united states department of the interior · vgs venice gathering system, l.l.c. 4200 research...

United States Department of the Interior BUREAU OF SAFETY AND ENVIRONMENTAL ENFORCEMENT

Gulf of Mexico OCS Region 1201 Elmwood Park Boulevard New Orleans, LA 70123-2394

Januarys, 2019 In Reply Refer To: GE 1035A

Connie Goers

Venice Gathering System, LLC 4200 Research Forest Drive. Suite 230 The Woodlands, TX 77381

Reference is made to Venice Gathering System, LLC's (VGS) Right-of-way (ROW) decommissioning application dated November 15, 2018, and received by this office on November 20, 2018. for Pipeline Segment Number (PSN) 10874. ROW No. OCS-G 15992.

Specifically, VGS requests to decommission PSN(s) 10874 in-place.

In accordance with 30 CFR 250.142, a departure is requested from 30 CFR 250.1751(d).

The table below describes the pipeline segment(s) pertaining to the aforementioned application:

PSN Size (NPS)

Length (feet)

Service Origin Termination

10874 20" 152.848 Gas Platform A

South Timbalier Block 265

Platform G South Timbalier

Block 151

Pursuant to 30 CFR 250.1751 (d), your request to decommission PSN(s) 10874 in-place is hereby denied due to the following: Pursuant to 30 CFR 250.1751 (d), BSEE will only allow seawater to remain in the pipeline i f decommissioning in place. In order to decommission this pipeline, it must be flushed and filled with seawater, or it must be removed.

Sincerely,

(for) Bryan A. Domangue Acting Regional Supervisor Regional Field Operations

VGS Venice Gathering System, L.L.C.

4200 Research Forest Drive, Suite 230 The Woodlands, Texas 77381

281.681.9500

November 15,2018

U.S. Department of the Interior tmm^w^bmm»ti^Mmi{M] Bureau of Safety and Environmental Enforcement R E C E I V E D 1201 Elmwood Park Boulevard New Orleans, Louisiana 70123-2394 NOV 20 201B

Attention: Forna Diphicyl ^ p ^ ^ T " Pipeline Section

RE: Request for Proposed Decommissioning of 20-Inch Gas Right-of-Way Pipeline (ROW No. G15992/Segment No. 10874) Originating at a Capped End in South Timbalier Block 265 and Terminating at South Timbalier Block 151 G-CMP Platform, OCS Federal Waters, Gulf of Mexico, Offshore, Louisiana

Mr. Diphicyl:

Venice Gathering System, L.L.C. (VGS) is requesting your review and consideration of the proposed decommissioning procedure and departure from Title 30 CFR Part 250.1751(d) pertaining to flushing the referenced pipeline segment with seawater.

Summani/Histon/

The referenced pipeiino segment was installed in 1996 and ultimately placed out of service in 2011 by the former VGS owners. Subsequently, your office approved a 5-year inactive right-of-way to determine future utility. VGS ultimately submitted a request to complete the decommissioning by leaving the inhibited seawater is place, and disconnecting the line pipe from the South Timbalier Block 151 G-CMP Platform; which was subsequently denied by your office. Subsequently, the VGS system was acquired by new owners; of which we submitted requests for time extensions to review for future utility and research the ongoing issues with the applicable agencies regarding denial of leaving inhibited seawater in place during decommissioning of the pipeline.

Prior to initiating the flush and fi l l operations, the prior VGS owners initiated a research toxicity tost in March 2010 using artificial soawator and Coastal Chemical's N-Spec 304 corrosion inhibitor mixed at 1000 ppm.

Request for Proposed Decommissioning oflO-bich Gas Right-of-Way Pipeline South Timbalier Block 265 Capped End to South Timbalier Block 151 G-CMP Platform ROW OCS-G 15992/Segtnent No. 10874) November 15,2018 Page Two

This test passed the EPA Region VI NPDES General Permit GMG290000 for discharging overboard. The pipeline was placed out of service during September 2011 by pigging, flushing and filling the pipeline with inhibited seawater, and disconnected from the South Timbalier Block 265 A Platform. A review of our records, and information supplemented by Coastal Chemical; the N-SPEC 304 was applied at +/-523 PPM in the flushing procedure with seawater (total volume of approximately 55,123 barrels).

The N-SPEC 304 chemical product is a film forming amine, which creates a tenacious bond with mild steel on the interior pipe wall to form a film barrier throughout the metal surface against corrosive conditions. To complete the final decommissioning as proposed, an additional acute toxicity test was initiated during October 2018 at a directed 50 PPM to address any potential residual entrained in the seawater which may not be bonded to the interior wall surfaces. This test was designed to replicate the amount of chemical exiting in the pipeline at 50 PPM and a worst case scenario discharge. That 50 PPM sample was created in the lab with fresh N-SPEC 304. -Based on the table provided in the NPDES GMG 2900000 General Permit, this test passed the highest Critical Dilution for any combination of pipe diameters and discharge rates. Therefore, whether the leak is a slow leak from a pinhole or results from a complete rupture of the pipeline, the worst case scenario is a dilution of 24.7% chemically treated water. This test not only passed at the 24.7% effluent level, but also passed at the 98% effluent level. In other words, the organisms had no survival issues in a 48-hour acute toxicity test when they were subjected to a concentration made of 98% of the chemically treated water mixed with just 2% lab created seawater. Copies of both toxicity test results are included for vour information; of which we could arrange a discussion or meeting with your office and a subject matter expert on the results cited above.

Enclosed is a proposed decommissioning application with supporting documentation to allow the inhibited seawater to remain in place based on the supporting test data and supporting technical data pertaining to the accidental discharge of this effluent.

• Proposed Decommissioning Procedure • Proposed Anchor Plot Drawing • Sherry and Element Laboratories Toxicity Test Reports • Pay Gov Receipt

Should you have any questions concerning this request, please contact Connie Goers, VGS Regulatory Representative at 281.210.30123 or [email protected].

ROW OCS-G 15992/Segment No. 10874) November 15,2018 Page Three

Sincerely,

Venice Gathering System, L.L.C.

Michael E. McCauley Operations General Manager

CJG/MEM Enclosures

2)

3)

4)

VGS South T i n k e r 265 to South T i m b a l i e r 1 5 1 G . C o i n p r e s s o r

Pipeline Abandonment SEGMENT NO. 10874

RESPONSIBLE PARTY

a. Pipeline Operator Name:

b. Address:

c. Contact Person(s).

PROPOSED PIPELINE ABANDONMENT

Venice Gathering System, LLC

d. Shore Base:

PIPELINE INFORMATIQN

a. Segment Number:

Origin

c

Structure Name: Area/Block: Coordinates:

Latitude: X

Terminus Structure Name: Area/Block: Coordinates:

Latitude X:

d. Install Date (Year):

e. Status:

f. Product:

g. Max Water Depth

PIPELINE DESCRIPTION

a. Configuration:

b. Size: Diameter:

c. Volume:

d. Buried:

PURPOSE

a. Descnption:

b. Reason:

4200 Reaearch Forest Drive Suite 230 The Woodlands. TX 77381

Connie Goers w/Arena-VGS Bryant Bradshaw w/ Arena-VGS"

Telephone No.(s): (281) 210-3123 (261) 2'io-3iT2"

GIS Dock, Fourchon. LA

10874 / ST-265-A (removed) to ST-151-G-Compressor / 20" Gas Condensate / 2220# MAOP

South Timbalier 265 "A" South Timbalier 265

28° 17' 54.637" 2.276,444.7

Complex ID No. ] OCS Lease:

Longitude: Y:

24246 12980

-90° 28' 28.690" •132,859.63

South Timbalier 151 G-Compressor South Timbalier 151

28° 37' 2.848" 2,347.870.22

Complex ID No.: " OCS Lease:

Longitude: 'V;

20618 00463

-90° 14' 57.692" -16,250.40

1996

OOS

Gas

200 ft

Capped end to Riser

20" Wall Thickness: 0.5

53.671 bbls

Length: 152,848'

(inclusive of 200 feet of riser on PF side)

Yos

Complete abandonment In place of SN10874 by removing tube tum at ST151 riser, installing plug in end of pipeline, and burying end to minimum 3' of cover.

Idle since 2011

c. Proposed Mod. Date: TBA

Issue Date: 11/14/18 Revision Page 1 of 2

VGS S o u t h T imba l ie r 265 to S o u t h T imba l ie r 151 G-Compresso r

P ipe l ine A b a n d o n m e n t

S E G M E N T NO. 10874

PROPOSED PIPELINE A B A N D O N M E N T (Con t i nued )

5) PROPOSED PROCEDURE

a. Brief description of the method to be used;

1) No te : S N I 0 8 7 4 has been p rev ious l y f l u shed to r emove al l h y d r o c a r b o n s (2011). The o r ig ina t ion p l a t f o r m ST265A has been removed (2013) and that end o f t h e l ine has been capped and bu r i ed .

2) ST 151 P la t fo rm Opera to rs to ver i fy SN10874 has been b leed d o w n to zero ps ig and is i so la ted f r o m all p ressure s o u r c e s on the p l a t f o rm .

3) Dive Suppo r t Vesse l (DSV) w i l l mob i l i ze to ST151 and set u p near SN10874 r iser.

