Method 1625C

Semivolatile Organic Compounds by Isotope Dilution GCMS

June 1989

U.S. Environmental Protection Agency
Office of Science and Technology
Engineering and Analysis Division
401 M Street S.W.
Washington, D.C. 20460


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Method 1625C
Semivolatile Organic Compounds
by Isotope Dilution GCMS

1.0	Scope and Application

1.1	This method is designed to meet the survey requirements of the USEPA ITD. The
method is used to determine the semivolatile toxic organic pollutants associated with the
Clean Water Act (as amended 1987); the Resource Conservation and Recovery Act (as
amended 1986); the Comprehensive Environmental Response, Compensation and Liability
Act (as amended 1986); and other compounds amenable to extraction and analysis by
capillary column gas chromatography-mass spectrometry (GCMS).

1.2	The chemical compounds listed in Tables 1-4 may be determined in waters, soils, and
municipal sludges by the method.

1.3	The detection limits of the method are usually dependent on the level of interferences
rather than instrumental limitations. The limits in Tables 5 and 6 typify the minimum
quantities that can be detected with no interferences present.

1.4	The GCMS portions of the method are for use only by analysts experienced with GCMS
or under the close supervision of such qualified persons. Laboratories unfamiliar with
analysis of environmental samples by GCMS should run the performance tests in
Reference 1 before beginning.

TABLE 1. BASE/NEUTRAL EXTRACTABLE COMPOUNDS DETERMINED BY GCMS
USING ISOTOPE DILUTION AND INTERNAL STANDARD TECHNIQUES

Pollutant	 Labeled Compound





CAS

EPA-







CAS

EPA-

Compound

Storet

Registry

EGD

NPDES

Analog

Registry

EGD

acenaphthene

34205

83-32-9

001

B

001

B

dio

15067-20-2

201 B

acenaphthylene

34200

208-96-8

077

B

002

B

d8

93951-97-4

277 B

anthracene

34220

120-12-7

078

B

003

B

dio

1719-06-8

278 B

benzidine

39120

92-87-5

005

B

004

B

d8

92890-63-6

205 B

benzo (a) anthracene

34526

56-55-3

072

B

005

B

diz

1718-53-2

272 B

benzo (b) fluoranthene

34230

205-99-2

074

B

007

B

diz

93951-98-5

274 B

benzo (k) fluoranthene

34242

207-08-9

075

B

009

B

diz

93952-01-3

275 B

benzo(a)pyrene

34247

50-32-8

073

B

006

B

di2

63466-71-7

273 B

benzo (ghi) perylene

34521

191-24-2

079

B

008

B

di2

93951-66-7

279 B

biphenyl (Appendix C)

81513

92-52-4

512

B





dio

1486-01-7

612 B

bis(2-chloroethyl) ether

34273

111-44-4

018

B

011

B

d8

93952-02-4

218 B

bis(2-chloroethoxy) methane

34278

111-91-1

043

B

010

B

d8

93966-78-0

243 B

bis(2-chloroisopropyl) ether

34283

108-60-1

042

B

012

B

di2

93951-67-8

242 B

bis(2-ethylhexyl) phthalate

39100

117-81-7

066

B

013

B

d4

93951-87-2

266 B

2

September 1989


-------
Method 1625C

TABLE 1. BASE/NEUTRAL EXTRACTABLE COMPOUNDS DETERMINED BY GCMS
USING ISOTOPE DILUTION AND INTERNAL STANDARD TECHNIQUES

Pollutant	 Labeled Compound





CAS

EPA-







CAS

EPA-

Compound

Storet

Registry

EGD

NPDES

Analog

Registry

EGD

4-bromophenyl phenyl ether

34636

101-55-3

041

B

014

B

d5

93951-83-8

241

B

butyl benzyl phthalate

34292

85-68-7

067

B

015

B

d4

93951-88-3

267

B

n-CIO (Appendix C)

77427

124-18-5

517

B





^22

16416-29-8

617

B

n-C12 (Appendix C)

77588

112-40-3

506

B





^26

16416-30-1

606

B

n-C14 (Appendix C)

77691

629-59-4

518

B

618

B









n-C16 (Appendix C)

77757

544-76-3

519

B





^34

15716-08-2

619

B

n-C18 (Appendix C)

77804

593-45-3

520

B

620

B









n-C20 (Appendix C)

77830

112-95-8

521

B





^42

62369-67-9

621

B

n-C22 (Appendix C)

77859

629-97-0

522

B

622

B









n-C24 (Appendix C)

77886

646-31-1

523

B





^50

16416-32-3

623

B

n-C26 (Appendix C)

77901

630-01-3

524

B

624

B









n-C28 (Appendix C)

78116

630-02-4

525

B

625

B









n-C30 (Appendix C)

78117

638-68-6

526

B





^62

93952-07-9

626

B

carbazole (4c)

77571

86-74-8

528

B





d8

38537-24-5

628

B

2-chloronaphthalene

34581

91-58-7

020

B

016

B

d7

93951-84-9

220

B

4-chlorophenyl phenyl ether

34641

7005-72-3

040

B

017

B

d5

93951-85-0

240

B

chrysene

34320

218-01-9

076

B

018

B

diz

1719-03-5

276

B

p-cymene (Appendix C)

77356

99-87-6

513

B





dM

93952-03-5

613

B

dibenzo (a,h) anthracene

34556

53-70-3

082

B

019

B

dM

13250-98-1

282

B

dibenzofuran

81302

132-64-9

505

B





d8

93952-04-6

605

B

(Appendix C & 4c)





















dibenzothiophene (Synfuel)

77639

132-65-0

504

B





d8

33262-29-2

604

B

di-n-butyl phthalate

39110

84-74-2

068

B

026

B

d4

93952-11-5

268

B

1,2-dichlorobenzene

34536

95-50-1

025

B

020

B

d4

2199-69-1

225

B

1,3-dichlorobenzene

34566

541-73-1

026

B

021

B

d4

2199-70-4

226

B

1,4-dichlorobenzene

34571

106-46-7

027

B

022

B

d4

3855-82-1

227

B

3,3'-dichlorobenzidine

34631

91-94-1

028

B

023

B

d6

93951-91-8

228

B

diethyl phthalate

34336

84-66-2

070

B

024

B

d4

93952-12-6

270

B

2,4-dimethylphenol

34606

105-67-9

034 A

003 A

d3

93951-75-8

234 A

dimethyl phthalate

34341

131-11-3

071

B

025

B

d4

93951-89-4

271

B

2,4-dinitrotoluene

34611

121-14-2

035

B

027

B

d3

93951-68-9

235

B

2,6-dinitrotoluene

34626

606-20-2

036

B

028

B

d3

93951-90-7

236

B

di-n-octyl phthalate

34596

117-84-0

069

B

029

B

d4

93952-13-7

269

B

diphenylamine

77579

122-39-4

507

B





dio

37055-51-9

607

B

(Appendix C)





















diphenyl ether

77587

101-84-8

508

B





dio

93952-05-7

608

B

(Appendix C)





















1,2-diphenylhydrazine

34346

122-66-7

037

B

030

B

dio

93951-92-9

237

B

fluoranthene

34376

206-44-0

039

B

031

B

dio

93951-69-0

231

B

fluorene

34381

86-73-7

080

B

032

B

dio

81103-79-9

280

B

hexachlorobenzene

39700

118-74-1

009

B

033

B

13C

93952-14-8

209

B

hexachlorobutadiene

34391

87-68-3

052

B

034

B

13c

4

93951-70-3

252

B

hexachloroethane

34396

67-72-1

012

B

036

B

13c

93952-15-9

212

B

hexachlorocyclopentadiene

34386

77-47-4

053

B

035

B

13c

4

93951-71-4

253

B

September 1989	3


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Method 1625C

TABLE 1. BASE/NEUTRAL EXTRACTABLE COMPOUNDS DETERMINED BY GCMS
USING ISOTOPE DILUTION AND INTERNAL STANDARD TECHNIQUES

Pollutant	 Labeled Compound





CAS

EPA-





CAS

EPA-

Compound

Storet

Registry

EGD

NPDES

Analog

Registry

EGD

indeno(l,2,3-cd)pyrene

34403

193-39-5

083 B

037 B







isophorone

34408

78-59-1

054 B

038 B

d8

93952-16-0

254 B

naphthalene

34696

91-20-3

055 B

039 B

d8

1146-65-2

255 B

beta-naphthylamine

82553

91-59-8

502 B



d7

93951-94-1

602 B

(Appendix C)















nitrobenzene

34447

98-95-3

056 B

040 B

d5

4165-60-0

256 B

N-nitrosodimethylamine

34438

62-75-9

061 B

041 B

d6

17829-05-9

261 B

N-nitrosodi-n-proplyamine

34428

621-64-7

063 B

042 B

di4

93951-96-3

263 B

N-nitrosodiphenylamine

34433

86-30-6

062 B

043 B

d6

93951-95-2

262 B

phenanthrene

34461

85-01-8

081 B

044 B

dio

1517-22-2

281 B

phenol

34694

108-95-2

065 A

010 A

d5

4165-62-2

265 A

alpha-picoline (Synfuel)

77088

109-06-8

503 B



d7

93951-93-0

603 B

pyrene

34469

129-00-0

084 B

045 B

dio

1718-52-1

284 B

styrene (Appendix C)

77128

100-42-5

510 B



d5

5161-29-5

610 B

alpha-terpineol

77493

98-55-5

509 B



d3

93952-06-8

609 B

(Appendix C)















1,2,3-trichlorobenzene (4c)

77613

87-61-6

529 B



d3

3907-98-0

629 B

1,2,4-trichlorobenzene

34551

120-82-1

008 B

046 B

d3

2199-72-6

208 B

TABLE 2. ACID EXTRACTABLE COMPOUNDS DETERMINED BY GCMS USING
ISOTOPE DILUTION AND INTERNAL STANDARD TECHNIQUES

Pollutant	 Labeled Compound





CAS

EPA-







CAS

EPA-

Compound

Storet

Registry

EGD

NPDES

Analog

Registry

EGD

4-chloro-3-methylphenol

34452

59-50-7

022

A

008

A

d2

93951-72-5

222

A

2-chlorophenol

34586

95-57-8

024

A

001

A

d4

93951-73-6

224

A

2,4-dichlorophenol

34601

120-83-2

031

A

002

A

d3

93951-74-7

231

A

2,4-dinitrophenol

34616

51-28-5

059

A

005

A

d3

93951-77-0

259

A

2-methyl-4,6-dinitrophenol

34657

534-52-1

060

A

004

A

d2

93951-76-9

260

A

2-nitrophenol

34591

88-75-5

057

A

006

A

d4

93951-75-1

257

A

4-nitrophenol
pentachlorophenol

34646
39032

100-02-7
87-86-5

058
064

A
A

007
009

A
A

d4

13c6

93951-79-2
85380-74-1

258
264

A
A

2,3,6-trichlorophenol (4c)

77688

933-75-5

530

A





d2

93951-81-6

630

A

2,4,5-trichlorophenol (4c)



95-95-4

531

A





d2

93951-82-7

631

A

2,4,6-trichlorophenol

34621

88-06-2

021

A

011

A

d2

93951-80-5

221

A

4

September 1989


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Method 1625C

TABLE 3. BASE/NEUTRAL EXTRACTABLE COMPOUNDS TO BE DETERMINED BY
REVERSE SEARCH AND QUANTITATION USING KNOWN RETENTION TIMES,
RESPONSE FACTORS, REFERENCE COMPOUND, AND MASS SPECTRA

EGD No.

Compound

CAS Registry

555

acetophenone

98-86-2

556

4-aminobiphenyl

92-67-1

557

aniline

62-53-3

558

o-anisidine

90-04-0

559

aramite

140-57-8

560

benzanthrone

82-05-3

561

l,3-benzenediol(resorcinol)

108-46-3

562

benzenethiol

108-98-5

563

2,3-benzofluorene

243-17-4

564

benzyl alcohol

100-51-6

565

2-bromochlorobenzene

694-80-4

566

3-bromochlorobenzene

108-37-2

567

4-chloro-2-nitroaniline

89-63-4

568

5-chloro-o-toluidine

95-79-4

569

4-chloroaniline

106-47-8

570

3-chloronitrobenzene

121-73-3

571

o-cresol

95-48-7

572

crotoxyphos

7700-17-6

573

2,6-di-tert-butyl-p-benzoquinone

719-22-2

574

2,4-diaminotoluene

95-80-7

575

1,2-dibromo-3-chloropropane

96-12-8

576

2,6-dichloro-4-nitroaniline

99-30-9

577

l,3-dichloro-2-propanol

96-23-1

578

2,3-dichloroaniline

608-27-5

579

2,3-dichloronitro-benzene

3209-22-1

580

l,2:3,4-diepoxybutane

1464-53-5

581

3,3'-dimethoxybenzidine

119-90-4

582

dimethyl sulfone

67-71-0

583

p-dimethylamino-azobenzene

60-11-7

584

7,12-dimethylbenz- (a) anthracene

57-97-6

585

N,N-dimethylformamide

68-12-2

586

3,6-dimethylphenanthrene

1576-67-6

587

1,4-dinitrobenzene

100-25-4

588

diphenyldisulfide

882-33-7

589

ethyl methanesulfonate

62-50-0

590

ethylenethiourea

96-45-7

591

ethynylestradiol3-methyl ether

72-33-3

592

hexachloropropene

1888-71-7

593

2-isopropylnaphthalene

2027-17-0

594

isosafrole

120-58-1

595

longifolene

475-20-7

596

malachite green

569-64-2

597

methapyrilene

91-80-5

598

methyl methanesulfonate

66-27-3

599

2-methylbenzothioazole

120-75-2

900

3-methylcholanthrene

56-49-5

September 1989

5


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Method 1625C

TABLE 3. BASE/NEUTRAL EXTRACTABLE COMPOUNDS TO BE DETERMINED BY
REVERSE SEARCH AND QUANTITATION USING KNOWN RETENTION TIMES,
RESPONSE FACTORS, REFERENCE COMPOUND, AND MASS SPECTRA

EGD No.

Compound

CAS Registry

901

4,4'-methylene-bis(2-chloroaniline)

101-14-4

902

4,5-methylene-phenanthrene

203-64-5

903

1 -methy lfluorene

1730-37-6

904

2-methylnaphthalene

91-57-6

905

1 -methy lphenanthrene

832-69-9

906

2-(methylthio)-benzothiazole

615-22-5

907

1,5-naphthalenediamine

2243-62-1

908

1,4-naphthoquinone

130-15-4

909

alpha-naphthylamine

134-32-7

910

5-nitro-o-toluidine

99-55-8

911

2-nitroaniline

88-74-4

912

3-nitroaniline

99-09-2

913

4-nitroaniline

100-01-6

914

4-nitrobiphenyl

92-93-3

915

N-nitrosodi-n-butylamine

924-16-3

916

N-nitrosodiethylamine

55-18-5

917

N-nitrosomethyl-ethylamine

10595-95-6

918

N-nitrosomethyl-phenylamine

614-00-6

919

N-nitrosomorpholine

59-89-2

920

N-nitrosopiperidine

100-75-4

921

pentachlorobenzene

608-93-5

922

pentachloroethane

76-01-7

923

pentamethylbenzene

700-12-9

924

perylene

198-55-0

925

phenacetin

62-44-2

926

phenothiazine

92-84-2

927

1 -phenylnaphthalene

605-02-7

928

2-phenylnaphthalene

612-94-2

929

pronamide

23950-58-5

930

pyridine

110-86-1

931

safrole

94-59-7

932

squalene

7683-64-9

933

1,2,4,5-tetra-chlorobenzene

95-94-3

934

thianaphthene (2,3-benzothiophene)

95-15-8

935

thioacetamide

62-55-5

936

thioxanthone

492-22-8

937

o-toluidine

95-53-4

938

1,2,3-trimethoxybenzene

634-36-6

939

2,4,5-trimethylaniline

137-17-7

940

triphenylene

217-59-4

941

tripropyleneglycolmethyl ether

20324-33-8

942

1,3,5-trithiane

291-21-4

6

September 1989


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Method 1625C

2.0	Summary of Method

2.1	The percent solids content of a sample is determined. Stable isotopically labeled analogs
of the compounds of interest are added to the sample. If the solids content is less than
1%, a 1 L sample is extracted at pH 12-13, then at pH <2 with methylene chloride using
continuous extraction techniques. If the solids content is 30% or less, the sample is
diluted to 1% solids with reagent water, homogenized ultrasonically, and extracted at pH
12-13, then at pH <2 with methylene chloride using continuous extraction techniques.
If the solids content is greater than 30%, the sample is extracted using ultrasonic
techniques. Each extract is dried over sodium sulfate, concentrated to a volume of 5 mL,
cleaned up using gel permeation chromatography (GPC), if necessary, and concentrated.
Extracts are concentrated to 1 mL if GPC is not performed, and to 0.5 mL if GPC is
performed. An internal standard is added to the extract, and a 1 |iL aliquot of the extract
is injected into the gas chromatograph (GC). The compounds are separated by GC and
detected by a mass spectrometer (MS). The labeled compounds serve to correct the
variability of the analytical technique.

TABLE 4. ACID EXTRACTABLE COMPOUNDS TO BE DETERMINED BY REVERSE
SEARCH AND QUANTITATION USING KNOWN RETENTION TIMES, RESPONSE
FACTORS, REFERENCE COMPOUND, AND MASS SPECTRA

EGD No.

Compound

CAS Registry

943

benzoic acid

65-85-0

944

p-cresol

106-44-5

945

3,5-dibromo-4-hydroxybenzonitrile

1689-84-5

946

2,6-dichlorophenol

87-65-0

947

hexanoic acid

142-62-1

948

2,3,4,6-tetrachlorophenol

58-90-2

2.2	Identification of a pollutant (qualitative analysis) is performed in one of three ways: (1)
For compounds listed in Tables 1 and 2, and for other compounds for which authentic
standards are available, the GCMS system is calibrated and the mass spectrum and
retention time for each standard are stored in a user created library. A compound is
identified when its retention time and mass spectrum agree with the library retention
time and spectrum. (2) For compounds listed in Tables 3 and 4, and for other
compounds for which standards are not available, a compound is identified when the
retention time and mass spectrum agree with those specified in this method. (3) For
chromatographic peaks which are not identified by (1) and (2) above, the background
corrected spectrum at the peak maximum is compared with spectra in the EPA/NIH
Mass Spectral File (Reference 2). Tentative identification is established when the
spectrum agrees (see Section 13).

