CCLME.ORG - 40 CFR PART 136—GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS OF POLLUTANTS
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n-C26 (Appendix C)........... 77901 630-01-3 524 B ........
n-C28 (Appendix C)........... 78116 630-02-4 525 B ........
n-C30 (Appendix C)........... 78117 638-68-6 526 B ........
Carbazole (4c)............... 77571 86-74-8 528 B ........
2-chloronaphthalene.......... 34581 91-58-7 020 B 016 B
4-chlorophenyl phenyl ether.. 34641 7005-72-3 040 B 017 B
Chrysene..................... 34320 218-01-9 076 B 018 B
P-cymene (Appendix C)........ 77356 99-87-6 513 B ........
Dibenzo(a,h)anthracene....... 34556 53-70-3 082 B 019 B
Dibenzofuran (Appendix C and 81302 132-64-9 505 B ........
4c).........................
Dibenzothiophene (Synfuel)... 77639 132-65-0 504 B ........
Di-n-butyl phthalate......... 39110 84-74-2 068 B 026 B
1,2-dichlorobenzene.......... 34536 95-50-1 025 B 020 B
1,3-dichlorobenzene.......... 34566 541-73-1 026 B 021 B
1,4-dichlorobenzene.......... 34571 106-46-7 027 B 022 B
3,3[prime]-dichlorobenzidine. 34631 91-94-1 028 B 023 B
Diethyl phthalate............ 34336 84-66-2 070 B 024 B
2,4-dimethylphenol........... 34606 105-67-9 034 A 003 A
Dimethyl phthalate........... 34341 131-11-3 071 B 025 B
2,4-dinitrotoluene........... 34611 121-14-2 035 B 027 B
2,6-dinitrotoluene........... 34626 606-20-2 036 B 028 B
Di-n-octyl phthalate......... 34596 117-84-0 069 B 029 B
Diphenylamine (Appendix C)... 77579 122-39-4 507 B ........
Diphenyl ether (Appendix C).. 77587 101-84-8 508 B ........
1,2-diphenylhydrazine........ 34346 122-66-7 037 B 030 B
Fluoranthene................. 34376 206-44-0 039 B 031 B
Fluorene..................... 34381 86-73-7 080 B 032 B
Hexachlorobenzene............ 39700 118-74-1 009 B 033 B
Hexachlorobutadiene.......... 34391 87-68-3 052 B 034 B
Hexachloroethane............. 34396 67-72-1 012 B 036 B
Hexachlorocyclopentadiene.... 34386 77-47-4 053 B 035 B
Indeno(1,2,3-cd)pyrene....... 34403 193-39-5 083 B 037 B
Isophorone................... 34408 78-59-1 054 B 038 B
Naphthalene.................. 34696 91-20-3 055 B 039 B
B-naphthylamine (Appendix C). 82553 91-59-8 502 B ........
Nitrobenzene................. 34447 98-95-3 056 B 040 B
N-nitrosodimethylamine....... 34438 62-75-9 061 B 041 B
N-nitrosodi-n-propylamine.... 34428 621-64-7 063 B 042 B
N-nitrosodiphenylamine....... 34433 86-30-3 062 B 043 B
Phenanthrene................. 34461 85-01-8 081 B 044 B
Phenol....................... 34694 108-95-2 065 A 010 A
a-Picoline (Synfuel)......... 77088 109-06-89 503 B ........
Pyrene....................... 34469 129-00-0 084 B 045 B
styrene (Appendix C)......... 77128 100-42-5 510 B ........
a-terpineol (Appendix C)..... 77493 98-55-5 509 B ........
1,2,3-trichlorobenzene (4c).. 77613 87-61-6 529 B ........
1,2,4-trichlorobenzene....... 34551 120-82-1 008 B 046 B
------------------------------------------------------------------------




Table 2_Acid Extractable Compounds
------------------------------------------------------------------------
CAS
Compound STORET registry EPA-EGD NPDES
------------------------------------------------------------------------
4-chloro-3-methylphenol...... 34452 59-50-7 022 A 008 A
2-chlorophenol............... 34586 95-57-8 024 A 001 A
2,4-dichlorophenol........... 34601 120-83-2 031 A 002 A
2,4-dinitrophenol............ 34616 51-28-5 059 A 005 A
2-methyl-4,6-dinitrophenol... 34657 534-52-1 060 A 004 A
2-nitrophenol................ 34591 88-75-5 057 A 006 A
4-nitrophenol................ 34646 100-02-7 058 A 007 A
Pentachlorophenol............ 39032 87-86-5 064 A 009 A
2,3,6-trichlorophenol (4c)... 77688 93-37-55 530 A ........
2,4,5-trichlorophenol (4c)... ........ 95-95-4 531 A ........