4) D ivers w i l l cu t t h e p ipe l ine w i t h i n 5' o f the tube tu rn on the r iser and the p ipe l ine s ide . The t u b e tu rn w i l l be

recovered and b r o u g h t to sho re .

5) D ivers w i l l ins ta l l p lug in end of p ipe l ine a n d then bury end o f p ipe to a m i n i m u m of 3' be low na tura l b o t t o m .

P n e u m o read ings w i l l be taken t o c o n f i r m dep th o f cover .

6) The end of the p ipe l ine w i l l be covered w i t h 3:1 c e m e n t ' s a n d bags

7) Divers w i l l con t i nue r e m o v i n g the rema in i ng p o r t i o n s o f t h e riser and assoc ia ted c lamps up to the -MO e leva t ion . A l l mater ia ls w i l l be recovered a n d b r o u g h t to s h o r e .

8) A b a n d o n m e n t in p lace o f SN10874 is comp le te .

b. If using an anchored vessel , provide an anchor plat or maximum radius of anchors. see a t t ached

| Issue Date: 11/14/18 | Revision B Page 2 of 2

m Element MaterlaK T»chnok)gy P 337 235 0483

P > 1 0 T T ^ O T ^ t " ' 2417 West Pinhook Road F 337 233 6540 Laf»v«tt«. LA T 800 737 2378 70S08-3344 USA lnto.lalayette®element.com

o)emew.coni

48 HOUR ACUTE TOXICITY TEST

F O R

ARENA OFFSHORE, LP

N SPEC 304

(OCTOBER 2018)

REQUESTED BY: MIKE MCCAULEY ARENA OFFSHORE. LP [email protected]

PREPARED BY:

APPROVED BY;

DIANNE BOURQUE f T 6ATE DivisjoN SECRETARY

KEVIN S. DISCHLER DATE

OPERATIONS MANAGER. BIOASSAY SERVICES

THE RESULTS OF THIS ANALYSIS RELATE ONLY TO THE REFERENCED SAMPLE, AS IT WAS SUBMITTED TO ELEMENT MATERIALS TECHNOLOGY LAFAYETTE, LLC.

STATE OF LOUISIANA LABORATORY ACCREDITATION CERTIFICATE NO. 01997

Job Number: 18100680

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EXECUTIVE SUMMARY

SAMPLE TESTED: N SPEC 304

DATE/TIME TESTS STARTED: Mysidopsis bahia -10.17.18 @ 1515

Menidia beryllina -10,17.18 @ 1520

The test concentrations for this test were set at 0% (Control) 0%, 6%, 12.5%, 24.7%, 49%, and 98% effluent. The effluent was saltwater treated with N Spec 304 at 50 ppm. That dosing took place at Element Lafayette.

"•Critical Dilution: 24.7% Effluent

'"This test was performed using the highest possible Critical Dilution based on the table published in the NPDES Permit GMG290000 for Chemically Treated Seawater. Based on the results below, seawater treated with N-Spec 304 at a concentration of 50 ppm would easily pass the 46 Hour Toxicity tests at any Cntical Dilution presented in the permit

Mysidopsis bahia

Parameter No. TEM3E Survival (Pass=01 Fail=1) 0

Parameter No. TOM3E NOEC Survival (% effluent) 98

Parameter No. TQM3E Highest Coef. of Variation {%) 0.0

Menidia beryllina

Parameter No. TEM6B Survival (Pass=0, Fail=1) 0

Parameter No. TOM6B NOEC Survival (% effluent) 98

Parameter No. TQM6B Highest Coef. of Variation (%) 0.0

Parameter No. 22414 Whole Effluent Toxicity 98

Unless othenvise noted, all analyses were conducted using EPA approved methodologies and all test results meet all requirements of NELAC

Report Number 16100680

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INDEX

Executive Summary 2 Index 3 Introduction 4 Report Form 5 Source of Effluent & Dilution Water 5 Test Methods 6 Test Organisms 7 Quality Assurance 7

APPENDIX

A. Effluent and Dilution Water Physical and Chemical Data 8 B. Raw Biological Data 9 C. Data On Results 10-12 D. Field Report and Chain-Of-Custody Form 13 E. Quality Assurance 14

Report Number 18100680 3 of 21

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INTRODUCTION:

1. Toxicity Testing Requirements of Permit: a. Mysidopsis bahia (Mysid shrimp) acute static renewal 48-hour definitive toxicity test

EPA-821-R-02-012, as modified by NPDES General Pennit No. GMG 290000.

b. Menidia beryllina (Inland silversides) acute static renewal 48-hour definitive toxicity test EPA/821-R-02-012, as modified by NPDES General Permit No. GMG 290uCG.

2. Sample ID: N SPEC 304

3. Contract Laboratory: Element Materials Technology Lafayette, LLC Bioassay Division 2417 West Pinhook Road Lafayette. LA 70508 Ph. 337-235-0483

SOURCE OF SAMPLE AND DILUTION WATER;

1. Sample: a. Company: Arena Offshore (Coastal Chemical) b. Sampling Point: N SPEC 304 c. Sample collection method: Grab d. Preservation: N/A e. Physical and chemical data: See Appendix A

2. Dilution Water a. Source: Synthetic sea water using Crystal Seas Marine Mix b. Pretreatment: Processed through a carbon bed, a 4-bBd deionlzer system

(Water 8i Power Technology Systems) c. Preservation: N/A d. Physical and chemical characteristics: See Appendix A


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REPORT FORM for

FROM OIL AND GAS PRODUCTION FACILITY

PART I, FACILITY INFORMATION

Company: Arena Offshore (Coastal Chemical)

Sample Collected (date/time): N/A

Sampler Name: N/A

PART II. PRODUCTION INFORMATION

Water production: 25 bbls/day

PART III. GENERAL INFORMATION

Sample ID: N SPEC 304

Diameter of overboard discharge pipe: N/A


5 Of 21

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TEST METHODS

- Mysidopsis bahia

1. Toxicity test method used: EPA-821-R-02-012 2. End points of test: Survival 3. Deviations from reference method, if any. and the reason(s): none 4. Date and time test started: 10.17.18 @ 1515 5. Date and time test terminated: 10.19.18 @ 1440 6. Type of test chambers: 400 ml plastic cups 7. Volume of solution used per test chamber. 200 ml 8. Number of organisms per test chamber: 8 9. Number of replicate test chambers per treatment: 5

10. Test temperatures: 25±1 0 C

- Menidia beryllina

1. Toxicity test method used: EPA-821-R-02-012 2. End points of test: Survival 3. Deviations from reference method, if any, and the reason(s): none 4. Date and time test started: 10.17.18 @ 1520 5. Date and time test terminated: 10.19.18 @ 1432 6. Type of test chambers: 400 ml plastic cups 7. Volume of solution used per test chamber 200 ml 8. Number of organisms per test chamber: 8 9. Number of replicate test chambers per treatment: 5

10. Test temperature: 25±10 C


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TEST ORGANISM

- Mysidopsis bahia

1. Scientific name; Mysidopsis bahia 2. Age: 4 days 3. Lifestage: Juvenile 4. Source: Element 5. Diseases and treatment: None

- Menidia beryllina

1. Scientific name: Menidia beryllina 2. Age: 13 days 3. Life stage: Juvenile 4. Source: Element 5. Diseases and treatment: None

QUALITY ASSURANCE

A. Mysidopsis bahia 1. Reference toxicant: Sodium Dodecyl Sulfate, Acres BOI 37422 2. Date of most recent test: 09.27.18 3. Dilution water used in test: Synthetic sea water 4. Results of test: NOEC Survival: 6 ppm

5. Physical and chemical test methods used: As required by test method.

B. Inland Silversides 1. Reference toxicant: Sodium Dodecyl Sulfate, Acres BOI37422 3. Date of most recent test: 09.27.18 3. Dilution water used in test: Synthetic sea water 4. Results of test: NOEC Survival: 6 ppm

5. Physical and chemical test methods used: As required by test method.


7 of 21

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APPENDIX A

Effluent Physical and Chemical Data:

Temperature: Ambient

pH: 7.93

Salinity: 24.9 ppt

Dilution Water Physical and Chemical Data:

Dilution water was synthetic seawater.