2.3	Quantitative analysis is performed in one of four ways by GCMS using extracted ion
current profile (EICP) areas: (1) For compounds listed in Tables 1 and 2, and for other
compounds for which standards and labeled analogs are available, the GCMS system is
calibrated and the compound concentration is determined using an isotope dilution
technique. (2) For compounds listed in Tables 1 and 2, and for other compounds for
which authentic standards but no labeled compounds are available, the GCMS system
is calibrated and the compound concentration is determined using an internal standard
technique. (3) For compounds listed in Tables 3 and 4, and for other compounds for
which standards are not available, compound concentrations are determined using

September 1989

7


-------
Method 1625C

known response factors. (4) For compounds for which neither standards nor known
response factors are available, compound concentration is determined using the sum of
the EICP areas relative to the sum of the EICP areas of the internal standard.

2.4 The quality of the analysis is assured through reproducible calibration and testing of the
extraction and GCMS systems.

TABLE 5. GAS CHROMATOGRAPHIC RETENTION TIMES AND DETECTION LIMITS
FOR BASE/NEUTRAL EXTRACTABLE COMPOUNDS

Method Detection
Retention Time	Limit4











Minimum

Low

High

EGD



Mean

EGD



Level3

solids

Solids

No.1

Compound

(sec)

Ref

Relative2

(l-ig/L)

(l-ig/kg)

(l-ig/kg)

164

2,2'-difluorobiphenyl (int std)

1163

164

1.000-1.000

10





930

pyridine

378

164

0.325







261

N-nitrosodimethylamine-d65

378

164

0.286- 0.364

50





361

N-nitrosodimethylamine5

385

261

1.006-1.028

50

16

27

585

N,N-dimethylformamide

407

164

0.350







580

l,2:3,4-diepoxybutane

409

164

0.352







603

alpha picoline-d7

417

164

0.326-0.393

50





703

alpha picoline

426

603

1.006-1.028

50

25

87

917

N-nitrosomethylethylamine

451

164

0.338







598

methyl methanesulfonate

511

164

0.439







610

styrene-d5

546

164

0.450-0.488

10





710

styrene

549

610

1.002-1.009

10

149*

17

916

N-nitrosodiethylamine

570

164

0.490







577

1,3-dichloro-2-propanol

589

164

0.506







589

ethyl methanesulfonate

637

164

0.548







582

dimethyl sulfone

649

164

0.558







562

benzenethiol

667

164

0.574







922

pentachloroethane

680

164

0.585







557

aniline

694

164

0.597







613

p-cymene-d14

742

164

0.624-0.652

10





713

p-cymene

755

613

1.008-1.023

10

426*

912*

265

phenol-d5

696

164

0.584-0.613

10





365

phenol

700

265

0.995-1.010

10

2501*

757*

218

bis(2-chloroethyl) ether-d8

696

164

0.584-0.607

10





318

bis(2-chloroethyl) ether

704

218

1.007-1.016

10

32

22

617

n-C10-d22

698

164

0.585-0.615

10





717

n-CIO

720

617

1.022-1.038

10

299*

1188*

226

1,3-dichlorobenzene-d4

722

164

0.605-0.636

10





326

1,3-dichlorobenzene

724

226

0.998-1.008

10

46

26

227

1,4-dichlorobenzene-d4

737

164

0.601-0.666

10





327

1,4-dichlorobenzene

740

227

0.997-1.009

10

35

20

225

1,2-dichlorobenzene-d4

758

164

0.632-0.667

10





325

1,2-dichlorobenzene

760

225

0.995-1.008

10

63

16

935

thioacetamide

768

164

0.660







564

benzyl alcohol

785

164

0.675







8

September 1989


-------
Method 1625C

TABLE 5. GAS CHROMATOGRAPHIC RETENTION TIMES AND DETECTION LIMITS
FOR BASE/NEUTRAL EXTRACTABLE COMPOUNDS

Retention Time

Method Detection
Limit4

EGD

No.1	Compound

242 bis(2-chloroisopropyl)

Mean
(sec)

EGD
Ref

Relative2

0.664-0.691

1.010-1.016
0.700

0.689-0.716

Minimum Low High
Level3 solids Solids
(l-ig/L) (ng/kg) (ng/kg)

342
571
263

363
555
212
312
937

919
575
256
356
566
565

941

254

354

942

920
234
334
243

343
208
308
558

255

355
934
609
709
606
706
629
729
252
352

ether-d12

bis(2-chloroisopropyl) ether

o-cresol

N-nitrosodi-n-

propylamine-d145

N-nitrosodi-n-propylamine5

acetophenone

hexachloroethane-13C

hexachloroethane

o-toluidine

N-nitrosomorpholine

1,2-dibromo-3-chloropropane

nitrobenzene-d5

nitrobenzene

3-bromochlorobenzene

2-bromochlorobenzene

tripropylene glycol

methyl ether

isophorone-d8

isophorone

1,3,5-trithiane

N-nitrosopiperidine

2,4-dimethylphenol-d3

2,4-dimethylphenol

bis(2-chloroethoxy)

methane-d65

bis(2-chloroethoxy) methane5

1,2,4-trichlorobenzene-d3

1,2,4-trichlorobenzene

o-anisidine

naphthalene-d8

naphthalene

thianapthene

alpha-terpineol-d3

alpha-terpineol

n-C12-d26

n-C12

l,2,3-trichlorobenzene-d35
1,2,3-trichlorobenzene5
hexachlorobutadiene-13C4
hexachlorobutadiene

788

799
814
817

164

242
164
164

10

10

20

24

39

830

263

1.008-1.023

20

46

47

818

164

0.703







819

164

0.690-0.717

10





823

212

0.999-1.001

10

58

55

830

164

0.714







834

164

0.717







839

164

0.721







845

164

0.706-0.727

10





849

256

1.002-1.007

10

39

28

854

164

0.734







880

164

0.757







881

164

0.758







881

164

0.747-0.767

10





889

254

0.999-1.017

10

8

5

889

164

0.764







895

164

0.770







921

164

0.781-0.803

10





924

234

0.999-1.003

10

26

13

933

164

0.792-0.807

10





939

243

1.000-1.013

10

26

23

955

164

0.813-0.830

10





958

208

1.000-1.005

10

49

24

962

164

0.827







963

164

0.819-0.836

10





967

255

1.001-1.006

10

62

42

971

164

0.835







973

164

0.829-0.844

10





975

609

0.998-1.008

10

nd

nd

953

164

0.730-0.908

10





981

606

0.986-1.051

10

860*

3885*

1000

164

0.852-0.868

10





1003

629

1.000-1.005

10

260*

164*

1005

164

0.856-0.871

10





1006

252

0.999-1.002

10

46

22

September 1989

9


-------
Method 1625C

TABLE 5. GAS CHROMATOGRAPHIC RETENTION TIMES AND DETECTION LIMITS
FOR BASE/NEUTRAL EXTRACTABLE COMPOUNDS

Retention Time

Method Detection
Limit4

EGD
No.1

Compound

Mean
(sec)

EGD
Ref

Relative;

Minimum Low
Level3 solids
(l-ig/L) (ng/kg)

High
Solids
(l-ig/kg)

918

N -nitrosomethy lphenylamine

1006

164

0.865







592

hexachloropropene

1013

164

0.871







569

4-chloroaniline

1016

164

0.874







570

3-chloronitrobenzene

1018

164

0.875







915

N-nitrosodi-n-butylamine

1063

164

0.914







923

pentamethylbenzene

1083

164

0.931







561

1,3-benzenediol

1088

164

0.936







931

safrole

1090

164

0.937







939

2,4,5-trimethylaniline

1091

164

0.938







904

2-methylnaphthalene

1098

164

0.944







599

2-methylbenzothiazole

1099

164

0.945







568

5-chloro-o-toluidine

1101

164

0.947







938

1,2,3-trimethoxy benzene

1128

164

0.970







933

1,2,4,5-tetr achlorobenzene

1141

164

0.981







253

hexachlorocyclo-
pentadiene-13C4

1147

164

0.976-0.986

10





353

hexachlorocyclopentadiene

1142

253

0.999-1.001

10

nd

nd

594

isosafrole (cis or trans)

1147

164

0.986







594

isosafrole (cis or trans)

1190

164

1.023







578

2,3-dichloroaniline

1160

164

0.997







574

2,4-diaminotoluene

1187

164

1.021







220

2-chloronaphthalene-d7

1185

164

1.014-1.024

10





320

2-chloronaphthalene

1200

220

0.997-1.007

10

80

59

518

n-C14

1203

164

1.034

10

256

3533

612

biphenyl-d10

1195

164

1.016-1.027

10





712

biphenyl

1205

612

1.001-1.006

10

67

55

608

diphenyl ether-d10

1211

164

1.036-1.047

10





708

diphenyl ether

1216

608

0.997-1.009

10

44

12

579

2,3-dichloronitrobenzene

1214

164

1.044







911

2-nitroaniline

1218

164

1.047







908

1,4-naphthoquinone

1224

164

1.052







595

longifolene

1225

164

1.053







277

acenaphthylene-d8

1265

164

1.080-1.095

10





377

acenaphthylene

1247

277

1.000-1.004

10

57

18

593

2-isopropylnaphthalene

1254

164

1.078







587

1,4-dinitrobenzene

1255

164

1.079







576

2,6-dichloro-4-nitroaniline

1259

164

1.083







271

dimethyl phthalate-d4

1269

164

1.083-1.102

10





371

dimethyl phthalate

1273

271

0.998-1.005

10

62

21

573

2,6-di-t-butyl-p-benzoquinone

1273

164

1.095







236

2,6-dinitrotoluene-d3

1283

164

1.090-1.112

10





336

2,6-dinitrotoluene

1300

236

1.001-1.005

10

55

47

912

3-nitroaniline

1297

164

1.115







10

September 1989


-------
Method 1625C

TABLE 5. GAS CHROMATOGRAPHIC RETENTION TIMES AND DETECTION LIMITS
FOR BASE/NEUTRAL EXTRACTABLE COMPOUNDS

Method Detection
Retention Time	Limit4











Minimum

Low

High

EGD



Mean

EGD



Level3

solids

Solids

No.1

Compound

(sec)

Ref

Relative2

(Pg/L)

(l-ig/kg)

(l-ig/kg)

201

acenaphthene-d10

1298

164

1.107-1.125

10





301

acenaphthene

1304

201

0.999-1.009

10

64

55

605

dibenzofuran-d8

1331

164

1.134-1.155

10





705

dibenzofuran

1335

605

0.998-1.007

10

77

210*

921

pentachlorobenzene

1340

164

1.152







909

alpha-naphthylamine

1358

164

1.168







235

2,4-dinitrotoluene-d3

1359

164

1.152-1.181

10





335

2,4-dinitrotoluene

1364

235

1.000-1.002

10

65

209*

602

beta-naphthylamine-d7

1368

164

1.163-1.189

50





702

beta-naphthylamine

1371

602

0.996-1.007

50

49

37

590

ethylenethiourea

1381

164

1.187







280

fluorene-d10

1395

164

1.185-1.214

10





380

fluorene

1401

281

0.999-1.008

10

69

61

240

4-chlorophenyl phenyl
ether-d5

1406

164

1.194-1.223

10





340

4-chlorophenyl phenyl ether

1409

240

0.990-1.015

10

73

59

270

diethyl phthalate-d4

1409

164

1.197-1.229

10





370

diethyl phthalate

1414

270

0.996-1.006

10

52

16

906

2- (methyl thio) benzothiazole

1415

164

1.217







567

4-chloro-2-nitroaniline

1421

164

1.222







910

5-nitro-o-toluidine

1422

164

1.223







913

4-nitroaniline

1430

164

1.230







619

n-C16-d34

1447

164

1.010-1.478

10





719

n-C16

1469

619

1.013-1.020

10

116*

644*

237

l,2-diphenylhydrazine-d8

1433

164

1.216-1.248

20





337

1,2-diphenylhydrazine6

1439

237

0.999-1.009

20

48

27

607

diphenylamine-d10

1437

164

1.213-1.249

20





707

diphenylamine

1439

607

1.000-1.007

20

58

54

262

N-nitrosodiphenylamine-d6

1447

164

1.225-1.252

20





362

N-nitrosodiphenylamine7

1464

262

1.000-1.002

20

55

36

241

4-bromophenyl phenyl
ether-d55

1495

164

1.271-1.307

10





341

4-bromophenyl phenyl ether5

1498

241

0.990-1.015

10

55

17

925

phenacetin

1512

164

1.300







903

1 -methy lfluorene

1514

164

1.302







209

hexachlorobenzene-13C6

1521

164

1.288-1.327

10





309

hexachlorobenzene

1522

209

0.999-1.001

10

51

48

556

4-aminobiphenyl

1551

164

1.334







929

pronamide

1578

164

1.357







281

phenanthrene-d10

1578

164

1.334-1.380

10





520

n-C18

1580

164

1.359

10

134*

844*

381

phenanthrene

1583

281

1.000-1.005

10

42

22

278

anthracene-d10

1588

164

1.342-1.388

10





September 1989

11


-------
Method 1625C

TABLE 5. GAS CHROMATOGRAPHIC RETENTION TIMES AND DETECTION LIMITS
FOR BASE/NEUTRAL EXTRACTABLE COMPOUNDS

Method Detection
Retention Time	Limit4











Minimum

Low

High

EGD



Mean

EGD



Level3

solids

Solids

No.1

Compound

(sec)

Ref

Relative2

(l-ig/L)

(l-ig/kg)

(l-ig/kg)

378

anthracene

1592

278

0.998-1.006

10

52

21

604

dibenzothiophene-d8

1559

164

1.314-1.361

10





704

dibenzothiophene

1564

604

1.000-1.006

10

72

71

588

diphenyldisulfide

1623

164

1.396







914

4-nitrobiphenyl

1639

164

1.409







927

1 -pheny lnaphthalene

1643

164

1.413







628

carbazole-d85

1645

164

1.388-1.439

20





728

carbazole5

1650

628

1.000-1.006

20

47

24

621

n-C20-d42

1655

164

1.184-1.662

10





721

n-C20

1677

621

1.010-1.021

10

83

229*

907

1,5-naphthalenediamine

1676

164

1.441







902

4,5-methylenephenanthrene

1690

164

1.453







905

1 -methy lphenanthrene

1697

164

1.459







268

di-n-butyl phthalate-d4

1719

164

1.446-1.510

10





368

di-n-butyl phthalate

1723

268

1.000-1.003

10

64

80

928

2-phenylnaphthalene

1733

164

1.490







586

3,6-dimethylphenanthrene

1763

164

1.516







597

methapyrilene

1781

164

1.531







926

phenothiazine

1796

164

1.544







239

fluoranthene-d10

1813

164

1.522-1.596

10





339

fluoranthene

1817

239

1.000-1.004

10

54

22

572

crotoxyphos

1822

164

1.567







936

thioxanthone

1836

164

1.579







284

pyrene-d10

1844

164

1.523-1.644

10





384

pyrene

1852

284

1.001-1.003

10

40

48

205

benzidine-d8

1854

164

1.549-1.632

50





305

benzidine

1853

205

1.000-1.002

50

nd

nd

522

n-C22

1889

164

1.624

10

432*

447*

559

aramite

1901

164

1.635







559

aramite

1916

164

1.647







583

p-dimethylaminoazobenzene

1922

164

1.653







563

2,3-benzofluorene

1932

164

1.661







623

n-C24-d50

1997

164

1.671-1.764

10





723

n-C24

2025

612

1.012-1.015

10

—

—

932

squalene

2039

164

1.753







267

butylbenzyl phthalate-d45

2058

164

1.715-1.824

10





367

butylbenzyl phthalate5

2060

267

1.000-1.002

10

60

65

276

chrysene-d12

2081

164

1.743-1.837

10





376

chrysene

2083

276

1.000-1.004

10

51

48

901

4,4'methylenebis
(2-chloroaniline)

2083

164

1.791







272

benzo(a)anthracene-d12

2082

164

1.735-1.846

10





372

benzo (a) anthracene

2090

272

0.999-1.007

10

61

47

12

September 1989


-------
Method 1625C

TABLE 5. GAS CHROMATOGRAPHIC RETENTION TIMES AND DETECTION LIMITS
FOR BASE/NEUTRAL EXTRACTABLE COMPOUNDS

Method Detection
Retention Time	Limit4











Minimum

Low

High

EGD



Mean

EGD



Level3

solids

Solids

No.1

Compound

(sec)

Ref

Relative2

(l-ig/L)

(l-ig/kg)

(l-ig/kg)

381

3,3'-dimethoxybenzidine

2090

164

1.797







228

3,3'-dichlorobenzidine-d6

2088

164

1.744-1.848

50





328

3,3'-dichlorobenzidine

2086

228

1.000-1.001

50

62

111

940

triphenylene

2088

164

1.795







560

benzan throne

2106

164

1.811







266

bis(2-ethylhexyl) phthalate-d4

2123

164

1.771-1.880

10





366

bis(2-ethylhexyl) phthalate

2124

266

1.000-1.002

10

553*

1310*

524

n-C26

2147

164

1.846

10

609*

886*

591

ethynylestradiol 3-methyl
ether

2209

164

1.899







269

di-n-octyl phthalate-d4

2239

164

1.867-1.982

10





369

di-n-octyl phthalate

2240

269

1.000-1.002

10

72

62

525

n-C28

2272

164

1.954

10

492*

1810*

584

7,12-dimethylbenz(a)-
anthracene

2284

164

1.964







274

benzo (b) fluoranthene-dj 2

2281

164

1.902-2.025

10





374

benzo (b) fluoranthene

2293

274

1.000-1.005

10

54

30

275

benzo (k) fluor anthene-dj 2

2287

164

1.906-2.033

10





375

benzo (k) fluoranthene

2293

275

1.000-1.005

10

95

20

924

perylene

2349

164

2.020







273

benzo (a) pyrene-dj 2

2351

164

1.954-2.088

10





373

benzo(a)pyrene

2350

273

1.000-1.004

10

52

15

626

n-C30-d62

2384

164

1.972-2.127

10





726

n-C30

2429

626

1.011-1.028

10

252*

658*

596

malachite green

2382

164

2.048







900

3-methylcholanthrene

2439

164

2.097







083

indeno(l,2,3-cd)pyrene

2650

164

2.279

20

67

263*

282

dibenzo(a,h)anthracene-d145

2649

164

2.107-2.445

20





382

dibenzo (a,h) anthracene5

2660

282

1.000-1.007

20

49

125

279

benzo(ghi)perylene-d12

2741

164

2.187-2.524

20





379

benzo (ghi) perylene

2750

279

1.001-1.006

20

44

nd

'Reference numbers beginning with 0, 1, 5, or 9 indicate a pollutant quantified by the internal
standard method; reference numbers beginning with 2 or 6 indicate a labeled compound
quantified by the internal standard method; reference numbers beginning with 3 or 7 indicate
a pollutant quantified by isotope dilution.

