------------------------------------------------------- (#) = qualifier out of range (m) = manual integration (+) = signals summed

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Data File: I:\MS09\Data\2015_07\13\07131513.D Acq On : 13 Jul 2015 18:41 Operator: SC Sample : 0.08ng TO-15 ICAL STD Misc : S29-07071501/S29-07111510 (8/9) ALS Vial : 3 Sample Multiplier: 1

Quant Time: Jul 14 10:43:33 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:34:59 2015 Response via : Initial Calibration DataAcq Meth:TO15.M

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600000

650000

700000

750000

800000

850000

900000

950000

1000000

1050000

1100000

1150000

1200000

Time-->


Hex

achl

orob

utad

iene

,Tn-

Dod

ecan

e,T

Nap

htha

lene

,T1,

2,4-

Tric

hlor

oben

zene

,T

n-U

ndec

ane,

T

n-Bu

tylb

enze

ne,T

d-Li

mon

ene,

T1,

2-D

ichl

orob

enze

ne,T

4-Is

opro

pylto

luen

e (p

-Cym

ene)

,T1,

2,3-

Trim

ethy

lben

zene

,Tse

c-Bu

tylb

enze

ne,T

1,4-

Dic

hlor

oben

zene

,T1,

3-D

ichl

orob

enze

ne,T

Benz

yl C

hlor

ide,

Tn-

Dec

ane,

Tte

rt-Bu

tylb

enze

ne,T

1,2,

4-Tr

imet

hylb

enze

ne,T

2-Et

hylto

luen

e,T

alph

a-M

ethy

lsty

rene

,T1,

3,5-

Trim

ethy

lben

zene

,T4-

Ethy

ltolu

ene,

T3-

Ethy

ltolu

ene,

Tn-

Prop

ylbe

nzen

e,T

alph

a-Pi

nene

,TC

umen

e,T

Brom

oflu

orob

enze

ne (S

S3),S

n-N

onan

e,T

o-Xy

lene

,T1,

1,2,

2-Te

trach

loro

etha

ne,T

Styr

ene,

TC

yclo

hexa

none

,TBr

omof

orm

,Tm

- & p

-Xyl

enes

,TEt

hylb

enze

ne,T

Chl

orob

enze

ne,T

Chl

orob

enze

ne-d

5 (IS

3),IR

Tetra

chlo

roet

hene

,Tn-

Oct

ane,

Tn-

Buty

l Ace

tate

,T1,

2-D

ibro

moe

than

e,T

Dib

rom

ochl

orom

etha

ne,T

2-H

exan

one,

TTo

luen

e,T

Tolu

ene-

d8 (S

S2),S

1,1,

2-Tr

ichl

oroe

than

e,T

trans

-1,3

-Dic

hlor

opro

pene

,T

4-M

ethy

l-2-p

enta

none

,Tci

s-1,

3-D

ichl

orop

rope

ne,T

n-H

epta

ne,T

Met

hyl M

etha

cryl

ate,

T2,

2,4-

Trim

ethy

lpen

tane

(Iso

octa

ne),T

1,4-

Dio

xane

,TTr

ichl

oroe

then

e,T

Brom

odic

hlor

omet

hane

,T1,

2-D

ichl

orop

ropa

ne,T

tert-

Am

yl M

ethy

l Eth

er,T

1,4-

Difl

uoro

benz

ene

(IS2)

,IRC

yclo

hexa

ne,T

Car

bon

Tetra

chlo

ride,

TBe

nzen

e,T

1-Bu

tano

l,TIs

opro

pyl A

ceta

te,T

1,1,

1-Tr

ichl

oroe

than

e,T

1,2-

Dic

hlor

oeth

ane,

T1,

2-D

ichl

oroe

than

e-d4

(SS1

),SEt

hyl t

ert-B

utyl

Eth

er,T

Tetra

hydr

ofur

an (T

HF)

,T

Chl

orof

orm

,TD

iisop

ropy

l Eth

er,T

Ethy

l Ace

tate

,Tn-

Hex

ane,

TBr

omoc

hlor

omet

hane

(IS1

),IR

cis-

1,2-

Dic

hlor

oeth

ene,

T2-

Buta

none

(MEK

),TVi

nyl A

ceta

te,T

Met

hyl t

ert-B

utyl

Eth

er,T

1,1-

Dic

hlor

oeth

ane,

Ttra

ns-1

,2-D

ichl

oroe

then

e,T

Tric

hlor

otrif

luor

oeth

ane,

TC

arbo

n D

isul

fide,

T3-

Chl

oro-

1-pr

open

e (A

llyl C

hlor

ide)

,T2-

Met

hyl-2

-Pro

pano

l (te

rt-Bu

tyl A

lcoh

ol,T

Met

hyle

ne C

hlor

ide,

T1,

1-D

ichl

oroe

then

e,T

Acry

loni

trile

,T2-

Prop

anol

(Iso

prop

anol

),TTr

ichl

orof

luor

omet

hane

,TAc

eton

e,T

Acro

lein

,TAc

eton

itrile

,TEt

hano

l,TC

hlor

oeth

ane,

TBr

omom

etha

ne,T

1,3-

Buta

dien

e,T

Viny

l Chl

orid

e,T

1,2-

Dic

hlor

o-1,

1,2,

2-te

traflu

oroe

than

e ,T

Chl

orom

etha

ne,T

Dic

hlor

odifl

uoro

met

hane

(CFC

12)

,TPr

open

e,T

R9071315.M Tue Jul 14 10:46:16 2015 Page: 3

83 of 128

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_07\13\07131514.D Acq On : 13 Jul 2015 19:15 Operator: SC Sample : 0.10ng TO-15 ICAL STD Misc : S29-07071501/S29-07111510 (8/9) ALS Vial : 3 Sample Multiplier: 1 Quant Time: Jul 14 10:41:40 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:34:59 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 1) Bromochloromethane (IS1) 8.98 130 132170 12.500 ng -0.02 37) 1,4-Difluorobenzene (IS2) 10.96 114 693587 12.500 ng -0.02 56) Chlorobenzene-d5 (IS3) 15.31 82 305376 12.500 ng 0.00 System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.76 65 266055 15.892 ng -0.02 Spiked Amount 12.500 Recovery = 127.12% 57) Toluene-d8 (SS2) 13.40 98 706645 12.638 ng 0.00 Spiked Amount 12.500 Recovery = 101.12% 73) Bromofluorobenzene (SS3) 16.92 174 212306 9.341 ng 0.00 Spiked Amount 12.500 Recovery = 74.72% Target Compounds Qvalue 2) Propene 3.80 42 2491 0.182 ng 99 3) Dichlorodifluoromethan... 3.89 85 3551 0.127 ng # 92 4) Chloromethane 4.09 50 2951 0.151 ng 97 5) 1,2-Dichloro-1,1,2,2-t... 4.24 135 1606 0.114 ng # 43 6) Vinyl Chloride 4.36 62 2308 0.126 ng 97 7) 1,3-Butadiene 4.54 54 1909 0.141 ng # 85 8) Bromomethane 4.84 94 1508 0.125 ng 90 9) Chloroethane 5.05 64 1346 0.140 ng # 43 10) Ethanol 5.23 45 7457 0.805 ng 99 11) Acetonitrile 5.45 41 4086 0.154 ng 93 12) Acrolein 5.58 56 1228 0.137 ng 97 13) Acetone 5.73 58 8124 0.835 ng 98 14) Trichlorofluoromethane 5.90 101 2829 0.119 ng 100 15) 2-Propanol (Isopropanol) 6.04 45 9642 0.303 ng 94 16) Acrylonitrile 6.24 53 2081 0.126 ng 87 17) 1,1-Dichloroethene 6.58 96 1486 0.121 ng 97 18) 2-Methyl-2-Propanol (t... 6.71 59 8682 0.283 ng 96 19) Methylene Chloride 6.71 84 3359 0.246 ng 99 20) 3-Chloro-1-propene (Al... 6.84 41 2972 0.174 ng 94 21) Trichlorotrifluoroethane 7.03 151 1220 0.107 ng 99 22) Carbon Disulfide 7.01 76 6340 0.113 ng 95 23) trans-1,2-Dichloroethene 7.73 61 2394 0.136 ng 98 24) 1,1-Dichloroethane 7.94 63 3191 0.135 ng 98 25) Methyl tert-Butyl Ether 8.07 73 4981 0.141 ng 94 26) Vinyl Acetate 8.14 86 1254 0.458 ng # 56 27) 2-Butanone (MEK) 8.40 72 1227 0.151 ng # 65 28) cis-1,2-Dichloroethene 8.81 61 2410 0.140 ng 98 29) Diisopropyl Ether 9.09 87 1471 0.138 ng # 88 30) Ethyl Acetate 9.08 61 1323 0.318 ng 96 31) n-Hexane 9.07 57 3275 0.165 ng # 91 32) Chloroform 9.12 83 2848 0.129 ng 96 34) Tetrahydrofuran (THF) 9.58 72 1193 0.143 ng # 84 35) Ethyl tert-Butyl Ether 9.63 87 1670 0.122 ng 91 36) 1,2-Dichloroethane 9.88 62 2235 0.140 ng 93 38) 1,1,1-Trichloroethane 10.15 97 2453 0.122 ng 93 39) Isopropyl Acetate 10.54 61 2176 0.277 ng # 89 40) 1-Butanol 10.57 56 4520 0.356 ng 97 41) Benzene 10.60 78 8296 0.159 ng 97 42) Carbon Tetrachloride 10.75 117 1936 0.111 ng 100 43) Cyclohexane 10.88 84 4651 0.235 ng 93 44) tert-Amyl Methyl Ether 11.23 73 4726 0.131 ng 98 45) 1,2-Dichloropropane 11.42 63 1814 0.135 ng 97 46) Bromodichloromethane 11.60 83 2044 0.117 ng 98 47) Trichloroethene 11.66 130 1513 0.103 ng 97 48) 1,4-Dioxane 11.68 88 1558 0.134 ng 79 49) 2,2,4-Trimethylpentane... 11.72 57 7723 0.136 ng 99

R9071315.M Tue Jul 14 10:42:39 2015 Page: 1

84 of 128

simon.cao

Simon

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_07\13\07131514.D Acq On : 13 Jul 2015 19:15 Operator: SC Sample : 0.10ng TO-15 ICAL STD Misc : S29-07071501/S29-07111510 (8/9) ALS Vial : 3 Sample Multiplier: 1 Quant Time: Jul 14 10:41:40 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:34:59 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 50) Methyl Methacrylate 11.86 100 1254 0.254 ng 95 51) n-Heptane 11.98 71 1583 0.129 ng # 89 52) cis-1,3-Dichloropropene 12.52 75 2495 0.125 ng 98 53) 4-Methyl-2-pentanone 12.57 58 1822 0.161 ng 92 54) trans-1,3-Dichloropropene 13.04 75 1880 0.096 ng # 43 55) 1,1,2-Trichloroethane 13.20 97 1468 0.112 ng 99 58) Toluene 13.50 91 6757 0.112 ng 99 59) 2-Hexanone 13.77 43 4585 0.164 ng 96 60) Dibromochloromethane 13.92 129 1518 0.098 ng 91 61) 1,2-Dibromoethane 14.17 107 1569 0.103 ng 99 62) n-Butyl Acetate 14.41 43 4846 0.152 ng 98 63) n-Octane 14.53 57 1479 0.124 ng 94 64) Tetrachloroethene 14.66 166 1572 0.088 ng 92 65) Chlorobenzene 15.36 112 4101 0.104 ng 97 66) Ethylbenzene 15.76 91 7072 0.108 ng 97 67) m- & p-Xylenes 15.95 91 11077 0.210 ng 100 68) Bromoform 16.01 173 998 0.071 ng 92 69) Styrene 16.34 104 3690 0.095 ng 99 70) o-Xylene 16.45 91 5618 0.104 ng 99 71) n-Nonane 16.70 43 3738 0.136 ng 96 72) 1,1,2,2-Tetrachloroethane 16.42 83 2666 0.099 ng 96 74) Cumene 17.07 105 6571 0.094 ng 96 75) alpha-Pinene 17.48 93 3280 0.100 ng # 26 76) n-Propylbenzene 17.60 91 8403 0.100 ng 99 77) 3-Ethyltoluene 17.71 105 6427 0.099 ng 99 78) 4-Ethyltoluene 17.75 105 6469 0.103 ng 99 79) 1,3,5-Trimethylbenzene 17.83 105 5745 0.105 ng 98 80) alpha-Methylstyrene 17.99 118 2290 0.081 ng 93 81) 2-Ethyltoluene 18.03 105 6473 0.098 ng 96 82) 1,2,4-Trimethylbenzene 18.26 105 5460 0.100 ng 96 83) n-Decane 18.38 57 3579 0.118 ng 91 84) Benzyl Chloride 18.40 91 3854 0.087 ng 95 85) 1,3-Dichlorobenzene 18.42 146 3083 0.095 ng 93 86) 1,4-Dichlorobenzene 18.50 146 2934 0.086 ng 97 87) sec-Butylbenzene 18.55 105 7448 0.103 ng 95 88) 4-Isopropyltoluene (p-... 18.72 119 7535 0.111 ng 99 89) 1,2,3-Trimethylbenzene 18.71 105 6123 0.108 ng 97 90) 1,2-Dichlorobenzene 18.85 146 2909 0.093 ng 98 91) d-Limonene 18.87 68 2206 0.109 ng 96 92) 1,2-Dibromo-3-Chloropr... 19.31 157 783 0.069 ng # 70 93) n-Undecane 19.71 57 3373 0.106 ng 96 94) 1,2,4-Trichlorobenzene 20.67 180 1772 0.075 ng # 86 95) Naphthalene 20.78 128 7574 0.094 ng 94 96) n-Dodecane 20.81 57 3214 0.106 ng 96 97) Hexachlorobutadiene 21.14 225 1104 0.068 ng 97 98) Cyclohexanone 16.11 55 2731 0.137 ng 96 99) tert-Butylbenzene 18.26 119 5273 0.100 ng 99 100) n-Butylbenzene 19.16 91 6408 0.113 ng 98 -------------------------------------------------------------------------- (#) = qualifier out of range (m) = manual integration (+) = signals summed

R9071315.M Tue Jul 14 10:42:39 2015 Page: 2

85 of 128




4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.000

50000

100000

150000

200000

250000

300000

350000

400000

450000

500000

550000

600000

650000

700000

750000

800000

850000

900000

950000

1000000

1050000

1100000

Time-->


Hex

achl

orob

utad

iene

,Tn-

Dod

ecan

e,T

Nap

htha

lene

,T1,

2,4-

Tric

hlor

oben

zene

,T

n-U

ndec

ane,

T1,

2-D

ibro

mo-

3-C

hlor

opro

pane

,Tn-

Buty

lben

zene

,Td-

Lim

onen

e,T

1,2-

Dic

hlor

oben

zene

,T4-

Isop

ropy

ltolu

ene

(p-C

ymen

e),T

1,2,

3-Tr

imet

hylb

enze

ne,T

sec-

Buty

lben

zene

,T1,

4-D

ichl

orob

enze

ne,T

1,3-

Dic

hlor

oben

zene

,TBe

nzyl

Chl

orid

e,T

n-D

ecan

e,T

1,2,

4-Tr

imet

hylb

enze

ne,T

tert-

Buty

lben

zene

,T2-

Ethy

ltolu

ene,

Tal

pha-

Met

hyls

tyre

ne,T

1,3,

5-Tr

imet

hylb

enze

ne,T

4-Et

hylto

luen

e,T

3-Et

hylto

luen

e,T

n-Pr

opyl

benz

ene,

Tal

pha-

Pine

ne,T

Cum

ene,

TBr

omof

luor

oben

zene

(SS3

),Sn-

Non

ane,

To-

Xyle

ne,T

1,1,

2,2-

Tetra

chlo

roet

hane

,TSt

yren

e,T

Cyc

lohe

xano

ne,T

Brom

ofor

m,T

m- &

p-X

ylen

es,T

Ethy

lben

zene

,TC

hlor

oben

zene

,TC

hlor

oben

zene

-d5

(IS3)

,IR

Tetra

chlo

roet

hene

,Tn-

Oct

ane,

Tn-

Buty

l Ace

tate

,T1,

2-D

ibro

moe

than

e,T

Dib

rom

ochl

orom

etha

ne,T

2-H

exan

one,

TTo

luen

e,T

Tolu

ene-

d8 (S

S2),S

1,1,

2-Tr

ichl

oroe

than

e,T

trans

-1,3

-Dic

hlor

opro

pene

,T

4-M

ethy

l-2-p

enta

none

,Tci

s-1,

3-D

ichl

orop

rope

ne,T

n-H

epta

ne,T

Met

hyl M

etha

cryl

ate,

T2,

2,4-

Trim

ethy

lpen

tane

(Iso

octa

ne),T

1,4-

Dio

xane

,TTr

ichl

oroe

then

e,T

Brom

odic

hlor

omet

hane

,T1,

2-D

ichl

orop

ropa

ne,T

tert-

Am

yl M

ethy

l Eth

er,T

1,4-

Difl

uoro

benz

ene

(IS2)

,IRC

yclo

hexa

ne,T

Car

bon

Tetra

chlo

ride,

TBe

nzen

e,T

1-Bu

tano

l,TIs

opro

pyl A

ceta

te,T

1,1,

1-Tr

ichl

oroe

than

e,T

1,2-

Dic

hlor

oeth

ane,

T1,

2-D

ichl

oroe

than

e-d4

(SS1

),SEt

hyl t

ert-B

utyl

Eth

er,T

Tetra

hydr

ofur

an (T

HF)

,T

Chl

orof

orm

,TD

iisop

ropy

l Eth

er,T

Ethy

l Ace

tate

,Tn-

Hex

ane,

TBr

omoc

hlor

omet

hane

(IS1

),IR

cis-

1,2-

Dic

hlor

oeth

ene,

T2-

Buta

none

(MEK

),TVi

nyl A

ceta

te,T

Met

hyl t

ert-B

utyl

Eth

er,T

1,1-

Dic

hlor

oeth

ane,

Ttra

ns-1

,2-D

ichl

oroe

then

e,T

Tric

hlor

otrif

luor

oeth

ane,

TC

arbo

n D

isul

fide,

T3-

Chl

oro-

1-pr

open

e (A

llyl C

hlor

ide)

,TM

ethy

lene

Chl

orid

e,T

2-M

ethy

l-2-P

ropa

nol (

tert-

Buty

l Alc

ohol

,T1,

1-D

ichl

oroe

then

e,T

Acry

loni

trile

,T2-

Prop

anol

(Iso

prop

anol

),TTr

ichl

orof

luor

omet

hane

,TAc

eton

e,T

Acro

lein

,TAc

eton

itrile

,TEt

hano

l,TC

hlor

oeth

ane,

TBr

omom

etha

ne,T

1,3-

Buta

dien

e,T

Viny

l Chl

orid

e,T

1,2-

Dic

hlor

o-1,

1,2,

2-te

traflu

oroe

than

e ,T

Chl

orom

etha

ne,T

Dic

hlor

odifl

uoro

met

hane

(CFC

12)

,TPr

open

e,T

R9071315.M Tue Jul 14 10:42:40 2015 Page: 3

86 of 128

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_07\13\07131515.D Acq On : 13 Jul 2015 19:49 Operator: SC Sample : 0.20ng TO-15 ICAL STD Misc : S29-07071501/S29-07111506 (8/9) ALS Vial : 4 Sample Multiplier: 1 Quant Time: Jul 14 10:40:22 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:34:59 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 1) Bromochloromethane (IS1) 8.98 130 124487 12.500 ng -0.02 37) 1,4-Difluorobenzene (IS2) 10.96 114 657964 12.500 ng -0.02 56) Chlorobenzene-d5 (IS3) 15.31 82 297869 12.500 ng 0.00 System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.76 65 258012 16.362 ng -0.02 Spiked Amount 12.500 Recovery = 130.88% 57) Toluene-d8 (SS2) 13.40 98 678900 12.447 ng 0.00 Spiked Amount 12.500 Recovery = 99.60% 73) Bromofluorobenzene (SS3) 16.92 174 205707 9.279 ng 0.00 Spiked Amount 12.500 Recovery = 74.24% Target Compounds Qvalue 2) Propene 3.79 42 4434 0.344 ng 96 3) Dichlorodifluoromethan... 3.88 85 7568 0.288 ng # 97 4) Chloromethane 4.08 50 6272 0.341 ng 100 5) 1,2-Dichloro-1,1,2,2-t... 4.23 135 3118 0.235 ng 95 6) Vinyl Chloride 4.35 62 5064 0.294 ng 100 7) 1,3-Butadiene 4.52 54 3999 0.312 ng 93 8) Bromomethane 4.83 94 3037 0.267 ng 99 9) Chloroethane 5.04 64 2690 0.298 ng 99 10) Ethanol 5.21 45 16319 1.869 ng 98 11) Acetonitrile 5.43 41 8367 0.336 ng 88 12) Acrolein 5.57 56 2557 0.302 ng 92 13) Acetone 5.71 58 15501 1.691 ng 97 14) Trichlorofluoromethane 5.89 101 5881 0.263 ng 97 15) 2-Propanol (Isopropanol) 6.03 45 20595 0.686 ng 82 16) Acrylonitrile 6.23 53 4919 0.317 ng 99 17) 1,1-Dichloroethene 6.58 96 3116 0.270 ng 99 18) 2-Methyl-2-Propanol (t... 6.69 59 18937 0.656 ng 97 19) Methylene Chloride 6.71 84 5176 0.403 ng 97 20) 3-Chloro-1-propene (Al... 6.84 41 5945 0.370 ng 95 21) Trichlorotrifluoroethane 7.03 151 2447 0.227 ng 97 22) Carbon Disulfide 7.01 76 12823 0.243 ng 99 23) trans-1,2-Dichloroethene 7.73 61 4886 0.294 ng 94 24) 1,1-Dichloroethane 7.94 63 6631 0.297 ng 99 25) Methyl tert-Butyl Ether 8.05 73 10342 0.311 ng 99 26) Vinyl Acetate 8.13 86 3130 1.214 ng # 77 27) 2-Butanone (MEK) 8.39 72 2243 0.293 ng # 75 28) cis-1,2-Dichloroethene 8.82 61 4991 0.307 ng 99 29) Diisopropyl Ether 9.08 87 3296 0.329 ng # 65 30) Ethyl Acetate 9.08 61 2718 0.694 ng 99 31) n-Hexane 9.08 57 6538 0.350 ng 98 32) Chloroform 9.12 83 6038 0.290 ng 100 34) Tetrahydrofuran (THF) 9.56 72 2285 0.291 ng # 83 35) Ethyl tert-Butyl Ether 9.63 87 3919 0.305 ng 95 36) 1,2-Dichloroethane 9.87 62 4662 0.311 ng 98 38) 1,1,1-Trichloroethane 10.14 97 4914 0.257 ng 99 39) Isopropyl Acetate 10.53 61 4637 0.623 ng # 93 40) 1-Butanol 10.56 56 8691 0.722 ng 97 41) Benzene 10.60 78 14275 0.288 ng 99 42) Carbon Tetrachloride 10.75 117 4315 0.262 ng 99 43) Cyclohexane 10.89 84 10211 0.544 ng 100 44) tert-Amyl Methyl Ether 11.22 73 9567 0.279 ng 97 45) 1,2-Dichloropropane 11.42 63 3890 0.305 ng 97 46) Bromodichloromethane 11.60 83 4605 0.278 ng 98 47) Trichloroethene 11.65 130 3463 0.248 ng 100 48) 1,4-Dioxane 11.67 88 2867 0.261 ng # 66 49) 2,2,4-Trimethylpentane... 11.72 57 15920 0.297 ng 99