Salinity = 26 ppt

pH = 7.9

Dissolved Oxygen = 6.6


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APPENDIX B

RAW BIOLOGICAL DATA

R e p o i t N u m b e r 1 8 1 0 0 6 8 0

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SUB-107 Rl

48 Hour Acute Toxicity under GMG290000 10-2011

Job Number:

Start Oate: End Date:

i v / i 7 / ( V ^ i m Source:

Client Name:

Test Species: F l « ^

i v i PFC

Hatch Date:

Job Number:

Start Oate: End Date: Source:

i v i PFC

Hatch Date:

•: 0 Hours . .y Concentration

•: 0 Hours . .y Control, 0% l l 1 % T M .1 % " 1 ^ % % Temperature "C (New) i ^ \ 1 "J s pH (New) i.Q 7.<! 79 Salinity ppt (New) 7 \ i s •? s l i DO mg/L (New) Lt Lt tL l-t L.t LL

0 Hours Survival A y B Y Y C Y f Jr y 5r y D r v Y \ E Y *

Technician h n ton 1 no r\n . n R

Control, 0% Is % l>.J % 41 % Temperature "C (New) 11 2 J 2 f > i pH (New) 1 V 79 7 ,9 Salinity ppt (New) V i \ i I i M DO mgn. (New) t.tr l .v l.Y ( y f> L l -Temperature °C (Old) X* DH (Old) •iu "7 t /> •ft* 1 w '/ w Salinity ppt (Old) 'din DO mg/L (Old) sstkj UK 24 Hours Survival

A « fl AS B •o V *& ' 0 C '0 f6 % D 'D $ E

Technician

Control, 0% L % ll.S % w % % Temperature X (Old) XX u pH (Old) Vvr > . * ? y 7. S-Salinity ppt (Old) U a 11 DO mg/L (Old) I., LA ts I i t i 48 Hours Survival

A s- Sr j? Sr B V Y C y Y V D Y Y y sr Y E V Sr Y Y Technician

Beginning DO acceptability: £4.0 mg/L Temperature Acceptability: 2WC. •If any replicate's D.O. falls below 4.0 mg/L, all concentrations will be aerated.* Ml ^ mililY

SLB-107 R l « Hour Acute Toxicity under eMG290000 For control ONLY - Salinity acceptability: 25 ±2 ppt

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SLB-107 Rl

Job Number:

Start Date: End Date:

48 Hour Acute Toxicity under 6M6290000 LlLSiLLkfl

10-2011

Source:

Client Name:

Test Species: Hatch Date: [ " f i / l f

Concenfrafeon

Control, 0% L % i i - r % i n % H % q sr % Temperature "C (New) ? c i i 7 i i s pH (New) 7.!l 7-9 7. 1 ) 7.< 7.9 Salinity ppt (New) \S \ J 2,1 7 X DO mg/L (New) t l t . t U t-t U 0 Hours Survival

A B V 0 y V sr sr 0 V V 5r E V V Technician n j i i i i —

24 Hours Control. 0% (, % \H.7% 4? % ^ % Temperature "C (New) ^ J 1 1 u l i pH (New) 1 Y 7 ir 75 Salinity ppt (New) M V u u Dd) mg/L (New) l.v- l.v u Lf Temperature "C ( d d )

pH (Old) •7.0 7-e? Salinity pp» (Old) iu 'Ac DO mg/L (Old) \i>.\ ie. 1 VC-l 24 Hours Survival

A B y, ft B % f l C D

E p 1

Technician •mn : : 48 Hours : Control, 0% L % U-S % l ^ . l % 41 %

Temperature a C (Old) > i xs 1 J IJ •i. S i s pH (Old) 7 V 7 V TV Salinity ppt (Old) I s ? t t l i t ? t. DO mg/L (Old) y LC LL i.r i , i -48 Hours Survival

A 5r ir Jr B > v- lr }r C Jr c V Sr D y Jr V E * V V Technician rtfi

Beginning DO acceptability: 24.0 mg/L Temperature Acceptability: 2S*1*C.

"If any replicate's 0.0. falls below 4.0 mg/L, all concentrations will be aerated.

For control ONLY - Salinity acceptability: 25 ± 2 ppt SLB-107 Rl 48 Hour Acute Toxldiy under GMG2900CO

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APPENDIX c

DATA ON RESULTS and

STATISTICAL PACKAGE

Repoit Number 18100680 12 Of 21

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TABLE 1 (Sheet 1 of 2)

Client: Arena Offshore Facility: N SPEC 304

MYSIDOPSIS BAHIA SURVIVAL

Date Initial Sample Collected: N/A

Test Initiated: (Date/Time) 10.17.18 @ 1515

DATA TABLE FOR MYSIDOPSIS BAHIA SURVIVAL

Effluent Concentrations Time of Reading REP

Control (0%) 6% 12.5% 24.7% 49% 98%

24Hours

A 100 100 100 100 100 100

24Hours B 100 100 100 100 100 100

24Hours 0 100 100 100 100 100 100 24Hours D 100 100 100 100 100 100

24Hours

E 100 100 100 100 100 100

48 Hours

A 100 100 100 100 100 100

48 Hours 6 100 100 100 100 100 100

48 Hours C 100 100 100 100 100 100 48 Hours D 100 100 100 100 100 100

48 Hours

E 100 100 100 100 100 100

Is the mean survival at 48 hours significantly less (p=:0.05) than the control survival at the critical dilution (24.7%)?: Yes X No

Result: NOEC Survival = 98% effluent


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TABLE 1 (Sheet 2 of 2)

Client: Arena Offshore Facility: N SPEC 304

MENIDIA BERYLLINA SURVIVAL

Date Initial Sample Collected: N/A

Test IniUated: (Date/Time) 10.17.18 @ 1520

DATA TABLE FOR INLAND SILVERSIDE SURVIVAL Effluent Concentrations

Time of Reading

REP Control (0%) 6% 12.5% 24.7% 49% 98%

24Hours

A 100 100 100 100 100 100

24Hours B 100 100 100 100 100 100

24Hours C 100 100 100 100 100 100 24Hours D 100 100 100 100 100 100

24Hours

E 100 100 100 100 100 100

48 Hours

A 100 100 100 100 100 100

48 Hours B 100 100 100 100 100 100

48 Hours C 100 100 75 100 100 100 48 Hours D 100 100 100 100 100 100

48 Hours

E 100 100 100 100 100 100

Is the mean survival at 48 hours significantly less (p=0.05) than the control survival at the critical dilution (24.7%)?: Yes X No

Result: NOEC Survival = 98% effluent

Report Nimber 18100680 14 Of 21

CETIS Analytical Report Report Date: Test Code:

23 0cM813:57 (p 1 of 2)

18100B80 102-0600-8546

Mysidopsis 96-h Acute Survival Test Element

Analysis ID: 18^303-6423 Endpoint: 48h Survival Rate CETIS Version: CETlSvl .8.7 Analyzed: 23 Oct-18 13:57 Analysis: Nonparametric-Control vs Treatments Official Results: Yos

Batch ID: 19-5326-1377 Test Type: Survival (96h) Analyst: Start Date: 23 Oct-1813:54 Protocol: EPA/821/R-02-012 (2002) Diluent: Laboratory Seawater Ending Date: 19Nov-18 Species: Mysidopsis bahia Brine: Crystal Sea Duration: 2Sd IDh Source: Element Age:

Sample ID: 08-2184-0105 Code: SW48MYS Client: Arena Sample Date: 17 Oct-1813:55 Material: Miscellaneous Discharge Project: Special Studies Receive Date: 1>Oct-1S Souree: GMG290000 Sample Age: 6d Station:

Sample Note: N-Spec 304 @ 50 PPM

Data Transform Zeta Alt Hyp Trials Seed NOEL LOEL TOEL TU

Angular (Corrected) NA Cs-T NA NA 58 >98 NA 1.02

Steel Many-One Rank Sum Test

Control vs C-% Test Stat Critical Ties DF P-Value P-Typo Declsion(a:5%)

SW Controi 6 27.6 16 1 8 0.8333 Asymp Non-Significant Effect 12.5 27.5 16 1 8 0.8333 Asymp Non-Significant Effect 24.7 27.6 16 1 8 0.8333 Asymp Non-Significant Effect 49 27.5 16 1 8 0.8333 Asymp Non-Significant Effect 98 27.5 16 1 8 0.8333 Asymp Non-Slgnlflcant Effect

ANOVA Table

Source Sum Squares Mean Square DF FStat P-Value Declsion(a:5%)

Between 0 0 5 65540 •O.0001 Signtficant Effect

Error 0 0 24 Total 0 29 "'

48h Survival Rate Summarv

C-% Control Type Count Mean S5% LGL 95% UCL Median Min Max Std Err CV% %Effect

0 SW Control 5 i i 1 1 1 1 0 0.0% 0.0%

6 5 i i 1 1 1 1 0 0.0% 0.0%

12.5 5 i i 1 1 1 1 0 0.0% 0.0%

24.7 5 i i 1 1 1 1 0 0.0% 0.0%

49 S i i 1 1 1 1 0 0.0% 0.0%

98 s i i 1 1 1 1 0 0.0% 0.0%

Angular (Corrected) Transformed Summary

C-% Control Type Count Mean 95% LCL 95% UCL Median Mln Max Std Err cv% %Effect

0 SW Control 5 1.393 1.393 1.393 1.393 1.393 1.393 0 0.0% 0.0%

6 5 1.393 1.393 1.393 1.393 1.393 1.393 0 0.0% 0.0%

12.5 6 1.393 1.393 1.393 1.393 1.393 1.393 0 0.0% 0.0%

24.7 5 1.393 1.393 1.393 1.393 1.393 1.393 0 0.0% 0.0%

49 5 1.393 1.393 1.393 1.393 1.393 1.393 0 0.0% 0.0%

98 5 1.393 1.393 1.393 1.393 1.393 1.393 0 0.0% 0.0%

48h Survival Rate Detail

C-% Control Type Rep 1 Rop 2 Rep 3 Rep 4 Rep 5

0 SW Control

6 1

1 1 1 1

1

1

1 1

12.5 i 1 1 1 1

24.7 i 1 1 1 1

49

98 ] 1 1

1 1 l 1

1

1

000-540-187-3 CETIS™ vl .8.7.14

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Analyst •.Jt. OA'