2Single values in this column are based on single laboratory data.

3This is a minimum level at which the analytical system shall give recognizable mass spectra
(background corrected) and acceptable calibration points. The concentration in the aqueous
or solid phase is determined using the equations in Section 14.0.

September 1989

13


-------
Method 1625C

4Method detection limits determined in digested sludge (low solids) and in filter cake or
compost (high solids).

Specification derived from related compound.

6Detected as azobenzene.

7Detected as diphenylamine.

nd = not detected when spiked into the sludge tested

*Background levels of these compounds were present in the sludge tested, resulting in higher
than expected MDL's. The MDL for these compounds is expected to be approximately
50 Hg/kg with no interferences present.

Column: 30 ±2 m x 0.25 ±0.02 mm i.d. 94% methyl, 4% phenyl, 1% vinyl bonded phase
fused silica capillary.

Temperature program: Five minutes at 30°C; 30-280°C at 8°C per min; isothermal at 280°C
until benzo(ghi)perylene elutes.

Gas velocity: 30 ±5 cm/sec at 30°C.

TABLE 6. GAS CHROMATOGRAPHIC RETENTION TIMES AND DETECTION
LIMITS FOR ACID EXTRACTABLE COMPOUNDS

Method Detection
Retention Time	Limit4











Minimum

Low

High

EGD



Mean

EGD



Level3

Solids

Solids

No.1

Compound

(sec)

Ref

Relative 2

(l-ig/L)

(l-ig/kg)

(l-ig/kg)

164

2,2'-difluorobiphenyl (int
std)

1163

164

1.000-1.000

10





224

2-chlorophenol-d4

701

164

0.587-0.618

10





324

2-chlorophenol

705

224

0.997-1.010

10

18

10

947

hexanoic acid

746

164

0.641







944

p-cresol

834

164

0.717







257

2-nitrophenol-d4

898

164

0.761-0.783

20





357

2-nitrophenol

900

257

0.994-1.009

20

39

44

231

2,4-dichlorophenol-d3

944

164

0.802-0.822

10





331

2,4-dichlorophenol

947

231

0.997-1.006

10

24

116

943

benzoic acid

971

164

0.835







946

2,6-dichlorophenol

981

164

0.844







222

4-chloro-3-methylphenol-d2

1086

164

0.930-0.943

10





322

4-chloro-3-methylphenol

1091

222

0.998-1.003

10

41

62

221

2,4,6-trichlorophenol-d2

1162

164

0.994-1.005

10

46

111

321

2,4,6-trichlorophenol

1165

221

0.998-1.004

10





631

2,4,5-trichlorophenol-d25

1167

164

0.998-1.009

10





731

2,4,5-trichlorophenol

1170

631

0.998-1.004

10

32

55

530

2,3,6-trichlorophenol

1195

164

1.028

10

58

37

259

2,4-dinitrophenol-d3

1323

164

1.127-1.149

50





359

2,4-dinitrophenol

1325

259

1.000-1.005

50

565

642

258

4-nitrophenol-d4

1349

164

1.147-1.175

50





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Method 1625C

TABLE 6. GAS CHROMATOGRAPHIC RETENTION TIMES AND DETECTION
LIMITS FOR ACID EXTRACTABLE COMPOUNDS

Method Detection
Retention Time	Limit4











Minimum

Low

High

EGD



Mean

EGD



Level3

Solids

Solids

No.1

Compound

(sec)

Ref

Relative 2

(l-ig/L)

(l-ig/kg)

(l-ig/kg)

358

4-nitrophenol

1354

2^8

0.997-1.006

50

287

11

948

2,3,4,6-tetrachlorophenol

1371

164

1.179







260

2-methyl-4,6-
dinitrophenol-d2

1433

164

1.216-1.249

20





360

2-methyl-4,6-dinitrophenol

1435

260

1.000-1.002

20

385

83

945

3,5-dibromo-
4-hydroxybenzonitrile

1481

164

1.273







264

pentachlorophenol-13C6

1559

164

1.320-1.363

50





364

pentachlorophenol

1561

264

0.998-1.002

50

51

207

Reference numbers beginning with 0, 1, 5, or 9 indicate a pollutant quantified by the
internal standard method; reference numbers beginning with 2 or 6 indicate a labeled
compound quantified by the internal standard method; reference numbers beginning with 3
or 7 indicate a pollutant quantified by isotope dilution.

2Single values in this column are based on single laboratory data.

3This is a minimum level at which the analytical system shall give recognizable mass spectra
(background corrected) and acceptable calibration points. The concentration in the aqueous
or solid phase is determined using the equations in section 14.

4Method detection limits determined in digested sludge (low solids) and in filter cake or
compost (high solids).

Specification derived from related compound.

Column: 30 ±2 m x 0.25 ±0.02 mm i.d. 94% methyl, 4% phenyl, 1% vinyl bonded phase
fused silica capillary.

Temperature program: Five minutes at 30°C; 30-250°C or until pentachlorophenol elutes.
Gas velocity: 30 ±5 cm/sec at 30°C.

3.0	Contamination And Interferences

3.1	Solvents, reagents, glassware, and other sample processing hardware may yield artifacts
and/or elevated baselines causing misinterpretation of chromatograms and spectra. All
materials used in the analysis shall be demonstrated to be free from interferences under
the conditions of analysis by running method blanks initially and with each sample lot
(samples started through the extraction process on a given eight hour shift, to a
maximum of 20). Specific selection of reagents and purification of solvents by distillation
in all-glass systems may be required. Glassware and, where possible, reagents are
cleaned by solvent rinse and baking at 450°C for one hour minimum.

September 1989

15


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Method 1625C

3.2 Interferences coextracted from samples will vary considerably from source to source,
depending on the diversity of the site being sampled.

4.0	Safety

4.1	The toxicity or carcinogenicity of each compound or reagent used in this method has not
been precisely determined; however, each chemical compound should be treated as a
potential health hazard. Exposure to these compounds should be reduced to the lowest
possible level. The laboratory is responsible for maintaining a current awareness file of
OSHA regulations regarding the safe handling of the chemicals specified in this method.
A reference file of data handling sheets should also be made available to all personnel
involved in these analyses. Additional information on laboratory safety can be found in
References 3-5.

4.2	The following compounds covered by this method have been tentatively classified as
known or suspected human or mammalian carcinogens: benzo(a)anthracene,
3,3'-dichlorobenzidine, dibenzo(a,h)anthracene, benzo(a)pyrene, N-nitrosodimethylamine,
and beta-naphthylamine. Primary standards of these compounds shall be prepared in
a hood, and a NIOSH/MESA approved toxic gas respirator should be worn when high
concentrations are handled.

5.0	Apparatus And Materials

5.1	Sampling Equipment—For discrete or composite sampling.

5.1.1	Sample bottles and caps

5.1.1.1	Liquid samples (waters, sludges and similar materials that contain less
than 5% solids)—Sample bottle, amber glass, 1.1 L minimum, with screw
cap.

5.1.1.2	Solid samples (soils, sediments, sludges, filter cake, compost, and similar
materials that contain more than 5% solids)—Sample bottle, wide mouth,
amber glass, 500 mL minimum.

5.1.1.3	If amber bottles are not available, samples shall be protected from light.

5.1.1.4	Bottle caps—Threaded to fit sample bottles. Caps shall be lined with
Teflon.

5.1.1.5	Cleaning

5.1.1.5.1	Bottles are detergent water washed, then solvent rinsed or
baked at 450°C for one hour minimum before use.

5.1.1.5.2	Cap liners are washed with detergent and water, rinsed
with reagent water (see Section 6.5.1) and then solvent, and
then baked for at least one hour at approximately 200°C.

5.1.2	Compositing equipment—Automatic or manual compositing system incorporating
glass containers cleaned per bottle cleaning procedure above. Sample containers

16

September 1989


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Method 1625C

are kept at 0-4°C during sampling. Only glass or Teflon tubing shall be used. If
the sampler uses a peristaltic pump, a minimum length of compressible silicone
rubber tubing may be used only in the pump. Before use, the tubing shall be
thoroughly rinsed with methanol, followed by repeated rinses with reagent water
(Section 6.5.1) to minimize sample contamination. An integrating flow meter is
used to collect proportional composite samples.

5.2	Equipment—For determining percent moisture.

5.2.1	Oven—Capable of maintaining a temperature of 110 ±5°C.

5.2.2	Desiccator.

5.3	Sonic Disruptor—375 watt with pulsing capability and 3/4 in. disruptor horn
(Ultrasonics, Inc, Model 375C, or equivalent).

5.4	Extraction Apparatus

5.4.1	Continuous liquid-liquid extractor—Teflon or glass connecting joints and
stopcocks without lubrication, 1.5-2 L capacity (Hershberg-Wolf Extractor, Ace
Glass 6841-10, or equivalent).

5.4.2	Beakers

5.4.2.1	1.5-2 L borosilicate glass beakers calibrated to 1 L.

5.4.2.2	400-500 mL borosilicate glass beakers.

5.4.2.3	Spatulas—Stainless steel.

5.4.3	Filtration apparatus

5.4.3.1	Glass funnel—125-250 mL.

5.4.3.2	Filter paper for above (Whatman 41, or equivalent)

5.5	Drying Column—15-20 mm i.d. Pyrex chromatographic column equipped with coarse
glass frit or glass wool plug.

5.6	Concentration Apparatus

5.6.1	Concentrator tube—Kuderna-Danish (K-D) 10 mL, graduated (Kontes K-570050-
1025, or equivalent) with calibration verified. Ground glass stopper (size 19/22
joint) is used to prevent evaporation of extracts.

5.6.2	Evaporation flask—Kuderna-Danish (K-D) 500 mL (Kontes K-570001-0500, or
equivalent), attached to concentrator tube with springs (Kontes K-662750-0012).

5.6.3	Snyder column—Kuderna-Danish (K-D) three-ball macro (Kontes K-503000-0232,
or equivalent).

September 1989

17


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Method 1625C

5.6.4	Snyder column—Kuderna-Danish (K-D) two-ball micro (Kontes K-469002-0219,
or equivalent).

5.6.5	Boiling chips—Approximately 10/40 mesh, extracted with methylene chloride and
baked at 450°C for one hour minimum.

5.6.6	Nitrogen evaporation device—Equipped with a water bath that can be maintained
at 35-40°C. The N-Evap by Organomation Associates, Inc., South Berlin, MA (or
equivalent) is suitable.

5.7	Water Bath—Heated, with concentric ring cover, capable of temperature control (±2°C),
installed in a fume hood.

5.8	Sample Vials—Amber glass, 2-5 mL with Teflon-lined screw cap.

5.9	Balances

5.9.1	Analytical—Capable of weighing 0.1 mg.

5.9.2	Top loading—Capable of weighing 10 mg.

5.10	Automated Gel Permeation Chromatograph—Analytical Biochemical Labs, Inc.,
Columbia, MO, Model GPC Autoprep 1002, or equivalent.

5.10.1	Column—600-700 mm x 25 mm i.d., packed with 70 g of SX-3 Bio-beads (Bio-Rad
Laboratories, Richmond, CA).

5.10.2	UV detectors—254 mu, preparative or semi-prep flow cell:

5.10.2.1	Schmadzu—5 mm path length.

5.10.2.2	Beckman—Altex 152W, 8 |iL micro-prep flow cell, 2 mm path.

5.10.2.3	Pharmacia UV-1— 3 mm flow cell.

5.10.2.4	LDC Milton-Roy UV-3—Monitor #1203.

5.11	Gas Chromatograph—Shall have splitless or on-column injection port for capillary
column, temperature program with 30°C hold, and shall meet all of the performance
specifications in Section 12.

5.11.1 Column—30 ±5 m x 0.25 ±0.02 mm i.d. 5% phenyl, 94% methyl, 1% vinyl silicone
bonded phase fused silica capillary column (J&W DB-5, or equivalent).

5.12	Mass Spectrometer—70 eV electron impact ionization, shall repetitively scan from 35-450
amu in 0.95-1.00 second, and shall produce a unit resolution (valleys between m/z 441-
442 less than 10 percent of the height of the 441 peak), background corrected mass
spectrum from 50 ng decafluorotriphenylphosphine (DFTPP) introduced through the GC
inlet. The spectrum shall meet the mass-intensity criteria in Table 7 (Reference 6). The
mass spectrometer shall be interfaced to the GC such that the end of the capillary column
terminates within one centimeter of the ion source but does not intercept the electron or

18

September 1989


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Method 1625C

ion beams. All portions of the column which connect the GC to the ion source shall
remain at or above the column temperature during analysis to preclude condensation of
less volatile compounds.

TABLE 7. DFTPP MASS-INTENSITY SPECIFICATIONS*

Mass

Intensity Required

51

8-82% of m/z 198

68

less than 2% of m/z 69

69

11-91% of m/z 198

70

less than 2% of m/z 69

127

32-59% of m/z 198

197

less than 1% of m/z 198

198

base peak, 100% abundance

199

4-9% of m/z 198

275

11-30% of m/z 198

441

44-110% of m/z 443

442

30-86% of m/z 198

443

14-24% of m/z 442

*Reference 6.

5.13 Data System—Shall collect and record MS data, store mass-intensity data in spectral
libraries, process GCMS data, generate reports, and shall compute and record response
factors.

5.13.1	Data acquisition—Mass spectra shall be collected continuously throughout the
analysis and stored on a mass storage device.

5.13.2	Mass spectral libraries—User created libraries containing mass spectra obtained
from analysis of authentic standards shall be employed to reverse search GCMS
runs for the compounds of interest (Section 7.2).

5.13.3	Data processing—The data system shall be used to search, locate, identify, and
quantify the compounds of interest in each GCMS analysis. Software routines
shall be employed to compute retention times and peak areas. Displays of
spectra, mass chromatograms, and library comparisons are required to verify
results.

5.13.4	Response factors and multipoint calibrations—The data system shall be used to
record and maintain lists of response factors (response ratios for isotope dilution)
and multi-point calibration curves (Section 7). Computations of relative standard
deviation (coefficient of variation) are used for testing calibration linearity.
Statistics on initial (Section 8.2) and on-going (Section 12.7) performance shall be
computed and maintained.

September 1989

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Method 1625C

6.0	Reagents and Standards

6.1	Reagents for Adjusting Sample pH

6.1.1	Sodium hydroxide—Reagent grade, 6 N in reagent water.

6.1.2	Sulfuric acid—Reagent grade, 6 N in reagent water.

6.2	Sodium Sulfate—Reagent grade, granular anhydrous, rinsed with methylene chloride (20
mL/g), baked at 450°C for one hour minimum, cooled in a desiccator, and stored in a
pre-cleaned glass bottle with screw cap which prevents moisture from entering.

6.3	Methylene Chloride—Distilled in glass (Burdick and Jackson, or equivalent).

6.4	GPC Calibration Solution—Containing 300 mg/mL corn oil, 15 mg/mL bis(2-ethylhexyl)
phthalate, 1.4 mg/mL pentachlorophenol, 0.1 mg/mL perylene, and 0.5 mg/mL sulfur.

6.5	Reference Matrices

6.5.1	Reagent water—Water in which the compounds of interest and interfering
compounds are not detected by this method.

6.5.2	High solids reference matrix—Playground sand or similar material in which the
compounds of interest and interfering compounds are not detected by this
method.

6.6	Standard Solutions—Purchased as solutions or mixtures with certification to their purity,
concentration, and authenticity, or prepared from materials of known purity and
composition. If compound purity is 96% or greater, the weight may be used without
correction to compute the concentration of the standard. When not being used, standards
are stored in the dark at -20 to -10°C in screw-capped vials with Teflon-lined lids. A
mark is placed on the vial at the level of the solution so that solvent evaporation loss can
be detected. The vials are brought to room temperature prior to use. Any precipitate is
redissolved and solvent is added if solvent loss has occurred.

6.7	Preparation of Stock Solutions—Prepare in methylene chloride, benzene, p-dioxane, or
a mixture of these solvents per the steps below. Observe the safety precautions in
Section 4. The large number of labeled and unlabeled acid and base/neutral compounds
used for combined calibration (Section 7) and calibration verification (Section 12.5) require
high concentrations (approximately 40 mg/mL) when individual stock solutions are
prepared, so that dilutions of mixtures will permit calibration with all compounds in a
single set of solutions. The working range for most compounds is 10-200 |ig/mL.
Compounds with a reduced MS response may be prepared at higher concentrations.

6.7.1 Dissolve an appropriate amount of assayed reference material in a suitable
solvent. For example, weigh 400 mg naphthalene in a 10 mL ground glass
stoppered volumetric flask and fill to the mark with benzene. After the
naphthalene is completely dissolved, transfer the solution to a 15 mL vial with
Teflon-lined cap.

20

September 1989


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Method 1625C

6.7.2	Stock standard solutions should be checked for signs of degradation prior to the
preparation of calibration or performance test standards. Quality control check
samples that can be used to determine the accuracy of calibration standards are
available from the US Environmental Protection Agency, Environmental
Monitoring and Support Laboratory, Cincinnati, Ohio 45268.

6.7.3	Stock standard solutions shall be replaced after six months, or sooner if
comparison with quality control check standards indicates a change in
concentration.

6.8	Labeled Compound Spiking Solution—From stock standard solutions prepared as above,
or from mixtures, prepare the spiking solution at a concentration of 200 \ig/mL, or at a
concentration appropriate to the MS response of each compound.

6.9	Secondary Standard—Using stock solutions (Section 6.7), prepare a secondary standard
containing all of the compounds in Tables 1 and 2 at a concentration of 400 |ig/mL, or
higher concentration appropriate to the MS response of the compound.

6.10	Internal Standard Solution—Prepare 2,2'-difluorobiphenyl (DFB) at a concentration of
10 mg/mL in benzene.

6.11	DFTPP Solution—Prepare at 50 |ig/mL in acetone.

6.12	Solutions for Obtaining Authentic Mass Spectra (Section 7.2)—Prepare mixtures of
compounds at concentrations which will assure authentic spectra are obtained for storage
in libraries.

6.13	Calibration Solutions—Combine 5 aliquots of 0.5 mL each of the solution in Section 6.8
with 25, 50, 125, 250, and 500 |iL of the solution in Section 6.9 and bring to 1.00 mL total
volume each. This will produce calibration solutions of nominal 10, 20, 50, 100 and 200
|ig/mL of the pollutants and a constant nominal 100 |ig/mL of the labeled compounds.
Spike each solution with 10 |iL of the internal standard solution (Section 6.10). These
solutions permit the relative response (labeled to unlabeled) to be measured as a function
of concentration (Section 7.4).

