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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY REGION I

ENVIRONMENTAL SERVICES DIVISION eo WESTVIF.W STREET, LEXINGTON. MASSACHUSETTS 02173·3185

DATE: November 1, 1991

Gas Chromatography-Mass Spectromet~~ Analysis of ExtractableSUBJ: p~n AqueM~~s - Solvent Recovery s:~ice

FROM: ~.payne Lee and~n Maas, . ESAT, and Dick Siscanaw, Chemistry section F-·l,· -\-.-~' ,p .M•

THRU: Dr. William J. Andrade, Chief, Chemistry Secti?~ J;;(,. ~ ~ ... ~,j. (M.~~"L.

TO: Dorothy Girten •

PROJECT NUMBER: 910256

ANALYTICAL PROCEDURE:

EPA Region 1 Procedure for Medium Level Analyses for Extractable Organics in Aqueous Samples. The samples are extracted by the RCRA method 3530, Liquid/liquid micro-extraction using methylenechloride. The extracts are analyzed on a gas chromatograph/mass spectrometer.

Date(s) Samples Received by the Laboratory: 9/23/91

Date Samples Analyzed: 9/26/91 - 10/2/91

File: K:\CHEMSTRY\REPORTS\FINAL\910256WA.BNA

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US llHVIllORHBNTAL PROTilC'l'ION AGENCY 10 westview street

Lexington, MA 02173

QUALITY CONTROL:

1. A laboratory blank was analyzed before the sampleanalysls.

2. Each sample was spiked with several surrogate compounds at approximately 4000 ug/1 concentration. The results for the surrogate recoveries are reported out for each sample.

3. One sample, 00554, was spiked as a matrix spike duplicatewith the following compounds at approximately 4000 ug/1concentration.

Compound Rec. QC Range comments (%) (%)

Acanaphthene 88 46-118 4-Chloro-3-methylphenol 33 23-97 = 2-Chlorophenol 25 27-123 = 1,4-Dichlorobenzene 83 36-97 c..J 2,4-Dinitrotoluene 85 24-96 4-Nitrophenol 0 10-80 N-Nitroaodipropylamine 81 41-116 Pentachlorophenol 6 9-.J.03 Phenol 26 12-89 Pyrena 79 26-127 1,2,4-Trichlorobenzene 91 39-98

COMPOUNDS NOT IN THE SPIKING SOLUTION:

TargetCompounds Cone.

(ug/L)

Bis(2-ethylhexyl)phthalate 99 ~i-n-butylphthalate -10 Isophorone -20

2

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VI BlfVIIlOlDIJDI'fAL PllO'l'ICTION AGDCY 10 We•tviev Street

LeziDgtoD, HA 02173

Tentatively Cone. Cone.Identified

Compounds (UCJ/L) (ug/L)

2-Pyrrolidlnone, 1-methyl- 100 50

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NOTE: Phthalate& (1,2-Benzenedicarboxylic esters) and adipates(hexanedioic eaters) are common method contaminants. Values at the detection levels are most likely due to method contamination.

SAMPLES ANALYZED: 00554

3

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US BNVIROHMBHTAL PROTBCTIOH AGENCY 10 westview street

Lexington, HA 02173

ANALYTICAL PARAMETERS

INSTRUMENTS:

Hewlett Packard 5890 Gas Chromatograph Hewlett Packard 5987 or 5988 Gas Chromatograph-Mass

Spectrometer

GC/FID screening conditions:

Gas: Hydrogen

capillary Column: DB-1, 30m, .32 mm ID, 0.10 micron film thickness

Injection Mode: Splitless

Temperature Program: Isothermal for 3 min at 40"C, programmed at 20"C/min to 350"C =

GC-MS Conditions: = w Gas: Helium

Capillary Column: DB-5, 60~, .25 mm ID, 0.25 micron film thickness

Injection Mode: Splitless

Temperature Program: I~othermal for 4 min at 40"C, programmed at 7"C/min to 300"C

Injector, Transfer Temperatures: 300"C, 290"C

Electron Energy: 70 v

Mass Range: 35-550

Scan Rate: 0.9 seconds

4

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SAMPLE NO.:

83-32-9 208-96-8 120-12-7 309-00-2 56-55-3 205-99-2 207-08-9 50-32-8 191-24-2 85-68-7 319-85-7 319-86-8 117-81-7 108-60-1 101-55-3 59-50-7 91-58-7 95-57-8 7005-72-3 218-01-9 72-54-8 72-55-9 50-29-3 53-70-3 84-74-2 541-73-1

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SOLVENT RECOVERY SERVICEFACILITY SAMPLED:

US ENVIRONMENTAL PROTECTION AGENCY REGION I LABORATORY GC/MS EXTRACTABLE ORGANIC ANALYSIS

Sample pH: 700554 Dilution FactorsSAMPLE LOCATION:

Base: 10DATE OF COLLECTION: Acid: 10TIME OF COLLECTION:

SAMPLE RESULTS: Compound Cone. PQL CommentsCAS

(ug/L) (Ug/L)NO.