23 Oct-18 13:67 (p 2 of 2) 18100680 1 02-0600-8546

Mysidopsis 96-h Acute Survival Test Element

Analysis ID: 18-0303-8423 Endpoint: 48h Survival Rata CETIS Version: CETlSvl.8.7

Analyzed: 23 Oct-18 13:57 Analysis: NonparametrioControl vs Treatments Official Results: Yes

Angular (Corrected) Transformed Detail

c.% Control Type Rep 1 Rop 2 Rep 3 Rep 4 Rep 5 0 SW Control 1.393 1.393 1.393 1.393 1.393 6 1.393 1.393 1.393 1.393 1.393 12.6 1.393 1.393 1.393 1.393 1.393 24,7 1.393 1.393 1.393 1.393 1.393 49 1.393 1.393 1.393 1.393 1.393 S3 1.393 1.393 1.393 1.393 1.393

Graphics

u ka

u

u

M

000-540-187-3 CETIS™ vl.a.7.14

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Analyst:. OA;


23Ocl-18 14:05(p1 of 2) 18100680mb 112-3516-0373

Inland Silverside 98-h Acute Survival Test Element Analysis 1D: 00-4801 -8383 Endpoint: 48h Survival Rate CETIS Version: CETlSvl.8.7 Analyzed: 23 Oct-1814:05 Analysis: Nonparametric-Contfol vs Troalments Official Results: Yes

Batch ID: 07-4712-8500 Test Typo: Survival (96h) Analyst: Start Date: 23 Oct-1813:58 Protocol: EPA/821/R-02.012 (2002) Diluent: Laboratory Seawater Ending Date: 19 Nov-18 Species: Menidia beryllina Brine Ciystal Sea Duration: 26d lOh Source: Element Age:

Sample ID: 10-4555-7873 Code; SW48MB Client : Arena Sample Date: 17 Oct-18 14:01 Material: Miscellaneous Discharge Project: Special Studies Receive Date: 17 Oct-18 Source: GMG290000

Sample Age: 6d Station:

Sample Note: N-Spec 304 6 50 PPM

Data Transform Zeta Alt Hyp Trials Seed NOEL LOEL TOEL TU

Angular (Corrected) NA O T NA NA 98 >98 NA 1.02

Steel Many-One Rank Sum Test

Control vs C-% Tost Stat Critical Ties DF P-Value P-Type D€clslon(a:5%)

SW Control 6 27,5 16 1 8 0.8333 Asymp Non-Significant Effect

12.5 27.5 16 1 8 0.8333 Asymp Non-Significant Effect

24.7 27.5 16 1 8 0.8333 Asymp Non-Slgnlflcant Effect

49 27.5 16 1 8 0.8333 Asymp Non-Significant Effect

98 27.6 16 1 8 0.8333 Asymp Non-Signiflcant Effect

ANOVA Table

Source Sum Squares Mean Square DF FStat P-Value DBCision(a;6°/e)

Between 0 0 5 65540 <0.0001 Significant Effect

Error 0 0 24 Total 0 '29 "

48h Survival Rate Summary

C-% Control Type Count Moan 95% LCL 95% UCL Median Min Max Std Err CV% %Effect

0 SW Conlrol 6 1 1 1 1 1 1 0 0.0% 0.0%

6 5 1 1 1 1 1 i 0 0,0% 0.0%

12.5 5 1 1 1 1 1 1 0 0,0% 0.0%

24.7 5 1 1 1 1 1 1 0 0,0% 0.0%

49 5 1 1 1 1 1 1 0 0,0% 0.0%

98 5 1 1 1 1 1 1 0 0,0% 0,0%

Angular (Corrected) Transformed Summary

C-% Control Typo Count Mean 95% LCL 95% UCL Median Mln Max Std Err cv% %Effect

0 SW Control 5 1.393 1.393 1.393 1.393 1.393 1.393 0 0,0% 0.0%

G 5 1.303 1.393 1.393 1.393 1.393 1.393 0 0.0% 0.0%

12.5 5 1,393 1.393 1.393 1,393 1.393 1.393 0 0.0% 0,0%

24.7 & 1 393 1.393 1.393 1.393 1.393 1.393 0 0.0% 0.0%

49 fa 1.393 1.393 1.393 1.393 1.393 1.393 0 0.0% 0.0%

96 5 1.393 1.393 1.393 1.393 1,393 1.393 0 0.0% 0.0%

48h Survival Rate Detail

C-% Control Type Rep 1 Rop 2 Rop 3 Rep 4 RepS

0 SW Confrol 1 1 1 1 1

6 1 1 1 1 1

12.5 1 \ 1 1 1

24.7 1 1 1 1 1

45 1 1 1 1 1

98 1 1 1 1 1

C0O-540-187-3 CETIS ' " v l ,8,7,14

17 Of 21

Analyst:. OA:.


23 Oct-IS 14:05 (p 2 Of 2) 18100680nib 112-3516-0373

Inland Slivorsido 96-h Acute Survival Test Element

Analysis ID: 00-4801-8383 Endpoint: 48h Survival Rate CETIS Version: CETlSvl .8.7 Analyzed: 23 Oct-1814:05 Analysis: Nonparametric-Control vs Treatments Official Results: Yes

Angular (Corrected) Transformed Detail

C-% Control Type Rop 1 Rop 2 Rep 3 Rep 4 RepS

0 SW Control 1.393 1 393 1.393 1.393 1.393 6 1.393 1,393 1.393 1.393 1.393

12.8 1.393 1,393 1.393 1.393 1.393 24.7 1.393 1.393 1.393 1.393 1.393

49 1,393 1.393 1.393 1.393 1.393

98 1.393 1.393 1.393 1.393 1.303

Graphics

I-I «

M

D l

J l

M 0 0

IU •M -J.o 4J 4$ |M M

000-540-167-3 CET IS« v l .8.7.14

18 Of 21

Ana l ys t . OA:.

element"

APPENDIX D

FIELD REPORT AND CHAIN OF CUSTODY FORMS


element" Chain of Custody Laboratory Number

Company Name:

Contact Name:

Address:

City. State Zip:

Phone Number

Fax Number:

E-mail Address:

Client Infonnation: Billing Infonnation: PO Number: Project Name/Number: Page of PO Number: Project Name/Number: Matrix Code

DW = Drinking Waler WW » Waste Water GW = Ground Water AQ - Aqueous OT • Other SL = Sludge SOL = Sold 0 - Oil SO = Soil F - Food SW = Swab NG • Natural Gas NGL • Natural Gas liquid PW= Produced Water CF = Compleiion Fluid

Quote Number;

Project Name/Number: Matrix Code


— f t *

Quote Number;

Sampler's Signature

Matrix Code


Required QC Level

Sampler's Signature

Matrix Code


Required QC Level

Sampler's Signature

Matrix Code


Ext Ext: Bill Monlhly

• Y e s

• N o

Shipping Melhod:

UPS / FedEx / NOW

Matrix Code


Bill Monlhly

• Y e s

• N o

Shipping Melhod:

UPS / FedEx / NOW

Matrix Code


Bill Monlhly

• Y e s

• N o DHL / Element/^ancp Mail

Matrix Code


to o o

Which Regulations Apply: • R C R A • P O T W •NPDES •USDA/FDA •RECAP/RISC

•Drinking Water •Distribution •Special •Stale •Other

Sample ID/Description.

Turn Time •S tandard RUSH • l Day • 2 Day • O t h e r

(Rush tum limes wi ' incur a surcharge and musl be pre-approved by lab.)

Collection Information

Dale Time Crab/ CompoBilo Matrix

Conta iner

fi 8 o

f >

i l o —

Rj f t- a. o

Pres. Reques ted Tests C o m m e n t s

Relinquished by Date/Time Received by Date/Time Reld Notes:

1

Reld Notes:

2 jZj^S-^ Received at lab on ice?

• Y e s H N o T e m p : ^ ^ _ 3

Received at lab on ice?

• Y e s H N o T e m p : ^ ^ _

All samples submitled to Element Materials Technology for analysis are accepted on a custodial basis only. Ownership of the malerial remains with the client submitting the samples. Element Materials Technology reserves the right to return unused sampla portions.

8800 Norlh US 31 Columbus, IN

47201 USA P 812-375J>531 F 812-37WJ731

328 Ley Road. Suite 100 Fort Wayne, IN

4G82S USA P 260-471-7000 F 260-471-7777

909 Exec j l i vo Dr Wareiw. IN 4G580 USA

P 574-267-3305 F S74-269.6S69

3371 Cleveland Road, Suite 100A South Bend. IN

46628 USA P 574-277-0707 F 574-273-5699

2417 W. Pinhook Rd Lalayelte, LA

70508 USA P 337-235-0483 F 337-233-6S40

elemenf

APPENDIX E

QUALITY ASSURANCE

1. EFFLUENT SAMPLING AND HANDLING: A grab sample was submitted to the laboratory. In between use, the sample was maintained In a refrigerator at 4 0C. The test was renewed at 24hrs. with fresh dilutions.