R9071315.M Tue Jul 14 10:41:21 2015 Page: 1

87 of 128

simon.cao

Simon

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_07\13\07131515.D Acq On : 13 Jul 2015 19:49 Operator: SC Sample : 0.20ng TO-15 ICAL STD Misc : S29-07071501/S29-07111506 (8/9) ALS Vial : 4 Sample Multiplier: 1 Quant Time: Jul 14 10:40:22 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:34:59 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 50) Methyl Methacrylate 11.86 100 2239 0.479 ng # 82 51) n-Heptane 11.98 71 3522 0.303 ng 99 52) cis-1,3-Dichloropropene 12.52 75 5249 0.277 ng 98 53) 4-Methyl-2-pentanone 12.56 58 3688 0.344 ng 90 54) trans-1,3-Dichloropropene 13.03 75 4187 0.225 ng 96 55) 1,1,2-Trichloroethane 13.21 97 3125 0.252 ng 99 58) Toluene 13.50 91 13892 0.235 ng 97 59) 2-Hexanone 13.77 43 9548 0.351 ng 96 60) Dibromochloromethane 13.91 129 3294 0.218 ng 98 61) 1,2-Dibromoethane 14.17 107 3438 0.231 ng 97 62) n-Butyl Acetate 14.41 43 10685 0.343 ng 95 63) n-Octane 14.52 57 3087 0.266 ng 97 64) Tetrachloroethene 14.66 166 3113 0.180 ng 97 65) Chlorobenzene 15.36 112 8490 0.222 ng 99 66) Ethylbenzene 15.76 91 14816 0.231 ng 100 67) m- & p-Xylenes 15.95 91 23153 0.451 ng 99 68) Bromoform 16.02 173 2459 0.180 ng 96 69) Styrene 16.33 104 7943 0.209 ng 97 70) o-Xylene 16.45 91 11509 0.219 ng 99 71) n-Nonane 16.69 43 8342 0.311 ng 94 72) 1,1,2,2-Tetrachloroethane 16.43 83 5650 0.216 ng 98 74) Cumene 17.07 105 14339 0.211 ng 100 75) alpha-Pinene 17.48 93 7261 0.226 ng # 62 76) n-Propylbenzene 17.60 91 18347 0.224 ng 98 77) 3-Ethyltoluene 17.71 105 13860 0.218 ng 96 78) 4-Ethyltoluene 17.75 105 13648 0.223 ng 99 79) 1,3,5-Trimethylbenzene 17.83 105 11710 0.219 ng 99 80) alpha-Methylstyrene 17.99 118 5653 0.205 ng 89 81) 2-Ethyltoluene 18.03 105 13928 0.215 ng 96 82) 1,2,4-Trimethylbenzene 18.26 105 11453 0.214 ng 95 83) n-Decane 18.38 57 7856 0.266 ng 98 84) Benzyl Chloride 18.40 91 8112 0.187 ng 94 85) 1,3-Dichlorobenzene 18.42 146 6293 0.198 ng 99 86) 1,4-Dichlorobenzene 18.49 146 6157 0.184 ng 98 87) sec-Butylbenzene 18.55 105 15911 0.226 ng 98 88) 4-Isopropyltoluene (p-... 18.72 119 14118 0.214 ng 99 89) 1,2,3-Trimethylbenzene 18.71 105 11853 0.215 ng 98 90) 1,2-Dichlorobenzene 18.85 146 6238 0.203 ng 99 91) d-Limonene 18.87 68 4831 0.245 ng 99 92) 1,2-Dibromo-3-Chloropr... 19.31 157 1797 0.161 ng # 77 93) n-Undecane 19.72 57 7699 0.249 ng 98 94) 1,2,4-Trichlorobenzene 20.66 180 3568 0.154 ng 98 95) Naphthalene 20.78 128 13120 0.166 ng 95 96) n-Dodecane 20.81 57 7506 0.254 ng 98 97) Hexachlorobutadiene 21.14 225 2584 0.164 ng 100 98) Cyclohexanone 16.11 55 5821 0.300 ng 96 99) tert-Butylbenzene 18.26 119 10932 0.212 ng 100 100) n-Butylbenzene 19.16 91 12860 0.232 ng 99 -------------------------------------------------------------------------- (#) = qualifier out of range (m) = manual integration (+) = signals summed

R9071315.M Tue Jul 14 10:41:21 2015 Page: 2

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4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.000

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R9071315.M Tue Jul 14 10:41:23 2015 Page: 3

89 of 128

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_07\13\07131516.D Acq On : 13 Jul 2015 20:23 Operator: SC Sample : 0.40ng TO-15 ICAL STD Misc : S29-07071501/S29-07111506 (8/9) ALS Vial : 4 Sample Multiplier: 1 Quant Time: Jul 14 10:39:09 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:34:59 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 1) Bromochloromethane (IS1) 8.97 130 118393 12.500 ng -0.03 37) 1,4-Difluorobenzene (IS2) 10.96 114 621109 12.500 ng -0.02 56) Chlorobenzene-d5 (IS3) 15.31 82 286296 12.500 ng 0.00 System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.76 65 247613 16.511 ng -0.02 Spiked Amount 12.500 Recovery = 132.08% 57) Toluene-d8 (SS2) 13.40 98 644962 12.303 ng 0.00 Spiked Amount 12.500 Recovery = 98.40% 73) Bromofluorobenzene (SS3) 16.92 174 200720 9.420 ng 0.00 Spiked Amount 12.500 Recovery = 75.36% Target Compounds Qvalue 2) Propene 3.78 42 8350 0.681 ng 97 3) Dichlorodifluoromethan... 3.88 85 13850 0.555 ng 99 4) Chloromethane 4.08 50 11518 0.658 ng 97 5) 1,2-Dichloro-1,1,2,2-t... 4.23 135 5452 0.432 ng 100 6) Vinyl Chloride 4.34 62 9288 0.567 ng 98 7) 1,3-Butadiene 4.52 54 7477 0.614 ng 92 8) Bromomethane 4.82 94 5035 0.466 ng 97 9) Chloroethane 5.03 64 4870 0.567 ng 97 10) Ethanol 5.20 45 28825 3.472 ng 99 11) Acetonitrile 5.43 41 15210 0.641 ng 95 12) Acrolein 5.56 56 4397 0.547 ng 99 13) Acetone 5.70 58 26762 3.070 ng 95 14) Trichlorofluoromethane 5.89 101 10562 0.497 ng 100 15) 2-Propanol (Isopropanol) 6.00 45 39691 1.390 ng 92 16) Acrylonitrile 6.21 53 8908 0.604 ng 96 17) 1,1-Dichloroethene 6.57 96 5899 0.537 ng 99 18) 2-Methyl-2-Propanol (t... 6.67 59 34987 1.274 ng 96 19) Methylene Chloride 6.70 84 7742 0.633 ng 96 20) 3-Chloro-1-propene (Al... 6.84 41 11168 0.731 ng 93 21) Trichlorotrifluoroethane 7.03 151 4735 0.462 ng 97 22) Carbon Disulfide 7.00 76 22884 0.455 ng 99 23) trans-1,2-Dichloroethene 7.73 61 9725 0.616 ng 99 24) 1,1-Dichloroethane 7.94 63 12499 0.589 ng 100 25) Methyl tert-Butyl Ether 8.04 73 19034 0.603 ng 97 26) Vinyl Acetate 8.12 86 6250 2.549 ng # 77 27) 2-Butanone (MEK) 8.39 72 4286 0.589 ng # 82 28) cis-1,2-Dichloroethene 8.81 61 9279 0.601 ng 99 29) Diisopropyl Ether 9.08 87 6063 0.636 ng # 65 30) Ethyl Acetate 9.07 61 5188 1.392 ng 100 31) n-Hexane 9.07 57 11761 0.661 ng 98 32) Chloroform 9.12 83 11457 0.578 ng 100 34) Tetrahydrofuran (THF) 9.55 72 4342 0.582 ng # 90 35) Ethyl tert-Butyl Ether 9.63 87 7064 0.578 ng 97 36) 1,2-Dichloroethane 9.87 62 8542 0.599 ng 99 38) 1,1,1-Trichloroethane 10.14 97 9193 0.509 ng 98 39) Isopropyl Acetate 10.53 61 8730 1.243 ng 95 40) 1-Butanol 10.55 56 15548 1.369 ng 93 41) Benzene 10.60 78 26353 0.563 ng 98 42) Carbon Tetrachloride 10.75 117 7776 0.499 ng 99 43) Cyclohexane 10.89 84 19043 1.076 ng 98 44) tert-Amyl Methyl Ether 11.22 73 17889 0.552 ng 97 45) 1,2-Dichloropropane 11.42 63 7100 0.589 ng 95 46) Bromodichloromethane 11.60 83 8539 0.546 ng 98 47) Trichloroethene 11.66 130 5992 0.455 ng 96 48) 1,4-Dioxane 11.65 88 5081 0.489 ng 97 49) 2,2,4-Trimethylpentane... 11.72 57 30150 0.595 ng 98

R9071315.M Tue Jul 14 10:40:05 2015 Page: 1

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simon.cao

Simon

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_07\13\07131516.D Acq On : 13 Jul 2015 20:23 Operator: SC Sample : 0.40ng TO-15 ICAL STD Misc : S29-07071501/S29-07111506 (8/9) ALS Vial : 4 Sample Multiplier: 1 Quant Time: Jul 14 10:39:09 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:34:59 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 50) Methyl Methacrylate 11.86 100 4343 0.984 ng 91 51) n-Heptane 11.98 71 6436 0.587 ng 98 52) cis-1,3-Dichloropropene 12.51 75 10160 0.568 ng 99 53) 4-Methyl-2-pentanone 12.55 58 6870 0.679 ng 96 54) trans-1,3-Dichloropropene 13.03 75 8602 0.490 ng 98 55) 1,1,2-Trichloroethane 13.21 97 5827 0.497 ng 100 58) Toluene 13.50 91 24830 0.437 ng 100 59) 2-Hexanone 13.76 43 17382 0.664 ng 98 60) Dibromochloromethane 13.91 129 6072 0.418 ng 99 61) 1,2-Dibromoethane 14.17 107 6697 0.468 ng 99 62) n-Butyl Acetate 14.40 43 19414 0.648 ng 98 63) n-Octane 14.52 57 6104 0.546 ng 99 64) Tetrachloroethene 14.66 166 5780 0.347 ng 99 65) Chlorobenzene 15.36 112 15573 0.423 ng 99 66) Ethylbenzene 15.76 91 27609 0.449 ng 100 67) m- & p-Xylenes 15.96 91 43806 0.887 ng 98 68) Bromoform 16.01 173 4543 0.345 ng 99 69) Styrene 16.33 104 15228 0.418 ng 100 70) o-Xylene 16.45 91 22077 0.438 ng 100 71) n-Nonane 16.69 43 15075 0.585 ng 98 72) 1,1,2,2-Tetrachloroethane 16.43 83 11146 0.442 ng 100 74) Cumene 17.07 105 26685 0.409 ng 100 75) alpha-Pinene 17.48 93 13654 0.443 ng 69 76) n-Propylbenzene 17.60 91 33925 0.431 ng 99 77) 3-Ethyltoluene 17.71 105 26194 0.430 ng 100 78) 4-Ethyltoluene 17.75 105 25783 0.439 ng 97 79) 1,3,5-Trimethylbenzene 17.83 105 22188 0.431 ng 99 80) alpha-Methylstyrene 17.99 118 10493 0.396 ng 88 81) 2-Ethyltoluene 18.03 105 25674 0.413 ng 100 82) 1,2,4-Trimethylbenzene 18.26 105 21380 0.416 ng 97 83) n-Decane 18.38 57 14723 0.519 ng 99 84) Benzyl Chloride 18.39 91 16070 0.385 ng 97 85) 1,3-Dichlorobenzene 18.42 146 11624 0.381 ng 97 86) 1,4-Dichlorobenzene 18.49 146 12009 0.374 ng 97 87) sec-Butylbenzene 18.54 105 30126 0.445 ng 98 88) 4-Isopropyltoluene (p-... 18.72 119 25584 0.404 ng 98 89) 1,2,3-Trimethylbenzene 18.71 105 22109 0.417 ng 100 90) 1,2-Dichlorobenzene 18.85 146 11331 0.384 ng 99 91) d-Limonene 18.87 68 9517 0.502 ng 100 92) 1,2-Dibromo-3-Chloropr... 19.31 157 3569 0.334 ng # 77 93) n-Undecane 19.71 57 14863 0.500 ng 97 94) 1,2,4-Trichlorobenzene 20.66 180 6844 0.307 ng 98 95) Naphthalene 20.78 128 23056 0.304 ng 98 96) n-Dodecane 20.81 57 14383 0.507 ng 98 97) Hexachlorobutadiene 21.14 225 4621 0.306 ng 100 98) Cyclohexanone 16.11 55 10429 0.560 ng 98 99) tert-Butylbenzene 18.26 119 21109 0.425 ng 100 100) n-Butylbenzene 19.16 91 25054 0.470 ng 98 -------------------------------------------------------------------------- (#) = qualifier out of range (m) = manual integration (+) = signals summed

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4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.000

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900000

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1000000

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Time-->


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m- &

p-X

ylen

es,T

Ethy

lben

zene

,TC

hlor

oben

zene

,TC

hlor

oben

zene

-d5

(IS3)

,IR

Tetra

chlo

roet

hene

,Tn-

Oct

ane,

Tn-

Buty

l Ace

tate

,T1,

2-D

ibro

moe

than

e,T

Dib

rom

ochl

orom

etha

ne,T

2-H

exan

one,

TTo

luen

e,T

Tolu

ene-

d8 (S

S2),S

1,1,

2-Tr

ichl

oroe

than

e,T

trans

-1,3

-Dic

hlor

opro

pene

,T

4-M

ethy

l-2-p

enta

none

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s-1,

3-D

ichl

orop

rope

ne,T

n-H

epta

ne,T

Met

hyl M

etha

cryl

ate,

T2,

2,4-

Trim

ethy

lpen

tane

(Iso

octa

ne),T

Tric

hlor

oeth

ene,

T1,

4-D

ioxa

ne,T

Brom

odic

hlor

omet

hane

,T1,

2-D

ichl

orop

ropa

ne,T

tert-

Am

yl M

ethy

l Eth

er,T

1,4-

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uoro

benz

ene

(IS2)

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yclo

hexa

ne,T

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bon

Tetra

chlo

ride,

TBe

nzen

e,T

1-Bu

tano

l,TIs

opro

pyl A

ceta

te,T

1,1,

1-Tr

ichl

oroe

than

e,T

1,2-

Dic

hlor

oeth

ane,

T1,

2-D

ichl

oroe

than

e-d4

(SS1

),SEt

hyl t

ert-B

utyl

Eth

er,T

Tetra

hydr

ofur

an (T

HF)

,T

Chl

orof

orm

,TDiis

opro

pyl E

ther

,TEt

hyl A

ceta

te,T

n-H

exan

e,T

Brom

ochl

orom

etha

ne (I

S1),I

Rci

s-1,

2-D

ichl

oroe

then

e,T

2-Bu

tano

ne (M

EK),T

Viny

l Ace

tate

,TM

ethy

l ter

t-But

yl E

ther

,T1,

1-D

ichl

oroe

than

e,T

trans

-1,2

-Dic

hlor

oeth

ene,

T

Tric

hlor

otrif

luor

oeth

ane,

TC

arbo

n D

isul

fide,

T3-

Chl

oro-

1-pr

open

e (A

llyl C

hlor

ide)

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lene

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orid

e,T

2-M

ethy

l-2-P

ropa

nol (

tert-

Buty

l Alc

ohol

,T1,

1-D

ichl

oroe

then

e,T

Acry

loni

trile

,T2-

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anol

(Iso

prop

anol

),TTr

ichl

orof

luor

omet

hane

,TAc

eton

e,T

Acro

lein

,TAc

eton

itrile

,TEt

hano

l,TC

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oeth

ane,

TBr

omom

etha

ne,T

1,3-

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dien

e,T

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l Chl

orid

e,T

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hlor

o-1,

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2-te

traflu

oroe

than

e ,T

Chl

orom

etha

ne,T

Dic

hlor

odifl

uoro

met

hane

(CFC

12)

,TPr

open

e,T

R9071315.M Tue Jul 14 10:40:07 2015 Page: 3

92 of 128

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_07\13\07131517.D Acq On : 13 Jul 2015 20:58 Operator: SC Sample : 1.0ng TO-15 ICAL STD Misc : S29-07071501/S29-07111505 (8/9) ALS Vial : 5 Sample Multiplier: 1 Quant Time: Jul 14 10:37:37 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:34:59 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 1) Bromochloromethane (IS1) 8.97 130 117797 12.500 ng -0.03 37) 1,4-Difluorobenzene (IS2) 10.96 114 620365 12.500 ng -0.02 56) Chlorobenzene-d5 (IS3) 15.31 82 284852 12.500 ng 0.00 System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.76 65 246760 16.538 ng -0.02 Spiked Amount 12.500 Recovery = 132.32% 57) Toluene-d8 (SS2) 13.40 98 642748 12.323 ng 0.00 Spiked Amount 12.500 Recovery = 98.56% 73) Bromofluorobenzene (SS3) 16.92 174 201161 9.489 ng 0.00 Spiked Amount 12.500 Recovery = 75.92% Target Compounds Qvalue 2) Propene 3.76 42 21028 1.724 ng 99 3) Dichlorodifluoromethan... 3.86 85 36347 1.463 ng 99 4) Chloromethane 4.06 50 29846 1.714 ng 99 5) 1,2-Dichloro-1,1,2,2-t... 4.22 135 14471 1.153 ng 100 6) Vinyl Chloride 4.33 62 24500 1.503 ng 100 7) 1,3-Butadiene 4.50 54 19748 1.631 ng 97 8) Bromomethane 4.80 94 14320 1.333 ng 96 9) Chloroethane 5.02 64 13141 1.538 ng 100 10) Ethanol 5.19 45 75327 9.119 ng 99 11) Acetonitrile 5.41 41 39058 1.656 ng 99 12) Acrolein 5.55 56 11528 1.441 ng 96 13) Acetone 5.68 58 70891 8.172 ng 97 14) Trichlorofluoromethane 5.88 101 27791 1.314 ng 99 15) 2-Propanol (Isopropanol) 5.99 45 100980 3.555 ng 92 16) Acrylonitrile 6.20 53 24702 1.682 ng 99 17) 1,1-Dichloroethene 6.57 96 15103 1.382 ng 98 18) 2-Methyl-2-Propanol (t... 6.64 59 90085 3.297 ng 92 19) Methylene Chloride 6.70 84 18501 1.521 ng 98 20) 3-Chloro-1-propene (Al... 6.83 41 29321 1.929 ng 97 21) Trichlorotrifluoroethane 7.03 151 12132 1.189 ng 99 22) Carbon Disulfide 6.99 76 62762 1.256 ng 100 23) trans-1,2-Dichloroethene 7.72 61 26163 1.665 ng 99 24) 1,1-Dichloroethane 7.94 63 32315 1.531 ng 99 25) Methyl tert-Butyl Ether 8.02 73 49156 1.564 ng 100 26) Vinyl Acetate 8.12 86 17375 7.122 ng # 86 27) 2-Butanone (MEK) 8.36 72 11170 1.542 ng # 92 28) cis-1,2-Dichloroethene 8.81 61 24926 1.623 ng 99 29) Diisopropyl Ether 9.06 87 16174 1.704 ng # 62 30) Ethyl Acetate 9.06 61 13352 3.601 ng 97 31) n-Hexane 9.07 57 31323 1.770 ng 99 32) Chloroform 9.12 83 28523 1.446 ng 98 34) Tetrahydrofuran (THF) 9.53 72 11201 1.510 ng 92 35) Ethyl tert-Butyl Ether 9.62 87 18661 1.534 ng 99 36) 1,2-Dichloroethane 9.87 62 22797 1.606 ng 100 38) 1,1,1-Trichloroethane 10.14 97 24614 1.366 ng 98 39) Isopropyl Acetate 10.52 61 23000 3.278 ng 96 40) 1-Butanol 10.54 56 38789 3.419 ng 93 41) Benzene 10.60 78 66429 1.421 ng 99 42) Carbon Tetrachloride 10.75 117 20996 1.350 ng 99 43) Cyclohexane 10.88 84 48705 2.755 ng 99 44) tert-Amyl Methyl Ether 11.21 73 46650 1.441 ng 97 45) 1,2-Dichloropropane 11.42 63 18906 1.570 ng 99 46) Bromodichloromethane 11.60 83 23094 1.478 ng 98 47) Trichloroethene 11.65 130 15746 1.197 ng 98 48) 1,4-Dioxane 11.65 88 12999 1.253 ng 100 49) 2,2,4-Trimethylpentane... 11.72 57 78000 1.541 ng 99