6.14	Precision and Recovery Standard—Used for determination of initial (Section 8.2) and on-
going (Section 12.7) precision and recovery. This solution shall contain the pollutants and
labeled compounds at a nominal concentration of 100 |ig/mL.

6.15	Stability of Solutions—All standard solutions (Sections 6.8 through 6.14) shall be analyzed
within 48 hours of preparation and on a monthly basis thereafter for signs of
degradation. Standards will remain acceptable if the peak area at the quantitation mass
relative to the DFB internal standard remains within ±15% of the area obtained in the
initial analysis of the standard.

7.0	Calibration

7.1	Assemble the GCMS and establish the operating conditions in Table 5. Analyze
standards per the procedure in Section 11 to demonstrate that the analytical system meets
the minimum levels in Tables 5 and 6, and the mass-intensity criteria in Table 7 for 50
ng DFTPP.

September 1989

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Method 1625C

12 Mass Spectral Libraries—Detection and identification of compounds of interest are
dependent upon spectra stored in user created libraries.

7.2.1	Obtain a mass spectrum of each pollutant, labeled compound, and the internal
standard by analyzing an authentic standard either singly or as part of a mixture
in which there is no interference between closely eluted components. Examine
the spectrum to determine that only a single compound is present. Fragments not
attributable to the compound under study indicate the presence of an interfering
compound.

7.2.2	Adjust the analytical conditions and scan rate (for this test only) to produce an
undistorted spectrum at the GC peak maximum. An undistorted spectrum will
usually be obtained if five complete spectra are collected across the upper half of
the GC peak. Software algorithms designed to "enhance" the spectrum may
eliminate distortion, but may also eliminate authentic masses or introduce other
distortion.

7.2.3	The authentic reference spectrum is obtained under DFTPP tuning conditions
(Section 7.1 and Table 7) to normalize it to spectra from other instruments.

7.2.4	The spectrum is edited by saving the five most intense mass spectral peaks and
all other mass spectral peaks greater than 10% of the base peak. The spectrum
may be further edited to remove common interfering masses. If five mass
spectral peaks cannot be obtained under the scan conditions given in Section 5.12,
the mass spectrometer may be scanned to an m/z lower than 35 to gain
additional spectral information. The spectrum obtained is stored for reverse
search and for compound confirmation.

7.2.5	For the compounds in Tables 3 and 4 and for other compounds for which the
mass spectra, quantitation m/z's, and retention times are known but the
instrument is not to be calibrated, add the retention time and reference compound
(Tables 5 and 6); the response factor and the quantitation m/z (Tables 8 and 9);
and spectrum (Appendix A) to the reverse search library. Edit the spectrum per
Section 7.2.4, if necessary.

7.3 Analytical Range—Demonstrate that 20 ng anthracene or phenanthrene produces an area
at m/z 178 approx one-tenth that required to exceed the linear range of the system. The
exact value must be determined by experience for each instrument. It is used to match
the calibration range of the instrument to the analytical range and detection limits
required, and to diagnose instrument sensitivity problems (Section 15.3). The 20 |ig/mL
calibration standard (Section 6.13) can be used to demonstrate this performance.

7.3.1 Polar compound detection—Demonstrate that unlabeled pentachlorophenol and
benzidine are detectable at the 50 |ig/mL level (per all criteria in Section 13). The
50 |ig/mL calibration standard (Section 6.13) can be used to demonstrate this
performance.

22

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Method 1625C

TABLE 8. CHARACTERISTIC M/Z's AND RESPONSE FACTORS OF BASE/NEUTRAL

EXTRACTABLE COMPOUNDS

Compound	Labeled Analog Primary m/z1	Response Factor2

acenaphthene

dio

154/164



acenaphthylene

d8

152/160



acetophenone



105

0.79

4-aminobiphenyl



169

0.81

aniline



93

1.04

o-anisidine



108

0.43

anthracene

dio

178/188



aramite



185

0.19

benzanthrone



230

0.15

1,3-benzenediol



110

0.78

benzenethiol



110

0.18

benzidine

d8

184/192



benzo (a) anthracene

diz

228/240



benzo (b) fluoranthene

diz

252/264



benzo (k) fluoranthene

d^

252/264



benzo(a)pyrene

d^

252/264



benzo (ghi) perylene

d^

276/288



2,3-benzofluorene



216

0.35

benzoic acid



105

0.16

benzyl alcohol



79

0.47

biphenyl

dio

154/164



bis(2-chloroethyl) ether

d8

93/101



bis(2-chloroethoxy)methane

d6

93/99



bis(2-chloroisopropyl) ether

d^

121/131



bis(2-ethylhexyl) phthalate

d4

149/153



2-bromochlorobenzene



111

0.33

3-bromochlorobenzene



192

0.40

4-bromophenyl phenyl ether

d5

248/253



butyl benzyl phthalate

d4

149/153



n-CIO

d22

57/82



n-C12

d26

57/66



n-C14



57



n-C16

d34

57/66



n-C18



57



n-C20

d42

57/66



n-C22



57



n-C24

dso

57/66



n-C26



57



n-C28



57



n-C30

d62

57/66



carbazole

d8

167/175



4-chloro-2-nitroaniline



172

0.20

5-chloro-o-toluidine



106

0.50

4-chloroaniline



127

0.73

2-chloronaphthalene

d7

162/169



3-chloronitrobenzene



157

0.18

4-chlorophenyl phenyl ether

d5

204/209



September 1989

23


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Method 1625C

TABLE 8. CHARACTERISTIC M/Z's AND RESPONSE FACTORS OF BASE/NEUTRAL

EXTRACTABLE COMPOUNDS

Compound

Labeled Analog

Primary m/z1

Response

3-chloropropionitrile



54

0.42

chrysene

diz

228/240



o-cresol



108

0.59

crotoxyphos



127

0.017

p-cymene

dM

119/130



2,6-di-tert-butyl-



220

0.078

p-benzoquinone







di-n-butyl phthalate

d4

149/153



2,4-diaminotoluene



122

0.059

dibenzo (a,h) anthracene

dM

278/292



dibenzofuran

d8

168/176



dibenzothiophene

d8

184/192



1,2-dibromo-3-chloropropane



157

0.22

2,6-dichloro-4-nitroaniline



124

0.019

l,3-dichloro-2-propanol



79

0.68

2,3-dichloroaniline



161

0.47

1,2-dichlorobenzene

d4

146/152



1,3-dichlorobenzene

d4

146/152



1,4-dichlorobenzene

d4

146/152



3,3'-dichlorobenzidine

d6

252/258



2,2'-difluorobiphenyl (int std)



190



2,3-dichloronitrobenzene



191

0.11

l,2:3,4-diepoxybutane



55

0.27

diethyl phthalate

d4

149/153



3,3'-dimethoxybenzidine



244

0.19

dimethyl phthalate

d4

163/167



dimethyl sulfone



79

0.40

p-dimethylaminoazobenzene



120

0.23

7,12-dimethylbenz(a)



256

0.58

anthracene







N,N-dimethylformamide



73

0.51

3,6-dimethylphenanthrene



206

0.72

2,4-dimethylphenol

d3

122/125



1,4-dinitrobenzene



168

0.24

2,4-dinitrotoluene

d3

165/168



2,6-dinitrotoluene

d3

165/167



di-n-octyl phthalate

d4

149/153



diphenylamine

dio

169/179



diphenyl ether

dio

170/180



diphenyldisulfide



218

0.25

1,2-diphenylhydrazine3

dio

77/82



ethyl methanesulfonate



109

0.28

ethylenethiourea



102

0.22

ethynylestradiol 3-methyl ether



227

0.28

fluoranthene

dio

202/212



fluorene

dio

166/176



hexachlorobenzene

13C

284/292



24

September 1989


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Method 1625C

TABLE 8. CHARACTERISTIC M/Z's AND RESPONSE FACTORS OF BASE/NEUTRAL

EXTRACTABLE COMPOUNDS

Compound

Labeled Analog

Primary m/z1

Response Factor2

hexachlorobutadiene

4

225/231



hexachloroethane

13c

201/204



hexachlorocyclopentadiene

13C4

237/241



hexachloropropene



213

0.23

indeno(l,2,3-cd)pyrene



276



isophorone

d8

82/88



2-isopropylnaphthalene



170

0.32

isosafrole



162

0.33

longifolene



161

0.14

malachite green



330



methapyrilene



97

0.43

methyl methanesulfonate



80

0.20

2-methylbenzothiazole



149

0.59

3-methylcholanthrene



268

0.59

4,4'-methylenebis



231

0.21

(2-chloroaniline)







4,5-methylenephenanthrene



190

0.44

1 -methy lfluorene



180

0.37

2-methylnaphthalene



142

0.99

1 -methy lphenanthrene



192

0.65

2-(methylthio)benzothiazole



181

0.42

naphthalene

d8

128/136



1,5-naphthalenediamine



158

0.085

1,4-naphthoquinone



158

0.021

alpha-naphthylamine



143

0.89

beta-naphthylamine

d7

143/150



5-nitro-o-toluidine



152

0.31

2-nitroaniline



138

0.39

3-nitroaniline



138

0.27

4-nitroaniline



138

0.11

nitrobenzene

d5

123/128



4-nitrobiphenyl



199

0.35

N-nitrosodi-n-butylamine



84

0.47

N-nitrosodi-n-propylamine

dM

70/78



N-nitrosodiethylamine



102

0.45

N-nitrosodimethylamine

d6

74/80



N-nitrosodiphenylamine4

d6

169/175



N-nitrosomethylethylamine



88

0.33

N-nitrosomethylphenylamine



106

0.024

N-nitrosomorpholine



56

0.49

N-nitrosopiperidine



114

0.41

pentachlorobenzene



248

0.25

pentachloroethane



117

0.20

pentamethylbenzene



148

0.42

perylene



252

0.30

phenacetin



108

0.38

phenanthrene

dio

178/188



September 1989

25


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Method 1625C

TABLE 8. CHARACTERISTIC M/Z's AND RESPONSE FACTORS OF BASE/NEUTRAL

EXTRACTABLE COMPOUNDS

Compound

Labeled Analog

Primary m/z1

Response Factor2

phenol

d5

94/71



phenothiazine



199

0.15

1 -pheny lnaphthalene



204

0.48

2-phenylnaphthalene



204

0.73

alpha-picoline

d7

93/100



pronamide



173

0.31

pyrene

dio

202/212



pyridine



79

0.68

safrole



162

0.45

squalene



69

0.042

styrene

d5

104/109



alpha-terpineol

d3

59/62



1,2,4,5-tetrachlorobenzene



216

0.43

thianaphthene



134

1.52

thioacetamide



75

0.28

thioxanthone



212

0.23

o-toluidine



106

1.04

1,2,3-trichlorobenzene

d3

180/183



1,2,4-trichlorobenzene

d3

180/183



1,2,3-trimethoxy benzene



168

0.48

2,4,5-trimethylaniline



120

0.28

triphenylene



228

1.32

tripropylene glycol methyl



59

0.092

ether







1,3,5-trithiane



138

0.15

Referenced to 2,2'-difluorobiphenyl
3Detected as azobenzene
4Detected as diphenylamine

NOTE: Because the composition and purity of commercially-supplied isotopically labeled standards
may vary, the primary m/z of the labeled analogs given in this table should be used as guidance. The
appropriate m/z of the labeled analogs should be determined prior to use for sample analysis.
Deviations from the m/z's listed here must be documented by the laboratory and submitted with the
data.

26

September 1989


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Method 1625C

TABLE 9. CHARACTERISTIC M/Z'S AND RESPONSE FACTORS OF ACID

EXTRACTABLE COMPOUNDS

Compound

Labeled Analog

Primary m/z1

Response Factor2

benzoic acid



105

0.16

4-chloro-3-methylphenol

d2

107/109



2-chlorophenol

d4

128/132



p-cresol



108

0.61

3,5-dibromo-4-hydroxybenzonitrile



277

0.12

2,4-dichlorophenol

d3

162/167



2,6-dichlorophenol



162

0.42

2,4-dinitrophenol

d3

184/187



hexanoic acid



60

0.62

2-methyl-4,6-dinitrophenol

d2

198/200



2-nitrophenol

d4

65/109



4-nitrophenol

d4

65/109



pentachlorophenol

13c6

266/272



2,3,4,6-tetrachlorophenol



232

0.17

2,3,6-trichlorophenol

d2

196/200



2,4,5-trichlorophenol

d2

196/200



2,4,6-trichlorophenol

d2

196/200



Native/labeled.

Referenced to 2,2'-difluorobiphenyl.

NOTE: Because the composition and purity of commercially-supplied isotopically labeled standards
may vary, the primary m/z of the labeled analogs given in this table should be used as guidance. The
appropriate m/z of the labeled analogs should be determined prior to use for sample analysis.

Deviations from the m/z's listed here must be documented by the laboratory and submitted with the
data.

7.4 Calibration with Isotope Dilution—Isotope dilution is used when 1) labeled compounds
are available, 2) interferences do not preclude its use, and 3) the quantitation m/z (Tables
8 and 9) extracted ion current profile (EICP) area for the compound is in the calibration
range. Alternate labeled compounds and quantitation m/z's may be used based on
availability. If any of the above conditions preclude isotope dilution, the internal
standard method (Section 7.5) is used.

7.4.1 A calibration curve encompassing the concentration range is prepared for each
compound to be determined. The relative response (pollutant to labeled) vs
concentration in standard solutions is plotted or computed using a linear
regression. The example in Figure 1 shows a calibration curve for phenol using
phenol-d5 as the isotopic diluent. Also shown are the ±10% error limits (dotted
lines). Relative Response (RR) is determined according to the procedures
described below. A minimum of five data points are employed for calibration.

September 1989

27


-------
Method 1625C

2	10 20 50 100 200

CONCENTRATION (ug/mL)

FIGURE 1 Relative Response Calibration Curve
for Phenol. The Dotted Lines Enclose a ± lO Per-
cent Error Window.

7.4.2 The relative response of a pollutant to its labeled analog is determined from
isotope ratio values computed from acquired data. Three isotope ratios are used
in this process:

Rx = the isotope ratio measured for the pure pollutant.

Ry = the isotope ratio measured for the labeled compound.

Rm = the isotope ratio of an analytical mixture of pollutant and labeled
compounds.

The m/z's are selected such that Rx > Ry. If is not between 2^ and 0.5^ , the
method does not apply and the sample is analyzed by the internal standard
method.

28

September 1989


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Method 1625C

7.4.3 Capillary columns usually separate the pollutant-labeled pair, with the labeled
compound eluted first (Figure 2). For this case,

AREA AT

FIGURE 2 Extracted Ion Current Profiles for
Chromatographically Resolved Labeled (m2/z)
and Unlabeled (rr^/z) Pairs.

[area m /z (at RT )]

R = 	-	—

X	1

1

R = 	

y [area m /z (at RT )]

R

[area m^/z (at RT^]

m [area mjz (at RT )]

as measured in the mixture of the pollutant and labeled compounds (Figure 2),
and RR = Rm.

7.4.4 Special precautions are taken when the pollutant-labeled pair is not separated, or
when another labeled compound with interfering spectral masses overlaps the
pollutant (a case which can occur with isomeric compounds). In this case, it is
necessary to determine the respective contributions of the pollutant and labeled
compounds to the respective EICP areas. If the peaks are separated well enough
to permit the data system or operator to remove the contributions of the
compounds to each other, the equations in Section 7.4.3 apply. This usually
occurs when the height of the valley between the two GC peaks at the same m/z
is less than 10% of the height of the shorter of the two peaks. If significant GC
and spectral overlap occur, RR is computed using the following equation:

September 1989

29


-------
Method 1625C

RR =

_ (Ry - Rm) (Rx + 1)
(Rm " Rx) (Ry +D

where,

Rx = Measured as shown in Figure 3A.
Ry = Measured as shown in Figure 3B.
Rm = Measured as shown in Figure 3C.

For the example,

R. =	= 9.644

4780

= _2650^ = 0 06()78
y 43600

R =	= 1.019

m 48300

RR = 1.115

The data from these analyses are reported to three significant figures (see Section
14.6). Therefore, in order to prevent rounding errors from affecting the values to
be reported, all calculations performed prior to the final determination of
concentrations should be carried out using at least four significant figures.

7.4.5	To calibrate the analytical system by isotope dilution, analyze a 1.0 |iL aliquot of
each of the calibration standards (Section 6.13) using the procedure in Section
11.0. Compute the RR at each concentration.

7.4.6	Linearity—If the ratio of relative response to concentration for any compound is
constant (less than 20% coefficient of variation) over the five-point calibration
range, an averaged relative response/concentration ratio may be used for that
compound; otherwise, the complete calibration curve for that compound shall be
used over the 5 point calibration range.

30

September 1989


-------
Method 1625C

(3A)

AREA = 46100

AREA = 4780

FIGURE 3 Extracted Ion Current Profiles for (3A)
Unlabeled Compound, (3B) Labeled Com-
pound, and (3C) Equal Mixture of Unlabeled
and Labeled Compounds.

7.5 Calibration by Internal Standard—Used when criteria for isotope dilution (Section 7.4)
cannot be met. The internal standard to be used for both acid and base/neutral analyses
is 2,2'-difluorobi-phenyl. The internal standard method is also applied to determination
of compounds having no labeled analog, and to measurement of labeled compounds for
intra-laboratory statistics (Sections 8.4 and 12.7.4).

7.5.1 Response factors—Calibration requires the determination of response factors (RF)
which are defined by the following equation:

(\ x cj

RF = —-	—

(Ais x Cs)

where,

As = The area of the characteristic mass for the compound in the daily
standard.

Ais = The area of the characteristric mass for the internal standard.

Cis = The concentration of the internal standard (]ig/mL).

Cs = The concentration of the compound in the daily standard (]ig/mL).

September 1989

31


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Method 1625C

7.5.1.1	The response factor is determined for at least five concentrations
appropriate to the response of each compound (Section 6.13); nominally,
10, 20, 50, 100, and 200 |ig/mL. The amount of internal standard added
to each extract is the same (100 |ig/mL) so that Cis remains constant. The
RF is plotted vs concentration for each compound in the standard (CJ to
produce a calibration curve.

7.5.1.2	Linearity—If the response factor (RF) for any compound is constant (less
than 35% coefficient of variation) over the five-point calibration range, an
averaged response factor may be used for that compound; otherwise, the
complete calibration curve for that compound shall be used over the five-
point range.