2. DILUTION WATER; The dilution water for the acute test was synthetic seawater.

3. TEST ORGANISMS: The Mysidopsis bahia and Menidia beryllina used In this test were from in-house cultures. Routine reference toxicant tests are mn to determine sensitivity of the test organisms. Organisms used in this test were positively identified to species when purchased to start cultures and as introduced to provide fresh breeding stock.

4. FACILITIES, EQUIPMENT, AND TEST CHAMBERS: Facilities are designed especially for bioassay testing and culture of test animals. There are two environmental chambers with temperature controlled at 25° C + 1° C. All equipment which comes in contact with the test fluid is as specified by EPA 821-R-02-012. Test vessels and any other laboratory equipment which come in contact with the effluent were prepared prior to use as follows:

a. Soak 15 minutes in tap water and scrub with detergent. b. Rinse twice with tap water. c. Carefully rinse with fresh dilute (20% V:V) hydrochloric add to remove scale,

metals and bases. d. Rinse twice with delonized water. e. Rinse once with full strength acetone to remove organic compounds. f. Rinse well with deionized water.

5. CHEMICAL AND PHYSICAL ANALYSIS: Routine chemical and physical analyses are conducted on culture, holding, acclimation and dilution waters as well as on effluents to be tested. All such tests required by EPA protocol are conducted as a minimum. Instruments used for these analyses are routinely calibrated to manufacturer's specifications as well as checked against EPA suggested standards.

6. TEST CONDITIONS: The physical and chemical parameters of the test were monitored at the start of the test and daily during the lesl to insure lhat none of these would affect the test end points.

7. TEST ACCEPTABILITY: The control (0% effluent) must have a survival equal to or greater than 90% to be considered as valid.

Report Numbar 18100680

210121

' • S H E R R Y L A B O R A T O R I E S "

Job No. B10020038

TESTING TODAY. PROTECTING TOMORROW

WWW.SHERRYLABS.COM

CHEMICALLY TREATED SEAWATER BIOASSAY REPORT 48 HOUR ACUTE TOXICITY TEST

FOR

COASTAL CHEMICAL CO, LLC/BRENNTAG N-SPEC 304

(RESEARCH TESTING)

REQUESTED BY: COASTAL CHEMICAL Co.

TYSON J. DUPUIS

6133 HWY 90 EAST

BROUSSARD, L A 70518

PREPARED BY: DiANiy, BOURQUE

DIVISION SECRETARY

)ATB

REVIEWED BY:

APPROVED BY:

PARLEY U

ASST. DIRECTOR OF BIOASSAY SERVICES

KEVINSTDISCHLER

DIRECTOR OF BIOASSAY SERVICES

DATE

DATE

THE RESULTS OF THIS ANALYSIS RELATE ONLY TO THE REFERENCED SAMPLE, AS IT WAS SUBMITTED TO SHERRY LABORATORIES-LOUISIAN A.

STATE OF LOUSISANA LABORATORY ACCREDITATION CERTIFICATE NO. 01997

Total number of pages in report /

Testing Facility: Sherry Laboratories @ 2417 West Pinhook Road. Lafayette. LA 70508 (Ph. 800.737.2378) This document shall nol be reproduced except in full, wilhout the wrillen approval of Sherry Laboratories. LLC.

Job No. G10020038

EXECUTIVE SUMMARY

PRODUCT TESTED: N-SPEC 304

DATE/TIME TESTS STARTED: Mysidopsis bahia - 02.23.10 @ 1000

Menidia beryllina - 02.09.10 @ 1535

NOTE: A sample of Nspec 304 was delivered to Sherry Laboratories on 2.01.10. A 1000 ppm dilution of Nspec 304 was prepared using artificial seawater. That dilution was tested at the following concentrations:

Control (0%), 5%, 10%, 20%, 40% and 80% ofthe 1000 ppm Dilution.

> Critical Dilution : 20% effluent

Mysidosis bahia:

NOEC Survival: 20% effluent

Pass or Fail Statement: Whereas the No Observed Effect Concentration (NOEC) for this test is not less than 20% effluent, this Acute Bioassay PASSES the requirements set by the permit for this test.

Menidia beryllina:

NOEC Survival: 20% Effluent

Pass or Fail Statement: Whereas the No Observed Effect Concentration (NOEC) for the Menidia beryllina test is not less than 20% effluent, this Acute Bioassay Passes thc requirements set by the permit for this test.

Unless otherwise noted, all analyses were conducted using EPA approved methodologies and all test results meet all requirements of NELAC.

Testing Facility: Sherry Laboratories @ 2417 West Pinhook Road, Lafayette, LA 70508 (Ph. 800.737.2378) 2 Thia document shall not be reproduced, except in fuil, without the wrillen approval of Sherry Laboratories, LLC.

Job No. B10020()38

INDEX

Executive Summary 2 Index 3 Report Form 4 Introduction 5 Source of Effluent & Dilution Water 5 Test Methods 6 Test Organisms 7 Quality Assurance 7 Results 8

APPENDIX

A. Effluent and Dilution Water Physical and Chemical Data 9 B. Raw Biological Data 10 C. Data On Results 11-13 D. Field Report and Chain-Of-Custody Form 14 E. Quality Assurance 15-16

Testing Facility: Sherry Laboratories @ 2417 West Pinhook Road, Lafayelte, LA 70508 (Ph. 800.737.2378) 3 77;ii documenl shall nol be reproduced excepl in full, without the wrillen approval of Sherry Laboratories, LLC.

Job No. B10020038

REPORT FORM for

PRODUCED WATER FROM OIL AND GAS PRODUCTION FACILITIES

PART I . FACILITY INFORMATION

Company: Coastal Chemical Co, LLC

Product: N-Spec 304

Sampler Name: Ty Dupuis

PART I I . DISCHARGE INFORMATION

Maximum Daily Discharge Rate: <3,000 bbl/day

PART I I I . GENERAL INFORMATION

Description of chemical treatment: N/A

Describe location of sampling point: N/A

Diameter of overboard discharge pipe: 8 inches

Sample Salinity: 24.2 ppt

Testing Facility: Sherry Laboratories @ 2417 West Pinhook Road, Lafayette. LA 70508 (Ph. 800.737.2378) 4 This doaimeni shali nol be reproduced, excepl in fuii. wilhoul ihe wrillen approval of Sherry Laboralories.LLC.

Job No. B10020038

INTRODUCTION:

1. Toxicity Testing Requirements of Permit: a. Mysidopsis bahia (Mysid shrimp) acute static renewal 48 hour definitive toxicity test

EPA-821-R-02-012, or the most recent update thereof.

b. Menidia beryllina (Inland silversides) acute static renewal 48 hour definitive toxicity test EPA/821-R-02-012, or the most recent update thereof.

2. Sample ID: N-Spec 304

3. Contract Laboratory: Sherry Laboratories-LA Bioassay Division 2417 West Pinhook Road Lafayette. LA 70508 Ph. 337-237-7700

SOURCE OF EFFLUENT AND DILUTION WATER:

1. Effluent Samples: a. Sampling point: N/A b. Collection date and time: N/A c. Sampie collection method: Grab d. Preservation: Chilled to <6 0 C e. Physical and chemical data: See Appendix A

2. Dilution Water: a. Source: Synthetic sea water using Hawaiian Marine Mix c. Pretreatment: Processed through a carbon bed, a 4-bed deionizer system

(Siemens Water Systems) c. Preservation: N/A d. Physical and chemical characteristics: See Appendix A

Testing Facilily: Sherry Laboratories @ 2417 West Pinhook Road, Lafayene, LA 70508 (Ph. 800.737.2378) This documenl shall not be reproduced, except in fuil. without ihu written approval of Sherry Laboralories.LLC.

Job No. BI0O2UO38

TEST METHODS

- Mysidopsis bahia

1. Toxicity test method used: EPA-821-R-02-012 2. End points of test: Survival 3. Deviations from reference method, if any, and the reason(s): none 4. Date and time test started: 02.23.10 @ 1000 5. Date and time test terminated: 02.25.10 @ 1005 6. Type of test chambers: 400 ml plastic cups 7. Volume of solution used per test chamber: 200 ml 8. Number of organisms per test chamber: 8 9. Number of replicate test chambers per treatment: 5

10. Test temperatures: 25±1 0C

- Menidia beryllina

1. Toxicity test method used: EPA-821-R-02-012 2. End points of test: Survival 3. Deviations from reference method, if any, and the reason(s): none 4. Date and time test started: 02.09.10 @ 1535 5. Date and time test terminated: 02.11.10 @ 1600 6. Type of test chambers: 400 ml plastic cups 7. Volume of solution used per test chamber: 200 ml 8. Number of organisms per test chamber: 8 9. Number of replicate test chambers per treatment: 5

10. Test temperature:: 25±1 0C

Testing Faciiity: Sherry Laboratories @ 2417 West Pinhook Road. Lafayette. LA 70508 (Ph. 800.737.2378) Thia document siiaii not be reproduced, excepl in full, wilhoul the written approval of Sherry Laboralories.LLC.