R9071315.M Tue Jul 14 10:38:50 2015 Page: 1

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simon.cao

Simon

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_07\13\07131517.D Acq On : 13 Jul 2015 20:58 Operator: SC Sample : 1.0ng TO-15 ICAL STD Misc : S29-07071501/S29-07111505 (8/9) ALS Vial : 5 Sample Multiplier: 1 Quant Time: Jul 14 10:37:37 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:34:59 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 50) Methyl Methacrylate 11.85 100 11791 2.675 ng 98 51) n-Heptane 11.98 71 17470 1.596 ng 98 52) cis-1,3-Dichloropropene 12.51 75 27727 1.552 ng 100 53) 4-Methyl-2-pentanone 12.55 58 17793 1.761 ng 97 54) trans-1,3-Dichloropropene 13.03 75 23427 1.336 ng 98 55) 1,1,2-Trichloroethane 13.20 97 15813 1.350 ng 100 58) Toluene 13.50 91 65237 1.154 ng 100 59) 2-Hexanone 13.76 43 46053 1.768 ng 99 60) Dibromochloromethane 13.91 129 16844 1.166 ng 98 61) 1,2-Dibromoethane 14.17 107 17356 1.219 ng 99 62) n-Butyl Acetate 14.40 43 50181 1.683 ng 99 63) n-Octane 14.52 57 16224 1.459 ng 97 64) Tetrachloroethene 14.66 166 15247 0.920 ng 99 65) Chlorobenzene 15.36 112 40786 1.113 ng 100 66) Ethylbenzene 15.76 91 73721 1.204 ng 99 67) m- & p-Xylenes 15.95 91 118140 2.405 ng 99 68) Bromoform 16.01 173 12927 0.987 ng 100 69) Styrene 16.33 104 42024 1.158 ng 100 70) o-Xylene 16.45 91 59685 1.190 ng 99 71) n-Nonane 16.69 43 41549 1.620 ng 96 72) 1,1,2,2-Tetrachloroethane 16.42 83 30024 1.198 ng 99 74) Cumene 17.07 105 71746 1.106 ng 99 75) alpha-Pinene 17.48 93 34881 1.137 ng 92 76) n-Propylbenzene 17.60 91 93434 1.193 ng 98 77) 3-Ethyltoluene 17.71 105 71448 1.177 ng 99 78) 4-Ethyltoluene 17.75 105 68943 1.179 ng 100 79) 1,3,5-Trimethylbenzene 17.83 105 58537 1.142 ng 99 80) alpha-Methylstyrene 17.99 118 27232 1.034 ng 90 81) 2-Ethyltoluene 18.03 105 69930 1.131 ng 99 82) 1,2,4-Trimethylbenzene 18.26 105 59494 1.163 ng 99 83) n-Decane 18.38 57 40249 1.425 ng 98 84) Benzyl Chloride 18.39 91 48144 1.160 ng 99 85) 1,3-Dichlorobenzene 18.42 146 32723 1.078 ng 99 86) 1,4-Dichlorobenzene 18.49 146 33256 1.040 ng 99 87) sec-Butylbenzene 18.55 105 82454 1.225 ng 99 88) 4-Isopropyltoluene (p-... 18.72 119 70908 1.124 ng 99 89) 1,2,3-Trimethylbenzene 18.71 105 61984 1.175 ng 100 90) 1,2-Dichlorobenzene 18.85 146 31955 1.090 ng 99 91) d-Limonene 18.87 68 23634 1.252 ng 98 92) 1,2-Dibromo-3-Chloropr... 19.31 157 11112 1.044 ng 89 93) n-Undecane 19.71 57 40268 1.361 ng 99 94) 1,2,4-Trichlorobenzene 20.66 180 21668 0.978 ng 99 95) Naphthalene 20.78 128 80155 1.063 ng 99 96) n-Dodecane 20.81 57 41414 1.466 ng 99 97) Hexachlorobutadiene 21.14 225 12889 0.857 ng 99 98) Cyclohexanone 16.11 55 27035 1.459 ng 99 99) tert-Butylbenzene 18.26 119 56019 1.135 ng 99 100) n-Butylbenzene 19.16 91 71653 1.350 ng 98 -------------------------------------------------------------------------- (#) = qualifier out of range (m) = manual integration (+) = signals summed

R9071315.M Tue Jul 14 10:38:50 2015 Page: 2

94 of 128




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Hex

achl

orob

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,Tn-

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Buty

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Tal

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Tal

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m,T

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Ethy

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hlor

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(IS3)

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hene

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ane,

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Buty

l Ace

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ochl

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one,

TTo

luen

e,T

Tolu

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d8 (S

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1,1,

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ichl

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than

e,T

trans

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hlor

opro

pene

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4-M

ethy

l-2-p

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none

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s-1,

3-D

ichl

orop

rope

ne,T

n-H

epta

ne,T

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hyl M

etha

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octa

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hlor

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ne,T

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odic

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yl M

ethy

l Eth

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uoro

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ene

(IS2)

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bon

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chlo

ride,

TBe

nzen

e,T

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S1),S

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l ter

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yl E

ther

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drof

uran

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F),T

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orm

,Tn-

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ane,

TD

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l Ace

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omoc

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omet

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ene,

T

2-Bu

tano

ne (M

EK),T

Viny

l Ace

tate

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ethy

l ter

t-But

yl E

ther

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1-D

ichl

oroe

than

e,T

trans

-1,2

-Dic

hlor

oeth

ene,

T

Tric

hlor

otrif

luor

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TC

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n D

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e (A

llyl C

hlor

ide)

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ethy

lene

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orid

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ethy

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nol (

tert-

Buty

l Alc

ohol

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ichl

oroe

then

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loni

trile

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lein

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R9071315.M Tue Jul 14 10:38:51 2015 Page: 3

95 of 128

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_07\13\07131518.D Acq On : 13 Jul 2015 21:32 Operator: SC Sample : 5.0ng TO-15 ICAL STD Misc : S29-07071501/S29-07111505 (8/9) ALS Vial : 5 Sample Multiplier: 1 Quant Time: Jul 14 10:35:16 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:34:59 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 1) Bromochloromethane (IS1) 8.98 130 114594 12.500 ng -0.02 37) 1,4-Difluorobenzene (IS2) 10.96 114 606138 12.500 ng -0.01 56) Chlorobenzene-d5 (IS3) 15.31 82 283127 12.500 ng 0.00 System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.77 65 243519 16.777 ng -0.02 Spiked Amount 12.500 Recovery = 134.24% 57) Toluene-d8 (SS2) 13.40 98 633811 12.226 ng 0.00 Spiked Amount 12.500 Recovery = 97.84% 73) Bromofluorobenzene (SS3) 16.92 174 205780 9.766 ng 0.00 Spiked Amount 12.500 Recovery = 78.16% Target Compounds Qvalue 2) Propene 3.75 42 92697 7.813 ng 99 3) Dichlorodifluoromethan... 3.86 85 161754 6.693 ng 99 4) Chloromethane 4.05 50 127262 7.513 ng 99 5) 1,2-Dichloro-1,1,2,2-t... 4.21 135 65537 5.366 ng 99 6) Vinyl Chloride 4.33 62 110348 6.957 ng 98 7) 1,3-Butadiene 4.50 54 89362 7.586 ng 96 8) Bromomethane 4.80 94 58207 5.569 ng 98 9) Chloroethane 5.01 64 48677 5.856 ng 100 10) Ethanol 5.20 45 328013 40.819 ng 99 11) Acetonitrile 5.41 41 171713 7.482 ng 99 12) Acrolein 5.54 56 53160 6.831 ng 100 13) Acetone 5.68 58 310086 36.745 ng 97 14) Trichlorofluoromethane 5.87 101 122479 5.951 ng 100 15) 2-Propanol (Isopropanol) 6.00 45 455398 16.482 ng 99 16) Acrylonitrile 6.21 53 111902 7.833 ng 99 17) 1,1-Dichloroethene 6.56 96 66330 6.241 ng 97 18) 2-Methyl-2-Propanol (t... 6.64 59 409969 15.423 ng 99 19) Methylene Chloride 6.70 84 73241 6.191 ng 97 20) 3-Chloro-1-propene (Al... 6.84 41 133631 9.037 ng 98 21) Trichlorotrifluoroethane 7.03 151 51807 5.221 ng 98 22) Carbon Disulfide 6.99 76 283548 5.831 ng 100 23) trans-1,2-Dichloroethene 7.73 61 116157 7.598 ng 98 24) 1,1-Dichloroethane 7.94 63 143541 6.992 ng 100 25) Methyl tert-Butyl Ether 8.02 73 223829 7.321 ng 99 26) Vinyl Acetate 8.12 86 86170 36.310 ng # 91 27) 2-Butanone (MEK) 8.36 72 50869 7.217 ng # 1 28) cis-1,2-Dichloroethene 8.82 61 110185 7.374 ng 98 29) Diisopropyl Ether 9.06 87 57529 6.230 ng # 95 30) Ethyl Acetate 9.06 61 60795 16.852 ng 98 31) n-Hexane 9.07 57 132843 7.715 ng 99 32) Chloroform 9.12 83 127932 6.668 ng 99 34) Tetrahydrofuran (THF) 9.52 72 47861 6.633 ng 98 35) Ethyl tert-Butyl Ether 9.62 87 82803 6.998 ng 98 36) 1,2-Dichloroethane 9.87 62 101770 7.368 ng 100 38) 1,1,1-Trichloroethane 10.14 97 108374 6.154 ng 99 39) Isopropyl Acetate 10.52 61 103129 15.044 ng # 94 40) 1-Butanol 10.53 56 183107 16.519 ng 97 41) Benzene 10.60 78 288888 6.324 ng 99 42) Carbon Tetrachloride 10.75 117 94288 6.203 ng 99 43) Cyclohexane 10.89 84 214875 12.438 ng 99 44) tert-Amyl Methyl Ether 11.21 73 216546 6.848 ng 99 45) 1,2-Dichloropropane 11.42 63 80861 6.872 ng 99 46) Bromodichloromethane 11.60 83 103730 6.793 ng 99 47) Trichloroethene 11.66 130 67433 5.246 ng 100 48) 1,4-Dioxane 11.64 88 58516 5.773 ng 100 49) 2,2,4-Trimethylpentane... 11.72 57 347016 7.018 ng 99

R9071315.M Tue Jul 14 10:36:21 2015 Page: 1

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simon.cao

Simon

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_07\13\07131518.D Acq On : 13 Jul 2015 21:32 Operator: SC Sample : 5.0ng TO-15 ICAL STD Misc : S29-07071501/S29-07111505 (8/9) ALS Vial : 5 Sample Multiplier: 1 Quant Time: Jul 14 10:35:16 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:34:59 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 50) Methyl Methacrylate 11.85 100 53771 12.487 ng 95 51) n-Heptane 11.98 71 75612 7.071 ng 100 52) cis-1,3-Dichloropropene 12.51 75 130745 7.492 ng 99 53) 4-Methyl-2-pentanone 12.55 58 78843 7.985 ng 95 54) trans-1,3-Dichloropropene 13.03 75 115165 6.721 ng 100 55) 1,1,2-Trichloroethane 13.21 97 70239 6.137 ng 100 58) Toluene 13.50 91 289128 5.148 ng 100 59) 2-Hexanone 13.75 43 216737 8.373 ng 98 60) Dibromochloromethane 13.91 129 79040 5.506 ng 98 61) 1,2-Dibromoethane 14.17 107 80530 5.689 ng 100 62) n-Butyl Acetate 14.39 43 239292 8.074 ng 98 63) n-Octane 14.52 57 70827 6.410 ng 98 64) Tetrachloroethene 14.66 166 66566 4.040 ng 100 65) Chlorobenzene 15.36 112 183105 5.029 ng 99 66) Ethylbenzene 15.76 91 334112 5.491 ng 99 67) m- & p-Xylenes 15.96 91 533928 10.934 ng 99 68) Bromoform 16.01 173 62227 4.780 ng 100 69) Styrene 16.33 104 198762 5.513 ng 99 70) o-Xylene 16.45 91 273140 5.477 ng 98 71) n-Nonane 16.69 43 189493 7.434 ng 97 72) 1,1,2,2-Tetrachloroethane 16.42 83 140900 5.655 ng 99 74) Cumene 17.07 105 328326 5.090 ng 99 75) alpha-Pinene 17.48 93 167918 5.509 ng 99 76) n-Propylbenzene 17.60 91 429680 5.521 ng 99 77) 3-Ethyltoluene 17.71 105 336854 5.585 ng 99 78) 4-Ethyltoluene 17.75 105 320883 5.521 ng 99 79) 1,3,5-Trimethylbenzene 17.83 105 274521 5.390 ng 99 80) alpha-Methylstyrene 17.99 118 131840 5.034 ng 99 81) 2-Ethyltoluene 18.03 105 330118 5.369 ng 99 82) 1,2,4-Trimethylbenzene 18.26 105 287350 5.652 ng 98 83) n-Decane 18.38 57 187294 6.671 ng 99 84) Benzyl Chloride 18.39 91 272254 6.599 ng 99 85) 1,3-Dichlorobenzene 18.42 146 154015 5.104 ng 100 86) 1,4-Dichlorobenzene 18.49 146 155837 4.904 ng 99 87) sec-Butylbenzene 18.55 105 388927 5.813 ng 99 88) 4-Isopropyltoluene (p-... 18.72 119 336752 5.371 ng 99 89) 1,2,3-Trimethylbenzene 18.71 105 301248 5.746 ng 99 90) 1,2-Dichlorobenzene 18.85 146 151054 5.182 ng 100 91) d-Limonene 18.87 68 116170 6.191 ng 99 92) 1,2-Dibromo-3-Chloropr... 19.31 157 56902 5.378 ng 93 93) n-Undecane 19.71 57 200585 6.820 ng 99 94) 1,2,4-Trichlorobenzene 20.66 180 112928 5.127 ng 100 95) Naphthalene 20.78 128 417419 5.570 ng 99 96) n-Dodecane 20.81 57 209544 7.462 ng 98 97) Hexachlorobutadiene 21.14 225 63964 4.280 ng 100 98) Cyclohexanone 16.10 55 126769 6.884 ng 98 99) tert-Butylbenzene 18.26 119 267828 5.458 ng 100 100) n-Butylbenzene 19.16 91 343825 6.516 ng 99 -------------------------------------------------------------------------- (#) = qualifier out of range (m) = manual integration (+) = signals summed

R9071315.M Tue Jul 14 10:36:21 2015 Page: 2

97 of 128




4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.000

50000

100000

150000

200000

250000

300000

350000

400000

450000

500000

550000

600000

650000

700000

750000

800000

850000

900000

950000

1000000

1050000

1100000

1150000

1200000

Time-->


Hex

achl

orob

utad

iene

,Tn-

Dod

ecan

e,T

Nap

htha

lene

,T1,

2,4-

Tric

hlor

oben

zene

,T

n-U

ndec

ane,

T1,

2-D

ibro

mo-

3-C

hlor

opro

pane

,Tn-

Buty

lben

zene

,Td-

Lim

onen

e,T

1,2-

Dic

hlor

oben

zene

,T4-

Isop

ropy

ltolu

ene

(p-C

ymen

e),T

1,2,

3-Tr

imet

hylb

enze

ne,T

sec-

Buty

lben

zene

,T1,

4-D

ichl

orob

enze

ne,T

1,3-

Dic

hlor

oben

zene

,TBe

nzyl

Chl

orid

e,Tn

-Dec

ane,

T1,

2,4-

Trim

ethy

lben

zene

,Tte

rt-Bu

tylb

enze

ne,T

2-Et

hylto

luen

e,T

alph

a-M

ethy

lsty

rene

,T1,

3,5-

Trim

ethy

lben

zene

,T4-

Ethy

ltolu

ene,

T3-

Ethy

ltolu

ene,

Tn-

Prop

ylbe

nzen

e,T

alph

a-Pi

nene

,TC

umen

e,T

Brom

oflu

orob

enze

ne (S

S3),S

n-N

onan

e,T

o-Xy

lene

,T1,

1,2,

2-Te

trach

loro

etha

ne,T

Styr

ene,

TC

yclo

hexa

none

,TBr

omof

orm

,Tm

- & p

-Xyl

enes

,TEt

hylb

enze

ne,T

Chl

orob

enze

ne,T

Chl

orob

enze

ne-d

5 (IS

3),IR

Tetra

chlo

roet

hene

,Tn-

Oct

ane,

Tn-

Buty

l Ace

tate

,T1,

2-D

ibro

moe

than

e,T

Dib

rom

ochl

orom

etha

ne,T2-H

exan

one,

TTo

luen

e,T

Tolu

ene-

d8 (S

S2),S

1,1,

2-Tr

ichl

oroe

than

e,T

trans

-1,3

-Dic

hlor

opro

pene

,T

4-M

ethy

l-2-p

enta

none

,Tci

s-1,

3-D

ichl

orop

rope

ne,T

n-H

epta

ne,T

Met

hyl M

etha

cryl

ate,

T2,

2,4-

Trim

ethy

lpen

tane

(Iso

octa

ne),T

Tric

hlor

oeth

ene,

T1,

4-D

ioxa

ne,T

Brom

odic

hlor

omet

hane

,T1,

2-D

ichl

orop

ropa

ne,T

tert-

Am

yl M

ethy

l Eth

er,T

1,4-

Difl

uoro

benz

ene

(IS2)

,IRC

yclo

hexa

ne,T

Car

bon

Tetra

chlo

ride,

TBe

nzen

e,T

1-Bu

tano

l,TIs

opro

pyl A

ceta

te,T

1,1,

1-Tr

ichl

oroe

than

e,T

1,2-

Dic

hlor

oeth

ane,

T1,

2-D

ichl

oroe

than

e-d4

(SS1

),SEt

hyl t

ert-B

utyl

Eth

er,T

Tetra

hydr

ofur

an (T

HF)

,TC

hlor

ofor

m,T

n-H

exan

e,TE

thyl

Ace

tate

,TD

iisop

ropy

l Eth

er,T

Brom

ochl

orom

etha

ne (I

S1),I

Rci

s-1,

2-D

ichl

oroe

then

e,T

2-Bu

tano

ne (M

EK),T

Viny

l Ace

tate

,TM

ethy

l ter

t-But

yl E

ther

,T1,

1-D

ichl

oroe

than

e,T

trans

-1,2

-Dic

hlor

oeth

ene,

T

Tric

hlor

otrif

luor

oeth

ane,

TC

arbo

n D

isul

fide,

T3-

Chl

oro-

1-pr

open

e (A

llyl C

hlor

ide)

,TM

ethy

lene

Chl

orid

e,T

2-M

ethy

l-2-P

ropa

nol (

tert-

Buty

l Alc

ohol

,T1,

1-D

ichl

oroe

then

e,T

Acry

loni

trile

,T2-

Prop

anol

(Iso

prop

anol

),TTr

ichl

orof

luor

omet

hane

,TAc

eton

e,T

Acro

lein

,TAc

eton

itrile

,TEt

hano

l,TC

hlor

oeth

ane,

TBr

omom

etha

ne,T

1,3-

Buta

dien

e,T

Viny

l Chl

orid

e,T

1,2-

Dic

hlor

o-1,

1,2,

2-te

traflu

oroe

than

e ,T

Chl

orom

etha

ne,TD

ichl

orod

ifluo

rom

etha

ne (C

FC 1

2),T

Prop

ene,

T

R9071315.M Tue Jul 14 10:36:22 2015 Page: 3

98 of 128

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_07\13\07131519.D Acq On : 13 Jul 2015 22:06 Operator: SC Sample : 25ng TO-15 ICAL STD Misc : S29-07071501/S29-07081503 (8/6) ALS Vial : 6 Sample Multiplier: 1 Quant Time: Jul 14 10:24:06 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:23:55 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 1) Bromochloromethane (IS1) 9.00 130 128760 12.500 ng 0.00 37) 1,4-Difluorobenzene (IS2) 10.97 114 676210 12.500 ng 0.00 56) Chlorobenzene-d5 (IS3) 15.31 82 325964 12.500 ng 0.00 System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.78 65 263284 16.773 ng 0.00 Spiked Amount 12.500 Recovery = 134.16% 57) Toluene-d8 (SS2) 13.41 98 715880 11.969 ng 0.00 Spiked Amount 12.500 Recovery = 95.76% 73) Bromofluorobenzene (SS3) 16.92 174 245432 9.857 ng 0.00 Spiked Amount 12.500 Recovery = 78.88% Target Compounds Qvalue 2) Propene 3.75 42 567450 49.565 ng 99 3) Dichlorodifluoromethan... 3.86 85 977843 38.001 ng 100 4) Chloromethane 4.06 50 818790 47.147 ng 100 5) 1,2-Dichloro-1,1,2,2-t... 4.22 135 417602 31.158 ng 100 6) Vinyl Chloride 4.33 62 687366 40.886 ng 100 7) 1,3-Butadiene 4.50 54 582739 47.240 ng 100 8) Bromomethane 4.81 94 365783 31.904 ng 99 9) Chloroethane 5.02 64 352337 40.209 ng 100 10) Ethanol 5.25 45 2020280 247.502 ng 99 11) Acetonitrile 5.44 41 1022926 44.932 ng 99 12) Acrolein 5.56 56 328349 41.156 ng 99 13) Acetone 5.71 58 1846461 214.638 ng 99 14) Trichlorofluoromethane 5.88 101 739389 33.269 ng 100 15) 2-Propanol (Isopropanol) 6.03 45 2787922 97.943 ng 98 16) Acrylonitrile 6.23 53 680063 45.261 ng 100 17) 1,1-Dichloroethene 6.57 96 411193 35.470 ng 99 18) 2-Methyl-2-Propanol (t... 6.67 59 2541793 91.643 ng 99 19) Methylene Chloride 6.72 84 440849 34.848 ng 99 20) 3-Chloro-1-propene (Al... 6.85 41 817445 53.933 ng 100 21) Trichlorotrifluoroethane 7.03 151 324255 29.353 ng 99 22) Carbon Disulfide 7.00 76 1695037 32.185 ng 99 23) trans-1,2-Dichloroethene 7.74 61 717022 44.237 ng 100 24) 1,1-Dichloroethane 7.96 63 871705 39.994 ng 100 25) Methyl tert-Butyl Ether 8.02 73 1354895 41.739 ng 100 26) Vinyl Acetate 8.14 86 529731 209.760 ng 100 27) 2-Butanone (MEK) 8.37 72 315264 41.975 ng 99 28) cis-1,2-Dichloroethene 8.83 61 684443 43.167 ng 99 29) Diisopropyl Ether 9.07 87 356363 35.802 ng 100 30) Ethyl Acetate 9.08 61 384041 103.598 ng 100 31) n-Hexane 9.08 57 824277 46.712 ng 100 32) Chloroform 9.15 83 789611 38.343 ng 100 34) Tetrahydrofuran (THF) 9.52 72 294486 38.129 ng 98 35) Ethyl tert-Butyl Ether 9.62 87 517073 40.859 ng 100 36) 1,2-Dichloroethane 9.89 62 620379 42.606 ng 100 38) 1,1,1-Trichloroethane 10.15 97 672510 35.394 ng 99 39) Isopropyl Acetate 10.53 61 643177 89.473 ng # 92 40) 1-Butanol 10.54 56 1153636 105.007 ng 88 41) Benzene 10.61 78 1776818 36.609 ng 100 42) Carbon Tetrachloride 10.76 117 594998 36.071 ng 100 43) Cyclohexane 10.89 84 1358962 73.308 ng 100 44) tert-Amyl Methyl Ether 11.21 73 1331922 39.481 ng 100 45) 1,2-Dichloropropane 11.43 63 510275 40.996 ng 100 46) Bromodichloromethane 11.61 83 660601 40.391 ng 100 47) Trichloroethene 11.66 130 435676 30.807 ng 100 48) 1,4-Dioxane 11.63 88 370585 33.710 ng 98 49) 2,2,4-Trimethylpentane... 11.73 57 2155833 41.439 ng 99