7.6 Combined Calibration—By using calibration solutions (Section 6.13) containing the
pollutants, labeled compounds, and the internal standard, a single set of analyses can be
used to produce calibration curves for the isotope dilution and internal standard
methods. These curves are verified each shift (Section 12.5) by analyzing the 100 |ig/mL
calibration standard (Section 6.13). Re-calibration is required only if calibration
verification (Section 12.5) criteria cannot be met.

8.0	Quality Assurance/Quality Control

8.1	Each laboratory that uses this method is required to operate a formal quality assurance
program (Reference 7). The minimum requirements of this program consist of an initial
demonstration of laboratory capability, analysis of samples spiked with labeled
compounds to evaluate and document data quality, and analysis of standards and blanks
as tests of continued performance. Laboratory performance is compared to established
performance criteria to determine if the results of analyses meet the performance
characteristics of the method. If the method is to be applied routinely to samples
containing high solids with very little moisture (e.g., soils, filter cake, compost), the high
solids reference matrix (Section 6.5.2) is substituted for the reagent water (Section 6.5.1)
in all performance tests, and the high solids method (Section 10) is used for these tests.

8.1.1	The analyst shall make an initial demonstration of the ability to generate
acceptable accuracy and precision with this method. This ability is established as
described in Section 8.2.

8.1.2	The analyst is permitted to modify this method to improve separations or lower
the costs of measurements, provided all performance specifications are met. Each
time a modification is made to the method, the analyst is required to repeat the
procedure in Section 8.2 to demonstrate method performance.

8.1.3	Analyses of blanks are required to demonstrate freedom from contamination. The
procedures and criteria for analysis of a blank are described in Section 8.5.

8.1.4	The laboratory shall spike all samples with labeled compounds to monitor
method performance. This test is described in Section 8.3. When results of these
spikes indicate atypical method performance for samples, the samples are diluted
to bring method performance within acceptable limits (Section 15).

32

September 1989


-------
Method 1625C

8.1.5	The laboratory shall, on an on-going basis, demonstrate through calibration
verification and the analysis of the precision and recovery standard (Section 6.14)
that the analysis system is in control. These procedures are described in Sections
12.1, 12.5, and 12.7.

8.1.6	The laboratory shall maintain records to define the quality of data that is
generated. Development of accuracy statements is described in Section 8.4.

8.2 Initial Precision and Accuracy—To establish the ability to generate acceptable precision

and accuracy, the analyst shall perform the following operations:

8.2.1	For low solids (aqueous samples), extract, concentrate, and analyze two sets of
four 1 L aliquots (eight aliquots total) of the precision and recovery standard
(Section 6.14) according to the procedure in Section 10. For high solids samples,
two sets of four 30 g aliquots of the high solids reference matrix are used.

8.2.2	Using results of the first set of four analyses, compute the average recovery (X)
in |ig/mL and the standard deviation of the recovery(s) in |ig/mL for each
compound, by isotope dilution for pollutants with a labeled analog, and by
internal standard for labeled compounds and pollutants with no labeled analog.

8.2.3	For each compound, compare s and X with the corresponding limits for initial
precision and accuracy in Table 10. If s and X for all compounds meet the
acceptance criteria, system performance is acceptable and analysis of blanks and
samples may begin. If, however, any individual s exceeds the precision limit or
any individual X falls outside the range for accuracy, system performance is
unacceptable for that compound.

NOTE: The large number of compounds in Table 10 present a substantial probability that one or more
will fail the acceptance criteria when all compounds are analyzed.

To determine if the analytical system is out of control, or if the failure can be
attributed to probability, proceed as follows:

8.2.4 Using the results of the second set of four analyses, compute s and X for only
those compounds which failed the test of the first set of four analyses
(Section 8.2.3). If these compounds now pass, system performance is acceptable
for all compounds and analysis of blanks and samples may begin. If, however,
any of the same compounds fail again, the analysis system is not performing
properly for these compounds. In this event, correct the problem and repeat the
entire test (Section 8.2.1).

8.3 The laboratory shall spike all samples with labeled compounds to assess method

performance on the sample matrix.

8.3.1	Analyze each sample according to the method beginning in Section 10.

8.3.2	Compute the percent recovery (P) of the labeled compounds using the internal
standard method (Section 7.5).

September 1989

33


-------
Method 1625C

8.3.3 Compare the labeled compound recovery for each compound with the
corresponding limits in Table 10. If the recovery of any compound falls outside
its warning limit, method performance is unacceptable for that compound in that
sample. Therefore, the sample is complex. Water samples are diluted, and
smaller amounts of soils, sludges, and sediments are reanalyzed per Section 15.

8.4 As part of the QA program for the laboratory, method accuracy for samples shall be
assessed and records shall be maintained. After the analysis of five samples of a given
matrix type (water, soil, sludge, sediment) for which the labeled compounds pass the
tests in Section 8.3, compute the average percent recovery (P) and the standard deviation
of the percent recovery (Sp) for the labeled compounds only. Express the accuracy
assessment as a percent recovery interval from P - 2sp to P + 2^ for each matrix.

For example: If P = 90% and sp = 10% for five analyses of compost, the accuracy interval
is expressed as 70-110%. Update the accuracy assessment for each
compound in each matrix on a regular basis (e.g., after each 5-10 new
accuracy measurements).

TABLE 10. ACCEPTANCE CRITERIA FOR PERFORMANCE TESTS





Labeled and native





Labeled and





compound initial

Labeled



native





precision and

compound

Calibration

compound







accuracy

recovery

verification

ongoing





(Section 8.2.3)

(Sections 8.3 _

(Section

accuracy

EGD
No.1





(ue/L)

and 14.2)

12.5)

(Section 12.7)

Compound

s

X

P (%)

(l-ig/L)

R (ng/L)

301

acenaphthene

21

79-134



80-125

72-144

201

acenaphthene-d10

38

38-147

20-270

71-141

30-180

377

acenaphthylene

38

69-186



60-166

61-207

277

acenaphthylene-d8

31

39-146

23-239

66-152

33-168

378

anthracene

41

58-174



60-168

50-199

278

anthracene-d10

49

31-194

14-419

58-171

23-242

305

benzidine

119

16-518



34-296

11-672

205

benzidine-d8

269

ns2-ns

ns-ns

ns-ns

ns-ns

372

benzo (a) anthracene

20

65-168



70-142

62-176

272

benzo (a) anthracene-dj 2

41

25-298

12-605

28-357

22-329

374

benzo (b) fluoranthene

183

32-545



61-164

20-ns

274

benzo (b) fluoranthene-dj 2

168

11-577

ns-ns

14-ns

ns-ns

375

benzo (k) fluoranthene

26

59-143



13-ns

53-155

275

benzo (k) fluoranthene-dj 2

114

15-514

ns-ns

13-ns

ns-685

373

benzo(a)pyrene

26

62-195



78-129

59-206

273

benzo(a)pyrene-d12

24

35-181

21-290

12-ns

32-194

379

benzo (ghi)perylene

21

72-160



69-145

58-168

279

benzo (ghi) pery lene-dj 2

45

29-268

14-529

13-ns

25-303

712

biphenyl (Appendix C)

41

75-148



58-171

62-176

612

biphenyl-d10

43

28-165

ns-ns

52-192

17-267

318

bis (2-chlor oethy 1) ether

34

55-196



61-164

50-213

218

bis(2-chloroethyl) ether d8

33

29-196

15-372

52-194

25-222

343

bis(2-chloroethoxy)
methane

27

43-153



44-228

39-166

34

September 1989


-------
Method 1625C

TABLE 10. ACCEPTANCE CRITERIA FOR PERFORMANCE TESTS





Labeled and native





Labeled and





compound initial

Labeled



native





precision and

compound

Calibration

compound







accuracy

recovery

verification

ongoing





(Section 8.2.3)

(Sections 8.3 _

(Section

accuracy







(ue/L)

and 14.2)

12.5)

(Section 12.7)

EjVjL)

No.1

Compound

s

X

P (%)

(l-ig/L)

R (ng/L)

243

bis(2-chloroethoxy)

33

29-196

15-372

52-194

25-222



methane3











342

bis(2-chloroisopropyl) ether

17

81-138



67-148

77-145

242

bis(2-chloroisopropyl)

27

35-149

20-260

44-229

30-169



ether-d12











366

bis(2-ethylhexyl) phthalate

31

69-220



76-131

64-232

266

bis(2-ethylhexyl) phthalate-

A

29

32-205

18-364

43-232

28-224

341

4

4-bromophenyl phenyl

44

44-140



52-193

35-172



ether











241

4-bromophenylphenyl

52

40-161

19-325

57-175

29-212



ether-d53











367

butyl benzyl phthalate

31

19-233



22-450

35-170

267

butyl benzyl phthalate-d43

29

32-205

18-364

43-232

28-224

717

n-CIO (Appendix C)

51

24-195



42-235

19-237

617

n-C10-d22

70

ns-298

ns-ns

44-227

ns-504

706

n-C12 (Appendix C)

74

35-369



60-166

29-424

606

n-C12-d26

53

ns-331

ns-ns

41-242

ns-408

518

n-C14 (Appendix C)3

109

ns-ns



37-268

ns-ns

719

n-C16 (Appendix C)

33

80-162



72-138

71-181

619

n-C16-d34

46

37-162

18-308

54-186

28-202

520

n-C18 (Appendix C)3

39

42-131



40-249

35-167

721

n-C20 (Appendix C)

59

53-263



54-184

46-301

621

n-C20-d42

34

34-172

19-306

62-162

29-198

522

n-C22 (Appendix C)3

31

45-152



40-249

39-195

723

n-C24 (Appendix C)

11

80-139



65-154

78-142

623

n-C24-d50

28

27-211

15-376

50-199

25-229

524

n-C26 (Appendix C)3

35

35-193



26-392

31-212

525

n-C28 (Appendix C)3

35

35-193



26-392

31-212

726

n-C30 (Appendix C)

32

61-200



66-152

56-215

626

n-C30-d62

41

27-242

13-479

24-423

23-274

728

carbazole (4c)

38

36-165



44-227

31-188

628

carbazole-d83

31

48-130

29-215

69-145

40-156

320

2-chloronaphthalene

100

46-357



58-171

35-442

220

2-chloronaphthalene-d7

41

30-168

15-324

72-139

24-204

322

4-chloro-3-methylphenol

37

76-131



85-115

62-159

222

4-chloro-3-methylphenol-d2

111

30-174

ns-613

68-147

14-314

324

2-chlorophenol

13

79-135



78-129

76-138

224

2-chlorophenol-d4

24

36-162

23-255

55-180

33-176

340

4-chlorophenyl phenyl

42

75-166



71-142

63-194

September 1989

35


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Method 1625C

TABLE 10. ACCEPTANCE CRITERIA FOR PERFORMANCE TESTS





Labeled and native





Labeled and





compound initial

Labeled



native





precision and

compound

Calibration

compound







accuracy

recovery

verification

ongoing





(Section 8.2.3)

(Sections 8.3 _

(Section

accuracy







(ue/L)

and 14.2)

12.5)

(Section 12.7)

EjVjL)

No.1

Compound

s

X

P (%)

(l-ig/L)

R (ng/L)

240

4-chlorophenyl phenyl

62

40-161

19-325

57-175

29-212



ether-d5











376

chrysene

51

59-186



70-142

48-221

276

chrysene-d12

69

33-219

13-512

24-411

23-290

713

p-cymene (Appendix C)

18

76-140



79-127

72-147

613

p-cymene-d14

67

ns-359

ns-ns

66-152

ns-468

382

dibenzo (a,h) anthracene

55

23-299



13-761

19-340

282

dibenzo(a.h)

45

29-268

14-529

13-ns

25-303



anthracene-d143











705

dibenzofuran (Appendix C)

20

85-136



73-136

79-146

605

dibenzofuran-d8

31

47-136

28-220

66-150

39-160

704

dibenzothiophene (Synfuel)

31

79-150



72-140

70-168

604

dibenzothiophene-d8

31

48-130

29-215

69-145

40-156

368

di-n-butyl phthalate

15

76-165



71-142

74-169

268

di-n-butyl phthalate-d4

23

23-195

13-346

52-192

22-209

325

1,2-dichlorobenzene

17

73-146



74-135

70-152

225

1,2-dichlorobenzene-d4

35

14-212

ns-494

61-164

11-247

326

1,3-dichlorobenzene

43

63-201



65-154

55-225

226

l,3-dichlorobenzene-d4

48

13-203

ns-550

52-192

ns-260

327

1,4-dichlorobenzene

42

61-194



62-161

53-219

227

l,4-dichlorobenzene-d4

48

15-193

ns-474

65-153

11-245

328

3,3'-dichlorobenzidine

26

68-174



77-130

64-185

228

3,3'-dichlorobenzidine-d6

80

ns-562

ns-ns

18-558

ns-ns

331

2,4-dichlorophenol

12

85-131



67-149

83-135

231

2,4-dichlorophenol-d3

28

38-164

24-260

64-157

34-182

370

diethyl phthalate

44

75-196



74-135

65-222

270

diethyl phthalate-d4

78

ns-260

ns-ns

47-211

ns-ns

334

2,4-dimethylphenol

13

62-153



67-150

60-156

234

2,4-dimethylphenol-d3

22

15-228

ns-449

58-172

14-242

371

dimethyl phthalate

36

74-188



73-137

67-207

271

dimethyl phthalate-d4

108

ns-640

ns-ns

50-201

ns-ns

359

2,4-dinitrophenol

18

72-134



75-133

68-141

259

2,4-dinitrophenol-d3

66

22-308

ns-ns

39-256

17-378

335

2,4-dinitrotoluene

18

75-158



79-127

72-164

235

2,4-dinitrotoluene-d3

37

22-245

10-514

53-187

19-275

336

2,6-dinitrotoluene

30

80-141



55-183

70-159

236

2,6-dinitrotoluene-d3

59

44-184

17-442

36-278

31-250

369

di-n-octyl phthalate

16

77-161



71-140

74-166

269

di-n-octyl phthalate-d4

46

12-383

ns-ns

21-467

10-433

707

diphenylamine (Appendix

n

45

58-205



57-176

51-231

607

diphenylamine-d10

42

27-206

11-488

59-169

21-249

36

September 1989


-------
Method 1625C

TABLE 10. ACCEPTANCE CRITERIA FOR PERFORMANCE TESTS

Labeled and native	Labeled and

Labeled	native

compound Calibration	compound

recovery verification	ongoing

(Sections 8.3 _ (Section	accuracy

and 14.2) 12.5)	(Section 12.7)

No.1	Compound	s	X	P (%)	(|Jg/L) R (pg/L)

708

diphenyl ether (Appendix

n

19

82-136



83-120

77-144

608

diphenyl ether-d10

37

36-155

19-281

77-129

29-186

337

1,2-dipheny lhydrazine

73

49-308



75-134

40-360

237

l,2-diphenylhy-drazine-d10

35

31-173

17-316

58-174

26-200

339

fluoranthene

33

71-177



67-149

64-194

239

fluoranthene-d10

35

36-161

20-278

47-215

30-187

380

fluorene

29

81-132



74-135

70-151

280

fluorene-d10

43

51-131

27-238

61-164

38-172

309

hexachlorobenzene

16

90-124



78-128

85-132

209

hexachlorobenzene-13C6

81

36-228

13-595

38-265

23-321

352

hexachlorobutadiene

56

51-251



74-135

43-287

252

hexachlorobutadiene-13C4

63

ns-316

ns-ns

68-148

ns-413

312

hexachloroethane

227

21-ns



71-141

13-ns

212

hexachloroethane-13C

77

ns-400

ns-ns

47-212

ns-563

353

hexachlorocyclo-pentadiene

15

69-144



77-129

67-148

253

hexachlorocyclo-

60

ns-ns

ns-ns

47-211

ns-ns



pentadiene-13C4











083

ideno(l,2,3-cd)pyrene3

55

23-299



13-761

19-340

354

isophorone

25

76-156



70-142

70-168

254

isophorone-d8

23

49-133

33-193

52-194

44-147

360

2-methyl-4,6-dinitrophenol

19

77-133



69-145

72-142

260

2-methyl-4,6-dinitrophenol-

A

64

36-247

16-527

56-177

28-307

355

2

naphthalene

20

80-139



73-137

75-149

255

naphthalene-d8

39

28-157

14-305

71-141

22-192

702

beta-naphthylamine

49

10-ns



39-256

ns-ns



(Appendix C)











602

beta-naphthylamine-d7

33

ns-ns

ns-ns

44-230

ns-ns

356

nitrobenzene

25

69-161



85-115

65-169

256

nitrobenzene-d5

28

18-265

ns-ns

46-219

15-314

357

2-nitrophenol

15

78-140



77-129

75-145

257

2-nitrophenol-d4

23

41-145

27-217

61-163

37-158

358

4-nitrophenol

42

62-146



55-183

51-175

258

4-nitrophenol-d4

188

14-398

ns-ns

35-287

ns-ns

361

N-nitrosodimethylamine

49

10-ns



39-256

ns-ns

261

N-nitrosodimethyl-amine-

A 3

33

ns-ns

ns-ns

44-230

ns-ns

363

6

N-nitrosodi-n-propylamine

45

65-142



68-148

53-173

263

N-nitrosodi-n-propylamine3

37

54-126

26-256

59-170

40-166

362

N-nitrosodiphenylamine

45

65-142



68-148

53-173

compound initial
precision and

accuracy
(Section 8.2.3)
lug/Ll

September 1989

37


-------
Method 1625C

TABLE 10. ACCEPTANCE CRITERIA FOR PERFORMANCE TESTS

EGD
No.1

Compound

Labeled and native
compound initial
precision and

accuracy
(Section 8.2.3)

lUg/Ll
s	X

Labeled
compound Calibration
recovery verification
(Sections 8.3 _ (Section
and 14.2)	12.5)

P (%)	(pg/L)

Labeled and

native
compound
ongoing
accuracy
(Section 12.7)

R (pg/L)

262	N -nitrosodiphenyl-amine-	37	54-126
d6

364	pentachlorophenol	21	76-140

264	pentachlorophenol-13C6	49	37-212
381	phenanthrene	13	93-119
281	phenanthrene-d10	40	45-130

365	phenol	36	77-127

265	phenol-d5	161	21-210
703	alpha-picoline (Synfuel)	38	59-149
603	alpha-picoline-d7	138	11-380
384	pyrene	19	76-152
284	pyrene-d10	29	32-176
710	styrene (Appendix C)	42	53-221
610	styrene-d5	49	ns-281
709	alpha-terpineol (Appendix	44	42-234

C)

609	alpha-terpineol-d3	48	22-292

729	1,2,3-trichloro-benzene (4c)	69	15-229

629	l,2,3-trichloro-benzene-d33	57	15-212

308	1,2,4-trichlorobenzene	19	82-136

208	l,2,4-trichlorobenzene-d3	57	15-212

530	2,3,6-trichloro-phenol (4c)3	30	58-137

731	2,4,5-trichlorophenol (4c)	30	58-137

631	2,4,5-trichlorophenol-d23	47	43-183

321	2,4,6-trichlorophenol	57	59-205

221	2,4,6-trichlorophenol-d2	47	43-183

26-256

18-412
24-241
ns-ns
ns-ns
18-303
ns-ns

ns-672
ns-592
ns-592

21-363
21-363

59-170

77-130
42-237

75-133
67-149
65-155
48-208

60-165
31-324

76-132
48-210
65-153
44-228
54-186

20-502

60-167

61-163

78-128
61-163
56-180
56-180
69-144
81-123
69-144

40-166

71-150
29-254
87-126
34-168
62-154
ns-ns

50-174
ns-608

72-159
28-196
48-244
ns-348
38-258

18-339
11-297
10-282
77-144
10-282

51-153
51-153
34-226
48-244
34-226

Reference numbers beginning with 0, 1 or 5 indicate a pollutant quantified by the internal
standard method; reference numbers beginning with 2 or 6 indicate a labeled compound
quantified by the internal standard method; reference numbers beginning with 3 or 7 indicate a
pollutant quantified by isotope dilution.