Job No. B10020038

TEST ORGANISM

- Mysidopsis bahia

1. Scientific name; Mysidopsis bahia 2. Age: 5 days 3. Life stage: Juvenile 4. Source: In-house culture 5. Diseases and treatment: None

- Menidia beryllina

1. Scientific name: Menidia beryllina 2. Age: 14 days 3. Lifestage: Juvenile 4. Source: CK & Associates 5. Diseases and treatment: None

QUALITY ASSURANCE

A. Mysidopsis bahia 1. Reference toxicant: Sodium Dodecyl Sulfate, Sigma Aldrich 077K0137 2. Date of most recent test: 01/4/10 3. Dilution water used in test: Synthetic sea water 4. Results of test: NOEC Survival: 8 ppm 5. Physical and chemical test methods used: As required by test method.

B. Inland Silversides I . Reference toxicant: Sodium Dodecyl Sulfate, Sigma Aldrich 077K0137 3. Date of most recent test: 01/07/10 3. Dilution water used in test: Synthetic sea water 4. Results of test: NOEC Survival: 3 ppm 5. Physical and chemical test methods used: As required by test method.

Testing Facility: Sheny Laboratories @ 2417 West Pinhook Road, Lafayette. LA 70508 (Ph. 800.737.2378) This documenl shali nol be reproduced, excepl in full, wilhoul ihe wriuen approval of Sheny Laboralories.LLC.

Job No. HI0020038

RESULTS:

1. Raw biological data:

See Appendix B

2. Data on results:

See Appendix D

3. Statistical methods used to calculate end points:

Methods are listed with each specific end point.

4. QAdata:

See Appendix E

Testing Faciiity: Sherry Laboratories @ 2417 West Pinhook Road. Ufayette, LA 70508 (Ph. 800.737.2378) 8 This documenl shall not be reproduced, except in full, wilhoul the wrillen approval of Sherry Laboratories,!^.

Job No. B 100200.18

APPENDIX A

Effluent Physical and Chemical Data::

The effluent as received into the laboratory was light brown in color

Dilution Water Physical and Chemical Data:

Dilution water was synthetic seawater.

Salinity = 24 ppt

pH -8.0

Dissolved Oxygen = 7.3

Testing Facility: Sheny Laboratories @ 2417 West Pinhook Road. Lafayelte. LA 70508 (Ph. 800.737.2378) 9 This document shall nol be reproduced, except in full, wilhoul Ihe wrillen approval of Sherry Laboralories.LLC.

Job No. HI0020(13X

APPENDIX B

RAW BIOLOGICAL DATA

Testing Facility: Sherry Laboratories @ 2417 West Pinhook Road, Lafayette, LA 70508 (Ph. 800.737.2378) 10 Tliis document shall not be reproduced, except in fuii, without the wrillen approval of Sherry Laboralories.LLC.

SLB-107

48 Hour Acute Toxicity under GMG290000 Job Number: < K / O O t P o o ^ &

Date: I S E Q Date: ' . 2 ' - 1 1 . \ D | U D C >

Dec-09

Client Name:

Start End Source:

Test Spedes:

£± : Hatch Date:

0 Hours Concen/rat/on

0 Hours Control, 0% 5 % i'O % <fe % s» % Temperature °C (New) pH (New) t o Vf.o Salinity ppt (New) DO mg/L (New) ' W 0 Hours So/v/va/ 1'-°

A r B %-C ft | 1 D E p a Technician n

24 Hours Control. 0% ^ % ; o % ^ 0 % % % Temperature "C (New) > -T 3 5 > r pH (New) z.o ^ L> •3 1 Salinity ppi (New) -J M 3 f DO mg/l (New) - 7 ( - > > •7 >- -7 > ~7>

Temperature 0C (Old) >S > T pH (Old) 7. . 7 r Salinity ppi (Old) 9 T 5' DO mo/L (Old) '7 . O •7.3. 24 Hours Survival

A Jf O CJ 6 n t> C « D •/ I E H v 7 O

Technician ^

48 Hours Temperalcre °C (Old)

pH (Old) Salinity ppi (Old)

DO mgl (Old)

Control, 0%

1 2m 3 1 3

% N

48 Wours Su/v/va/ 7 z 2

%

z

A 6 6 8 a C <r D J O 0

E i Technician

SLB-107 48 Hour Acute Toxicity under GMG290000 xls

SLB-107

48 Hour Acute Toxicity under GMG290000 Job Number: Client Name: T c f i g ^ gbaMf ld i

Test Species: fttotlQi Source: SO^ . Hate

Dec-09

Start Date: t 2 ^ - \ T \ M - m End Date: j - Z S . i n >gr :ch Date;

Concentration Control, 0% S % t O % l o % H D %

Temperature "C (New) I S 1ft pH (New) f t * - = » . ^ S-.o V - 1 Salinity ppt (New) ±M DO mg/L (New) o . r ^ - O 3uS2 0 Hours Survival

A 9?-B

C f D 0 ft E > k Technician

24 Howrs Control, 0% / O % ^ . 0 % «V-o % % Temperature °C (New) 5 5 -pH (New) •7. i <i 0 e • * 1 Salinity ppi (New) 7 U v v t ;>>-. ^ «4 DO mo/L (New) "M Temperature "C (Old) ?< pH (Old) 7 ^ Salinity ppt (Old) §4 SI 5 ^ DO mg/L (Old) - 7 •£> 1

24 Hours Survival

A « « B i n C 1 4 D V 5 f k E 5 i P 7 Technician

48 Hours Control, 0% * % 10 % i o % MO % %

Temperature °C (Old) i.5 2^ A S

pH (Old) 1.1

Salinity ppt (Old) ^9 DO mg/L (Old) 1* in. 1.7. f t ? 48 Hours Survival

A y V g H \

B I ? O C r> D 5f 4. 9 E Z- a Technician J t u | 1

SLB-107 48 Hour Acute Toxialy under GMG290000.xls

Job No. B10020038

APPENDIX C

DATA ON RESULTS and

STATISTICAL PACKAGE

Testing Facility: Sheny Laboratories @ 2417 West Pinhook Road. Ufayette. LA 70508 (Ph. 800.737.2378) 11 77J/J documenl shall nol be reproduced excepl in full, wilhoul the written approval of Sherry Laboralories.LLC.

JobNo. U10020038

TABLE 1 (Sheet lof 2)

Client : Coastal Chemical CO, LLC Producl: N-Spcc 304

MYSIDOPSIS BAHIA SURVIVAL


DATA TABLE FOR MYSIDOPSIS BAHIA SURVIVAL

Effluent Concentrations Time of Reading

REP Control(0%) 5% 10% 20% 40% 80%

24Hours

A 100 100 100 100 100 87.5

24Hours B 100 100 100 100 100 87.5

24Hours C 100 100 100 100 100 50 24Hours D 100 100 100 100 62.5 100

24Hours

E 100 100 100 100 75 87.5

48 Hours

A 100 100 100 100 50 12.5

48 Hours B 10 100 100 100 25 0

48 Hours C 100 100 100 87.5 37.5 0 48 Hours D 87.5 100 100 75 25 0

48 Hours

E 87.5 100 100 87.5 25 0

Is the mean survival at 48 hours significanlly less (p=0.05) than the conlrol survival at the critical dilution (20%)?: Yes X No

NOEC Survival = 20% effluent

Testing Facility: Sherry Laboratories @ 2417 West Pinhook Road. Ufayette. LA 70508 (Ph. 800.737.2378) This documenl shall noi be reproduced excepl in full, wilhoul ihe wrillen approval of Sherry Laboralories.LLC.

12

JobNo. B10020038

TABLE 1 (Sheet 2 ofl)

Client : Coastal Chemical CO, LLC Product: N-Spcc 304

MENIDIA BKRYLLINA SURVIVAL


DATA TABLE FOR INLAND SILVERSIDE SURVIVAL Effluent Concentrations

Time of Reading REP

Control(0%) 5% 10% 20% 40% 80%

24Hours

A 100 100 100 100 0 0

24Hours B 100 87.5 100 100 37.5 0

24Hours C 100 100 100 87.5 37.5 0 24Hours D 100 100 100 100 12.5 0

24Hours

E 100 100 100 87.5 50 0

48 Hours

A 100 100 100 100 0 0

48 Hours B 100 87.5 100 100 25 0

48 Hours C 87.5 100 100 87.5 25 0 48 Hours D 100 100 100 100 0 0

48 Hours

E 87.5 100 100 S7.5 50 0

Is tlie mean survival at 48 hours significantly less (p=0.05) than the control survival at the critical dilution (20%)?: Yes _X_No

NOEC Survival - 20% effluent

Testing Facility: Sheny Laboratories @ 2417 West Pinhook Road, Lafayette, LA 70508 (Ph. 800.737.2378) nUl document shall not be reproduced except in full, without the written approval of Sherry Laboratories, LLC.