Priority Pollutants

Acenaphthene ND 62 Acenaphthylene ND 62 Anthracene ND 62

62Aldrin ND Benzo(a)anthracene ND 62 Benzo(b)fluoranthene ND 62 Benzo(k)fluoranthene ND 62 Benzo (a) pyrene ND 62

0

Benzo(ghi)perylene ND 62 Benzyl butyl phthalate ND 62 = beta-BHC ND 62 =

0delta-BHC ND 62 CAl Bia(2-ethylhezyl)phthalate -30 u Bis(2-chloroisopropyl)ether ND 60 4-Bromophenylphenyl ether ;:.. ND 60 4-Chloro-3-methylphenol ND 250 2-Chloronaphthalene ND 60 2-Chlorophenol ND 120 4-Chlorophenylphenyl ether ND 62 Chrysene ND 62

04,4'-DDD ND 62 4,4'-DDE ND 62

624,4'-DDT ND Dibenzo(a,h)anthracene ND 62 Di-n-butylphthalate -10 u 1,3-Dichlorobenzene ND 62

(cont.)

US ENVIRONMENTAL PROTECTION AGENCY REGION I LABORATORY

5

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·. -,I

ND 62 ND 62 ND 500 ND 120 ND 62 ND 62 ND 120 ND 62 ND 250 ND 62 ND 62 ND 62 ND 62 = ND 62 = ND 62 w ND 62 ND 62 NO 62

·..- ND 62 NO 62 NO 62

-20 62 NO 62 ND 62 ND 62 ND 120 ND 250 ND 62 ND 62 NO 250 ND 62 ND 120 ND 62

I'""'\US ENVIRONMENTAL PROTECTION AGENCY REGION I LABORATORY GC/MS EXTRACTABLE ORGANIC ANALYSIS

SAMPLE NO.: 00554 sample Results Continued:

CAS Compound Cone. PQL Comments NO. (ug/L) (ug/L)

95-50-1 106-46-7 91-94-1 120-83-2 60-57-1 84-66-2 105-67-9 131-11-3 51-28-5 121-14-2 606-20-2 117-84-0 206-44-0 86-73-7 76-44-8 1024-57-3 118-74-1 87-68-3 77-47-4 67-72-1 193-39-5 78-51-1 534-52-1 91-20-3 98-95-3 88-75-5 100-02-7 86-30-3 621-64-7 87-86-5 85-01-8 108-95-2 129-00-0

1,2-Dichlorobenzene 1,4-Dichlorobenzene 3,3'-Dichlorobenzidine 2,4-Dichlorophenol Dieldrin Diethylphthalate 2,4-Dimethylphenol Dimethylphthalate 2,4-Dinitrophenol2,4-Dinitrotoluene 2,6-Dinitrotoluene Di-n-octylphtha~ate Fluoranthene Fluorene HeptachlorHeptachlor epoxide Hexachlorobenzene Hexachlorobutadiene Hexachlorocyclopentadiene Hexachloroethane Indeno(1,2,3-cd)pyrene

' I•opborone2-Methyl-4,6-dinitrophenol Naphthalene Nitrobenzene 2-Nitrophenol 4-NitrophenolN-Nitrosodiphenylamine N-Nitrosodi-n-propylamine Pentachlorophenol Phenanthrene Phenol Pyrena

(cont.)

6

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US ENVIRONMENTAL PROTECTION AGENCY REGION I LABORATORY GC/MS EXTRACTABLE ORGANIC ANALYSIS

SAMPLE NO.: 00554 Sample Results Continued:

Compound Cone. PQL CommentsCAS NO. {ug/L) {Ug/L)

120-82-1 88-06-2

65-53-3 65-85-0 100-51-6 106-47-8 132-64-9 534-52-1 91-57-6 95-48-7 106-44-5 88-74-4 99-09-2 100-01-6 95-95-4

1,2,4-Trichlorobenzene 2,4,6-Trichlorophenol

Hazardous Substances

Aniline Benzoic Acid Benzyl Alcohol 4-Chloroaniline Oibanzofuran 4,6-0initro-2-methylphenol 2-Mathylnaphthalene2-Methylphenol4-Mathylphenol2-Nitroaniline 3-Nitroaniline 4-Nitroaniline 2,4,5-Trichlorophenol

~O.,..th,...a_r_C~o-m_p_o_u_n-:-ds-Q~u-a_n...,.t....l..,.t-a.,..t-ed~

Diphenylhydrazine(azobenzene)

Tentatively Identified Compounds

2-Pyrrolidinone, 1-methyl-

NO NO

ND NO ND ND NO ND ND ND NO ND NO NO NO

·-·

NO

Est. Cone.

(ug/L)

90

62 120

120 500 120 120

62 250

62 62 62

250 250 500 120

62

Est. PQL

(ug/L)

50

7

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US ENVIRONMENTAL PROTECTION AGENCY REGION I LABORATORY GC/MS EXTRACTABLE ORGANIC ANALYSIS

SAMPLE NO.: 00554 Sample Results Continued:

Sample Recoveries For Recoveries surroqate compounds: <'>

2-Fluorophenol 1 21-100 Phenol,d5 1 10-94 Nitrobenzene,d5 94 35-114 Fluorobiphenyl 63 43-116 2,4,6-Tribromophenol 6 10-123 p-Terphenyl,d14 107 33-141

Notes: NO • none detected

- • approximate < • less . than > • qreater than c

NA • not available, due to sample dilution or interference

8