R9071315.M Tue Jul 14 10:25:07 2015 Page: 1

99 of 128

simon.cao

Simon

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_07\13\07131519.D Acq On : 13 Jul 2015 22:06 Operator: SC Sample : 25ng TO-15 ICAL STD Misc : S29-07071501/S29-07081503 (8/6) ALS Vial : 6 Sample Multiplier: 1 Quant Time: Jul 14 10:24:06 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:23:55 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 50) Methyl Methacrylate 11.86 100 347680 74.278 ng 99 51) n-Heptane 11.99 71 479679 42.697 ng 99 52) cis-1,3-Dichloropropene 12.52 75 842203 45.259 ng 100 53) 4-Methyl-2-pentanone 12.55 58 499398 48.412 ng 99 54) trans-1,3-Dichloropropene 13.03 75 740149 41.199 ng 100 55) 1,1,2-Trichloroethane 13.21 97 444906 35.913 ng 99 58) Toluene 13.51 91 1862456 29.377 ng 99 59) 2-Hexanone 13.75 43 1322028 47.351 ng 100 60) Dibromochloromethane 13.91 129 520684 31.589 ng 99 61) 1,2-Dibromoethane 14.17 107 520486 32.266 ng 99 62) n-Butyl Acetate 14.40 43 1497177 46.804 ng 100 63) n-Octane 14.53 57 455793 37.568 ng 100 64) Tetrachloroethene 14.66 166 439442 22.979 ng 100 65) Chlorobenzene 15.36 112 1191095 28.635 ng 99 66) Ethylbenzene 15.76 91 2173278 31.687 ng 100 67) m- & p-Xylenes 15.96 91 3511129 64.014 ng 98 68) Bromoform 16.02 173 435432 28.795 ng 99 69) Styrene 16.33 104 1340810 32.789 ng 100 70) o-Xylene 16.45 91 1774863 31.661 ng 99 71) n-Nonane 16.70 43 1180587 43.209 ng 99 72) 1,1,2,2-Tetrachloroethane 16.43 83 905011 32.366 ng 99 74) Cumene 17.07 105 2156553 29.537 ng 100 75) alpha-Pinene 17.48 93 1126907 32.805 ng 100 76) n-Propylbenzene 17.60 91 2777908 31.816 ng 100 77) 3-Ethyltoluene 17.71 105 2156253 31.459 ng 100 78) 4-Ethyltoluene 17.75 105 2166290 33.290 ng 99 79) 1,3,5-Trimethylbenzene 17.83 105 1803196 31.332 ng 100 80) alpha-Methylstyrene 17.99 118 984744 33.165 ng 94 81) 2-Ethyltoluene 18.03 105 2123577 30.610 ng 99 82) 1,2,4-Trimethylbenzene 18.26 105 1917900 33.756 ng 99 83) n-Decane 18.38 57 1215548 39.756 ng 95 84) Benzyl Chloride 18.40 91 1840750 40.049 ng 99 85) 1,3-Dichlorobenzene 18.42 146 1016382 29.479 ng 100 86) 1,4-Dichlorobenzene 18.49 146 1027092 28.238 ng 100 87) sec-Butylbenzene 18.55 105 2503838 33.287 ng 100 88) 4-Isopropyltoluene (p-... 18.72 119 2307553 32.974 ng 99 89) 1,2,3-Trimethylbenzene 18.71 105 2025916 34.655 ng 99 90) 1,2-Dichlorobenzene 18.85 146 1000976 30.182 ng 100 91) d-Limonene 18.87 68 847820 41.220 ng 99 92) 1,2-Dibromo-3-Chloropr... 19.31 157 382959 31.634 ng 97 93) n-Undecane 19.72 57 1296052 40.412 ng 99 94) 1,2,4-Trichlorobenzene 20.66 180 759414 30.020 ng 100 95) Naphthalene 20.78 128 2677593 31.891 ng 100 96) n-Dodecane 20.81 57 1322002 43.703 ng 99 97) Hexachlorobutadiene 21.14 225 439334 25.333 ng 100 98) Cyclohexanone 16.10 55 805668 39.720 ng 99 99) tert-Butylbenzene 18.26 119 1811226 32.933 ng 100 100) n-Butylbenzene 19.16 91 2204225 37.547 ng 100 -------------------------------------------------------------------------- (#) = qualifier out of range (m) = manual integration (+) = signals summed

R9071315.M Tue Jul 14 10:25:07 2015 Page: 2

100 of 128


Data File: I:\MS09\Data\2015_07\13\07131519.D Acq On : 13 Jul 2015 22:06 Operator: SC Sample : 25ng TO-15 ICAL STD Misc : S29-07071501/S29-07081503 (8/6) ALS Vial : 6 Sample Multiplier: 1


4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.000

500000

1000000

1500000

2000000

2500000

3000000

3500000

4000000

4500000

5000000

5500000

6000000

6500000

7000000

7500000

8000000

Time-->


Hex

achl

orob

utad

iene

,Tn-

Dod

ecan

e,T

Nap

htha

lene

,T1,

2,4-

Tric

hlor

oben

zene

,T

n-U

ndec

ane,

T1,

2-D

ibro

mo-

3-C

hlor

opro

pane

,Tn-

Buty

lben

zene

,Td-

Lim

onen

e,T

1,2-

Dic

hlor

oben

zene

,T4-

Isop

ropy

ltolu

ene

(p-C

ymen

e),T

1,2,

3-Tr

imet

hylb

enze

ne,T

sec-

Buty

lben

zene

,T1,

4-D

ichl

orob

enze

ne,T

1,3-

Dic

hlor

oben

zene

,TBe

nzyl

Chl

orid

e,T

n-D

ecan

e,T

1,2,

4-Tr

imet

hylb

enze

ne,T

tert-

Buty

lben

zene

,T2-

Ethy

ltolu

ene,

Tal

pha-

Met

hyls

tyre

ne,T

1,3,

5-Tr

imet

hylb

enze

ne,T

4-Et

hylto

luen

e,T

3-Et

hylto

luen

e,T

n-Pr

opyl

benz

ene,

Tal

pha-

Pine

ne,T

Cum

ene,

TBr

omof

luor

oben

zene

(SS3

),Sn-

Non

ane,

To-

Xyle

ne,T

1,1,

2,2-

Tetra

chlo

roet

hane

,TSt

yren

e,T

Cyc

lohe

xano

ne,T

Brom

ofor

m,T

m- &

p-X

ylen

es,T

Ethy

lben

zene

,TC

hlor

oben

zene

,TC

hlor

oben

zene

-d5

(IS3)

,IR

Tetra

chlo

roet

hene

,Tn-

Oct

ane,

Tn-

Buty

l Ace

tate

,T1,

2-D

ibro

moe

than

e,T

Dib

rom

ochl

orom

etha

ne,T

2-H

exan

one,

TTo

luen

e,T

Tolu

ene-

d8 (S

S2),S

1,1,

2-Tr

ichl

oroe

than

e,T

trans

-1,3

-Dic

hlor

opro

pene

,T

4-M

ethy

l-2-p

enta

none

,Tci

s-1,

3-D

ichl

orop

rope

ne,T

n-H

epta

ne,T

Met

hyl M

etha

cryl

ate,

T2,

2,4-

Trim

ethy

lpen

tane

(Iso

octa

ne),T

Tric

hlor

oeth

ene,

T1,

4-D

ioxa

ne,T

Brom

odic

hlor

omet

hane

,T1,

2-D

ichl

orop

ropa

ne,T

tert-

Am

yl M

ethy

l Eth

er,T

1,4-

Difl

uoro

benz

ene

(IS2)

,IRC

yclo

hexa

ne,T

Car

bon

Tetra

chlo

ride,

TBe

nzen

e,T

1-Bu

tano

l,TIs

opro

pyl A

ceta

te,T

1,1,

1-Tr

ichl

oroe

than

e,T

1,2-

Dic

hlor

oeth

ane,

T1,

2-D

ichl

oroe

than

e-d4

(SS1

),SEt

hyl t

ert-B

utyl

Eth

er,T

Tetra

hydr

ofur

an (T

HF)

,TC

hlor

ofor

m,T

n-H

exan

e,T

Ethy

l Ace

tate

,TD

iisop

ropy

l Eth

er,T

Brom

ochl

orom

etha

ne (I

S1),I

Rci

s-1,

2-D

ichl

oroe

then

e,T

2-Bu

tano

ne (M

EK),T

Viny

l Ace

tate

,TM

ethy

l ter

t-But

yl E

ther

,T1,

1-D

ichl

oroe

than

e,T

trans

-1,2

-Dic

hlor

oeth

ene,

T

Tric

hlor

otrif

luor

oeth

ane,

TC

arbo

n D

isul

fide,

T3-

Chl

oro-

1-pr

open

e (A

llyl C

hlor

ide)

,TM

ethy

lene

Chl

orid

e,T

2-M

ethy

l-2-P

ropa

nol (

tert-

Buty

l Alc

ohol

,T1,

1-D

ichl

oroe

then

e,T

Acry

loni

trile

,T2-

Prop

anol

(Iso

prop

anol

),TTr

ichl

orof

luor

omet

hane

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eton

e,T

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lein

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eton

itrile

,TEtha

nol,T

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oroe

than

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omet

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nyl C

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ide,

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than

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orom

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ne,T

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(CFC

12)

,TPr

open

e,T

R9071315.M Tue Jul 14 10:25:08 2015 Page: 3

101 of 128

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_07\13\07131520.D Acq On : 13 Jul 2015 22:40 Operator: SC Sample : 50ng TO-15 ICAL STD Misc : S29-07071501/S29-07081503 (8/6) ALS Vial : 6 Sample Multiplier: 1 Quant Time: Jul 14 10:47:27 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:34:59 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 1) Bromochloromethane (IS1) 9.01 130 154307 12.500 ng 0.00 37) 1,4-Difluorobenzene (IS2) 10.97 114 808190 12.500 ng 0.00 56) Chlorobenzene-d5 (IS3) 15.31 82 368993 12.500 ng 0.00 System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.79 65 292155 14.947 ng 0.00 Spiked Amount 12.500 Recovery = 119.60% 57) Toluene-d8 (SS2) 13.41 98 832412 12.320 ng 0.00 Spiked Amount 12.500 Recovery = 98.56% 73) Bromofluorobenzene (SS3) 16.92 174 279023 10.160 ng 0.00 Spiked Amount 12.500 Recovery = 81.28% Target Compounds Qvalue 2) Propene 3.75 42 1148146 71.864 ng 99 3) Dichlorodifluoromethan... 3.86 85 2016347 61.959 ng 99 4) Chloromethane 4.06 50 1632621 71.574 ng 99 5) 1,2-Dichloro-1,1,2,2-t... 4.22 135 955887 58.118 ng 100 6) Vinyl Chloride 4.33 62 1499547 70.214 ng 100 7) 1,3-Butadiene 4.51 54 1282733 80.865 ng 97 8) Bromomethane 4.81 94 858120 60.967 ng 99 9) Chloroethane 5.02 64 789738 70.552 ng 100 10) Ethanol 5.26 45 4256228 393.345 ng 98 11) Acetonitrile 5.45 41 2162687 69.982 ng 99 12) Acrolein 5.57 56 720560 68.763 ng 100 13) Acetone 5.72 58 4016149 353.427 ng 90 14) Trichlorofluoromethane 5.88 101 1653010 59.647 ng 99 15) 2-Propanol (Isopropanol) 6.05 45 5852285 157.296 ng 100 16) Acrylonitrile 6.24 53 1488029 77.352 ng 99 17) 1,1-Dichloroethene 6.57 96 948731 66.292 ng 93 18) 2-Methyl-2-Propanol (t... 6.69 59 5528976 154.463 ng 98 19) Methylene Chloride 6.73 84 1009549 63.379 ng 93 20) 3-Chloro-1-propene (Al... 6.85 41 1739677 87.370 ng 96 21) Trichlorotrifluoroethane 7.03 151 774940 57.993 ng 96 22) Carbon Disulfide 7.00 76 3850365 58.801 ng 100 23) trans-1,2-Dichloroethene 7.75 61 1594618 77.467 ng 97 24) 1,1-Dichloroethane 7.96 63 1928784 69.776 ng 100 25) Methyl tert-Butyl Ether 8.02 73 3063658 74.413 ng 99 26) Vinyl Acetate 8.15 86 1207045 377.720 ng # 71 27) 2-Butanone (MEK) 8.38 72 710669 74.874 ng # 88 28) cis-1,2-Dichloroethene 8.84 61 1498946 74.494 ng 96 29) Diisopropyl Ether 9.08 87 817591 65.757 ng # 77 30) Ethyl Acetate 9.08 61 846806 174.322 ng 97 31) n-Hexane 9.08 57 1814922 78.278 ng 100 32) Chloroform 9.15 83 1752931 67.854 ng 100 34) Tetrahydrofuran (THF) 9.52 72 663316 68.267 ng 93 35) Ethyl tert-Butyl Ether 9.62 87 1191006 74.749 ng 94 36) 1,2-Dichloroethane 9.90 62 1331545 71.588 ng 99 38) 1,1,1-Trichloroethane 10.15 97 1504209 64.059 ng 99 39) Isopropyl Acetate 10.53 61 1438570 157.383 ng # 87 40) 1-Butanol 10.55 56 2554053 172.805 ng 94 41) Benzene 10.61 78 4002592 65.718 ng 100 42) Carbon Tetrachloride 10.76 117 1343384 66.280 ng 100 43) Cyclohexane 10.89 84 3104826 134.787 ng 97 44) tert-Amyl Methyl Ether 11.21 73 2996795 71.078 ng 98 45) 1,2-Dichloropropane 11.43 63 1125749 71.758 ng 100 46) Bromodichloromethane 11.62 83 1471009 72.254 ng 100 47) Trichloroethene 11.67 130 1017750 59.386 ng 100 48) 1,4-Dioxane 11.64 88 850604 62.933 ng 98 49) 2,2,4-Trimethylpentane... 11.73 57 4713321 71.491 ng 98

R9071315.M Tue Jul 14 10:48:24 2015 Page: 1

102 of 128

simon.cao

Simon

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_07\13\07131520.D Acq On : 13 Jul 2015 22:40 Operator: SC Sample : 50ng TO-15 ICAL STD Misc : S29-07071501/S29-07081503 (8/6) ALS Vial : 6 Sample Multiplier: 1 Quant Time: Jul 14 10:47:27 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:34:59 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 50) Methyl Methacrylate 11.86 100 802986 139.855 ng 95 51) n-Heptane 11.99 71 1071870 75.179 ng 98 52) cis-1,3-Dichloropropene 12.52 75 1875623 80.604 ng 99 53) 4-Methyl-2-pentanone 12.55 58 1095573 83.220 ng 94 54) trans-1,3-Dichloropropene 13.03 75 1641932 71.861 ng 99 55) 1,1,2-Trichloroethane 13.21 97 1001506 65.631 ng 99 58) Toluene 13.51 91 4128273 56.396 ng 99 59) 2-Hexanone 13.75 43 2746443 81.412 ng 97 60) Dibromochloromethane 13.92 129 1168776 62.471 ng 99 61) 1,2-Dibromoethane 14.17 107 1163682 63.074 ng 100 62) n-Butyl Acetate 14.40 43 3110918 80.541 ng 98 63) n-Octane 14.53 57 982106 68.201 ng 97 64) Tetrachloroethene 14.66 166 1010798 47.071 ng 99 65) Chlorobenzene 15.36 112 2678128 56.437 ng 100 66) Ethylbenzene 15.76 91 4756543 59.981 ng 99 67) m- & p-Xylenes 15.96 91 7702787 121.039 ng 99 68) Bromoform 16.02 173 993513 58.561 ng 100 69) Styrene 16.33 104 2945899 62.690 ng 99 70) o-Xylene 16.45 91 3850320 59.242 ng 99 71) n-Nonane 16.70 43 2398219 72.188 ng 97 72) 1,1,2,2-Tetrachloroethane 16.43 83 1954171 60.175 ng 100 74) Cumene 17.07 105 4687867 55.767 ng 99 75) alpha-Pinene 17.48 93 2461398 61.956 ng 99 76) n-Propylbenzene 17.60 91 5921876 58.383 ng 99 77) 3-Ethyltoluene 17.71 105 4833792 61.496 ng 99 78) 4-Ethyltoluene 17.76 105 4533675 59.855 ng 99 79) 1,3,5-Trimethylbenzene 17.84 105 3927105 59.162 ng 99 80) alpha-Methylstyrene 17.99 118 2159548 63.275 ng 99 81) 2-Ethyltoluene 18.04 105 4586328 57.239 ng 99 82) 1,2,4-Trimethylbenzene 18.27 105 4202133 63.415 ng 100 83) n-Decane 18.39 57 2495069 68.190 ng 98 84) Benzyl Chloride 18.40 91 4001782 74.424 ng 99 85) 1,3-Dichlorobenzene 18.42 146 2223868 56.544 ng 100 86) 1,4-Dichlorobenzene 18.49 146 2220020 53.606 ng 100 87) sec-Butylbenzene 18.55 105 5354448 61.403 ng 100 88) 4-Isopropyltoluene (p-... 18.72 119 4970994 60.833 ng 99 89) 1,2,3-Trimethylbenzene 18.72 105 4398825 64.377 ng 100 90) 1,2-Dichlorobenzene 18.85 146 2161457 56.897 ng 100 91) d-Limonene 18.87 68 1796667 73.468 ng 98 92) 1,2-Dibromo-3-Chloropr... 19.31 157 826767 59.952 ng 95 93) n-Undecane 19.72 57 2642865 68.946 ng 99 94) 1,2,4-Trichlorobenzene 20.66 180 1654072 57.626 ng 99 95) Naphthalene 20.78 128 5717327 58.534 ng 100 96) n-Dodecane 20.81 57 2709346 74.033 ng 98 97) Hexachlorobutadiene 21.14 225 970009 49.800 ng 100 98) Cyclohexanone 16.11 55 1714304 71.428 ng 97 99) tert-Butylbenzene 18.26 119 3961384 61.946 ng 99 100) n-Butylbenzene 19.16 91 4610182 67.041 ng 99 -------------------------------------------------------------------------- (#) = qualifier out of range (m) = manual integration (+) = signals summed

R9071315.M Tue Jul 14 10:48:24 2015 Page: 2

103 of 128




4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.000

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Hex

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R9071315.M Tue Jul 14 10:48:26 2015 Page: 3

104 of 128

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_07\13\07131521.D Acq On : 13 Jul 2015 23:14 Operator: SC Sample : 100ng TO-15 ICAL STD Misc : S29-07071501/S29-07081503 (8/6) ALS Vial : 6 Sample Multiplier: 1 Quant Time: Jul 14 10:48:40 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:34:59 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 1) Bromochloromethane (IS1) 9.02 130 173236 12.500 ng 0.02 37) 1,4-Difluorobenzene (IS2) 10.98 114 895601 12.500 ng 0.00 56) Chlorobenzene-d5 (IS3) 15.32 82 394731 12.500 ng 0.00 System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.79 65 310031 14.129 ng 0.01 Spiked Amount 12.500 Recovery = 113.04% 57) Toluene-d8 (SS2) 13.41 98 907246 12.552 ng 0.00 Spiked Amount 12.500 Recovery = 100.40% 73) Bromofluorobenzene (SS3) 16.92 174 304467 10.364 ng 0.00 Spiked Amount 12.500 Recovery = 82.88% Target Compounds Qvalue 2) Propene 3.76 42 2398768 133.737 ng 98 3) Dichlorodifluoromethan... 3.86 85 4120655 112.786 ng 99 4) Chloromethane 4.06 50 3026903 118.199 ng 99 5) 1,2-Dichloro-1,1,2,2-t... 4.22 135 2032489 110.072 ng 100 6) Vinyl Chloride 4.34 62 3156147 131.634 ng 99 7) 1,3-Butadiene 4.51 54 2612495 146.698 ng 95 8) Bromomethane 4.82 94 1857692 117.562 ng 100 9) Chloroethane 5.03 64 1481632 117.900 ng 100 10) Ethanol 5.29 45 8373653 689.305 ng 98 11) Acetonitrile 5.47 41 4394936 126.676 ng 100 12) Acrolein 5.58 56 1491803 126.808 ng 100 13) Acetone 5.73 58 7936627 622.119 ng # 80 14) Trichlorofluoromethane 5.89 101 3504390 112.636 ng 99 15) 2-Propanol (Isopropanol) 6.07 45 11232565 268.918 ng 99 16) Acrylonitrile 6.26 53 3098113 143.451 ng 99 17) 1,1-Dichloroethene 6.58 96 2042986 127.155 ng 89 18) 2-Methyl-2-Propanol (t... 6.71 59 10176210 253.230 ng 97 19) Methylene Chloride 6.74 84 2153865 120.443 ng 89 20) 3-Chloro-1-propene (Al... 6.86 41 3577960 160.058 ng 93 21) Trichlorotrifluoroethane 7.04 151 1709487 113.951 ng 95 22) Carbon Disulfide 7.00 76 8176684 111.227 ng 99 23) trans-1,2-Dichloroethene 7.75 61 3353722 145.122 ng 95 24) 1,1-Dichloroethane 7.98 63 4054309 130.644 ng 99 25) Methyl tert-Butyl Ether 8.03 73 6534137 141.365 ng 99 26) Vinyl Acetate 8.16 86 2544062 709.122 ng # 26 27) 2-Butanone (MEK) 8.39 72 1504129 141.156 ng # 81 28) cis-1,2-Dichloroethene 8.85 61 3152224 139.541 ng 94 29) Diisopropyl Ether 9.08 87 1724162 123.519 ng # 46 30) Ethyl Acetate 9.10 61 1639614 300.647 ng 91 31) n-Hexane 9.08 57 3479769 133.684 ng 98 32) Chloroform 9.16 83 3708543 127.868 ng 99 34) Tetrahydrofuran (THF) 9.53 72 1416028 129.810 ng # 89 35) Ethyl tert-Butyl Ether 9.63 87 2580549 144.261 ng # 90 36) 1,2-Dichloroethane 9.90 62 2749138 131.652 ng 99 38) 1,1,1-Trichloroethane 10.16 97 3203272 123.102 ng 98 39) Isopropyl Acetate 10.54 61 2940676 290.317 ng # 76 40) 1-Butanol 10.57 56 5252228 320.679 ng 89 41) Benzene 10.62 78 8485639 125.726 ng 100 42) Carbon Tetrachloride 10.77 117 2895311 128.907 ng 100 43) Cyclohexane 10.90 84 6609734 258.937 ng 93 44) tert-Amyl Methyl Ether 11.22 73 6389993 136.766 ng 96 45) 1,2-Dichloropropane 11.44 63 2367421 136.177 ng 100 46) Bromodichloromethane 11.62 83 3117344 138.174 ng 100 47) Trichloroethene 11.67 130 2247856 118.362 ng 100 48) 1,4-Dioxane 11.64 88 1852241 123.665 ng 95 49) 2,2,4-Trimethylpentane... 11.74 57 9777507 133.830 ng 96