13

Misc. Discharge 48 Hour Acute-48 Hr Surv lv l B10020038

s Start Dale: End Date: Sample Date: Comments:

2/9/201015:35 Test ID: B10020038 Sample ID: 2/11/2010 16:00 Lab ID: -SHERRY LABORATORIES- Sample Type:

Protocol: FW-Acute-EPA821-R-02-012 Test Species:

Coastal Chemical-NSpeG304 / a , MISC-Miscellaneous ^ / MY. MyBldopcic b t i h igy^ / '

Conc-% 1 2 3 4 5 .C-Lab Control 1.0000 1.0000 0.8750 1.0000 0.8750

5 1.0000 0.8750 1.0000 1.0000 1.0000 10 1.0000 1.0000 1.0000 1.0000 1.0000 20 1.0000 1.0000 0.8750 1.0000 0.8750 40 0.0000 0.2500 0.2500 0.0000 0.5000 80 0.0000 0.0000 0.0000 0.0000 0.0000

Transform: Arcs In Square Root Rank 1-Tailed Conc-% Mean N-Mean Mean Mln Max CV% N Sum Critical

.C-Lab Control 0.9500 1.0000 1.3196 1.2094 1.3931 7.623 5 5 0.9750 1.0263 1.3564 1.2094 1.3931 6.055 G 30.00 17.00

10 1.0000 1.0526 1.3931 1.3931 1.3931 0.000 32.50 17.00 20 0.9500 1.0000 1.3196 1.2094 1.3931 7.623 5 27.50 17.00

•40 0.2000 0.2105 0.4376 0.1777 0.7854 59.463 6 15.00 17.00 80 0.0000 0.0000 0.1777 0.1777 0.1777 0.000 5

Auxiliary Tests Statistic Critical Skew Kurt Shapiro-Wilk's Test indicates non-normal distribution (p <= 0.01) 0.88424 0.888 0.05222 1.97935 Equality of variance cannot be confirmed Hvoothesis Test (1-tall, 0.05) NOEC LOEC ChV TU Steel's Many-One Rank Test 20 40 28.2843 5 Treatments vs LC-Lab Control

Page 1 ToxCalc V5.0.23 Reviewed by:_

Misc. Discharge 48 Hour Acute-48 Hr Survival Start Date: End Date: Sample Date: Comments:

2/9/201015:35 Test ID: Bl0020038 Sample ID: 2/11/2010 16:00 Lab ID: -SHERRY LABORATORIES- Sample Type:

Protocol: FW-Acute-EPA821-R-02-012 Test Species:

Coastal Chemical-NSpec304 MISC-Miscellaneo.us _ /

Conc-% 1 2 3 4 5 C-Lab Control 1.0000 1.0000 0.8750 1.0000 0.8750

5 1.0000 0.8750 1.0000 1.0000 1.0000 10 1.0000 1.0000 1.0000 1.0000 1.0000 20 1.0000 1.0000 0.8750 1.0000 0.8750 40 0.0000 0.2500 0.2500 0.0000 0.5000 80 0.0000 0.0000 0.0000 0.0000 0.0000

Transform: Arcsln Square Root Number Total Conc-% Mean N-Mean Mean Mln Max CV% N Resp Number

.C-Lab Control 0.9500 1.0000 1.3196 1.2094 1.3931 7.623 5 2 40 5 0.9750 1.0263 1.3564 1.2094 1.3931 6.055 5 1 40

10 1.0000 1.0526 1.3931 1.3931 1.3931 0.000 5 0 40 20 0.9500 1.0000 1.3196 1.2094 1.3931 7.623 5 2 40 40 0.2000 0.2105 0.4376 0.1777 0.7854 59.463 5 32 40 80 0.0000 0.0000 0.1777 0.1777 0.1777 0.000 5 40 40

Auxiliary Tests Statistic Critical Skew Kurt Shapiro-Wilk's Test Indicates non-normal distribution (p <= 0.01) Equality of variance cannot be confirmed

0.88424 0.888 0,05222 1.97935

Trimmed Spearman-Karbor Trim Level ECSO 95% CL

0.0% 5.0%

10.0% 20.0%

Auto-0.0%

32.031 31.700 31.196 30.668 32.031

29.127 28.764 28.239 28.225 29.127

35.225 34.934 34.463 33.322 35.225

Page 1 ToxCalc V5.0.23 Reviewed by

Test: MD48HRACU-Misc. Discharge 48 Hour Acute Test ID: B10020038 Species: MY-Mysidopsis bahia Protocol: FW-Acute-EPA821-R-02-012 Sample ID: Coastal Chemical-NSpec304 Sample Type: MISC-Miscellaneous Start Date: 2/9/2010 15:35 End Date: 2/11/2010 16:00 Lab ID: -SHERRY LABORATORIES-LA

Pos ID Rep Group Start 24 hr 48 Hr 72 Hr 96 Hr 10 Day Notes 1 1 LC-Lab Control 8 8 8 2 2 LC-Lab Control 8 8 8 3 3 LC-Lab Control 8 8 7 4 4 LC-Lab Control 8 8 8 5 5 LC-Lab Control 8 8 7 6 1 5.000 8 8 8 7 2 5.000 8 7 7 8 3 5.000 8 8 8 9 4 5.000 8 8 8 10 5 5.000 8 8 8 11 1 10.000 8 8 8 12 2 10.000 8 8 8 13 3 10.000 8 8 8 14 4 10.000 8 8 8 15 5 10.000 8 8 8 16 1 20.000 8 8 8 17 2 20.000 8 8 8 18 3 20.000 8 7 7 19 4 20.000 8 8 8 20 5 20.000 8 7 7 21 1 40.000 8 0 0 22 2 40.000 8 3 2 23 3 40.000 8 3 2 24 4 40.000 8 1 0 25 5 40.000 8 4 4

26 1 80.000 8 0 0 27 2 80.000 8 0 0 28 3 80.000 8 0 0 29 4 80.000 8 0 0 30 5 80.000 8 0 0

Comments:

Pagel ToxCalc 5.0 Reviewed by:.

Acute Fish Test-48 Hr Survival start Date: 2/23/2010 Test ID: 1E+07 Sample ID: Coastal Chemical End Date: 2/25/2010 Lab ID: SL-Sherry Laboratories Sample Type: PW-Produced Water Toxicity Sample Date: Protocol: EPAA 91-EPA/600/4-90/027F Test Species: MY-Mysldopsis bahia Comments:

MY-Mysldopsis bahia

Conc-% 1 2 3 4 5 B-Control 1.0000 1.0000 1.0000 0.8750 0.8750

5 1.0000 1.0000 1.0000 1.0000 1.0000 10 1.0000 1.0000 1.0000 1.0000 1.0000 20 1.0000 1.0000 0.8750 0.7500 0.8750 40 0.5000 0.2500 0.3750 0.2500 0.2500 80 0.1250 0.0000 0.0000 0.0000 0.0000

Transform: Arcsin Square Root Rank 1-Tailed Conc-% Mean N-Mean Mean Min Max CV% N Sum Critical

B-Control 0.9500 1.0000 1.3196 1.2094 1.3931 7.623 5 5 1.0000 1.0526 1.3931 1.3931 1.3931 0.000 5 32.50 16.00

10 1.0000 1.0526 1.3931 1.3931 1.3931 0.000 5 32.50 16.00 20 0.9000 0.9474 1.2504 1.0472 1.3931 11.683 5 24.00 16.00

*40 0.3250 0.3421 0.6031 0.5236 0.7854 19.502 5 15.00 16.00 •80 0.0250 0.0263 0.2144 0.1777 0.3614 38.301 5 15.00 16.00

Auxiliary Tests Statistic Critical Skew Kurt Shapiro-Wilk's Test indicates normal distribution (p > 0.01) 0.94437 0.9 0.21211 0.47546 Equality of variance cannot be confirmed Hypothesis Test (1-tail, 0.05) NOEC LOEC ChV TU Steel's Many-One Rank Test 20 40 28.2843 5 Treatments vs B-Control

Dose-Response Plot

e 1 ToxCalc V5.0.23 Reviewed

,, „_ _ Acute Fish Test-48 Hr Survival Start Date: 2/23/2010 Test ID: 1E+07 Sample ID: Coastal Chemical End Date: 2/25/2010 Lab ID: SL-Sherry Laboratories Sample Type: PW-Produced Water Toxicity Sample Date: Protocol: EPAA 91-EPA/600/4-90/027FTest Species: MY-Mysidopsis bahia Comments:

MY-Mysidopsis bahia

Conc-% 1 2 3 4 5 B-Control 1.0000 1.0000 1.0000 0.8750 0.8750

5 1.0000 1.0000 i.oooo 1.0000 1.0000 10 1.0000 1.0000 1.0000 1.0000 1.0000 20 1.0000 1.0000 0.8750 0.7500 0.8750 40 0.5000 0.2500 0.3750 0.2500 0.2500 80 0.1250 0.0000 0.0000 0.0000 0.0000

Transform: Arcsin Square Root Number Total Conc-% Mean ^J-Mean Mean Min Max CV% N Resp Number

B-Control 0.9500 1.0000 1.3196 1.2094 1.3931 7.623 5 2 40 5 1.0000 1.0526 1.3931 1.3931 1.3931 0.000 5 0 40

10 1.0000 1.0526 1.3931 1.3931 1.3931 0.000 5 0 40 20 0.9000 0.9474 1.2504 1.0472 1.3931 11.683 5 4 40 40 0.3250 0.3421 0.6031 0.5236 0.7854 19.502 5 27 40 80 0.0250 0.0263 0.2144 0.1777 0.3614 38.301 5 39 40