2ns = no specification: limit is outside the range that can be measured reliably.

3This compound is to be determined by internal standard; specification is derived from related

compound.

Blanks—Reagent water and high solids reference matrix blanks are analyzed to
demonstrate freedom from contamination.

8.5.1 Extract and concentrate a 1 L reagent water blank or a high solids reference
matrix blank with each sample lot (samples started through the extraction process

38

September 1989


-------
Method 1625C

on the same eight hour shift, to a maximum of 20 samples). Analyze the blank
immediately after analysis of the precision and recovery standard (Section 6.14)
to demonstrate freedom from contamination.

8.5.2 If any of the compounds of interest (Tables 1-4) or any potentially interfering
compound is found in an aqueous blank at greater than 10 Hg/L, or in a high
solids reference matrix blank at greater than 100 \ig/kg (assuming a response
factor of 1 relative to the internal standard for compounds not listed in Tables 1-
4), analysis of samples is halted until the source of contamination is eliminated
and a blank shows no evidence of contamination at this level.

8.6	The specifications contained in this method can be met if the apparatus used is calibrated
properly, then maintained in a calibrated state. The standards used for calibration
(Section 7), calibration verification (Section 12.5), and for initial (Section 8.2) and on-going
(Section 12.7) precision and recovery should be identical, so that the most precise results
will be obtained. The GCMS instrument in particular will provide the most reproducible
results if dedicated to the settings and conditions required for the analyses of
semivolatiles by this method.

8.7	Depending on specific program requirements, field replicates may be collected to
determine the precision of the sampling technique, and spiked samples may be required
to determine the accuracy of the analysis when the internal standard method is used.

9.0	Sample Collection, Preservation, and Handling

9.1	Collect samples in glass containers following conventional sampling practices (Reference
8). Aqueous samples which flow freely are collected in refrigerated bottles using
automatic sampling equipment. Solid samples are collected as grab samples using wide
mouth jars.

9.2	Maintain samples at 0-4°C from the time of collection until extraction. If residual
chlorine is present in aqueous samples, add 80 mg sodium thiosulfate per liter of water.
EPA Methods 330.4 and 330.5 may be used to measure residual chlorine (Reference 9).

9.3	Begin sample extraction within seven days of collection, and analyze all extracts within
40 days of extraction.

10.0	Sample Extraction, Concentration, and Cleanup

Samples containing 1% solids or less are extracted directly using continuous liquid/liquid
extraction techniques (Section 10.2.1 and Figure 4). Samples containing 1-30% solids are
diluted to the 1% level with reagent water (Section 10.2.2) and extracted using continuous
liquid/liquid extraction techniques. Samples containing greater than 30% solids are
extracted using ultrasonic techniques (Section 10.2.5)

10.1	Determination of Percent Solids

10.1.1	Weigh 5-10 g of sample into a tared beaker.

10.1.2	Dry overnight (12 hours minimum) at 110 ±5°C, and cool in a desiccator.

September 1989

39


-------
Method 1625C

10.1.3 Determine percent solids as follows:

% solids = weight of dry sample x 1Q0

weight of wet sample

10.2 Preparation of Samples for Extraction

10.2.1 Samples containing 1% solids or less—Extract sample directly using continuous

liquid/liquid extraction techniques.

10.2.1.1	Measure 1.00 ±0.01 L of sample into a clean 1.5-2.0 L beaker.

10.2.1.2	Dilute aliquot—For samples which are expected to be difficult to
extract, concentrate, or clean-up, measure an additional 100.0 ±1.0
mL into a clean 1.5-2.0 L beaker and dilute to a final volume of
1.00 ±0.1 L with reagent water.

10.2.1.3	Spike 0.5 mL of the labeled compound spiking solution
(Section 6.8) into the sample aliquots. Proceed to preparation of
the QC aliquots for low solids samples (Section 10.2.3).

40

September 1989


-------
Method 1625C

STANDARD

BLANK

SAMPLE

[10.2.3.1]

[10.2.1.3,10.2.3.2]

[10.2.3.3]

[10.2.4]

[10.3.2]

[10.3.4]

[10.5]

SPIKE
1.0 mL
OF STANDARDS

STIR AND
EQUILIBRATE

STANDARD OR BLANK

EXTRACT BASE
NEUTRAL

ORGANIC

AQUEOUS

CONCENTRATE
TO 2-4 mL

EXTRACT ACID

CONCENTRATE
TO 2-4 mL

1 L REAGENT
WATER

SPIKE 500 jjL
OF 200 jjg/mL
ISOTOPES

STIR AND
EQUILIBRATE

1 L ALIQUOT

SPIKE 500 pL
OF 200 ng/mL
ISOTOPES

ORGANIC

>

STIR
EQUILI

'

AND
BRATE





EXTRACT BASE/
NEUTRAL

AQUEOUS

1



J,

>

'



'

[10.6]

CONCENTRATE
TO 1.0 mL



CONCENTRATE
T01.0 mL



CONCENTRATE
TO 1.0 mL



*

r . _



f



f

[11.3]

ADD INTERNAL
STANDARD



ADD INTERNAL
STANDARD



ADD INTERNAL
STANDARD





/

N

'



t

[11.41

INJECT



INJECT



INJECT

FIGURE 4 Flow Chart for Extraction/Concentration of Low Solids Precision and Recovery Standard, Blank, and
Sample by Method 1625. Numbers in Brackets [ ] Refer to Section Numbers in the Method.

September 1989

41


-------
Method 1625C

10.2.2 Samples containing 1-30% solids

10.2.2.1	Mix sample thoroughly.

10.2.2.2	Using the percent solids found in Section 10.1.3, determine the
weight of sample required to produce 1 L of solution containing
1% solids as follows:

sample weight, (grams) =

% solids

10.2.2.3	Discard all sticks, rocks, leaves and other foreign material prior to
weighing. Place the weight determined in Section 10.2.2.2 in a
clean 1.5-2.0 L beaker.

10.2.2.4	Dilute aliquot—For samples which are expected to be difficult to
extract, concentrate, or clean up, weigh an amount of sample equal
to one-tenth the amount determined in Section 10.2.2.2 into a
second clean 1.5-2.0 L beaker. When diluted to 1.0 L, this dilute
aliquot will contain 0.1% solids.

10.2.2.5	Bring the sample aliquot(s) above to 100-200 mL volume with
reagent water.

10.2.2.6	Spike 0.5 mL of the labeled compound spiking solution
(Section 6.8) into each sample aliquot.

10.2.2.7	Using a clean metal spatula, break any solid portions of the sample
into small pieces.

10.2.2.8	Place the 3/4 inch horn on the ultrasonic probe approx Vz inch
below the surface of each sample aliquot and pulse at 50% for
three minutes at full power. If necessary, remove the probe from
the solution and break any large pieces using the metal spatula or
a stirring rod and repeat the sonication. Clean the probe with
methylene chloride:acetone (1:1) between samples to preclude
cross-contamination.

10.2.2.9	Bring the sample volume to 1.0 ±0.1 L with reagent water.

10.2.3 Preparation of QC aliquots for samples containing low solids (<30%).

10.2.3.1	For each sample or sample lot (to a maximum of 20) to be
extracted at the same time, place three 1.0 ±0.01 L aliquots of
reagent water in clean 1.5-2.0 L beakers.

10.2.3.2	Spike 0.5 mL of the labeled compound spiking solution
(Section 6.8) into one reagent water aliquot. This aliquot will serve
as the blank.

42

September 1989


-------
Method 1625C

10.2.3.3	Spike 1.0 mL of the precision and recovery standard (Section 6.14)

into the two remaining reagent water aliquots.

10.2.4	Stir and equilibrate all sample and QC solutions for one to two hours. Extract the
samples and QC aliquots per Section 10.3.

10.2.5	Samples containing 30% solids or greater

10.2.5.1	Mix the sample thoroughly.

10.2.5.2	Discard all sticks, rocks, leaves and other foreign material prior to
weighing. Weigh 30 ±0.3 g into a clean 400-500 mL beaker.

10.2.5.3	Dilute aliquot—For samples which are expected to be difficult to
extract, concentrate, or clean-up, weigh 3 ±0.03 g into a clean
400-500 mL beaker.

10.2.5.4	Spike 0.5 mL of the labeled compound spiking solution
(Section 6.8) into each sample aliquot.

10.2.5.5	QC aliquots—For each sample or sample lot (to a maximum of 20)
to be extracted at the same time, place three 30 ±0.3 g aliquots of
the high solids reference matrix in clean 400-500 mL beakers.

10.2.5.6	Spike 0.5 mL of the labeled compound spiking solution
(Section 6.8) into one high solids reference matrix aliquot. This
aliquot will serve as the blank.

10.2.5.7	Spike 1.0 mL of the precision and recovery standard (Section 6.14)
into the two remaining high solids reference matrix aliquots.
Extract, concentrate, and clean up the high solids samples and QC
aliquots per Sections 10.4 through 10.8.

10.3 Continuous Extraction of Low Solids (Aqueous) Samples—Place 100-150 mL methylene
chloride in each continuous extractor and 200-300 mL in each distilling flask.

10.3.1 Pour the sample(s), blank, and QC aliquots into the extractors. Rinse the glass
containers with 50-100 mL methylene chloride and add to the respective
extractors. Include all solids in the extraction process.

10.3.2 Base/neutral extraction—Adjust the pH of the waters in the extractors to 12-13
with 6 N NaOH while monitoring with a pH meter. Begin the extraction by
heating the flask until the methylene chloride is boiling. When properly adjusted,
one to two drops of methylene chloride per second will fall from the condensor
tip into the water. Test and adjust the pH of the waters during the first to second
hour and during the fifth to tenth hour of extraction. Extract for 24-48 hours.

10.3.3 Remove the distilling flask, estimate and record the volume of extract (to the
nearest 100 mL), and pour the contents through a drying column containing 7-10
cm anhydrous sodium sulfate. Rinse the distilling flask with 30-50 mL of
methylene chloride and pour through the drying column. Collect the solution in

September 1989

43


-------
Method 1625C

a 500 mL K-D evaporator flask equipped with a 10 mL concentrator tube. Seal,
label as the base/neutral fraction, and concentrate per Sections 10.5 through 10.6.

10.3.4 Acid extraction—Adjust the pH of the waters in the extractors to 2 or less using
6 N sulfuric acid. Charge clean distilling flasks with 300-400 mL of methylene
chloride. Test and adjust the pH of the waters during the first one to two hours
and during the fifth to tenth hour of extraction. Extract for 24-48 hours. Repeat
Section 10.3.3, except label as the acid fraction.

10.4	Ultrasonic Extraction of High Solids Samples

10.4.1	Add 60 g of anhydrous sodium sulfate the sample and QC aliquot(s)
(Section 10.2.5) and mix thoroughly.

10.4.2	Add 100 ±10 mL of acetone:methylene chloride (1:1) to the sample and mix
thoroughly.

10.4.3	Place the 3/4 in. horn on the ultrasonic probe approx Vz in. below the surface of
the solvent but above the solids layer and pulse at 50% for three minutes at full
power. If necessary, remove the probe from the solution and break any large
pieces using the metal spatula or a stirring rod and repeat the sonication.

10.4.4	Decant the extracts through Whatman 41 filter paper using glass funnels and
collect in 500-1000 mL graduated cylinders.

10.4.5	Repeat the extraction steps (Sections 10.4.2 through 10.4.4) twice more for each
sample and QC aliquot. On the final extraction, swirl the sample or QC aliquot,
pour into its respective glass funnel, and rinse with acetone:methylene chloride.
Record the total extract volume.

10.4.6	Pour each extract through a drying column containing 7-10 cm of anhydrous
sodium sulfate. Rinse the graduated cylinder with 30-50 mL of methylene
chloride and pour through the drying column. Collect each extract in a 500 mL
K-D evaporator flask equipped with a 10 mL concentrator tube. Seal and label
as the high solids semivolatile fraction. Concentrate and clean up the samples
and QC aliquots per Sections 10.5 through 10.8.

10.5	Macro Concentration—Concentrate the extracts in separate 500 mL K-D flasks equipped

with 10 mL concentrator tubes.

10.5.1 Add one to two clean boiling chips to the flask and attach a three-ball macro
Snyder column. Prewet the column by adding approx 1 mL of methylene
chloride through the top. Place the K-D apparatus in a hot water bath so that the
entire lower rounded surface of the flask is bathed with steam. Adjust the
vertical position of the apparatus and the water temperature as required to
complete the concentration in 15-20 minutes. At the proper rate of distillation, the
balls of the column will actively chatter but the chambers will not flood. When
the liquid has reached an apparent volume of 1 mL, remove the K-D apparatus
from the bath and allow the solvent to drain and cool for at least 10 minutes.
Remove the Snyder column and rinse the flask and its lower joint into the

44

September 1989


-------
Method 1625C

concentrator tube with 1-2 mL of methylene chloride. A 5 mL syringe is
recommended for this operation.

10.5.2 For performance standards (Sections 8.2 and 12.7) and for blanks (Section 8.5),
combine the acid and base/neutral extracts for each at this point. Do not combine
the acid and base/neutral extracts for aqueous samples.

10.6 Micro Concentration

10.6.1	Kuderna-Danish (K-D)—Add a clean boiling chip and attach a two-ball micro
Snyder column to the concentrator tube. Prewet the column by adding approx
0.5 mL methylene chloride through the top. Place the apparatus in the hot water
bath. Adjust the vertical position and the water temperature as required to
complete the concentration in 5-10 minutes. At the proper rate of distillation, the
balls of the column will actively chatter but the chambers will not flood. When
the liquid reaches an apparent volume of approx 0.5 mL, remove the apparatus
from the water bath and allow to drain and cool for at least 10 minutes. Remove
the micro Snyder column and rinse its lower joint into the concentrator tube with
approx 0.2 mL of methylene chloride. Adjust the final volume to 5.0 mL if the
extract is to be cleaned up by GPC, to 1.0 mL if it does not require clean-up, or
to 0.5 mL if it has been cleaned up.

10.6.2	Nitrogen blowdown—Place the concentrator tube in a warm water bath (35°C)
and evaporate the solvent volume using a gentle stream of clean, dry nitrogen
(filtered through a column of activated carbon).

CAUTION: New plastic tubing must not be used between the carbon trap and the sample, since it may
introduce interferences.

The internal wall of the tube must be rinsed down several times with methylene
chloride during the operation. During evaporation, the tube solvent level must
be kept below the water level of the bath. The extract must never be allowed to
become dry. Adjust the final volume to 5.0 mL if the extract is to be cleaned up
by GPC, to 1.0 mL if it does not require clean-up, or to 0.5 mL if it has been
cleaned up.

10.7	Transfer the concentrated extract to a clean screw-cap vial. Seal the vial with a Teflon-
lined lid, and mark the level on the vial. Label with the sample number and fraction,
and store in the dark at -20 to -10°C until ready for analysis.

10.8	GPC Setup and Calibration
10.8.1 Column packing

10.8.1.1	Place 75 ±5 g of SX-3 Bio-beads in a 400-500 mL beaker.

10.8.1.2	Cover the beads and allow to swell overnight (12 hours minimum).

10.8.1.3	Transfer the swelled beads to the column and pump solvent
through the column, from bottom to top, at 4.5-5.5 mL/min prior
to connecting the column to the detector.

September 1989

45


-------
Method 1625C

10.8.1.4	After purging the column with solvent for one to two hours, adjust

the column head pressure to 7-10 psig, and purge for four to five
hours to remove air from the column. Maintain a head pressure
of 7-10 psig. Connect the column to the detector.

10.8.2 Column calibration

10.8.2.1	Load 5 mL of the calibration solution (Section 6.4) into the sample
loop.

10.8.2.2	Inject the calibration solution and record the signal from the
detector. The elution pattern will be corn oil, bis(2-ethylhexyl)
phthalate, pentachlorophenol, perylene, and sulfur.

10.8.2.3	Set the "dump time" to allow >85% removal of the corn oil and
>85% collection of the phthalate.

10.8.2.4	Set the "collect time" to the peak minimum between perylene and
sulfur.

10.8.2.5	Verify the calibration with the calibration solution after every

20 extracts. Calibration is verified if the recovery of the
pentachlorophenol is greater than 85%. If calibration is not
verified, the system shall be recalibrated using the calibration
solution, and the previous 20 samples shall be re-extracted and
cleaned up using the calibrated GPC system.

10.9 Extract Cleanup

10.9.1	Filter the extract or load through the filter holder to remove particulates. Load
the 5.0 mL extract onto the column. The maximum capacity of the column is 0.5-
1.0 g. If necessary, split the extract into multiple aliquots to prevent column
overload.

10.9.2	Elute the extract using the calibration data determined in Section 10.8.2. Collect
the eluate in a clean 400-500 mL beaker.

10.9.3	Concentrate the cleaned up extract to 5.0 mL per Section 10.5.

10.9.4	Rinse the sample loading tube thoroughly with methylene chloride between
extracts to prepare for the next sample.

10.9.5	If a particularly dirty extract is encountered, a 5.0 mL methylene chloride blank
shall be run through the system to check for carry-over.

10.9.6	Concentrate the extract to 0.5 mL and transfer to a screw-cap vial per
Sections 10.6 and 10.7. Concentrating extracts cleaned up by GPC to 0.5 mL will
place the analytes in the same part of the GCMS calibration range as in samples
not subjected to GPC.