2,4,6-trichlorophenol........ 34621 88-06-2 021 A 011 A
------------------------------------------------------------------------




Table 3_Gas Chromatography of Base/Neutral Extractable Compounds
------------------------------------------------------------------------
Retention time Detection
EGD ------------------------------------ limit \2\
No. Compound Mean (µg/
\1\ (sec) EGD Ref Relative L)
------------------------------------------------------------------------
164 2,2[prime]- 1163 164 1.000-1.000 10
difluorobipheny
l (int std)....
061 N- 385 164 ns 50
nitrosodimethyl
amine..........
603 alpha picoline- 417 164 0.326-0.393 50
d7.............
703 alpha picoline.. 426 603 1.006-1.028 50
610 styrene-d5...... 546 164 0.450-0.488 10
710 styrene......... 549 610 1.002-1.009 10
613 p-cymene-d14.... 742 164 0.624-0.652 10
713 p-cymene........ 755 613 1.008-1.023 10
265 phenol-d5....... 696 164 0.584-0.613 10
365 phenol.......... 700 265 0.995-1.010 10
218 bis(2- 696 164 0.584-0.607 10
chloroethyl)
ether-d8.......
318 bis(2- 704 218 1.007-1.016 10
chloroethyl)
ether..........
617 n-decane-d22.... 698 164 0.585-0.615 10
717 n-decane........ 720 617 1.022-1.038 10
226 1,3- 722 164 0.605-0.636 10
dichlorobenzene-
d4.............
326 1,3- 724 226 0.998-1.008 10
dichlorobenzene
227 1,4- 737 164 0.601-0.666 10
dichlorobenzene-
d4.............
327 1,4- 740 227 0.997-1.009 10
dichlorobenzene
225 1,2- 758 164 0.632-0.667 10
dichlorobenzene-
d4.............
325 1,2- 760 225 0.995-1.008 10
dichlorobenzene
242 bis(2- 788 164 0.664-0.691 10
chloroisopropyl
) ether-d12....
342 bis(2- 799 242 1.010-1.016 10
chloroisopropyl
) ether........
212 hexachloroethane- 819 164 0.690-0.717 10
13C............
312 hexachloroethane 823 212 0.999-1.001 10
063 N-nitrosodi-n- 830 164 ns 20
propylamine....
256 nitrobenzene-d5. 845 164 0.706-0.727 10
356 nitrobenzene.... 849 256 1.002-1.007 10
254 isophorone-d8... 881 164 0.747-0.767 10
354 isophorone...... 889 254 0.999-1.017 10
234 2,4-dimethyl 921 164 0.781-0.803 10
phenol-d3......
334 2,4- 924 234 0.999-1.003 10
dimethylphenol.
043 bis(2- 939 164 ns 10
chloroethoxy)
methane........
208 1,2,4- 955 164 0.813-0.830 10
trichlorobenzen
e-d3...........
308 1,2,4- 958 208 1.000-1.005 10
trichlorobenzen
e..............
255 naphthalene-d8.. 963 164 0.819-0.836 10
355 naphthalene..... 967 255 1.001-1.006 10
609 alpha-terpineol- 973 164 0.829-0.844 10
d3.............
709 alpha-terpineol. 975 609 0.998-1.008 10
606 n-dodecane-d26.. 953 164 0.730-0.908 10
706 n-dodecane...... 981 606 0.986-1.051 10
529 1,2,3- 1003 164 ns 10
trichlorobenzen
e..............
252 hexachlorobutadi 1005 164 0.856-0.871 10
ene-13C4.......
352 hexachlorobutadi 1006 252 0.999-1.002 10
ene............
253 hexachlorocyclop 1147 164 0.976-0.986 10
entadiene-13C4.
353 hexachlorocyclop 1142 253 0.999-1.001 10
entadiene......
220 2- 1185 164 1.014-1.024 10
chloronaphthale
ne-d7..........
320 2- 1200 220 0.997-1.007 10
chloronaphthale
ne.............
518 n-tetradecane... 1203 164 ns 10
612 Biphenyl-d10.... 1205 164 1.016-1.027 10
712 Biphenyl........ 1195 612 1.001-1.006 10
608 Diphenyl ether- 1211 164 1.036-1.047 10
d10............
708 Diphenyl ether.. 1216 608 0.997-1.009 10
277 Acenaphthylene- 1265 164 1.080-1.095 10
d8.............
377 Acenaphthylene.. 1247 277 1.000-1.004 10
271 Dimethyl 1269 164 1.083-1.102 10
phthalate-d4...
371 Dimethyl 1273 271 0.998-1.005 10
phthalate......