Auxiliary Tests Statistic Critical Skew 0.21211

Kurt Shapiro-Wilk's Test indicates normal distribution (p > 0.01) 0.94437 Equality of variance cannot be confirmed

0.47546

Parameter Value Maximum Likelihood-Probit

SE 95% Fiducial Limits Control Ch!-Sq Critical P-value Mu Sigma Iter Slope 5.69766 0.89393 3.94555 7.44976 0.05 1.59994 Intercept -3.7457 1.39544 -6.4807 -1.0106 TSCR 0.01647 0.01185 -0.0067 0.0397 1.0 • Point Probits % 95% Fiducial Limits 0.9-EC01 2.674 13.3864 8.40231 17.3445

0.9-

EC05 3.355 17.6309 12.3941 21.6047 0.8 -EC10 3.718 20.4191 15.2053 24.3565 0.7-EC15 3.964 22.5454 17.4208 26.4587

C EC20 4.158 24.3921 19.3787 28.3034 C

EC25 4.326 26.0965 21.2003 30.034 oo.s-

| 0.4 -EC40 4.747 30.9384 26.341 35.2041 oo.s-

| 0.4 -EC50 5.000 34.2739 29.7445 39.0875

oo.s-

| 0.4 -

ECSO 5.253 37.9689 33.3003 43.7738 0.3-EC75 5.674 45.0135 39.4476 53.816 0.2-ECSO 5.842 48.1589 41.9792 58.7073

0.2-

EC85 6.036 52.1037 45.0203 65.1393 0.1 -EC90 6.282 57.5293 49.0186 74.4592 0.0-EC95 6.645 66.6273 55.3839 91.147 EC99 7.326 87.753 69.1346 134.163

7.81472 0.66 1.53496 0.17551

1000 Dose %

Page 1 ToxCalc V5.0.23 Reviewed by:.

JobNo. B10020O38

APPENDIX D

FIELD REPORT A N D CHAIN OF CUSTODY FORMS

Testing Facility: Sherry Laboratories @ 2417 West Pinhook Road. Ufayette. LA 70508 (Ph. 800.737.2378) 14 This documenl shall nol be reproduced, excepl in full, wilhoul ihe wrillen approval of Sherry Laboralories.LLC.

rr SHERmrL^joratories Sherry Laboratories - Chain of Custody Record Labomiory Number:

Compuiy Name:

Conlacl Name

Addie«:

City. Sute. Zip:

Phone Number

Fix Number.

E-nuil Aikkesa:

Client Information: Billing Information: PO Number: Project Name/Number: Page of

I CX V C 1 ( r - f f h l ' C , |

PO Number: Project Name/Number: Matrix Code DW = Drinking Waier WW =r Wane Water GW« Ground Water AQ = Aqaoiu» OT> Other SL = Sludge SOL = Solid O-Ofl SO-Soil F = r-ood SW . Swab NO = Natural Gn NGL » Natural Cas Liquid PW t Pmdoced Water CF m Camptetion Fluid

Quote Number:

Project Name/Number: Matrix Code DW = Drinking Waier WW =r Wane Water GW« Ground Water AQ = Aqaoiu» OT> Other SL = Sludge SOL = Solid O-Ofl SO-Soil F = r-ood SW . Swab NO = Natural Gn NGL » Natural Cas Liquid PW t Pmdoced Water CF m Camptetion Fluid

_ J

Quote Number:

Sampler's Signature

Matrix Code DW = Drinking Waier WW =r Wane Water GW« Ground Water AQ = Aqaoiu» OT> Other SL = Sludge SOL = Solid O-Ofl SO-Soil F = r-ood SW . Swab NO = Natural Gn NGL » Natural Cas Liquid PW t Pmdoced Water CF m Camptetion Fluid

Required QC Level

Sampler's Signature


Required QC Level

Sampler's Signature


Ex«: Ext: Bill Monthly

• Y e s

• N o

Shipping Method:

UPS / FedEx / Airbome

DHL / Sherry / Hand / Mail


Bill Monthly

• Y e s

• N o

Shipping Method:




Bill Monthly

• Y e s

• N o

Shipping Method:




Which RegulaUons Apply: •RCRA •Drinking Water

•PCrrW •Disuibution

D NPDES DSpecial •USDA/FDA •State •RECAP/RISC •other

Turn Time (Rush tum • Standard times will incur RLTSH a surcharse and • 1 Day must be pre-• 2 Day approved by nother lab.)

Container Pres. KKItu slcd V M i Comments Which RegulaUons Apply: •RCRA •Drinking Water

•PCrrW •Disuibution

D NPDES DSpecial •USDA/FDA •State •RECAP/RISC •other

Turn Time (Rush tum • Standard times will incur RLTSH a surcharse and • 1 Day must be pre-• 2 Day approved by nother lab.) j 9

i

w <£

%0

Sample ID/Description Collection Infonmilion

Matrix

j 9 i

w <£

%0

Sample ID/Description Dale Time Cinlu Matrix

j 9 i

w <£

%0

X

%0 %0 %0 %0 %0 %0 %0 %0 %0 %0

Relinquished by Date/Time Received by Dale/Time Field Notes:

i

Field Notes:

2 Rcceivctl at lab on ice? t . b---r-

• V e s H N o Temp: 3 1~ : 1 ; • ;

Rcceivctl at lab on ice? t . b---r-

• V e s H N o Temp:

Al! samples submitled lo Sheny Laboratories for analysis are accepted on a custodial basis only. Ownership of ihe malerial remains with the clieni submitting the samples. Sherry Laboratories reserves the right to rctura unused sample portions.

MOl Imratatinn Dr»c. Suite 125 POBoxMV

Dalei Uie. IN 473M-0S69 765-378^103

Fax:

629WasMn|!lonSL Kullf m

ColunlHU. IN 472111 I12-37M831

ta «12-375-n731

2121 F. Wa-hioslnn Bltd. Fort WMlM^MMMl

Fax: 260-471-7777

560 South /.imnirr Road P.O. Box 1849

Watsao. IN 46581-1849 S74-267-3.W

Fax: 574-269-6569

2417 W. Plnlumk Rd Ijirnyrtle, LA 7*508

JJ7-235-048.»

Fax: vnta WW

1701 North Ironwooil Drive Suite I South Bead I.V 466S3

574-273-4599 Fax: 574-273-4599

KM

Job No. B10020038

APPENDIX E

QUALITY ASSURANCE

I . EFFLUENT SAMPLING AND HANDLING:A grab sample which was less than 36 hours old at the start ofthe test was used to start the test. The renewal fluid used on day two ofthe test was from the same sample. Immediately after the dilution was made, the sample was cooled and stored at the laboratory. In between use, the sample was maintained in a refrigerator at <6 0 C.

2. DILUTION WATER: The dilution water for thc acute test was synthetic seawater.

3. TEST ORGANISMS: The Mysidopsis bahia used in this test were from in-house cultures. The Menidia beryllina were out from an outside source. Routine reference toxicant tests are run to determine sensitivity ofthe test organisms. Organisms in this tests are fed 24 hour old artemia. Organisms used in this test were positively identified lo species when purchased to start cultures and as introduced to provide fresh breeding stock.

4. FACILITIES, EQUIPMENT, AND TEST CHAMBERS: Facilities are designed especially for bioassay testing and culture of test animals. There are two environmental chambers with

temperature controlled at 25-26° C. All equipment which comes in contact with the test fluid is as specified by EPA 82I-R-02-012. Test vessels and any other laboratory equipment which come in contact with the effluent were prepared prior to use as follows:

a. Soak 15 minutes, and scrub wilh detergent in tap waler. b. Rinse twice with lap waler. c. Rinse vvith Acetone d. Rinse with tap water e. Rinse with deionized water f. Soak in fresh dilute (10% V:V) hydrochloric acid to remove scale,

metals and bases for a minimum of 4 hours. g. Rinse five times wilh tap water. h. Rinse five with deionized water.

Testing Facility: Sherry Laboratories @ 2417 West Pinhook Road. Lafayene, LA 70508 (Ph. 800.737.2378) 15 This Joctwwiu shall nui be ruproJuceJ. excepl in full, wilhoul ihe wrillen approval of Sherry Laboratories, LLC.

JobNo. B10020038

5. CHEMICAL AND PHYSICAL ANALYSIS: Routine chemical and physical analyses are conducted on culture, holding, acclimation and dilution waters as well as on effluents lo be tested. All such tests required by EPA protocol are conducted as a minimum. Instruments used for these analyses are routinely calibrated to manufacturer's specifications as well as checked against EPA suggested standards.

6. TEST CONDITIONS: The physical and chemical parameters ofthe test were monitored at the start ofthe test and daily during the test to insure that none of these would affect thc test end points.

7. TEST ACCEPTABILITY: The control (0% effluent) must have a survival equal to or greater than 90% to be considered as valid.

Testing Facility: Sheny Laboratories @ 2417 West Pinhook Road, Lafayene. LA 70508 (Ph. 800.7372378) 16 This documenl shall nol be reproduced excepl in full, wilhoul ihe wrillen approval of Sherry Laboralories.LLC.

Connie Goers

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