11.0 GCMS Analysis

46

September 1989


-------
Method 1625C

11.1	Establish the operating conditions given in Tables 5 or 6 for analysis of the base/neutral
or acid extracts, respectively. For analysis of combined extracts (Sections 10.5.2 and
10.9.6), use the operating conditions in Table 5.

11.2	Bring the concentrated extract (Section 10.7) or standard (Sections 6.13 through 6.14) to
room temperature and verify that any precipitate has redissolved. Verify the level on the
extract (Sections 6.6 and 10.7) and bring to the mark with solvent if required.

11.3	Add the internal standard solution (Section 6.10) to the extract (use 1.0 pL of solution per
0.1 mL of extract) immediately prior to injection to minimize the possibility of loss by
evaporation, adsorption, or reaction. Mix thoroughly.

11.4	Inject a volume of the standard solution or extract such that 100 ng of the internal
standard will be injected, using on-column or splitless injection. For 1 mL extracts, this
volume will be 1.0 |iL. Start the GC column initial isothermal hold upon injection. Start
MS data collection after the solvent peak elutes. Stop data collection after the
benzo(ghi)perylene or pentachlorophenol peak elutes for the base/neutral (or semi-
volatile) or acid fraction, respectively. Return the column to the initial temperature for
analysis of the next sample.

12.0	System and Laboratory Performance

12.1	At the beginning of each 8 hr shift during which analyses are performed, GCMS system
performance and calibration are verified for all pollutants and labeled compounds. For
these tests, analysis of the 100 |ig/mL calibration standard (Section 6.13) shall be used
to verify all performance criteria. Adjustment and/or recalibration (per Section 7) shall
be performed until all performance criteria are met. Only after all performance criteria
are met may samples, blanks, and precision and recovery standards be analyzed.

12.2	DFTPP Spectrum Validity—Inject 1 |iL of the DFTPP solution (Section 6.11) either
separately or within a few seconds of injection of the standard (Section 12.1) analyzed at
the beginning of each shift. The criteria in Table 7 shall be met.

12.3	Retention Times—The absolute retention time of 2,2'-difluorobiphenyl shall be within the
range of 1078-1248 seconds and the relative retention times of all pollutants and labeled
compounds shall fall within the limits given in Tables 5 and 6.

12.4	GC Resolution—The valley height between anthracene and phenanthrene at m/z 178 (or
the analogs at m/z 188) shall not exceed 10 percent of the taller of the two peaks.

12.5	Calibration Verification—Compute the concentration of each pollutant (Tables 1 and 2)
by isotope dilution (Section 7.4) for those compounds which have labeled analogs.
Compute the concentration of each pollutant which has no labeled analog by the internal
standard method (Section 7.5). Compute the concentration of the labeled compounds by
the internal standard method. These concentrations are computed based on the
calibration data determined in Section 7.

12.5.1 For each pollutant and labeled compound being tested, compare the concentration
with the calibration verification limit in Table 10. If all compounds meet the
acceptance criteria, calibration has been verified and analysis of blanks, samples,
and precision and recovery standards may proceed. If, however, any compound

September 1989

47


-------
Method 1625C

fails, the measurement system is not performing properly for that compound. In
this event, prepare a fresh calibration standard or correct the problem causing the
failure and repeat the test (Section 12.1), or recalibrate (Section 7).

12.6	Multiple Peaks—Each compound injected shall give a single, distinct GC peak.

12.7	On-going Precision and Accuracy

12.7.1	Analyze the extract of one of the pair of precision and recovery standards (Section
10) prior to analysis of samples from the same lot.

12.7.2	Compute the concentration of each pollutant (Tables 1 and 2) by isotope dilution
(Section 7.4) for those compounds which have labeled analogs. Compute the
concentration of each pollutant which has no labeled analog by the internal
standard method (Section 7.5). Compute the concentration of the labeled
compounds by the internal standard method.

12.7.3	For each pollutant and labeled compound, compare the concentration with the
limits for on-going accuracy in Table 10. If all compounds meet the acceptance
criteria, system performance is acceptable and analysis of blanks and samples may
proceed. If, however, any individual concentration falls outside of the range
given, system performance is unacceptable for that compound.

NOTE: The large number of compounds in Table 10 present a substantial probability that one or more
will fail when all compounds are analyzed.

To determine if the extraction/concentration system is out of control or if the
failure is caused by probability, proceed as follows:

12.7.3.1	Analyze the second aliquot of the pair of precision and recovery
standards (Section 10).

12.7.3.2	Compute the concentration of only those pollutants or labeled
compounds that failed the previous test (Section 12.7.3). If these
compounds now pass, the extraction/concentration processes are
in control and analysis of blanks and samples may proceed. If,
however, any of the same compounds fail again, the
extraction/concentration processes are not being performed
properly for these compounds. In this event, correct the problem,
re-extract the sample lot (Section 10) and repeat the on-going
precision and recovery test (Section 12.7).

12.7.4 Add results which pass the specifications in Section 12.7.3 to initial and previous
on-going data for each compound in each matrix. Update QC charts to form a
graphic representation of continued laboratory performance (Figure 5). Develop
a statement of laboratory accuracy for each pollutant and labeled compound in
each matrix type by calculating the average percent recovery (R) and the standard
deviation of percent recovery (sr). Express the accuracy as a recovery interval
from R-2sr to R+2§. For example, if R = 95% anjd s = 5%, the accuracy is 85-
105%.

48

September 1989


-------
Method 1625C

s

N

2

K
<

<
LL)
CC
<
*
<
UJ
(V

45,000

35,000 -<~

J	1	L	I	I	i

ANTHRACENED,,,

J	L

25,000 1	1	1	1	1	,	j	,	1	r

123456789 10
ANALYSIS NUMBER

• + 3s

3s

8|

P

UJ <
cr oc

»-
z
<

1 10

1 00



_L

_L

ANTHRACENE

g go 	1	1	,	,	1	1	,	,	p

6/1 6/1 6/1 6/1 6/2 6/2 6/3 6/3 6/4 6/5
DATE ANALYZED

¦ + 3s
- 3s

FIGURE 5 Quality Control Charts Showing Area
(top graph) and Relative Response of
Anthracene to Anthracene-d10 (lower graph)
Plotted as a Function of Time or Analysis
Number.

13.0	Qualitative Determination

Identification is accomplished by comparison of data from analysis of a sample or blank
with data stored in the mass spectral libraries. For compounds for which the relative
retention times and mass spectra are known, identification is confirmed per Sections 13.1
and 13.2. For unidentified GC peaks, the spectrum is compared to spectra in the
EPA/NIH mass spectral file per Section 13.3.

13.1	Labeled Compounds and Pollutants Having No Labeled Analog (Tables 1-4)

13.1.1	The signals for all characteristic m/z's stored in the spectral library (Section 7.2.4)
shall be present and shall maximize within the same two consecutive scans.

13.1.2	Either (1) the background corrected EICP areas, or (2) the corrected relative
intensities of the mass spectral peaks at the GC peak maximum shall agree within
a factor of two (one-half to two times) for all masses stored in the library.

13.1.3	For the compounds for which the system has been calibrated (Tables 1 and 2), the
retention time shall be within the windows specified in Tables 5 and 6, or within

September 1989

49


-------
Method 1625C

±15 scans or ±15 seconds (whichever is greater) for compounds for which no
window is specified.

13.1.4 The system has not been calibrated for the compounds listed in Tables 3 and 4,
however, the relative retention times and mass spectra of these compounds are
known. Therefore, for a compound in Table 3 or 4 to be identified, its retention
time relative to the internal standard 2,2'-difluorobiphenyl must fall within a
retention time window of ±30 seconds, or ±30 scans (whichever is greater) of the
nominal retention time of the compound specified in Table 5 or 6.

13.2	Pollutants Having a Labeled Analog (Tables 1 and 2)

13.2.1	The signals for all characteristic m/z's stored in the spectral library (Section 7.2.4)
shall be present and shall maximize within the same two consecutive scans.

13.2.2	Either (1) the background corrected EICP areas, or (2) the corrected relative
intensities of the mass spectral peaks at the GC peak maximum shall agree within
a factor of two for all masses stored in the spectral library.

13.2.3	The relative retention time between the pollutant and its labeled analog shall be
within the windows specified in Tables 5 and 6.

13.3	Unidentified GC Peaks

13.3.1	The signals for masses specific to a GC peak shall all maximize within ±1 scan.

13.3.2	Either (1) the background corrected EICP areas, or (2) the corrected relative
intensities of the mass spectral peaks at the GC peak maximum shall agree within
a factor of two with the masses stored in the EPA/NIH Mass Spectral File.

13.4	The m/z's present in the experimental mass spectrum that are not present in the
reference mass spectrum shall be accounted for by contaminant or background ions. If
the experimental mass spectrum is contaminated, or if identification is ambiguous, an
experienced spectrometrist (Section 1.4) is to determine the presence or absence of the
compound.

14.0	Quantitative Determination

14.1	Isotope Dilution—Because the pollutant and its labeled analog exhibit the same effects
upon extraction, concentration, and gas chromatography, correction for recovery of the
pollutant can be made by adding a known amount of a labeled compound to every
sample prior to extraction. Relative response (RR) values for sample mixtures are used
in conjunction with the calibration curves described in Section 7.4 to determine
concentrations directly, so long as labeled compound spiking levels are constant. For the
phenol example given in Figure 1 (Section 7.4.1), RR would be equal to 1.114. For this
RR value, the phenol calibration curve given in Figure 1 indicates a concentration of 27
\ig/mL in the sample extract (Cex).

14.2	Internal Standard—Compute the concentration in the extract using the response factor
determined from calibration data (Section 7.5) and the following equation:

50

September 1989


-------
Method 1625C

(A x C.)

Cex (MgtoL) = ' "

(A. x RF)

where,

Cex = The concentration of the compound in the extract, and the other terms
are as defined in Section 7.5.1.

14.3 The concentration of the pollutant in the solid phase of the sample is computed using the
concentration of the pollutant in the extract and the weight of the solids (Section 10), as
follows:

(C x V )

Concentration in solid (ug/kg) = ——	—

W

where,

Vex = The extract volume in mL, and Ws is the sample weight in kg.

14.4	Dilution of Samples—If the EICP area at the quantitation m/z for any compound exceeds
the calibration range of the system, the extract of the dilute aliquot (Section 10) is
analyzed by isotope dilution. For water samples, where the base/neutral and acid
extracts are not combined, re-analysis is only required for the extract (B/N or A) in
which the compound exceeds the calibration range. If further dilution is required and
the sample holding time has not been exceeded, a smaller sample aliquot is extracted per
Sections 14.4.1 through 14.4.3. If the sample holding time has been exceeded, the sample
extract is diluted by successive factors of 10, internal standard is added to give a
concentration of 100 \ig/mL in the diluted extract, and the diluted extract is analyzed by
the internal standard method.

14.4.1	For samples containing one percent solids or less for which the holding time has
not been exceeded, dilute 10 mL, 1.0 mL, 0.1 mL etc. of sample to one liter with
reagent water and extract per Section 10.2.1.

14.4.2	For samples containing 1-30% solids for which the holding time has not been
exceeded, extract an amount of sample equal to 1/100 the amount determined in
Section 10.2.2.2. Extract per Section 10.2.2.

14.4.3	For samples containing 30% solids or greater for which the holding time has not
been exceeded, extract 0.30 ±0.003 g of sample per Section 10.2.5.

14.5	Dilution of samples containing high concentrations of compounds to be identified per
Section 13.3—When the EICP area of the quantitation m/z of a compound to be
identified per Section 13.3 exceeds the linear range of the GCMS system, or when any
peak is saturated, dilute the sample per Sections 14.4.1 through 14.4.3.

September 1989

51


-------
Method 1625C

14.6 Results are reported to three significant figures for all pollutants, labeled compounds, and
tentatively identified compounds found in all standards, blanks, and samples. For
aqueous samples, the units are Hg/L, and for samples containing one percent solids or
greater (soils, sediments, filter cake, compost), the units are |ig/kg, based on the dry
weight of the solids.

14.6.1 Results for samples which have been diluted are reported at the least dilute level
at which the area at the quantitation m/z is within the calibration range (Section
14.4), or at which no m/z in the spectrum is saturated (Section 14.5). For
compounds having a labeled analog, results are reported at the least dilute level
at which the area at the quantitation m/z is within the calibration range (Section
14.4) and the labeled compound recovery is within the normal range for the
method (Section 15.4).

15.0	Analysis of Complex Samples

15.1	Some samples may contain high levels (>1000 Hg/L) of the compounds of interest,
interfering compounds, and/or polymeric materials. Some samples will not concentrate
to 1 mL (Section 10.6); others will overload the GC column and/or mass spectrometer.

15.2	Analyze the dilute aliquot (Section 10) when the sample will not concentrate to 1.0 mL.
If a dilute aliquot was not extracted, and the sample holding time (Section 9.3) has not
been exceeded, dilute an aliquot of an aqueous sample with reagent water, or weigh a
dilute aliquot of a high solids sample and re-extract (Section 10); otherwise, dilute the
extract (Section 14.4) and analyze by the internal standard method (Section 14.2).

15.3	Recovery of Internal Standard—The EICP area of the internal standard should be within
a factor of two of the area in the shift standard (Section 12.1). If the absolute areas of the
labeled compounds are within a factor of two of the respective areas in the shift
standard, and the internal standard area is less than one-half of its respective area, then
loss of the internal standard in the extract has occurred. In this case, use one of the
labeled compounds (preferably a polynuclear aromatic hydrocarbon) to compute the
concentration of a pollutant with no labeled analog.

15.4	Recovery of Labeled Compounds—In most samples, labeled compound recoveries will
be similar to those from reagent water or from the high solids reference matrix (Section
12.7). If the labeled compound recovery is outside the limits given in Table 10, the
extract from the dilute aliquot (Section 10) is analyzed as in Section 14.4. If the recoveries
of all labeled compounds and the internal standard are low (per the criteria above), then
a loss in instrument sensitivity is the most likely cause. In this case, the 100 |ig/mL
calibration standard (Section 12.1) shall be analyzed and calibration verified (Section 12.5).
If a loss in sensitivity has occurred, the instrument shall be repaired, the performance
specifications in Section 12 shall be met, and the extract reanalyzed. If a loss in
instrument sensitivity has not occurred, the method does not apply to the sample being
analyzed, and the result may not be reported for regulatory compliance purposes.

16.0	Method Performance

16.1	Interlaboratory performance for this method is detailed in Reference 10. Reference mass
spectra, retention times, and response factors are from References 11 and 12. Results of
initial tests of this method on municipal sludge can be found in Reference 13.

52

September 1989


-------
Method 1625C

16.2 A chromatogram of the 100 |ig/mL acid/base/neutral calibration standard (Section 6.13)
is shown in Figure 6.

References

1.	"Performance Tests for the Evaluation of Computerized Gas Chromatography/Mass
Spectrometry Equipment and Laboratories" USEPA, EMSL Cincinnati, Ohio 45268,
EPA 600/4-80-025 (April 1980).

2.	National Standard Reference Data System, "Mass Spectral Tape Format", US National
Bureau of Standards (1979 and later attachments).

3.	"Working with Carcinogens," DHEW, PHS, CDC, NIOSH, Publication 77-206,
(August 1977).

4.	"OSHA Safety and Health Standards, General Industry" OSHA 2206, 29 CFR 1910
(January 1976).

5.	"Safety in Academic Chemistry Laboratories," ACS Committee on Chemical Safety (1979).

6.	"Inter-laboratory Validation of U. S. Environmental Protection Agency Method 1625A,
Addendum Report", SRI International, Prepared for Analysis and Evaluation Division
(WH-557), USEPA, 401 M St SW, Washington, DC 20460 (January 1985).

7.	"Handbook of Analytical Quality Control in Water and Wastewater Laboratories,"
USEPA, EMSL, Cincinnati, OH 45268, EPA 600/4-79-019 (March 1979).

8.	"Standard Practice for Sampling Water," ASTM Annual Book of Standards, ASTM,
Philadelphia, PA, 76 (1980).

9.	"Methods 330.4 and 330.5 for Total Residual Chlorine," USEPA, EMSL, Cincinnati,
OH 45268, EPA 600/4-70-020 (March 1979).

10.	"Inter-laboratory Validation of US Environmental Protection Agency Method 1625,"
USEPA, Effluent Guidelines Division, Washington, DC 20460 (June 15, 1984).

11.	"Narrative for Episode 1036: Paragraph 4© Mass Spectra, Retention Times, and Response
Factors", U S Testing Co, Inc, Prepared for W. A. Telliard, Industrial Technology Division
(WH-552), USEPA, 401 M St SW, Washington, DC 20460 (October 1985).

12.	"Narrative for SAS 109: Analysis of Extractable Organic Pollutant Standards by Isotope
Dilution GC/MS", S-CUBED Division of Maxwell Laboratories, Inc., Prepared for
W.A. Telliard, Industrial Technology Division (WH-552), USEPA, 401 M St SW,
Washington, DC 20460 (July 1986).

13.	Colby, Bruce N., and Ryan, Philip W. "Initial Evaluation of Methods 1634 and 1635 for
the analysis of Municipal Wastewater Treatment Sludges by Isotope Dilution GCMS",
Pacific Analytical Inc., Prepared for W.A. Telliard, Industrial Technology Division (WH-
552), USEPA, 401 M St SW, Washington DC 20460 (July 1986).

September 1989

53


-------
Method 1625C

SCANS

100.0

RIC	DATA: ABNID116S »1

93/13/84 5:24:80	CALIs ABN1DI166 #1

SAMPLE: AB,G,UER,00100,00,C,NA:Hh.NAS
CONDS.: 1S25A,30^0.251111,5630,30-28088,156280,30CIVSI
RANGE: G 1,3200 LABEL: N 2, 3.0 GUAN: A 2, 2.0 J 0 BASE: U 20,

1 TO 3200

RIC

V-





u

715776.

11

Ul



500
7:55

1000
15:50

1500

23:45

2000
31:48

2500
39:35

3006
47:30

SCAN
TIME

FIGURE 6 Chromatogram of Combined Acid/Base/Neutral Standard.