R9071315.M Tue Jul 14 10:49:34 2015 Page: 1

105 of 128

simon.cao

Simon

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_07\13\07131521.D Acq On : 13 Jul 2015 23:14 Operator: SC Sample : 100ng TO-15 ICAL STD Misc : S29-07071501/S29-07081503 (8/6) ALS Vial : 6 Sample Multiplier: 1 Quant Time: Jul 14 10:48:40 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:34:59 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 50) Methyl Methacrylate 11.87 100 1747000 274.576 ng # 89 51) n-Heptane 11.99 71 2273473 143.894 ng 97 52) cis-1,3-Dichloropropene 12.52 75 3989198 154.703 ng 99 53) 4-Methyl-2-pentanone 12.56 58 2286208 156.712 ng 89 54) trans-1,3-Dichloropropene 13.04 75 3489586 137.820 ng 99 55) 1,1,2-Trichloroethane 13.22 97 2147997 127.025 ng 98 58) Toluene 13.51 91 8803136 112.417 ng 98 59) 2-Hexanone 13.76 43 5496625 152.310 ng 94 60) Dibromochloromethane 13.92 129 2550656 127.443 ng 99 61) 1,2-Dibromoethane 14.18 107 2507139 127.031 ng 100 62) n-Butyl Acetate 14.40 43 6209833 150.289 ng 95 63) n-Octane 14.53 57 2038632 132.340 ng 95 64) Tetrachloroethene 14.67 166 2279071 99.211 ng 99 65) Chlorobenzene 15.37 112 5794776 114.152 ng 99 66) Ethylbenzene 15.77 91 10104496 119.112 ng 97 67) m- & p-Xylenes 15.97 91 16402179 240.933 ng 97 68) Bromoform 16.03 173 2200171 121.230 ng 99 69) Styrene 16.34 104 6321866 125.761 ng 99 70) o-Xylene 16.46 91 8208334 118.061 ng 98 71) n-Nonane 16.70 43 4654189 130.959 ng 92 72) 1,1,2,2-Tetrachloroethane 16.43 83 4145957 119.342 ng 100 74) Cumene 17.08 105 9966393 110.829 ng 98 75) alpha-Pinene 17.48 93 5284118 124.334 ng 98 76) n-Propylbenzene 17.61 91 12256211 112.954 ng 98 77) 3-Ethyltoluene 17.71 105 10354040 123.136 ng 98 78) 4-Ethyltoluene 17.76 105 9526075 117.566 ng 98 79) 1,3,5-Trimethylbenzene 17.84 105 8387513 118.119 ng 98 80) alpha-Methylstyrene 18.00 118 4665192 127.778 ng 99 81) 2-Ethyltoluene 18.04 105 9716599 113.359 ng 98 82) 1,2,4-Trimethylbenzene 18.28 105 8573449 120.947 ng 100 83) n-Decane 18.39 57 4689327 119.802 ng 94 84) Benzyl Chloride 18.41 91 8328274 144.788 ng 96 85) 1,3-Dichlorobenzene 18.43 146 4867214 115.685 ng 100 86) 1,4-Dichlorobenzene 18.50 146 4840606 109.262 ng 100 87) sec-Butylbenzene 18.56 105 11122496 119.233 ng 98 88) 4-Isopropyltoluene (p-... 18.73 119 9820466 112.343 ng 99 89) 1,2,3-Trimethylbenzene 18.72 105 8884597 121.548 ng 100 90) 1,2-Dichlorobenzene 18.86 146 4658740 114.637 ng 100 91) d-Limonene 18.87 68 3624519 138.548 ng 94 92) 1,2-Dibromo-3-Chloropr... 19.32 157 1777025 120.458 ng 90 93) n-Undecane 19.72 57 5144808 125.465 ng 96 94) 1,2,4-Trichlorobenzene 20.66 180 3589993 116.916 ng 100 95) Naphthalene 20.78 128 11724113 112.205 ng 99 96) n-Dodecane 20.81 57 5236636 133.761 ng 95 97) Hexachlorobutadiene 21.15 225 2162253 103.771 ng 99 98) Cyclohexanone 16.11 55 3545277 138.085 ng 95 99) tert-Butylbenzene 18.27 119 8055084 117.748 ng 98 100) n-Butylbenzene 19.16 91 9395141 127.715 ng 97 -------------------------------------------------------------------------- (#) = qualifier out of range (m) = manual integration (+) = signals summed

R9071315.M Tue Jul 14 10:49:34 2015 Page: 2

106 of 128




4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.000

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2.8e+07

3e+07

3.2e+07

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ropy

ltolu

ene

(p-C

ymen

e),T

1,2,

3-Tr

imet

hylb

enze

ne,T

sec-

Buty

lben

zene

,T1,

4-D

ichl

orob

enze

ne,T

1,3-

Dic

hlor

oben

zene

,TBe

nzyl

Chl

orid

e,T

n-D

ecan

e,T

1,2,

4-Tr

imet

hylb

enze

ne,T

tert-

Buty

lben

zene

,T2-

Ethy

ltolu

ene,

Tal

pha-

Met

hyls

tyre

ne,T

1,3,

5-Tr

imet

hylb

enze

ne,T

4-Et

hylto

luen

e,T

3-Et

hylto

luen

e,T

n-Pr

opyl

benz

ene,

Tal

pha-

Pine

ne,T

Cum

ene,

TBr

omof

luor

oben

zene

(SS3

),Sn-

Non

ane,

To-

Xyle

ne,T

1,1,

2,2-

Tetra

chlo

roet

hane

,TSt

yren

e,T

Cyc

lohe

xano

ne,T

Brom

ofor

m,T

m- &

p-X

ylen

es,T

Ethy

lben

zene

,TC

hlor

oben

zene

,TC

hlor

oben

zene

-d5

(IS3)

,IR

Tetra

chlo

roet

hene

,Tn-

Oct

ane,

Tn-

Buty

l Ace

tate

,T1,

2-D

ibro

moe

than

e,T

Dib

rom

ochl

orom

etha

ne,T

2-H

exan

one,

TTo

luen

e,T

Tolu

ene-

d8 (S

S2),S

1,1,

2-Tr

ichl

oroe

than

e,T

trans

-1,3

-Dic

hlor

opro

pene

,T

4-M

ethy

l-2-p

enta

none

,Tci

s-1,

3-D

ichl

orop

rope

ne,T

n-H

epta

ne,T

Met

hyl M

etha

cryl

ate,

T2,

2,4-

Trim

ethy

lpen

tane

(Iso

octa

ne),T

Tric

hlor

oeth

ene,

T1,

4-D

ioxa

ne,T

Brom

odic

hlor

omet

hane

,T1,

2-D

ichl

orop

ropa

ne,T

tert-

Am

yl M

ethy

l Eth

er,T

1,4-

Difl

uoro

benz

ene

(IS2)

,IRC

yclo

hexa

ne,T

Car

bon

Tetra

chlo

ride,

TBe

nzen

e,T

1-Bu

tano

l,TIs

opro

pyl A

ceta

te,T

1,1,

1-Tr

ichl

oroe

than

e,T

1,2-

Dic

hlor

oeth

ane,

T1,

2-D

ichl

oroe

than

e-d4

(SS1

),SEt

hyl t

ert-B

utyl

Eth

er,T

Tetra

hydr

ofur

an (T

HF)

,TC

hlor

ofor

m,T

Ethy

l Ace

tate

,TD

iisop

ropy

l Eth

er,T

n-H

exan

e,T

Brom

ochl

orom

etha

ne (I

S1),I

Rcis-

1,2-

Dic

hlor

oeth

ene,

T

2-Bu

tano

ne (M

EK),T

Viny

l Ace

tate

,TM

ethy

l ter

t-But

yl E

ther

,T1,

1-D

ichl

oroe

than

e,T

trans

-1,2

-Dic

hlor

oeth

ene,

T

Tric

hlor

otrif

luor

oeth

ane,

TC

arbo

n D

isul

fide,

T3-

Chl

oro-

1-pr

open

e (A

llyl C

hlor

ide)

,TM

ethy

lene

Chl

orid

e,T

2-M

ethy

l-2-P

ropa

nol (

tert-

Buty

l Alc

ohol

,T1,

1-D

ichl

oroe

then

e,T

Acr

ylon

itrile

,T2-

Prop

anol

(Iso

prop

anol

),TTr

ichl

orof

luor

omet

hane

,TAc

eton

e,T

Acro

lein

,TAc

eton

itrile

,TEt

hano

l,TC

hlor

oeth

ane,

TBr

omom

etha

ne,T

1,3-

Buta

dien

e,T

Viny

l Chl

orid

e,T

1,2-

Dic

hlor

o-1,

1,2,

2-te

traflu

oroe

than

e ,T

Chl

orom

etha

ne,TD

ichl

orod

ifluo

rom

etha

ne (C

FC 1

2),T

Prop

ene,

T

R9071315.M Tue Jul 14 10:49:36 2015 Page: 3

107 of 128

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_07\13\07131523.D Acq On : 14 Jul 2015 12:34 Operator: SC Sample : 25ng TO-15 ICV STD Misc : S29-07071501/S29-07141502 (8/12) ALS Vial : 16 Sample Multiplier: 1 Quant Time: Jul 14 12:59:59 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 1) Bromochloromethane (IS1) 9.00 130 177499 12.500 ng -0.02 37) 1,4-Difluorobenzene (IS2) 10.97 114 930349 12.500 ng 0.00 56) Chlorobenzene-d5 (IS3) 15.31 82 387310 12.500 ng 0.00 System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.78 65 307257 10.766 ng -0.01 Spiked Amount 12.500 Recovery = 86.16% 57) Toluene-d8 (SS2) 13.41 98 925122 13.150 ng 0.00 Spiked Amount 12.500 Recovery = 105.20% 73) Bromofluorobenzene (SS3) 16.92 174 298175 13.333 ng 0.00 Spiked Amount 12.500 Recovery = 106.64% Target Compounds Qvalue 2) Propene 3.75 42 590593 20.033 ng 98 3) Dichlorodifluoromethan... 3.86 85 1039330 22.027 ng 100 4) Chloromethane 4.05 50 928642 23.563 ng 99 5) 1,2-Dichloro-1,1,2,2-t... 4.22 135 534936 26.845 ng 100 6) Vinyl Chloride 4.33 62 863641 26.234 ng 100 7) 1,3-Butadiene 4.50 54 711364 28.051 ng 95 8) Bromomethane 4.81 94 513338 26.943 ng 100 9) Chloroethane 5.02 64 441008 25.983 ng 100 10) Ethanol 5.25 45 2273040 115.270 ng 98 11) Acetonitrile 5.44 41 1134618 22.066 ng 99 12) Acrolein 5.56 56 379712 24.924 ng 99 13) Acetone 5.71 58 2271973 126.137 ng # 83 14) Trichlorofluoromethane 5.88 101 904725 23.844 ng 99 15) 2-Propanol (Isopropanol) 6.03 45 3201222 50.179 ng 100 16) Acrylonitrile 6.23 53 816710 26.309 ng 99 17) 1,1-Dichloroethene 6.57 96 552080 28.487 ng 87 18) 2-Methyl-2-Propanol (t... 6.68 59 3141530 54.680 ng 97 19) Methylene Chloride 6.72 84 587711 25.527 ng 86 20) 3-Chloro-1-propene (Al... 6.85 41 930822 25.602 ng 92 21) Trichlorotrifluoroethane 7.03 151 460927 30.048 ng 93 22) Carbon Disulfide 7.00 76 2030802 23.270 ng 100 23) trans-1,2-Dichloroethene 7.74 61 860828 26.600 ng 93 24) 1,1-Dichloroethane 7.96 63 1084433 25.880 ng 99 25) Methyl tert-Butyl Ether 8.02 73 1760054 27.593 ng 98 26) Vinyl Acetate 8.14 86 718468 138.511 ng # 58 27) 2-Butanone (MEK) 8.37 72 410818 27.247 ng # 78 28) cis-1,2-Dichloroethene 8.83 61 838449 26.828 ng 92 29) Diisopropyl Ether 9.07 87 478202 25.381 ng # 65 30) Ethyl Acetate 9.08 61 477450 53.425 ng 93 31) n-Hexane 9.08 57 1027866 26.005 ng 99 32) Chloroform 9.14 83 1006504 27.541 ng 100 34) Tetrahydrofuran (THF) 9.52 72 407342 26.576 ng # 86 35) Ethyl tert-Butyl Ether 9.62 87 697666 29.181 ng # 90 36) 1,2-Dichloroethane 9.89 62 737065 25.437 ng 100 38) 1,1,1-Trichloroethane 10.15 97 854811 26.896 ng 98 39) Isopropyl Acetate 10.53 61 820755 58.139 ng # 78 40) 1-Butanol 10.54 56 1361734 51.990 ng 92 41) Benzene 10.61 78 2337821 27.327 ng 100 42) Carbon Tetrachloride 10.76 117 753401 28.255 ng 100 43) Cyclohexane 10.89 84 1798936 56.764 ng 93 44) tert-Amyl Methyl Ether 11.21 73 1723641 27.868 ng 96 45) 1,2-Dichloropropane 11.43 63 641587 26.942 ng 100 46) Bromodichloromethane 11.61 83 816382 28.371 ng 100 47) Trichloroethene 11.66 130 599360 28.633 ng 100 48) 1,4-Dioxane 11.63 88 501938 28.677 ng 94 49) 2,2,4-Trimethylpentane... 11.73 57 2651977 26.127 ng 95

R9071315.M Tue Jul 14 13:01:02 2015 Page: 1

108 of 128

simon.cao

Simon

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_07\13\07131523.D Acq On : 14 Jul 2015 12:34 Operator: SC Sample : 25ng TO-15 ICV STD Misc : S29-07071501/S29-07141502 (8/12) ALS Vial : 16 Sample Multiplier: 1 Quant Time: Jul 14 12:59:59 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 50) Methyl Methacrylate 11.85 100 472254 58.939 ng # 89 51) n-Heptane 11.98 71 611354 28.091 ng 96 52) cis-1,3-Dichloropropene 12.52 75 963477 28.595 ng 100 53) 4-Methyl-2-pentanone 12.55 58 607116 26.812 ng 90 54) trans-1,3-Dichloropropene 13.03 75 884544 27.064 ng 100 55) 1,1,2-Trichloroethane 13.21 97 579038 28.943 ng 98 58) Toluene 13.51 91 2414892 30.766 ng 99 59) 2-Hexanone 13.75 43 1485933 28.551 ng 94 60) Dibromochloromethane 13.91 129 658441 34.149 ng 100 61) 1,2-Dibromoethane 14.17 107 668973 33.076 ng 100 62) n-Butyl Acetate 14.39 43 1684641 29.541 ng 96 63) n-Octane 14.53 57 544300 29.067 ng 94 64) Tetrachloroethene 14.66 166 596720 30.525 ng 100 65) Chlorobenzene 15.36 112 1561991 32.257 ng 100 66) Ethylbenzene 15.76 91 2753643 31.655 ng 98 67) m- & p-Xylenes 15.96 91 4368647 61.966 ng 98 68) Bromoform 16.02 173 544405 31.882 ng 100 69) Styrene 16.33 104 1695985 34.617 ng 98 70) o-Xylene 16.45 91 2181444 30.184 ng 98 71) n-Nonane 16.69 43 1288608 26.616 ng 94 72) 1,1,2,2-Tetrachloroethane 16.42 83 1090754 29.701 ng 99 74) Cumene 17.07 105 2658121 30.028 ng 99 75) alpha-Pinene 17.48 93 1411588 32.112 ng 98 76) n-Propylbenzene 17.60 91 3326256 29.336 ng 98 77) 3-Ethyltoluene 17.71 105 2643208 31.116 ng 99 78) 4-Ethyltoluene 17.75 105 2619237 31.875 ng 99 79) 1,3,5-Trimethylbenzene 17.83 105 2201263 31.066 ng 98 80) alpha-Methylstyrene 17.99 118 1210926 34.020 ng 99 81) 2-Ethyltoluene 18.03 105 2569999 30.597 ng 99 82) 1,2,4-Trimethylbenzene 18.26 105 2318546 31.947 ng 99 83) n-Decane 18.38 57 1358814 28.728 ng 98 84) Benzyl Chloride 18.39 91 2178846 33.233 ng 98 85) 1,3-Dichlorobenzene 18.42 146 1267470 33.351 ng 100 86) 1,4-Dichlorobenzene 18.49 146 1249381 31.653 ng 100 87) sec-Butylbenzene 18.55 105 2963774 30.850 ng 99 88) 4-Isopropyltoluene (p-... 18.72 119 2731108 28.827 ng 98 89) 1,2,3-Trimethylbenzene 18.71 105 2379236 30.852 ng 99 90) 1,2-Dichlorobenzene 18.85 146 1203353 31.833 ng 100 91) d-Limonene 18.87 68 969325 32.110 ng 97 92) 1,2-Dibromo-3-Chloropr... 19.31 157 444734 29.849 ng 90 93) n-Undecane 19.71 57 1370162 27.708 ng 98 94) 1,2,4-Trichlorobenzene 20.66 180 823908 28.465 ng 100 95) Naphthalene 20.78 128 2764006 25.920 ng 100 96) n-Dodecane 20.81 57 1273098 25.352 ng 98 97) Hexachlorobutadiene 21.14 225 473891 27.322 ng 100 98) Cyclohexanone 16.10 55 917566 28.729 ng 95 99) tert-Butylbenzene 18.26 119 2171852 31.663 ng 99 100) n-Butylbenzene 19.16 91 2491002 30.713 ng 99 -------------------------------------------------------------------------- (#) = qualifier out of range (m) = manual integration (+) = signals summed

R9071315.M Tue Jul 14 13:01:02 2015 Page: 2

109 of 128


Data File: I:\MS09\Data\2015_07\13\07131523.D Acq On : 14 Jul 2015 12:34 Operator: SC Sample : 25ng TO-15 ICV STD Misc : S29-07071501/S29-07141502 (8/12) ALS Vial : 16 Sample Multiplier: 1


4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 23.00 24.000

500000

1000000

1500000

2000000

2500000

3000000

3500000

4000000

4500000

5000000

5500000

6000000

6500000

7000000

7500000

8000000

8500000

9000000

Time-->


Hex

achl

orob

utad

iene

,Tn-

Dod

ecan

e,T

Nap

htha

lene

,T1,

2,4-

Tric

hlor

oben

zene

,T

n-U

ndec

ane,

T1,

2-D

ibro

mo-

3-C

hlor

opro

pane

,Tn-

Buty

lben

zene

,Td-

Lim

onen

e,T

1,2-

Dic

hlor

oben

zene

,T4-

Isop

ropy

ltolu

ene

(p-C

ymen

e),T

1,2,

3-Tr

imet

hylb

enze

ne,T

sec-

Buty

lben

zene

,T1,

4-D

ichl

orob

enze

ne,T

1,3-

Dic

hlor

oben

zene

,TBe

nzyl

Chl

orid

e,T

n-D

ecan

e,T

1,2,

4-Tr

imet

hylb

enze

ne,T

tert-

Buty

lben

zene

,T2-

Ethy

ltolu

ene,

Tal

pha-

Met

hyls

tyre

ne,T

1,3,

5-Tr

imet

hylb

enze

ne,T

4-Et

hylto

luen

e,T

3-Et

hylto

luen

e,T

n-Pr

opyl

benz

ene,

Tal

pha-

Pine

ne,TCum

ene,

TBr

omof

luor

oben

zene

(SS3

),Sn-

Non

ane,

To-

Xyle

ne,T

1,1,

2,2-

Tetra

chlo

roet

hane

,TSt

yren

e,T

Cyc

lohe

xano

ne,T

Brom

ofor

m,T

m- &

p-X

ylen

es,T

Ethy

lben

zene

,TC

hlor

oben

zene

,TC

hlor

oben

zene

-d5

(IS3)

,IR

Tetra

chlo

roet

hene

,Tn-

Oct

ane,

Tn-

Buty

l Ace

tate

,T1,

2-D

ibro

moe

than

e,T

Dib

rom

ochl

orom

etha

ne,T

2-H

exan

one,

TTo

luen

e,T

Tolu

ene-

d8 (S

S2),S

1,1,

2-Tr

ichl

oroe

than

e,T

trans

-1,3

-Dic

hlor

opro

pene

,T

4-M

ethy

l-2-p

enta

none

,Tci

s-1,

3-D

ichl

orop

rope

ne,T

n-H

epta

ne,T

Met

hyl M

etha

cryl

ate,

T2,

2,4-

Trim

ethy

lpen

tane

(Iso

octa

ne),T

Tric

hlor

oeth

ene,

T1,

4-D

ioxa

ne,T

Brom

odic

hlor

omet

hane

,T1,

2-D

ichl

orop

ropa

ne,T

tert-

Am

yl M

ethy

l Eth

er,T

1,4-

Difl

uoro

benz

ene

(IS2)

,IRC

yclo

hexa

ne,T

Car

bon

Tetra

chlo

ride,

TBe

nzen

e,T

1-Bu

tano

l,TIs

opro

pyl A

ceta

te,T

1,1,

1-Tr

ichl

oroe

than

e,T

1,2-

Dic

hlor

oeth

ane,

T1,

2-D

ichl

oroe

than

e-d4

(SS1

),SEt

hyl t

ert-B

utyl

Eth

er,T

Tetra

hydr

ofur

an (T

HF)