236 2,6- 1283 164 1.090-1.112 10
dinitrotoluene-
d3.............
336 2,6- 1300 236 1.001-1.005 10
dinitrotoluene.
201 Acenaphthene-d10 1298 164 1.107-1.125 10
301 Acenaphthene.... 1304 201 0.999-1.009 10
605 Dibenzofuran-d8. 1331 164 1.134-1.155 10
705 Dibenzofuran.... 1335 605 0.998-1.007 10
602 Beta- 1368 164 1.163-1.189 50
naphthylamine-
d7.............
702 Beta- 1371 602 0.996-1.007 50
naphthylamine..
280 Fluorene-d10.... 1395 164 1.185-1.214 10
380 Fluorene........ 1401 281 0.999-1.008 10
240 4-chlorophenyl 1406 164 1.194-1.223 10
phenyl ether-d5
340 4-chlorophenyl 1409 240 0.990-1.015 10
phenyl ether...
270 Diethyl 1409 164 1.197-1.229 10
phthalate-d4...
370 Diethyl 1414 270 0.996-1.006 10
phthalate......
619 n-hexadecane-d34 1447 164 1.010-1.478 10
719 n-hexadecane.... 1469 619 1.013-1.020 10
235 2,4- 1359 164 1.152-1.181 10
dinitrotoluene-
d3.............
335 2,4- 1344 235 1.000-1.002 10
dinitrotoluene.
237 1,2- 1433 164 1.216-1.248 20
diphenylhydrazi
ne-d8..........
337 1,2- 1439 237 0.999-1.009 20
diphenylhydrazi
ne (\3\).......
607 Diphenylamine- 1437 164 1.213-1.249 20
d10............
707 Diphenylamine... 1439 607 1.000-1.007 20
262 N- 1447 164 1.225-1.252 20
nitrosodiphenyl
amine-d6.......
362 N- 1464 262 1.000-1.002 20
nitrosodiphenyl
amine (\4\)....
041 4-bromophenyl 1498 164 1.271-1.307 10
phenyl ether...
209 Hexachlorobenzen 1521 164 1.288-1.327 10
e-13C6.........
309 Hexachlorobenzen 1522 209 0.999-1.001 10
e..............
281 Phenanthrene-d10 1578 164 1.334-1.380 10
520 n-octadecane.... 1580 164 ns 10
381 Phenanthrene.... 1583 281 1.000-1.005 10
278 Anthracene-d10.. 1588 164 1.342-1.388 10
378 Anthracene...... 1592 278 0.998-1.006 10
604 Dibenzothiophene- 1559 164 1.314-1.361 10
d8.............
704 Dibenzothiophene 1564 604 1.000-1.006 10
528 Carbazole....... 1650 164 ns 20
621 n-eicosane-d42.. 1655 164 1.184-1.662 10
721 n-eicosane...... 1677 621 1.010-1.021 10
268 Di-n-butyl 1719 164 1.446-1.510 10
phthalate-d4...
368 Di-n-butyl 1723 268 1.000-1.003 10
phthalate......
239 Fluoranthene-d10 1813 164 1.522-1.596 10
339 Fluoranthene.... 1817 239 1.000-1.004 10
284 Pyrene-d10...... 1844 164 1.523-1.644 10
384 Pyrene.......... 1852 284 1.001-1.003 10
205 Benzidine-d8.... 1854 164 1.549-1.632 50
305 Benzidine....... 1853 205 1.000-1.002 50
522 n-docosane...... 1889 164 ns 10
623 n-tetracosane- 1997 164 1.671-1.764 10
d50............
723 n-tetracosane... 2025 612 1.012-1.015 10
067 Butylbenzyl 2060 164 ns 10
phthalate......
276 Chrysene-d12.... 2081 164 1.743-1.837 10
376 Chrysene........ 2083 276 1.000-1.004 10
272 Benzo(a)anthrace 2082 164 1.735-1.846 10
ne-d12.........
372 Benzo(a)anthrace 2090 272 0.999-1.007 10
ne.............
228 3,3[prime]- 2088 164 1.744-1.848 50
dichlorobenzidi
ne-d6..........
328 3,3[prime]- 2086 228 1.000-1.001 50
dichlorobenzidi
ne.............
266 Bis(2- 2123 164 1.771-1.880 10
ethylhexyl)
phthalate-d4...
366 Bis(2- 2124 266 1.000-1.002 10
ethylhexyl)
phthalate......
524 n-hexacosane.... 2147 164 ns 10
269 di-n-octyl 2239 164 1.867-1.982 10
phthalate-d4...
369 di-n-octyl 2240 269 1.000-1.002 10
phthalate......
525 n-octacosane.... 2272 164 ns 10
274 Benzo(b)fluorant 2281 164 1.902-2.025 10
hene-d12.......