54

September 1989


-------
Method 1625C

Appendix A

Mass Spectra in the Form of Mass/Intensity Lists

555 acetophenone

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

42

21

43

245

49

19

50

221

51

524

52

75

61

13

62

26

63

422

65

31

73

13

74

64

75

36

76

62

77

941

78

11

89

12

91

22

105

1000

106

87

120

479

121

38









556 4-aminobiphenyl



















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

51

55

63

65

72

82

83

73

85

163

115

142

139

65

141

132

167

163

168

280

169

1000

170

216

557 aniline























int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z























40

65

41

66

42

16

46

11

47

75

50

40

51

47

52

54

53

12

54

40

61

17

62

28

63

59

64

33

65

226

66

461

74

11

78

14

91

10

92

136

93

1000

94

73









558 o-

anisidine





















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

40

22

41

43

42

10

50

60

51

106

52

202

53

286

54

39

61

12

62

25

63

43

64

24

65

142

66

20

76

13

77

36

68

32

79

25

80

915

81

41

92

47

93

14

94

18

105

18

108

1000

109

55

122

123

844

124

56







559 aramite





















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

41

606

57

758

59

328

63

782

65

285

74

113

77

155

91

339

105

153

107

239

121

107

123

120

163

143

175

182

185

1000

187

328

191

346

197

191

319

270

334

137

















560 benzanthrone



















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

74

69

75

71

87

97

88

160

99

69

100

215

101

278

150

58

174

67

199

63

200

350

201

236

202

762

203

126

230

1000

231

177









September 1989

55


-------
Method 1625C

Appendix A

Mass Spectra in the Form of Mass/Intensity Lists

561 1,3-benzenediol

m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

40 64

41

19

52

42

43

36

49

11

50

43

51 54

52

29

53

184

54

89

55

97

61

15

62 27

63

74

64

61

65

13

68

56

69

119

71 16

81

201

82

251

95

13

109

11

110

1000

111 51





















562 benzenethiol



















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

45 128

50

149

51

205

65

175

66

505

69

114

77 161

84

259

109

316

110

1000

111

102





563 2,3-benzofluorene



















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

74 52

81

69

94

143

95

253

106

60

107

205

108 491

187

75

189

90

213

233

214

60

215

987

216 1000

217

166

















943 benzoic acid



















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

45 29

50

221

51

413

52

45

66

11

74

53

75 25

76

81

77

778

78

76

105

1000

122

868

564 benzyl alcohol



















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

40 17

59

16

50

155

51

319

52

78

53

84

61 11

62

31

63

70

64

12

65

75

74

35

75 13

76

18

77

565

78

116

79

1000

80

73

89 65

90

64

91

125

105

38

106

18

107

523

108 737

109

43

















565 2-bromochlorobenzene

















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

49 237

50

890

51

183

73

158

74

506

75

1000

76 202

111

961

113

287

190

638

192

809

194

193

56

September 1989


-------
Method 1625C

Appendix A

Mass Spectra in the Form of Mass/Intensity Lists

566 3-bromochlorobenzene

















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

49

201

50

834

51

174

73

169

74

509

75

914

76

197

111

1000

113

301

190

625

192

802

194

191

567 4-chloro-2-nitroaniline

















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

49

119

50

174

51

260

52

531

61

205

62

394

63

1000

64

315

65

192

73

290

74

105

75

156

76

127

78

152

90

724

91

253

101

232

114

312

126

766

128

234

142

211

172

915

174

289





568 5-chloro-o

-toluidine



















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

50

115

51

261

52

257

53

137

77

420

78

134

79

140

89

152

106

1000

140

599

141

964

142

265

143

313





















569 4-chloroaniline



















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

41

60

62

55

63

147

64

135

65

329

73

51

91

63

92

186

99

67

100

115

127

1000

128

81

129

292





















570 3-chloronitrobenzene

















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

50

619

51

189

73

144

74

330

75

1000

76

169

85

101

99

258

111

851

113

266

157

424

159

137

571 o-

cresol





















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

50

102

51

181

53

144

77

358

79

380

80

159

89

114

90

231

107

783

108

1000









944 p-

-cresol





















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

50

136

51

224

52

106

53

196

77

420

79

308

80

145

90

122

107

822

108

1000









572 crotoxyphos



















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

40

633

44

448

67

42

77

70

79

41

104

100

105

484

109

21

127

1000

166

180

193

401

194

20

September 1989	57


-------
Method 1625C

Appendix A

Mass Spectra in the Form of Mass/Intensity Lists

573 2,6-di-t-butyl-p-benzoquinone















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

51

392

53

586

55

325

57

668

65

416

67

927

77

376

79

308

91

456

95

322

107

248

121

255

135

538

136

240

149

429

163

292

177

1000

205

203

220

410





















574 2,4-diaminotoluene



















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

40

70

42

55

51

76

52

70

53

51

61

91

67

50

77

147

78

69

93

63

94

224

104

128

105

134

106

67

121

958

122

1000

123

79





575 l,2-dibromo-3-chloropropane















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

42

38

59

341

51

104

61

38

75

1000

76

75

77

331

81

43

93

117

95

106

97

12

105

67

106

17

119

74

121

66

155

635

157

784

158

20

159

204

187

10

















945 3,5-dibromo-4-hydroxybenzonitrile















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

53

148

61

193

62

222

88

632

117

137

168

152

170

141

275

489

277

1000

279

451









576 2,6-dichloro-4-nitroaniline

















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

41

206

52

1000

61

523

62

828

63

588

73

470

65

137

89

218

90

443

97

458

124

954

126

401

133

218

160

401

176

431

178

134

206

378





58

September 1989


-------
Method 1625C

Appendix A

Mass Spectra in the Form of Mass/Intensity Lists

577 l,3-dichloro-2-propanol

















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

40 14

42

55

43

503

44

22

47

12

58

15

49 113

50

15

51

37

57

10

61

12

75

14

78 11

79

1000

80

25

81

310









578 2,3-dichloroaniline



















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

52 138

61

151

62

265

63

455

64

142

65

105

73 130

90

460

99

202

125

108

126

149

161

1000

163 626

165

101

















579 2,3-dichloronitrobenzene

















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

49 220

50

257

61

150

62

120

63

173

73

336

74 976

75

743

84

351

85

166

86

125

109

1000

110 204

111

303

133

701

135

435

145

580

147

368

161 190

163

121

191

411

193

263









946 2,6-dichlorophenol



















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

49 111

62

160

63

714

73

132

98

293

99

117

126 260

162

1000

164

613

166

101









580 l,2:3,4-diepoxybutane

















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

40 37

41

29

42

83

43

60

55

1000

56

67

57 155

58

16

85

13













581 3,3'-dimethoxybenzidine

















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

65 44

79

222

85

69

93

84

107

46

115

110

122 115

158

154

186

144

201

552

229

162

244

1000

245 152





















September 1989

59


-------
Method 1625C

Appendix A

Mass Spectra in the Form of Mass/Intensity Lists

582 dimethyl sulfone



















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

44 10

45

94

46

29

47

18

48

69

62

14

63 69

64

22

65

19

79

1000

81

36

94

528

96 23





















583 p-dimethylaminoazobenzene















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

42 483

51

181

77

447

78

120

79

147

91

109

104 142

105

190

120

1000

148

160

225

676





584 7,12-dimethylbenzo(a)anthracene















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

101 24

112

34

113

112

114

38

119

212

120

296

125 46

126

81

127

60

128

76

215

24

226

47

237 23

239

313

240

230

241

433

242

61

250

32

252 68

253

33

255

84

256

1000

257

180





585 N,N-dimethylformamide

















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

40 58

41

79

42

497

43

115

44

1000

45

19

57 17

58

83

72

89

73

994

74

35





586 3,6-dimethylphenanthrene

















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

76 113

89

129

94

179

101

142

102

151

189

388

190 193

191

430

205

246

206

1000

207

159





587 1,4-dinitrobenzene



















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

50 1000

51

131

63

228

64

218

74

311

75

623

76 664

92

240

122

166

168

399









588 diphenyldisulfide



















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

50 153

51

293

65

671

59

282

77

141

109

1000

110 132

154

191

185

117

218

418









60	September 1989


-------
Method 1625C

Appendix A

Mass Spectra in the Form of Mass/Intensity Lists

589 ethyl methanesulfonate

















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

42

16

43

72

45

208

48

40

59

19

63

23

64

22

65

93

79

1000

80

127

81

42

96

16

97

206

109

579

111

18

123

15

124

33





590 ethylenethiourea



















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

41

46

42

126

45

97

46

42

59

14

72

89

73

151

102

1000

















591 ethynylestradiol 3-methyl ether















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

41

155

53

101

91

157

115

143

147

226

159

132

160

115

173

199

174

313

227

1000

228

149

242

153

310

516





















592 hexachloropropene



















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

47

131

71

333

106

334

108

200

117

329

119

320

141

206

143

196

211

631

213

1000

215

623

217

186

947 hexanoic acid



















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

41

627

42

535

43

214

45

186

46

19

55

128

56

90

57

102

60

1000

61

66

69

21

70

20

73

412

74

56

87

98













593 2-isopropylnaphthalene

















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

51

100

63

Ill

76

157

77

129

115

147

127

131

128

216

152

133

153

184

154

114

155

1000

156

139

170

368





















594 isosafrole





















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

50

110

51

222

63

127

77

277

78

208

103

355

104

441

131

371

132

107

135

129

161

250

162

1000

595 longifolene





















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

53

438

55

719

65

346

67

453

77

566

69

713

91

1000

93

611

94

546

95

404

105

614

107

475

119

394

133

338

161

568

204

172









September 1989	61


-------
Method 1625C

Appendix A

Mass Spectra in the Form of Mass/Intensity Lists

596 malachite

green



















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

118 113

126

313

165

369

208

135

209

233

210

181

237 158

253

1000

254

160

329

189

330

775

331

170

597 methapyriline



















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

42 72

45

47

53

40

58

1000

71

188

72

225

78 54

79

48

97

516

190

40

191

67





598 methyl methanesulfonate

















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

45 178

56

15

48

108

50

26

63

35

64

48

65 285

78

27

79

821

80

1000

81

44

82

33

95 137

109

59

110

60













599 2-methylbenzothiozole

















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

45 152

50

133

58

153

62

106

63

309

69

513

82 204

108

392

109

102

148

279

149

1000

150

110

900 3-methylcholanthrene

















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

113 58

119

55

125

83

126

305

132

99

133

122

134 160

250

56

252

322

253

271

263

59

265

106

266 50

267

192

268

1000

269

185









901 4,4'-methylenebis(2-chloroaniline)















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

77 190

84

107

98

299

104

133

115

226

140

316

195 352

229

228

231

1000

233

227

265

171

266

631

267 144

268

358

















902 4,5-methylenephenanthrene















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

50 50

62

55

63

95

74

69

81

145

86

53

87 60

94

255

95

659

163

80

187

213

188

137

189 900 190 1000

62

September 1989


-------
Method 1625C

Appendix A

Mass Spectra in the Form of Mass/Intensity Lists

903 1-methylfluorene



















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

50

66

51

87

62

57

63

137

74

64

75

85

76

196

83

135

87

53

88

78

89

203

90

58

139

54

151

73

152

124

163

57

164

58

165

1000

166

136

176

96

177

52

178

202

179

182

180

686

181

99





















904 2-methylnaphthalene

















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

50

29

51

39

57

28

58

47

62

26

63

65

65

19

69

56

70

25

71

126

74

25

75

23

76

14

77

15

86

13

87

18

89

42

113

19

114

13

115

303

116

25

126

13

139

98

140

24

141

748

142

1000

143

105













905 1-methylphenanthrene

















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

51

54

63

86

70

62

74

51

81

52

83

164

96

132

163

55

165

217

189

165

191

532

192

1000

193

152





















906 2-(methylthio)benzothiazole















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

45

790

50

212

63

383

69

578

82

233

108

627

136

239

148

938

180

250

181

1000









907 1,5-naphthalenediamine

















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

51 48 65

83

77

75

79

111

103

86

118

52

130 262 131

40

141

43

157

89

158

1000

159

117

908 1,4-naphthoquinone



















m/z int. m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

50 445 51

62

52

52

66

69

74

189

75

205

76 590 101

51

102

613

103

52

104

550

130

433

158 1000 159

100

















909 alpha-naphthylamine

















m/z int. m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

50 25 51

31

57

36

59

46

62

28

63

59

65 27 71

58

72

104

89

62

113

22

114

34

115 401 116

212

142

53

143

1000

144

101





September 1989

63


-------
Method 1625C

Appendix A

Mass Spectra in the Form of Mass/Intensity Lists

910 5-nitro-o-toluidine



















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

51 194

52

159

53

121

77

766

78

176

79

619

94 168

104

120

106

691

152

1000









911 2-nitroaniline



















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

41 64

50

51

51

89

52

207

53

74

62

58

63 181

64

155

65

960

66

96

80

212

91

86

92 566

108

170

138

1000

139

63









912 3-nitroaniline



















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

41 101

52

120

53

59

62

58

63

143

64

121

65 1000

66

114

80

169

91

62

92

764

93

62

108 87

138

717

139

51













913 4-nitroaniline



















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

52 228

53

160

62

110

63

216

64

164

65

1000

66 124

80

266

92

300

108

636

138

520





914 4-nitrobiphenyl



















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

51 131

63

104

76

179

115

134

141

277

151

259

152 902

153

284

169

374

199

1000

200

125





915 N-nitroso-di-n-butylamine

















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

41 1000

42

536

43

570

44

313

55

129

56

167

57 994

84

985

86

103

99

197

115

158

116

237

158 161





















916 N-nitrosodiethylamine

















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

41 170

42

079

43

69

44

1000

45

20

54

18

56 525

57

492

70

24

71

28

85

25

87

31

102 807

103

35

















917 N-nitrosomethylethylamine















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

40 117

42

1000

43

667

44

26

54

17

56

189

57 99

59

13

71

60

73

57

88

772

89

20

64

September 1989


-------
Method 1625C

Appendix A

Mass Spectra in the Form of Mass/Intensity Lists

918 N-nitrosomethylphenylamine















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

50 181

51

434

52

104

63

110

77

1000

78

194

79 331

104

147

106

673

107

220

212

137





919 N-nitrosomorpholine

















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

41 181

42

192

43

52

44

17

54

85

55

95

56 1000

57

49

85

13

86

333

87

14

116

337

920 N-nitrosopiperidine



















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

41 320

42

1000

43

43

51

14

52

12

53

32

54 58

55

444

56

224

57

17

67

21

82

26

83 28

84

47

114

491

115

26









921 pentachlorobenzene



















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

73 160

108

239

125

102

178

102

213

179

215

218

217 106

248

648

250

1000

252

642

254

199





922 pentachloroethane



















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

47 203

60

398

62

119

83

378

85

218

94

114

95 165

117

1000

119

979

121

306

130

293

132

272

165 716

167

901

169

422













923 pentamethylbenzene

















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

51 126

53

84

63

61

65

99

77

145

79

64

91 218

105

128

115

120

117

91

133

1000

134

105

147 60

148

420

















924 perylene





















m/z int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

74 33

111

43

112

70

113

Ill

124

132

125

251

126 243

224

49

248

75

249

52

250

284

251

86

252 1000

253

219

















925 phenacetin

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

43

443

51

33

52

112

53

164

63

39

64

30

65

47

79

31

80

179

31

154

108

1000

109

196

110

50

137

461

138

40

179

672

180

64





September 1989

65


-------
Method 1625C

Appendix A

Mass Spectra in the Form of Mass/Intensity Lists

926 phenothiazine^



















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

50

145

51

120

63

134

69

190

100

128

154

149

166

240

167

607

198

186

199

1000

200

143





927 1-phenylnaphthalene

















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

50

132

51

156

63

148

74

124

75

142

76

136

87

101

88

183

89

162

100

155

101

527

102

111

200

144

201

136

202

643

203

1000

204

999

205

159

928 2-phenylnaphthalene

















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

51

108

63

101

76

136

88

133

89

158

101

333

102

188

202

398

203

270

204

1000

205

157





929 pronamide





















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

41

270

66

109

74

112

75

137

84

194

109

186

145

334

147

198

173

1000

175

615

254

133

255

211

256

102

257

122

















930 pyridine





















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

40

45

48

11

49

62

50

324

51

414

52

879

53

112

54

12

55

16

75

21

76

19

77

22

78

151

79

1000

80

101

81

58









931 safrole





















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

50

132

51

369

63

108

77

391

78

228

103

348

104

477

105

130

131

437

132

166

161

298

162

1000

163

109





















932 squalene





















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

53

62

55

94

67

105

68

119

69

1000

70

57

79

43

81

465

82

52

93

70

95

104

107

43

109

47

121

46

137

41













933 1,2,4,5-tetrachlorobenzene

















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

47

125

49

176

61

127

72

183

73

332

74

448

84

197

108

284

109

231

143

194

145

117

179

237

181

224

214

791

216

1000

218

482

220

101





66	September 1989


-------
Method 1625C

Appendix A

Mass Spectra in the Form of Mass/Intensity Lists

948 2,3,4,6-tetrachlorophenol

















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

61

234

65

167

66

105

83

134

84

178

96

202

97

107

131

463

133

270

166

298

168

273

194

168

196

164

230

793

232

1000

234

471









934 thianaphthene



















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

45

80

50

91

51

65

62

82

63

162

67

78

69

139

74

55

89

191

90

136

108

82

134

1000

135

104

136

52

















935 thioacetamide



















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

40

225

42

485

43

44

46

18

57

36

58

93

59

165

60

437

75

1000

76

25

77

43





936 thioxanthone



















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

50

262

63

180

69

320

74

116

69

176

82

121

92

188

108

129

139

385

152

227

183

112

184

951

185

137

212

1000

213

145













937 o-

toluidine





















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

40

51

41

38

42

35

49

10

50

88

51

169

52

164

53

192

53

86

62

26

63

68

64

30

65

59

66

24

74

19

65

14

76

21

77

313

78

113

79

243

80

80

89

107

90

76

91

52

104

45

106

1000

107

90













938 1,2,3-trimethoxybenzene

















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

50

257

51

459

52

139

53

276

63

112

65

341

67

114

77

246

79

132

82

117

93

483

95

801

107

190

108

144

110

898

125

578

153

759

168

1000

939 2,4,5-trimethylaniline

















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

41

80

52

58

51

63

53

66

65

150

67

74

79

62

91

167

93

51

117

54

118

65

119

93

120

1000

121

87

134

670

135

978

136

99





September 1989

67


-------
Method 1625C

Appendix A

Mass Spectra in the Form of Mass/Intensity Lists

940 triphenylene

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

74

52

87

55

100

107

101

108

112

131

113

244

114

181

200

67

202

56

224

84

225

56

226

313

227

132

228

1000

229

184













941 tripropylene glycol

methyl

ether















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

45

492

46

15

47

19

55

17

57

68

58

43

59

1000

60

34

71

16

72

44

73

363

74

232

103

57

117

92

161

21













942 1,3,5-trithiane



















m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

m/z

int.

46

1000

47

150

48

98

59

93

60

76

64

136

73

102

91

92

92

111

110

58

138

259





68

September 1989


-------