,TC

hlor

ofor

m,T

n-H

exan

e,T

Ethy

l Ace

tate

,TD

iisop

ropy

l Eth

er,T

Brom

ochl

orom

etha

ne (I

S1),I

Rci

s-1,

2-D

ichl

oroe

then

e,T

2-Bu

tano

ne (M

EK),T

Viny

l Ace

tate

,TM

ethy

l ter

t-But

yl E

ther

,T1,

1-D

ichl

oroe

than

e,T

trans

-1,2

-Dic

hlor

oeth

ene,

T

Tric

hlor

otrif

luor

oeth

ane,

TC

arbo

n D

isul

fide,

T3-

Chl

oro-

1-pr

open

e (A

llyl C

hlor

ide)

,TM

ethy

lene

Chl

orid

e,T

2-M

ethy

l-2-P

ropa

nol (

tert-

Buty

l Alc

ohol

,T1,

1-D

ichl

oroe

then

e,T

Acry

loni

trile

,T2-

Prop

anol

(Iso

prop

anol

),TTr

ichl

orof

luor

omet

hane

,TAc

eton

e,T

Acro

lein

,TAc

eton

itrile

,TEtha

nol,T

Chl

oroe

than

e,T

Brom

omet

hane

,T1,

3-Bu

tadi

ene,

TVi

nyl C

hlor

ide,

T1,2-

Dic

hlor

o-1,

1,2,

2-te

traflu

oroe

than

e ,T

Chl

orom

etha

ne,T

Dic

hlor

odifl

uoro

met

hane

(CFC

12)

,TPr

open

e,T

R9071315.M Tue Jul 14 13:01:08 2015 Page: 3

110 of 128

of 2 I:\MS09\0-Instrument Info\0-Security Certificates\ICV_07141501.CRT 7/14/15 1:48 PM

INITIAL CALIBRATION VERIFICATION CHECK SHEET

Data File Name: 07131523.D Acq. Method File: TO15.MData File Path: I:\MS09\Data\2015_07\13\ Sample Name: 25ng TO-15 ICV STD

Operator: SC Misc Info: S29-07071501/S29-07141502 (Date Acquired: 7/14/15 12:34 Instrument Name: MS09

Compound Ret. Amt. Spike % Lower Upper * OR# Name Time (ng) Amt.(ng) Rec. Limit Limit Fail2) Propene 3.75 20.0 24.50 82 70 130 *3) Dichlorodifluoromethane (CFC 12 3.86 22.0 23.50 94 70 130 *4) Chloromethane 4.05 23.6 25.00 94 70 130 *5) 1,2-Dichloro-1,1,2,2-tetrafluoroeth 4.22 26.8 25.50 105 70 130 *6) Vinyl Chloride 4.33 26.2 25.00 105 70 130 *7) 1,3-Butadiene 4.50 28.1 25.75 109 70 130 *8) Bromomethane 4.81 26.9 25.25 107 70 130 *9) Chloroethane 5.02 26.0 25.00 104 70 130 *

10) Ethanol 5.25 115 124.75 92 70 130 *11) Acetonitrile 5.44 22.1 26.50 83 70 130 *12) Acrolein 5.56 24.9 26.75 93 70 130 *13) Acetone 5.71 126 134.75 94 70 130 *14) Trichlorofluoromethane 5.88 23.8 27.00 88 70 130 *15) 2-Propanol (Isopropanol) 6.03 50.2 52.25 96 70 130 *16) Acrylonitrile 6.23 26.3 26.50 99 70 130 *17) 1,1-Dichloroethene 6.57 28.5 27.00 106 70 130 *18) 2-Methyl-2-Propanol (tert-Butyl Alco 6.68 54.7 50.00 109 70 130 *19) Methylene Chloride 6.72 25.5 27.75 92 70 130 *20) 3-Chloro-1-propene (Allyl Chlorid 6.85 25.6 27.25 94 70 130 *21) Trichlorotrifluoroethane 7.03 30.0 27.50 109 70 130 *22) Carbon Disulfide 7.00 23.3 26.25 89 70 130 *23) trans-1,2-Dichloroethene 7.74 26.6 26.25 101 70 130 *24) 1,1-Dichloroethane 7.96 25.9 26.50 98 70 130 *25) Methyl tert-Butyl Ether 8.02 27.6 27.00 102 70 130 *26) Vinyl Acetate 8.14 139 129.75 107 70 130 *27) 2-Butanone (MEK) 8.37 27.2 27.50 99 70 130 *28) cis-1,2-Dichloroethene 8.83 26.8 27.25 98 70 130 *29) Diisopropyl Ether 9.07 25.4 27.00 94 70 130 *30) Ethyl Acetate 9.08 53.4 53.50 100 70 130 *31) n-Hexane 9.08 26.0 26.50 98 70 130 *32) Chloroform 9.14 27.5 28.00 98 70 130 *34) Tetrahydrofuran (THF) 9.52 26.6 27.50 97 70 130 *35) Ethyl tert-Butyl Ether 9.62 29.2 26.75 109 70 130 *36) 1,2-Dichloroethane 9.89 25.4 26.75 95 70 130 *38) 1,1,1-Trichloroethane 10.15 26.9 26.25 102 70 130 *39) Isopropyl Acetate 10.53 58.1 57.25 101 70 130 *40) 1-Butanol 10.54 52.0 51.25 101 70 130 *41) Benzene 10.61 27.3 28.25 97 70 130 *42) Carbon Tetrachloride 10.76 28.3 28.75 98 70 130 *43) Cyclohexane 10.89 56.8 53.00 107 70 130 *44) tert-Amyl Methyl Ether 11.21 27.9 26.75 104 70 130 *45) 1,2-Dichloropropane 11.43 26.9 27.00 100 70 130 *46) Bromodichloromethane 11.61 28.4 27.25 104 70 130 *47) Trichloroethene 11.66 28.6 27.00 106 70 130 *48) 1,4-Dioxane 11.63 28.7 26.25 109 70 130 *49) 2,2,4-Trimethylpentane (Isooctane) 11.73 26.1 26.75 98 70 130 *

111 of 128

simon.cao

Simon

of 2 I:\MS09\0-Instrument Info\0-Security Certificates\ICV_07141501.CRT 7/14/15 1:48 PM

INITIAL CALIBRATION VERIFICATION CHECK SHEET

Data File Name: 07131523.D Acq. Method File: TO15.MData File Path: I:\MS09\Data\2015_07\13\ Sample Name: 25ng TO-15 ICV STD

Operator: SC Misc Info: S29-07071501/S29-07141502 (Date Acquired: 7/14/15 12:34 Instrument Name: MS09

Compound Ret. Amt. Spike % Lower Upper * OR# Name Time (ng) Amt.(ng) Rec. Limit Limit Fail

50) Methyl Methacrylate 11.85 58.9 52.75 112 70 130 *51) n-Heptane 11.98 28.1 27.00 104 70 130 *52) cis-1,3-Dichloropropene 12.52 28.6 26.00 110 70 130 *53) 4-Methyl-2-pentanone 12.55 26.8 27.50 97 70 130 *54) trans-1,3-Dichloropropene 13.03 27.1 26.25 103 70 130 *55) 1,1,2-Trichloroethane 13.21 28.9 27.00 107 70 130 *58) Toluene 13.51 30.8 27.25 113 70 130 *59) 2-Hexanone 13.75 28.6 27.50 104 70 130 *60) Dibromochloromethane 13.91 34.1 27.50 124 70 130 *61) 1,2-Dibromoethane 14.17 33.1 27.25 121 70 130 *62) n-Butyl Acetate 14.39 29.5 28.25 104 70 130 *63) n-Octane 14.53 29.1 26.25 111 70 130 *64) Tetrachloroethene 14.66 30.5 25.25 121 70 130 *65) Chlorobenzene 15.36 32.3 27.50 117 70 130 *66) Ethylbenzene 15.76 31.7 27.25 116 70 130 *67) m- & p-Xylenes 15.96 62.0 53.50 116 70 130 *68) Bromoform 16.02 31.9 28.50 112 70 130 *69) Styrene 16.33 34.6 27.75 125 70 130 *70) o-Xylene 16.45 30.2 26.25 115 70 130 *71) n-Nonane 16.69 26.6 25.50 104 70 130 *72) 1,1,2,2-Tetrachloroethane 16.42 29.7 26.25 113 70 130 *74) Cumene 17.07 30.0 26.00 115 70 130 *75) alpha-Pinene 17.48 32.1 26.50 121 70 130 *76) n-Propylbenzene 17.60 29.3 25.50 115 70 130 *77) 3-Ethyltoluene 17.71 31.1 26.75 116 70 130 *78) 4-Ethyltoluene 17.75 31.9 26.75 119 70 130 *79) 1,3,5-Trimethylbenzene 17.83 31.1 26.75 116 70 130 *80) alpha-Methylstyrene 17.99 34.0 26.25 130 70 130 *81) 2-Ethyltoluene 18.03 30.6 26.75 114 70 130 *82) 1,2,4-Trimethylbenzene 18.26 31.9 27.25 117 70 130 *83) n-Decane 18.38 28.7 26.25 109 70 130 *84) Benzyl Chloride 18.39 33.2 27.50 121 70 130 *85) 1,3-Dichlorobenzene 18.42 33.4 28.50 117 70 130 *86) 1,4-Dichlorobenzene 18.49 31.7 26.00 122 70 130 *87) sec-Butylbenzene 18.55 30.9 27.25 113 70 130 *88) 4-Isopropyltoluene (p-Cymene) 18.72 28.8 26.00 111 70 130 *89) 1,2,3-Trimethylbenzene 18.71 30.9 26.50 117 70 130 *90) 1,2-Dichlorobenzene 18.85 31.8 27.50 116 70 130 *91) d-Limonene 18.87 32.1 26.25 122 70 130 *92) 1,2-Dibromo-3-Chloropropane 19.31 29.8 27.25 109 70 130 *93) n-Undecane 19.71 27.7 25.25 110 70 130 *94) 1,2,4-Trichlorobenzene 20.66 28.5 28.75 99 70 130 *95) Naphthalene 20.78 25.9 27.25 95 70 130 *96) n-Dodecane 20.81 25.4 27.25 93 70 130 *97) Hexachlorobutadiene 21.14 27.3 28.75 95 70 130 *98) Cyclohexanone 16.10 28.7 27.50 104 70 130 *99) tert-Butylbenzene 18.26 31.7 26.75 119 70 130 *

100) n-Butylbenzene 19.16 30.7 28.00 110 70 130 *

Bold = 75 Compound List* = Pass

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Evaluate Continuing Calibration Report Data File: I:\MS09\Data\2015_08\04\08041502.D Acq On : 4 Aug 2015 6:14 Operator: SC Sample : CCV R9080415_25ng Misc : S29-07071501/S29-07081503 (8/6) ALS Vial : 15 Sample Multiplier: 1 Quant Time: Aug 04 09:11:26 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Min. RRF : 0.000 Min. Rel. Area : 50% Max. R.T. Dev 0.33min Max. RRF Dev : 30% Max. Rel. Area : 200% Compound AvgRF CCRF %Dev Area% Dev(min) ------------------------------------------------------------------------- 1 IR Bromochloromethane (IS1) 1.000 1.000 0.0 116 -0.02 2 T Propene 2.076 1.534 26.1 81 0.00 3 T Dichlorodifluoromethane (CF 3.323 2.888 13.1 90 0.00 4 T Chloromethane 2.775 2.217 20.1 80 0.00 5 T 1,2-Dichloro-1,1,2,2-tetraf 1.403 1.407 -0.3 104 -0.01 6 T Vinyl Chloride 2.318 2.026 12.6 89 0.00 7 T 1,3-Butadiene 1.786 1.531 14.3 84 -0.01 8 T Bromomethane 1.342 1.371 -2.2 113 0.00 9 T Chloroethane 1.195 1.109 7.2 95 0.00 10 T Ethanol 1.389 1.111 20.0 84 -0.04 11 T Acetonitrile 3.621 2.806 22.5 84 -0.04 12 T Acrolein 1.073 0.926 13.7 90 -0.02 13 T Acetone 1.268 1.032 18.6 90 -0.03 14 T Trichlorofluoromethane 2.672 2.415 9.6 97 0.00 15 T 2-Propanol (Isopropanol) 4.493 3.737 16.8 84 -0.04 16 T Acrylonitrile 2.186 1.966 10.1 90 -0.03 17 T 1,1-Dichloroethene 1.365 1.315 3.7 103 0.00 18 T 2-Methyl-2-Propanol (tert-B 4.046 3.592 11.2 89 -0.04 19 T Methylene Chloride 1.621 1.361 16.0 100 -0.02 20 T 3-Chloro-1-propene (Allyl C 2.560 2.117 17.3 85 -0.01 21 T Trichlorotrifluoroethane 1.080 1.096 -1.5 109 0.00 22 T Carbon Disulfide 6.146 5.619 8.6 97 0.00 23 T trans-1,2-Dichloroethene 2.279 2.083 8.6 92 -0.01 24 T 1,1-Dichloroethane 2.951 2.607 11.7 93 -0.02 25 T Methyl tert-Butyl Ether 4.492 4.137 7.9 97 0.00 26 T Vinyl Acetate 0.365 0.346 5.2 100 -0.03 27 T 2-Butanone (MEK) 1.062 0.940 11.5 96 -0.02 28 T cis-1,2-Dichloroethene 2.201 1.949 11.4 91 -0.01 29 T Diisopropyl Ether 1.327 1.113 16.1 102 -0.01 30 T Ethyl Acetate 0.629 0.548 12.9 91 -0.02 31 T n-Hexane 2.783 2.438 12.4 93 0.00 32 T Chloroform 2.574 2.312 10.2 95 -0.02 33 S 1,2-Dichloroethane-d4(SS1) 2.010 1.700 15.4 97 -0.01 34 T Tetrahydrofuran (THF) 1.079 0.931 13.7 98 0.00 35 T Ethyl tert-Butyl Ether 1.684 1.646 2.3 101 0.00 36 T 1,2-Dichloroethane 2.041 1.728 15.3 88 -0.01 37 IR 1,4-Difluorobenzene (IS2) 1.000 1.000 0.0 114 0.00 38 T 1,1,1-Trichloroethane 0.427 0.402 5.9 96 -0.01 39 T Isopropyl Acetate 0.190 0.178 6.3 93 -0.01 40 T 1-Butanol 0.352 0.303 13.9 90 -0.04 41 T Benzene 1.149 1.019 11.3 97 -0.01 42 T Carbon Tetrachloride 0.358 0.350 2.2 97 0.00 43 T Cyclohexane 0.426 0.416 2.3 99 -0.01 44 T tert-Amyl Methyl Ether 0.831 0.795 4.3 96 0.00 45 T 1,2-Dichloropropane 0.320 0.291 9.1 93 0.00 46 T Bromodichloromethane 0.387 0.372 3.9 94 -0.01 47 T Trichloroethene 0.281 0.286 -1.8 105 0.00 48 T 1,4-Dioxane 0.235 0.219 6.8 99 0.00 49 T 2,2,4-Trimethylpentane (Iso 1.364 1.226 10.1 91 0.00 50 T Methyl Methacrylate 0.108 0.109 -0.9 101 -0.01 51 T n-Heptane 0.292 0.281 3.8 97 0.00 52 T cis-1,3-Dichloropropene 0.453 0.460 -1.5 95 0.00 53 T 4-Methyl-2-pentanone 0.304 0.269 11.5 90 -0.01 54 T trans-1,3-Dichloropropene 0.439 0.415 5.5 93 0.00

R9071315.M Tue Aug 04 09:16:44 2015 Page: 1

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Evaluate Continuing Calibration Report Data File: I:\MS09\Data\2015_08\04\08041502.D Acq On : 4 Aug 2015 6:14 Operator: SC Sample : CCV R9080415_25ng Misc : S29-07071501/S29-07081503 (8/6) ALS Vial : 15 Sample Multiplier: 1 Quant Time: Aug 04 09:11:26 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Min. RRF : 0.000 Min. Rel. Area : 50% Max. R.T. Dev 0.33min Max. RRF Dev : 30% Max. Rel. Area : 200% Compound AvgRF CCRF %Dev Area% Dev(min) ------------------------------------------------------------------------- 55 T 1,1,2-Trichloroethane 0.269 0.267 0.7 98 0.00 56 IR Chlorobenzene-d5 (IS3) 1.000 1.000 0.0 100 0.00 57 S Toluene-d8 (SS2) 2.271 2.360 -3.9 108 0.00 58 T Toluene 2.533 2.589 -2.2 96 0.00 59 T 2-Hexanone 1.680 1.498 10.8 82 -0.01 60 T Dibromochloromethane 0.622 0.720 -15.8 99 0.00 61 T 1,2-Dibromoethane 0.653 0.726 -11.2 99 0.00 62 T n-Butyl Acetate 1.841 1.680 8.7 82 0.00 63 T n-Octane 0.604 0.597 1.2 89 0.00 64 T Tetrachloroethene 0.631 0.711 -12.7 105 0.00 65 T Chlorobenzene 1.563 1.675 -7.2 99 0.00 66 T Ethylbenzene 2.807 2.945 -4.9 94 0.00 67 T m- & p-Xylenes 2.275 2.362 -3.8 92 0.00 68 T Bromoform 0.551 0.622 -12.9 101 -0.01 69 T Styrene 1.581 1.764 -11.6 94 0.00 70 T o-Xylene 2.332 2.404 -3.1 91 0.00 71 T n-Nonane 1.563 1.446 7.5 81 0.00 72 T 1,1,2,2-Tetrachloroethane 1.185 1.252 -5.7 91 0.00 73 S Bromofluorobenzene (SS3) 0.722 0.796 -10.2 106 0.00 74 T Cumene 2.857 3.042 -6.5 94 0.00 75 T alpha-Pinene 1.419 1.557 -9.7 94 0.00 76 T n-Propylbenzene 3.659 3.818 -4.3 91 0.00 77 T 3-Ethyltoluene 2.742 2.912 -6.2 94 0.00 78 T 4-Ethyltoluene 2.652 2.872 -8.3 92 0.00 79 T 1,3,5-Trimethylbenzene 2.287 2.404 -5.1 92 0.00 80 T alpha-Methylstyrene 1.149 1.345 -17.1 93 0.00 81 T 2-Ethyltoluene 2.711 2.852 -5.2 92 0.00 82 T 1,2,4-Trimethylbenzene 2.342 2.532 -8.1 91 0.00 83 T n-Decane 1.527 1.505 1.4 83 0.00 84 T Benzyl Chloride 2.116 2.276 -7.6 88 -0.01 85 T 1,3-Dichlorobenzene 1.227 1.346 -9.7 94 0.00 86 T 1,4-Dichlorobenzene 1.274 1.391 -9.2 94 0.00 87 T sec-Butylbenzene 3.101 3.277 -5.7 92 0.00 88 T 4-Isopropyltoluene (p-Cymen 3.058 3.165 -3.5 91 0.00 89 T 1,2,3-Trimethylbenzene 2.489 2.632 -5.7 89 0.00 90 T 1,2-Dichlorobenzene 1.220 1.338 -9.7 94 0.00 91 T d-Limonene 0.974 1.062 -9.0 86 0.00 92 T 1,2-Dibromo-3-Chloropropane 0.481 0.538 -11.9 95 0.00 93 T n-Undecane 1.596 1.624 -1.8 83 0.00 94 T 1,2,4-Trichlorobenzene 0.934 1.019 -9.1 92 0.00 95 T Naphthalene 3.442 3.736 -8.5 89 0.00 96 T n-Dodecane 1.621 1.662 -2.5 83 0.00 97 T Hexachlorobutadiene 0.560 0.583 -4.1 93 0.00 98 T Cyclohexanone 1.031 0.958 7.1 86 0.00 99 T tert-Butylbenzene 2.214 2.413 -9.0 92 0.00 100 T n-Butylbenzene 2.618 2.705 -3.3 88 0.00 -------------------------------------------------------------------------- (#) = Out of Range SPCC's out = 0 CCC's out = 0

R9071315.M Tue Aug 04 09:16:44 2015 Page: 2

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Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_08\04\08041502.D Acq On : 4 Aug 2015 6:14 Operator: SC Sample : CCV R9080415_25ng Misc : S29-07071501/S29-07081503 (8/6) ALS Vial : 15 Sample Multiplier: 1 Quant Time: Aug 04 09:11:26 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 1) Bromochloromethane (IS1) 9.00 130 149787 12.500 ng -0.02 37) 1,4-Difluorobenzene (IS2) 10.97 114 769681 12.500 ng 0.00 56) Chlorobenzene-d5 (IS3) 15.31 82 327176 12.500 ng 0.00 System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.78 65 254681 10.574 ng -0.01 Spiked Amount 12.500 Recovery = 84.56% 57) Toluene-d8 (SS2) 13.41 98 772146 12.993 ng 0.00 Spiked Amount 12.500 Recovery = 103.92% 73) Bromofluorobenzene (SS3) 16.92 174 260354 13.781 ng 0.00 Spiked Amount 12.500 Recovery = 110.24% Target Compounds Qvalue 2) Propene 3.75 42 459534 18.471 ng 97 3) Dichlorodifluoromethan... 3.85 85 882499 22.163 ng 99 4) Chloromethane 4.05 50 657577 19.772 ng 99 5) 1,2-Dichloro-1,1,2,2-t... 4.21 135 434237 25.823 ng 100 6) Vinyl Chloride 4.33 62 613059 22.068 ng 99 7) 1,3-Butadiene 4.50 54 490782 22.933 ng 94 8) Bromomethane 4.81 94 414938 25.807 ng 99 9) Chloroethane 5.02 64 335401 23.417 ng 100 10) Ethanol 5.25 45 1693903 101.794 ng 98 11) Acetonitrile 5.43 41 857290 19.757 ng 99 12) Acrolein 5.56 56 296848 23.090 ng 99 13) Acetone 5.70 58 1669222 109.818 ng # 83 14) Trichlorofluoromethane 5.88 101 716274 22.369 ng 99 15) 2-Propanol (Isopropanol) 6.03 45 2350783 43.666 ng 100 16) Acrylonitrile 6.23 53 612575 23.384 ng 99 17) 1,1-Dichloroethene 6.57 96 421671 25.784 ng # 86 18) 2-Methyl-2-Propanol (t... 6.67 59 2270421 46.829 ng 97 19) Methylene Chloride 6.72 84 440488 22.672 ng 85 20) 3-Chloro-1-propene (Al... 6.85 41 691314 22.533 ng 90 21) Trichlorotrifluoroethane 7.03 151 354486 27.385 ng 92 22) Carbon Disulfide 7.00 76 1649774 22.401 ng 100 23) trans-1,2-Dichloroethene 7.74 61 661394 24.218 ng 92 24) 1,1-Dichloroethane 7.96 63 812269 22.972 ng 99 25) Methyl tert-Butyl Ether 8.02 73 1313713 24.406 ng 97 26) Vinyl Acetate 8.14 86 529991 121.079 ng # 54 27) 2-Butanone (MEK) 8.37 72 304176 23.907 ng # 76 28) cis-1,2-Dichloroethene 8.83 61 624887 23.694 ng 92 29) Diisopropyl Ether 9.07 87 363450 22.859 ng # 60 30) Ethyl Acetate 9.07 61 351046 46.548 ng 94 31) n-Hexane 9.08 57 766849 22.991 ng 99 32) Chloroform 9.14 83 747898 24.251 ng 99 34) Tetrahydrofuran (THF) 9.52 72 287203 22.205 ng # 86 35) Ethyl tert-Butyl Ether 9.62 87 522692 25.907 ng # 88 36) 1,2-Dichloroethane 9.89 62 543437 22.224 ng 100 38) 1,1,1-Trichloroethane 10.15 97 643339 24.468 ng 97 39) Isopropyl Acetate 10.53 61 599008 51.289 ng # 80 40) 1-Butanol 10.54 56 1038900 47.944 ng 90 41) Benzene 10.61 78 1725785 24.384 ng 99 42) Carbon Tetrachloride 10.76 117 576279 26.123 ng 99 43) Cyclohexane 10.89 84 1350106 51.495 ng 92 44) tert-Amyl Methyl Ether 11.21 73 1284377 25.101 ng 95 45) 1,2-Dichloropropane 11.43 63 474052 24.062 ng 100 46) Bromodichloromethane 11.61 83 618494 25.981 ng 100 47) Trichloroethene 11.67 130 458339 26.467 ng 100 48) 1,4-Dioxane 11.63 88 368130 25.423 ng 92 49) 2,2,4-Trimethylpentane... 11.73 57 1962970 23.376 ng 95

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Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_08\04\08041502.D Acq On : 4 Aug 2015 6:14 Operator: SC Sample : CCV R9080415_25ng Misc : S29-07071501/S29-07081503 (8/6) ALS Vial : 15 Sample Multiplier: 1 Quant Time: Aug 04 09:11:26 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 50) Methyl Methacrylate 11.86 100 352676 53.204 ng # 88 51) n-Heptane 11.99 71 463012 25.716 ng 96 52) cis-1,3-Dichloropropene 12.52 75 799452 28.680 ng 99 53) 4-Methyl-2-pentanone 12.55 58 451045 24.078 ng 89 54) trans-1,3-Dichloropropene 13.03 75 689957 25.517 ng 99 55) 1,1,2-Trichloroethane 13.21 97 435612 26.319 ng 97 58) Toluene 13.51 91 1795629 27.081 ng 99 59) 2-Hexanone 13.75 43 1088404 24.757 ng 94 60) Dibromochloromethane 13.92 129 518011 31.803 ng 100 61) 1,2-Dibromoethane 14.17 107 512778 30.013 ng 99 62) n-Butyl Acetate 14.40 43 1231082 25.555 ng 95 63) n-Octane 14.53 57 406456 25.695 ng 93 64) Tetrachloroethene 14.66 166 460366 27.878 ng 100 65) Chlorobenzene 15.36 112 1184065 28.947 ng 100 66) Ethylbenzene 15.76 91 2042751 27.799 ng 98 67) m- & p-Xylenes 15.96 91 3245637 54.498 ng 96 68) Bromoform 16.02 173 439265 30.452 ng 99 69) Styrene 16.33 104 1258343 30.405 ng 98 70) o-Xylene 16.45 91 1620088 26.537 ng 97 71) n-Nonane 16.69 43 955692 23.368 ng 94 72) 1,1,2,2-Tetrachloroethane 16.42 83 827768 26.683 ng 100 74) Cumene 17.07 105 2030193 27.150 ng 99 75) alpha-Pinene 17.48 93 1059765 28.540 ng 97 76) n-Propylbenzene 17.60 91 2523597 26.348 ng 98 77) 3-Ethyltoluene 17.71 105 2020050 28.151 ng 98 78) 4-Ethyltoluene 17.76 105 1992225 28.701 ng 99 79) 1,3,5-Trimethylbenzene 17.84 105 1667613 27.860 ng 98 80) alpha-Methylstyrene 17.99 118 915632 30.452 ng 98 81) 2-Ethyltoluene 18.03 105 1959422 27.615 ng 99 82) 1,2,4-Trimethylbenzene 18.27 105 1739635 28.376 ng 98 83) n-Decane 18.39 57 1014539 25.392 ng 97 84) Benzyl Chloride 18.40 91 1623339 29.311 ng 97 85) 1,3-Dichlorobenzene 18.42 146 960356 29.914 ng 100 86) 1,4-Dichlorobenzene 18.49 146 964934 28.940 ng 100 87) sec-Butylbenzene 18.55 105 2294401 28.272 ng 98 88) 4-Isopropyltoluene (p-... 18.72 119 2091607 26.135 ng 97 89) 1,2,3-Trimethylbenzene 18.71 105 1808468 27.761 ng 98 90) 1,2-Dichlorobenzene 18.85 146 936728 29.334 ng 99 91) d-Limonene 18.87 68 729725 28.616 ng 96 92) 1,2-Dibromo-3-Chloropr... 19.31 157 362594 28.809 ng 87 93) n-Undecane 19.72 57 1073297 25.694 ng 97 94) 1,2,4-Trichlorobenzene 20.66 180 699932 28.626 ng 100 95) Naphthalene 20.78 128 2395688 26.595 ng 100 96) n-Dodecane 20.81 57 1098093 25.886 ng 98 97) Hexachlorobutadiene 21.15 225 408287 27.866 ng 100 98) Cyclohexanone 16.10 55 696025 25.798 ng 94 99) tert-Butylbenzene 18.26 119 1673777 28.887 ng 99 100) n-Butylbenzene 19.16 91 1929555 28.163 ng 98 -------------------------------------------------------------------------- (#) = qualifier out of range (m) = manual integration (+) = signals summed

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Data File: I:\MS09\Data\2015_08\04\08041502.D Acq On : 4 Aug 2015 6:14 Operator: SC Sample : CCV R9080415_25ng Misc : S29-07071501/S29-07081503 (8/6) ALS Vial : 15 Sample Multiplier: 1


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R9071315.M Tue Aug 04 09:16:34 2015 Page: 3

117 of 128

Evaluate Continuing Calibration Report Data File: I:\MS09\Data\2015_08\05\08051502.D Acq On : 5 Aug 2015 4:14 Operator: SC Sample : CCV R9080515_25ng Misc : S29-07071501/S29-07081503 (8/6) ALS Vial : 15 Sample Multiplier: 1 Quant Time: Aug 05 09:14:18 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Min. RRF : 0.000 Min. Rel. Area : 50% Max. R.T. Dev 0.33min Max. RRF Dev : 30% Max. Rel. Area : 200% Compound AvgRF CCRF %Dev Area% Dev(min) ------------------------------------------------------------------------- 1 IR Bromochloromethane (IS1) 1.000 1.000 0.0 125 -0.02 2 T Propene 2.076 1.455 29.9 82 -0.02 3 T Dichlorodifluoromethane (CF 3.323 2.741 17.5 92 -0.01 4 T Chloromethane 2.775 2.126 23.4 83 -0.02 5 T 1,2-Dichloro-1,1,2,2-tetraf 1.403 1.373 2.1 109 -0.01 6 T Vinyl Chloride 2.318 1.949 15.9 92 -0.01 7 T 1,3-Butadiene 1.786 1.502 15.9 89 -0.01 8 T Bromomethane 1.342 1.332 0.7 118 -0.01 9 T Chloroethane 1.195 1.075 10.0 99 -0.01 10 T Ethanol 1.389 1.063 23.5 86 -0.05 11 T Acetonitrile 3.621 2.672 26.2 86 -0.04 12 T Acrolein 1.073 0.891 17.0 93 -0.02 13 T Acetone 1.268 0.992 21.8 93 -0.03 14 T Trichlorofluoromethane 2.672 2.317 13.3 100 -0.01 15 T 2-Propanol (Isopropanol) 4.493 3.572 20.5 86 -0.04 16 T Acrylonitrile 2.186 1.882 13.9 93 -0.03 17 T 1,1-Dichloroethene 1.365 1.279 6.3 107 -0.01 18 T 2-Methyl-2-Propanol (tert-B 4.046 3.460 14.5 92 -0.04 19 T Methylene Chloride 1.621 1.335 17.6 105 -0.02 20 T 3-Chloro-1-propene (Allyl C 2.560 2.016 21.3 86 -0.02 21 T Trichlorotrifluoroethane 1.080 1.084 -0.4 116 -0.01 22 T Carbon Disulfide 6.146 5.435 11.6 101 0.00 23 T trans-1,2-Dichloroethene 2.279 2.001 12.2 95 -0.01 24 T 1,1-Dichloroethane 2.951 2.510 14.9 96 -0.02 25 T Methyl tert-Butyl Ether 4.492 4.004 10.9 101 -0.01 26 T Vinyl Acetate 0.365 0.336 7.9 104 -0.03 27 T 2-Butanone (MEK) 1.062 0.914 13.9 101 -0.02 28 T cis-1,2-Dichloroethene 2.201 1.871 15.0 94 -0.01 29 T Diisopropyl Ether 1.327 1.074 19.1 106 -0.01 30 T Ethyl Acetate 0.629 0.527 16.2 94 -0.03 31 T n-Hexane 2.783 2.318 16.7 95 0.00 32 T Chloroform 2.574 2.229 13.4 98 -0.02 33 S 1,2-Dichloroethane-d4(SS1) 2.010 1.638 18.5 100 -0.01 34 T Tetrahydrofuran (THF) 1.079 0.892 17.3 100 -0.01 35 T Ethyl tert-Butyl Ether 1.684 1.607 4.6 106 -0.02 36 T 1,2-Dichloroethane 2.041 1.641 19.6 89 -0.02 37 IR 1,4-Difluorobenzene (IS2) 1.000 1.000 0.0 122 0.00 38 T 1,1,1-Trichloroethane 0.427 0.387 9.4 98 -0.01 39 T Isopropyl Acetate 0.190 0.172 9.5 96 -0.01 40 T 1-Butanol 0.352 0.292 17.0 93 -0.04 41 T Benzene 1.149 0.997 13.2 101 -0.01 42 T Carbon Tetrachloride 0.358 0.340 5.0 100 -0.01 43 T Cyclohexane 0.426 0.408 4.2 104 -0.01 44 T tert-Amyl Methyl Ether 0.831 0.774 6.9 100 0.00 45 T 1,2-Dichloropropane 0.320 0.281 12.2 96 0.00 46 T Bromodichloromethane 0.387 0.359 7.2 97 -0.01 47 T Trichloroethene 0.281 0.284 -1.1 111 -0.01 48 T 1,4-Dioxane 0.235 0.215 8.5 104 0.00 49 T 2,2,4-Trimethylpentane (Iso 1.364 1.183 13.3 94 -0.01 50 T Methyl Methacrylate 0.108 0.107 0.9 107 -0.01 51 T n-Heptane 0.292 0.272 6.8 100 0.00 52 T cis-1,3-Dichloropropene 0.453 0.445 1.8 98 0.00 53 T 4-Methyl-2-pentanone 0.304 0.259 14.8 93 -0.01 54 T trans-1,3-Dichloropropene 0.439 0.401 8.7 96 0.00

R9071315.M Wed Aug 05 09:15:26 2015 Page: 1

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Simon

Evaluate Continuing Calibration Report Data File: I:\MS09\Data\2015_08\05\08051502.D Acq On : 5 Aug 2015 4:14 Operator: SC Sample : CCV R9080515_25ng Misc : S29-07071501/S29-07081503 (8/6) ALS Vial : 15 Sample Multiplier: 1 Quant Time: Aug 05 09:14:18 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Min. RRF : 0.000 Min. Rel. Area : 50% Max. R.T. Dev 0.33min Max. RRF Dev : 30% Max. Rel. Area : 200% Compound AvgRF CCRF %Dev Area% Dev(min) ------------------------------------------------------------------------- 55 T 1,1,2-Trichloroethane 0.269 0.262 2.6 102 0.00 56 IR Chlorobenzene-d5 (IS3) 1.000 1.000 0.0 107 0.00 57 S Toluene-d8 (SS2) 2.271 2.353 -3.6 115 0.00 58 T Toluene 2.533 2.528 0.2 100 0.00 59 T 2-Hexanone 1.680 1.425 15.2 83 -0.01 60 T Dibromochloromethane 0.622 0.704 -13.2 104 0.00 61 T 1,2-Dibromoethane 0.653 0.705 -8.0 102 0.00 62 T n-Butyl Acetate 1.841 1.601 13.0 83 0.00 63 T n-Octane 0.604 0.575 4.8 91 0.00 64 T Tetrachloroethene 0.631 0.702 -11.3 110 0.00 65 T Chlorobenzene 1.563 1.646 -5.3 104 0.00 66 T Ethylbenzene 2.807 2.865 -2.1 97 0.00 67 T m- & p-Xylenes 2.275 2.293 -0.8 96 0.00 68 T Bromoform 0.551 0.615 -11.6 106 -0.01 69 T Styrene 1.581 1.730 -9.4 98 0.00 70 T o-Xylene 2.332 2.337 -0.2 94 -0.01 71 T n-Nonane 1.563 1.383 11.5 82 0.00 72 T 1,1,2,2-Tetrachloroethane 1.185 1.216 -2.6 95 0.00 73 S Bromofluorobenzene (SS3) 0.722 0.813 -12.6 115 0.00 74 T Cumene 2.857 2.956 -3.5 97 0.00 75 T alpha-Pinene 1.419 1.519 -7.0 98 0.00 76 T n-Propylbenzene 3.659 3.708 -1.3 94 0.00 77 T 3-Ethyltoluene 2.742 2.836 -3.4 97 0.00 78 T 4-Ethyltoluene 2.652 2.796 -5.4 95 0.00 79 T 1,3,5-Trimethylbenzene 2.287 2.338 -2.2 96 0.00 80 T alpha-Methylstyrene 1.149 1.314 -14.4 97 0.00 81 T 2-Ethyltoluene 2.711 2.765 -2.0 95 0.00 82 T 1,2,4-Trimethylbenzene 2.342 2.454 -4.8 94 0.00 83 T n-Decane 1.527 1.438 5.8 85 0.00 84 T Benzyl Chloride 2.116 2.204 -4.2 91 -0.01 85 T 1,3-Dichlorobenzene 1.227 1.318 -7.4 98 0.00 86 T 1,4-Dichlorobenzene 1.274 1.362 -6.9 98 0.00 87 T sec-Butylbenzene 3.101 3.179 -2.5 95 0.00 88 T 4-Isopropyltoluene (p-Cymen 3.058 3.060 -0.1 93 0.00 89 T 1,2,3-Trimethylbenzene 2.489 2.541 -2.1 92 0.00 90 T 1,2-Dichlorobenzene 1.220 1.301 -6.6 97 0.00 91 T d-Limonene 0.974 1.024 -5.1 88 0.00 92 T 1,2-Dibromo-3-Chloropropane 0.481 0.524 -8.9 98 0.00 93 T n-Undecane 1.596 1.554 2.6 84 0.00 94 T 1,2,4-Trichlorobenzene 0.934 0.989 -5.9 95 0.00 95 T Naphthalene 3.442 3.605 -4.7 92 0.00 96 T n-Dodecane 1.621 1.581 2.5 84 0.00 97 T Hexachlorobutadiene 0.560 0.567 -1.2 96 0.00 98 T Cyclohexanone 1.031 0.921 10.7 88 -0.01 99 T tert-Butylbenzene 2.214 2.346 -6.0 96 0.00 100 T n-Butylbenzene 2.618 2.606 0.5 90 0.00 -------------------------------------------------------------------------- (#) = Out of Range SPCC's out = 0 CCC's out = 0

R9071315.M Wed Aug 05 09:15:26 2015 Page: 2

119 of 128

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_08\05\08051502.D Acq On : 5 Aug 2015 4:14 Operator: SC Sample : CCV R9080515_25ng Misc : S29-07071501/S29-07081503 (8/6) ALS Vial : 15 Sample Multiplier: 1 Quant Time: Aug 05 09:14:18 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 1) Bromochloromethane (IS1) 9.00 130 160733 12.500 ng -0.02 37) 1,4-Difluorobenzene (IS2) 10.97 114 821657 12.500 ng 0.00 56) Chlorobenzene-d5 (IS3) 15.31 82 348336 12.500 ng 0.00 System Monitoring Compounds 33) 1,2-Dichloroethane-d4(... 9.78 65 263291 10.187 ng -0.01 Spiked Amount 12.500 Recovery = 81.52% 57) Toluene-d8 (SS2) 13.41 98 819699 12.955 ng 0.00 Spiked Amount 12.500 Recovery = 103.68% 73) Bromofluorobenzene (SS3) 16.92 174 283304 14.085 ng 0.00 Spiked Amount 12.500 Recovery = 112.72% Target Compounds Qvalue 2) Propene 3.74 42 467829 17.524 ng 97 3) Dichlorodifluoromethan... 3.85 85 898704 21.033 ng 100 4) Chloromethane 4.05 50 676546 18.957 ng 99 5) 1,2-Dichloro-1,1,2,2-t... 4.21 135 454552 25.191 ng 100 6) Vinyl Chloride 4.33 62 632802 21.227 ng 99 7) 1,3-Butadiene 4.50 54 516562 22.494 ng 93 8) Bromomethane 4.80 94 432497 25.068 ng 100 9) Chloroethane 5.01 64 349069 22.711 ng 100 10) Ethanol 5.24 45 1738588 97.364 ng 99 11) Acetonitrile 5.43 41 876130 18.817 ng 98 12) Acrolein 5.55 56 306407 22.210 ng 99 13) Acetone 5.70 58 1721200 105.526 ng # 80 14) Trichlorofluoromethane 5.88 101 737327 21.459 ng 99 15) 2-Propanol (Isopropanol) 6.03 45 2411304 41.740 ng 100 16) Acrylonitrile 6.23 53 629231 22.384 ng 99 17) 1,1-Dichloroethene 6.57 96 440104 25.078 ng # 84 18) 2-Methyl-2-Propanol (t... 6.67 59 2346672 45.105 ng 96 19) Methylene Chloride 6.72 84 463620 22.238 ng 82 20) 3-Chloro-1-propene (Al... 6.84 41 706440 21.458 ng 89 21) Trichlorotrifluoroethane 7.02 151 376304 27.091 ng 90 22) Carbon Disulfide 7.00 76 1712107 21.664 ng 100 23) trans-1,2-Dichloroethene 7.74 61 681803 23.265 ng 90 24) 1,1-Dichloroethane 7.96 63 839236 22.118 ng 99 25) Methyl tert-Butyl Ether 8.02 73 1364314 23.620 ng 97 26) Vinyl Acetate 8.14 86 553065 117.746 ng # 49 27) 2-Butanone (MEK) 8.37 72 317249 23.236 ng # 72 28) cis-1,2-Dichloroethene 8.83 61 643723 22.746 ng 90 29) Diisopropyl Ether 9.07 87 376450 22.064 ng # 56 30) Ethyl Acetate 9.07 61 362355 44.775 ng 93 31) n-Hexane 9.07 57 782470 21.862 ng 99 32) Chloroform 9.14 83 774031 23.389 ng 99 34) Tetrahydrofuran (THF) 9.52 72 295200 21.269 ng # 85 35) Ethyl tert-Butyl Ether 9.62 87 547602 25.293 ng # 86 36) 1,2-Dichloroethane 9.89 62 553993 21.113 ng 99 38) 1,1,1-Trichloroethane 10.15 97 661152 23.554 ng 97 39) Isopropyl Acetate 10.52 61 615337 49.354 ng # 78 40) 1-Butanol 10.54 56 1071593 46.325 ng 88 41) Benzene 10.61 78 1802812 23.861 ng 99 42) Carbon Tetrachloride 10.76 117 597336 25.365 ng 100 43) Cyclohexane 10.89 84 1413973 50.519 ng 90 44) tert-Amyl Methyl Ether 11.21 73 1335959 24.457 ng 95 45) 1,2-Dichloropropane 11.43 63 489772 23.288 ng 100 46) Bromodichloromethane 11.61 83 637847 25.099 ng 100 47) Trichloroethene 11.66 130 484954 26.233 ng 100 48) 1,4-Dioxane 11.63 88 385765 24.956 ng 92 49) 2,2,4-Trimethylpentane... 11.73 57 2021276 22.547 ng 94

R9071315.M Wed Aug 05 09:15:16 2015 Page: 1

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Simon

Quantitation Report (QT Reviewed) Data File: I:\MS09\Data\2015_08\05\08051502.D Acq On : 5 Aug 2015 4:14 Operator: SC Sample : CCV R9080515_25ng Misc : S29-07071501/S29-07081503 (8/6) ALS Vial : 15 Sample Multiplier: 1 Quant Time: Aug 05 09:14:18 2015 Quant Method : I:\MS09\Methods\R9071315.M Quant Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) QLast Update : Tue Jul 14 10:53:11 2015 Response via : Initial Calibration DataAcq Meth:TO15.M Internal Standards R.T. QIon Response Conc Units Dev(Min) -------------------------------------------------------------------------- 50) Methyl Methacrylate 11.86 100 370673 52.381 ng # 86 51) n-Heptane 11.99 71 477398 24.838 ng 95 52) cis-1,3-Dichloropropene 12.52 75 825942 27.756 ng 99 53) 4-Methyl-2-pentanone 12.55 58 464209 23.213 ng 87 54) trans-1,3-Dichloropropene 13.03 75 712157 24.672 ng 100 55) 1,1,2-Trichloroethane 13.21 97 455969 25.806 ng 96 58) Toluene 13.51 91 1867135 26.449 ng 99 59) 2-Hexanone 13.75 43 1102151 23.547 ng 92 60) Dibromochloromethane 13.92 129 539187 31.093 ng 100 61) 1,2-Dibromoethane 14.17 107 530790 29.180 ng 99 62) n-Butyl Acetate 14.40 43 1249360 24.359 ng 94 63) n-Octane 14.53 57 416627 24.739 ng 92 64) Tetrachloroethene 14.66 166 484283 27.545 ng 100 65) Chlorobenzene 15.36 112 1238663 28.442 ng 100 66) Ethylbenzene 15.76 91 2115748 27.043 ng 97 67) m- & p-Xylenes 15.96 91 3354134 52.899 ng 96 68) Bromoform 16.02 173 463021 30.149 ng 99 69) Styrene 16.33 104 1313882 29.818 ng 97 70) o-Xylene 16.45 91 1676824 25.798 ng 96 71) n-Nonane 16.69 43 973400 22.355 ng 92 72) 1,1,2,2-Tetrachloroethane 16.42 83 855647 25.906 ng 100 74) Cumene 17.07 105 2100222 26.381 ng 98 75) alpha-Pinene 17.48 93 1100855 27.845 ng 97 76) n-Propylbenzene 17.60 91 2608922 25.584 ng 97 77) 3-Ethyltoluene 17.71 105 2094657 27.417 ng 98 78) 4-Ethyltoluene 17.75 105 2064951 27.942 ng 98 79) 1,3,5-Trimethylbenzene 17.84 105 1726239 27.088 ng 97 80) alpha-Methylstyrene 17.99 118 951697 29.729 ng 98 81) 2-Ethyltoluene 18.03 105 2022952 26.779 ng 98 82) 1,2,4-Trimethylbenzene 18.27 105 1795330 27.506 ng 98 83) n-Decane 18.39 57 1031558 24.249 ng 96 84) Benzyl Chloride 18.40 91 1673713 28.384 ng 97 85) 1,3-Dichlorobenzene 18.42 146 1000747 29.279 ng 100 86) 1,4-Dichlorobenzene 18.49 146 1005645 28.329 ng 100 87) sec-Butylbenzene 18.55 105 2369392 27.423 ng 98 88) 4-Isopropyltoluene (p-... 18.72 119 2153144 25.269 ng 97 89) 1,2,3-Trimethylbenzene 18.71 105 1858505 26.796 ng 97 90) 1,2-Dichlorobenzene 18.85 146 969713 28.522 ng 100 91) d-Limonene 18.87 68 749293 27.599 ng 96 92) 1,2-Dibromo-3-Chloropr... 19.31 157 375798 28.045 ng 86 93) n-Undecane 19.72 57 1093277 24.582 ng 97 94) 1,2,4-Trichlorobenzene 20.66 180 723141 27.779 ng 100 95) Naphthalene 20.78 128 2461591 25.666 ng 99 96) n-Dodecane 20.81 57 1112738 24.637 ng 97 97) Hexachlorobutadiene 21.15 225 422817 27.105 ng 100 98) Cyclohexanone 16.10 55 712541 24.806 ng 93 99) tert-Butylbenzene 18.26 119 1732132 28.078 ng 98 100) n-Butylbenzene 19.16 91 1978857 27.128 ng 98 -------------------------------------------------------------------------- (#) = qualifier out of range (m) = manual integration (+) = signals summed

R9071315.M Wed Aug 05 09:15:16 2015 Page: 2

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Data File: I:\MS09\Data\2015_08\05\08051502.D Acq On : 5 Aug 2015 4:14 Operator: SC Sample : CCV R9080515_25ng Misc : S29-07071501/S29-07081503 (8/6) ALS Vial : 15 Sample Multiplier: 1


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1000000

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R9071315.M Wed Aug 05 09:15:16 2015 Page: 3

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BFB

Data Path : I:\MS09\Data\2015_07\13\ Data File : 07131512.D Acq On : 13 Jul 2015 18:07 Operator : SC Sample : 12.5ng TO-15 BFB STD Misc : S29-07071501 ALS Vial : 2 Sample Multiplier: 1

Integration File: RTEINT.P

Method : I:\MS09\Methods\R9071315.M Title : EPA TO-15 per SOP VOA-TO15 (CASS TO-15/GC-MS) Last Update : Tue Jul 14 10:34:59 2015

15.00 15.20 15.40 15.60 15.80 16.00 16.20 16.40 16.60 16.80 17.00 17.20 17.40 17.60 17.80 18.00 18.20 18.40 18.60 18.800

200000

400000

600000

800000

1000000

Time-->


30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 1850

20000

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m/z-->

Abundance Average of 16.911 to 16.921 min.: 07131512.D\data.ms (-)95

174

75

50

698737 6257 81 14345 117106 128 148 155137 161111

AutoFind: Scans 2509, 2510, 2511; Background Corrected with Scan 2499

| Target | Rel. to | Lower | Upper | Rel. | Raw | Result || Mass | Mass | Limit% | Limit% | Abn% | Abn | Pass/Fail |----------------------------------------------------------------------| 50 | 95 | 8 | 40 | 18.5 | 28411 | PASS || 75 | 95 | 30 | 66 | 47.1 | 72395 | PASS || 95 | 95 | 100 | 100 | 100.0 | 153771 | PASS || 96 | 95 | 5 | 9 | 6.6 | 10092 | PASS || 173 | 174 | 0.00 | 2 | 0.0 | 0 | PASS || 174 | 95 | 50 | 120 | 77.2 | 118707 | PASS || 175 | 174 | 4 | 9 | 7.8 | 9286 | PASS || 176 | 174 | 93 | 101 | 95.4 | 113213 | PASS || 177 | 176 | 5 | 9 | 6.4 | 7281 | PASS |----------------------------------------------------------------------

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Data Path : I:\MS09\Data\2015_08\04\ Data File : 08041502.D Acq On : 4 Aug 2015 6:14 Operator : SC Sample : CCV R9080415_25ng Misc : S29-07071501/S29-07081503 (8/6) ALS Vial : 15 Sample Multiplier: 1



15.00 15.20 15.40 15.60 15.80 16.00 16.20 16.40 16.60 16.80 17.00 17.20 17.40 17.60 17.80 18.00 18.20 18.40 18.60 18.800

1000000

2000000

3000000

4000000

5000000

Time-->


25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 1850

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m/z-->


174

75

5069

876137 8156 14345 117104 128 148 155137 161



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BFB

Data Path : I:\MS09\Data\2015_08\05\ Data File : 08051502.D Acq On : 5 Aug 2015 4:14 Operator : SC Sample : CCV R9080515_25ng Misc : S29-07071501/S29-07081503 (8/6) ALS Vial : 15 Sample Multiplier: 1



15.00 15.20 15.40 15.60 15.80 16.00 16.20 16.40 16.60 16.80 17.00 17.20 17.40 17.60 17.80 18.00 18.20 18.40 18.60 18.800

1000000

2000000

3000000

4000000

5000000

6000000

Time-->


25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 105 110 115 120 125 130 135 140 145 150 155 160 165 170 175 180 1850

50000

100000

150000

m/z-->


174

75

5068

8737 61 8156 14145 117 128106 148 155135 160112



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Date/Time File Name Sample ID Misc Info Operator Vial Comment

1 7/13/15 11:31 07131501.D Blank (100mL) S29-07071501 SC 2

2 7/13/15 12:05 07131502.D Blank (100mL) S29-07071501 SC 2

3 7/13/15 12:39 07131503.D Blank (100mL) S29-07071501 SC 2

4 7/13/15 13:12 07131504.D Blank (100mL) S29-07071501 SC 2

5 7/13/15 13:46 07131505.D Blank (100mL) S29-07071501 SC 2

6 7/13/15 14:28 07131506.D Blank (100mL) S29-07071501 SC 2

7 7/13/15 15:18 07131507.D Blank (100mL) S29-07071501 SC 2

8 7/13/15 15:51 07131508.D Blank (100mL) S29-07071501 SC 2

9 7/13/15 16:25 07131509.D 0.5ng std check S29-07071501 SC 5

10 7/13/15 16:59 07131510.D 25ng std check S29-07071501 SC 6

11 7/13/15 17:33 07131511.D Blank (100mL) S29-07071501 SC 2

12 7/13/15 18:07 07131512.D 12.5ng TO-15 BFB STD S29-07071501 SC 2

13 7/13/15 18:41 07131513.D 0.08ng TO-15 ICAL STD S29-07071501/S29-07111510 (8/9) SC 3






19 7/13/15 22:06 07131519.D 25ng TO-15 ICAL STD S29-07071501/S29-07081503 (8/6) SC 6



22 7/14/15 12:01 07131522.D Blank (100mL) S29-07071501 SC 2

23 7/14/15 12:34 07131523.D 25ng TO-15 ICV STD S29-07071501/S29-07141502 (8/12) SC 16

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1 8/4/15 5:40 08041501.D System Check S29-07071501/S29-07081503 (8/6) SC 15 Pass

2 8/4/15 6:14 08041502.D CCV R9080415_25ng S29-07071501/S29-07081503 (8/6) SC 15 Pass

3 8/4/15 6:48 08041503.D CCV C9080415_5.0ng S29-07071501/S29-07131504 (8/11) SC 2 Pass

4 8/4/15 7:22 08041504.D MB R9080415_1000mL S29-07071501 SC 2 Pass

5 8/4/15 7:55 08041505.D LCS R9080415_25ng S29-07071501/S29-07141502 (8/12) SC 16 Pass

6 8/4/15 8:29 08041506.D LCSD R9080415_25ng S29-07071501/S29-07141502 (8/12) SC 16 Pass

7 8/4/15 9:10 08041507.D P1503087-001Dil (0.1mL) S29-07071501 SC 1

8 8/4/15 9:46 08041508.D P1503117-001Dil (2.0mL) S29-07071501 SC 1

9 8/4/15 10:22 08041509.D P1503034-003Dil (10mL) S29-07071501 SC 1

10 8/4/15 10:56 08041510.D P1503034-001Dil (25mL) S29-07071501 SC 5

11 8/4/15 11:29 08041511.D P1503034-002Dil (25mL) S29-07071501 SC 6

12 8/4/15 12:03 08041512.D P1503117-002 (1000mL) S29-07071501 SC 12

13 8/4/15 12:37 08041513.D P1503085-002Dil (10mL) S29-07071501 SC 1

14 8/4/15 13:11 08041514.D P1503149-005 (100mL) S29-07071501 SC 5

15 8/4/15 13:45 08041515.D P1503155-001 (100mL) S29-07071501 SC 6

16 8/4/15 14:18 08041516.D P1503155-002 (100mL) S29-07071501 SC 7

17 8/4/15 14:52 08041517.D P1503155-003 (35mL) S29-07071501 SC 8

18 8/4/15 15:26 08041518.D P1503155-003 dup(35mL) S29-07071501 SC 8 Pass

19 8/4/15 15:59 08041519.D P1503155-001Dil (25mL) S29-07071501 SC 6

20 8/4/15 17:01 08041520.D P1503087-002Dil (4.0mL) S29-07071501 SC 1 cf

21 8/4/15 17:34 08041521.D P1503149-001 (400mL) S29-07071501 SC 9

22 8/4/15 18:08 08041522.D P1503149-002 (400mL) S29-07071501 SC 10

23 8/4/15 18:42 08041523.D P1503149-003 (400mL) S29-07071501 SC 11

24 8/4/15 19:16 08041524.D P1503149-004 (400mL) S29-07071501 SC 12

25 8/4/15 19:50 08041525.D P1503012-001 (20mL) S29-07071501 SC 13

26 8/4/15 20:24 08041526.D P1503012-002 (20mL) S29-07071501 SC 14

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1 8/5/15 3:40 08051501.D System Check S29-07071501/S29-07081503 (8/6) SC 15 Pass

2 8/5/15 4:14 08051502.D CCV R9080515_25ng S29-07071501/S29-07081503 (8/6) SC 15 Pass

3 8/5/15 4:48 08051503.D CCV C9080515_5.0ng S29-07071501/S29-07131504 (8/11) SC 2 Pass

4 8/5/15 5:22 08051504.D MB R9080515_1000mL S29-07071501 SC 2 Pass

5 8/5/15 5:56 08051505.D LCS R9080515_25ng S29-07071501/S29-07141502 (8/12) SC 16 Pass

6 8/5/15 6:30 08051506.D LCSD R9080515_25ng S29-07071501/S29-07141502 (8/12) SC 16 Pass

7 8/5/15 7:03 08051507.D P1503113-001 (1000mL) S29-07071501 SC 3

8 8/5/15 7:37 08051508.D P1503113-002 (1000mL) S29-07071501 SC 4

9 8/5/15 8:11 08051509.D P1503113-003 (1000mL) S29-07071501 SC 5

10 8/5/15 8:45 08051510.D P1503113-004 (1000mL) S29-07071501 SC 6

11 8/5/15 9:19 08051511.D P1503113-005 (1000mL) S29-07071501 SC 7

12 8/5/15 9:53 08051512.D P1503113-006 (1000mL) S29-07071501 SC 8

13 8/5/15 10:27 08051513.D P1503113-006dup (1000mL) S29-07071501 SC 8 Pass

14 8/5/15 11:01 08051514.D P1503149-003Dil (40mL) S29-07071501 SC 11

15 8/5/15 11:35 08051515.D P1503149-004Dil (40mL) S29-07071501 SC 12

16 8/5/15 12:08 08051516.D P1503012-001 (200mL) S29-07071501 SC 13

17 8/5/15 12:49 08051517.D P1503087-002Dil (4.0mL) S29-07071501 SC 1

18 8/5/15 13:23 08051518.D P1503155-001 (80mL) S29-07071501 SC 9

19 8/5/15 13:57 08051519.D CCV Me9080515_50ng S29-07071501/S29-07271505 (8/26) SC 12 Pass

20 8/5/15 14:31 08051520.D P1503192-001 (100mL) S29-07071501 SC 10

21 8/5/15 15:04 08051521.D P1503192-002 (100mL) S29-07071501 SC 11

22 8/5/15 15:39 08051522.D Chamber QC (1000mL) S29-07071501 SC 13

23 8/5/15 16:30 08051523.D Blank (100mL) S29-07071501 SC 2

24 8/5/15 17:11 08051524.D MB Me9080515_1000mL S29-07071501 SC 2 Pass

25 8/5/15 17:46 08051525.D LCS Me9080515_100ng S29-07071501/S29-07271507 (8/26) SC 14 Pass

26 8/5/15 18:20 08051526.D LCSD Me9080515_100ng S29-07071501/S29-07271507 (8/26) SC 14 Pass

27 8/5/15 18:54 08051527.D P1502638-001 (1000mL) S29-07071501 SC 9

28 8/5/15 19:28 08051528.D P1502817-001 (1000mL) S29-07071501 SC 10

29 8/5/15 20:02 08051529.D P1502884-001 (1000mL) S29-07071501 SC 11

30 8/5/15 20:37 08051530.D P1502885-001 (1000mL) S29-07071501 SC 12

31 8/5/15 21:11 08051531.D P1502934-001 (1000mL) S29-07071501 SC 13

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ATTACHMENT 3

Tier 2 Air Screening Risk Assessment for VOCs to Nearest Receptor, Approximately 75 Meters from Stack, Pemaco Superfund Site,

Maywood, California

Attachment3Tier2ScreeningRiskAssessmentforVOCstoNearestReceptor

Approximately75MetersfromStackPemacoSuperfundSite,MaywoodCalifornia

Effluent 1 Mass flow rate2Average Air

Concentration3 Predicted Inhalation DoseCancerPotency4

Maximum Individual Cancer Risk

Chronic Reference Exposure Level

Chronic Hazard Index

Acute Reference Exposure Level4

Acute Hazard Index4

Compound Concentration Qlbs Qton Cair Concentrations DI CP MICR RELC HIC RELA HIAug/m3 lbs/yr ton/yr mg/m3 ppmv mg/kg/day (mg/kg‐day)‐1 ǳƎ/m 3

1,1,1‐Trichloroethane 4.3 2.4E‐02 1.20E‐05 8.2E‐05 0.0000000151 2.4E‐08 NR NA 1000 8.24E‐08 3900 8.7E‐111,1,2,2‐Tetrachloroethane 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 2.0E‐01 0.0E+00 NR NA NR NA1,1,2‐Trichloro‐1,2,2‐Trifluoroethane (Freon 113) 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA1,1,2‐Trichloroethane 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA1,1‐Dichloroethane 8.6 4.8E‐02 2.40E‐05 1.6E‐04 0.0000000407 4.8E‐08 5.7E‐03 2.7E‐10 NR NA NR NA1,1‐Dichloroethene 55 3.1E‐01 1.54E‐04 1.1E‐03 0.0000002660 3.1E‐07 NR NA 70 1.51E‐05 NR NA1,2,4‐Trichlorobenzene 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA1,2,4‐Trimethylbenzene 1.2 6.7E‐03 3.35E‐06 2.3E‐05 0.0000000047 6.7E‐09 NR NA NR NA NR NA1,2‐Dibromoethane 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 2.5E‐01 0.0E+00 0.8 0.00E+00 NR NA1,2‐Dichlorobenzene 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA1,2‐Dichloroethane 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 7.2E‐02 0.0E+00 400 0.00E+00 NR NA1,2‐Dichloropropane 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA1,2‐Dichlorotetrafluoroethane (Freon 114) 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA1,3,5‐Trimethylbenzene 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NA1,3‐Dichlorobenzene 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA 3900 0.0E+001,4‐Dichlorobenzene 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 4.0E‐02 0.0E+00 800 0.00E+00 NR NA1,4‐Dioxane 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 2.7E‐02 0.0E+00 3000 0.00E+00 3000 0.0E+002‐Butanone (Methyl ethyl ketone) 5.5 3.1E‐02 1.54E‐05 1.1E‐04 0.0000000358 3.1E‐08 NR NA NR NA 13000 3.3E‐11Acetone 69 3.9E‐01 1.93E‐04 1.3E‐03 0.0000002009 3.8E‐07 NR NA NR NA NR NABenzene 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 1.0E‐01 0.0E+00 60 0.00E+00 1300 0.0E+00Bromomethane 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 5 0.00E+00 NR NACarbon Disulfide 0.81 4.5E‐03 2.26E‐06 1.6E‐05 0.0000000050 4.5E‐09 NR NA 800 1.94E‐08 6200 1.0E‐11Carbon tetrachloride 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 1.5E‐01 0.0E+00 40 0.00E+00 NR NAChlorobenzene 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 1000 0.00E+00 1900 0.0E+00Chloroethane 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 30000 0.00E+00 NR NAChloroform 5.2 2.9E‐02 1.45E‐05 1.0E‐04 0.0000000204 2.9E‐08 1.9E‐02 5.5E‐10 300 3.32E‐07 NR NAChloromethane 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NAcis‐1,2‐Dichloroethene 160 8.9E‐01 4.47E‐04 3.1E‐03 0.0000007737 8.9E‐07 NR NA NR NA NR NAcis‐1,3‐Dichloropropene 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NACyclohexane 450 2.5E+00 1.26E‐03 8.6E‐03 0.0000025064 2.5E‐06 NR NA NR NA NR NADichlorodifluoromethane (Freon 12) 0.74 4.1E‐03 2.07E‐06 1.4E‐05 0.0000000027 4.1E‐09 NR NA NR NA NR NADimethyl octane 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NAEthyl benzene 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 8.7E‐03 0.0E+00 2000 0.00E+00 NR NAHexachloro‐1,3‐Butadiene 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NAIsopropanol 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 7000 0.00E+00 150 0.0E+00m/p Xylene 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 700 0.00E+00 22000 0.0E+00Methyl ethyl benzene 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NAMethylene chloride 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 30000 0.00E+00 3200 0.0E+00N‐Hexane 160 8.9E‐01 4.47E‐04 3.1E‐03 0.0000008703 8.9E‐07 NR NA 7000 4.38E‐07 NR NAo‐Xylene 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 700 0.00E+00 22000 0.0E+00Propylene 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 3000 0.00E+00 NR NAStyrene 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 900 0.00E+00 21000 0.0E+00Tert‐Butyl Methyl Ether (MTBE) 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 1.8E‐03 0.0E+00 8000 0.00E+00 NR NATetrachloroethene 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 2.1E‐02 0.0E+00 35 0.00E+00 NR NAToluene 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 300 0.00E+00 37000 0.0E+00trans‐1,2‐Dichloroethene 5.0 2.8E‐02 1.40E‐05 9.6E‐05 0.0000000242 2.8E‐08 NR NA NR NA NR NAtrans‐1,3‐Dichloropropene 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NATrichloroethene 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 7.0E‐03 0.0E+00 600 0.00E+00 NR NATrichlorofluoromethane 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA NR NA NR NAVinyl Chloride 0.56 3.1E‐03 1.56E‐06 1.1E‐05 0.0000000042 3.1E‐09 2.7E‐01 8.4E‐10 NR NA 180000 2.5E‐13Xylenes (total) 0 0.0E+00 0.00E+00 0.0E+00 0.0000000000 0.0E+00 NR NA 700 0.00E+00 22000 0.0E+00

Total 0.0000047700 1.66E‐09 1.59E‐05 1.31E‐10

Notes:1. Mass flux rate is based on a volumetric flow rate of 170.2 standard cubic feet per minute (scfm).2. Average air concentration and dispersion factor at nearest receptor approximately 75 meters from stack. 6. Zero was used for the non‐detected results.3. Cancer Risk and Chronic Hazard Index to nearest receptor approximately 75 meters from stack. 7. NA = not applicable; NR = not reported.

Results for vapor sample collected at SP‐108 (final effluent) on 7/23/2015 (TO‐15SIM method)

Source: Earth Tech, Inc. 2007. SCAQMD ‐ Tier 2 Toxic Air Contaminant Emissions Modeling, Pemaco Superfund Site, 5050 East Saluson Avenue, Maywood, Calidfornia. February.

5. Bolded results indicate positive detection.

4. South Coast Air Quality Management District, July 1, 2005 Risk Assessment Procedures for Rules 1401 and 212 Version7.0, Permit Application Package "L" Rules 1401 and 212 Version 7.0,

8. The COCs 2‐Hexanone, Ethanol, Naphthalene, and Tetrahydrofuran were not included in the original Tier 2 Screening Risk Assessment model. Detected concentrations ofthese COCs in plant vapor effluent during the July 2015 sampling event (0.95 J ug/m 3 for 2‐hexanone, 4.8 J ug/m3 for Ethanol, 1.2 J ug/m3 for Naphthalene, and 14 ug/m3 for Tetrahydrofuran) were assessed using the highest Cancer Potency factor from the original model (2.7E‐01, for Vinyl Chloride). The resulting total Maximum Individual Cancer Risk (approximately 3.31E‐8) remains far below the one‐in‐a‐million (1.0E‐6) threshold.

OTIE

Attachment 3Tier 2 Screening Risk Assessment for VOCs to Nearest Receptor

Page 1 of 1