354 Benzo(b)fluorant 2293 274 1.000-1.005 10
hene...........
275 Benzo(k)fluorant 2287 164 1.906-2.033 10
hene-d12.......
375 Benzo(k)fluorant 2293 275 1.000-1.005 10
hene...........
273 Benzo(a)pyrene- 2351 164 1.954-2.088 10
d12............
373 Benzo(a)pyrene.. 2350 273 1.000-1.004 10
626 N-triacontane- 2384 164 1.972-2.127 10
d62............
726 N-triacontane... 2429 626 1.011-1.028 10
083 Indeno(1,2,3- 2650 164 ns 20
cd)pyrene......
082 Dibenzo(a,h)anth 2660 164 ns 20
racene.........
279 Benzo(ghi)peryle 2741 164 2.187-2.524 20
ne-d12.........
379 Benzo(ghi)peryle 2750 279 1.001-1.006 20
ne.............
------------------------------------------------------------------------
\1\ 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.
\2\ This is a minimum level at which the entire GC/MS system must give
recognizable mass spectra (background corrected) and acceptable
calibration points.
\3\ Detected as azobenzene.
\4\ Detected as diphenylamine.
ns = specification not available at time of release of method.
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: 5 min 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.




Table 4_Gas Chromatography of Acid Extractable Compounds
------------------------------------------------------------------------
Retention time Detection
EGD ------------------------------------ limit 2
No. 1 Compound Mean (µg/
(sec) EGD Ref Relative L)
------------------------------------------------------------------------
164 2,2[prime]- 1163 164 1.000-1.000 10
difluorobipheny
l (int std)....
224 2-chlorophenol- 701 164 0.587-0.618 10
d4.............
324 2-chlorophenol.. 705 224 0.997-1.010 10
257 2-nitrophenol-d4 898 164 0.761-0.783 20
357 2-nitrophenol... 900 257 0.994-1.009 20
231 2,4- 944 164 0.802-0.822 10
dichlorophenol-
d3.............
331 2,4- 947 231 0.997-1.006 10
dichlorophenol.
222 4-chloro-3- 1086 164 0.930-0.943 10
methylphenol-d2
322 4-chloro-3- 1091 222 0.998-1.003 10
methylphenol...
221 2,4,6- 1162 164 0.994-1.005 10
trichlorophenol-
d2.............
321 2,4,6- 1165 221 0.998-1.004 10
trichlorophenol
531 2,4,5- 1170 164 ns 10
trichlorophenol
530 2,3,6- 1195 164 ns 10
trichlorophenol
259 2,4- 1323 164 1.127-1.149 50
dinitrophenol-
d3.............
359 2,4- 1325 259 1.000-1.005 50
dinitrophenol..
258 4-nitrophenol-d4 1349 164 1.147-1.175 50
358 4-nitrophenol... 1354 258 0.997-1.006 50
260 2-methyl-4,6- 1433 164 1.216-1.249 20
dinitrophenol-
d2.............
360 2-methyl-4,6- 1435 260 1.000-1.002 20
dinitrophenol..
264 Pentachloropheno 1559 164 1.320-1.363 50
l-13C6.........
364 Pentachloropheno 1561 264 0.998-1.002 50
l..............
------------------------------------------------------------------------
1 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.
2 This is a minimum level at which the entire GC/MS system must give
recognizable mass spectra (background corrected) and acceptable
calibration points.
ns=specification not available at time of release of method.
Column: 30 ±2mx0.25 ±0.02mm i.d. 94% methyl, 4% phenyl, 1%
vinyl bonded phase fused silica capillary.
Temperature program: 5 min at 30 °C; 8 °C/min. to 250°C or
until pentachlorophenol elutes.
Gas velocity: 30 ±5 cm/sec.




Table 5_DFTPP Mass Intensity Specifications
------------------------------------------------------------------------
Mass Intensity required
------------------------------------------------------------------------
51 30-60 percent of mass 198.
68 Less than 2 percent of mass 69.
70 Less than 2 percent of mass 69.
127 40-60 percent of mass 198.
197 Less than 1 percent of mass 198.
199 5-9 percent of mass 198.
275 10-30 percent of mass 198.
365 greater than 1 percent of mass 198
441 present and less than mass 443
442 40-100 percent of mass 198.
443 17-23 percent of mass 442.
------------------------------------------------------------------------




Table 6_Base/Neutral Extractable Compound Characteristic Masses
------------------------------------------------------------------------
Labeled Primary m/
Compound analog z
------------------------------------------------------------------------
Acenaphthene..................................... d10 154/164
Acenaphthylene................................... d8 152/160
Anthracene....................................... d10 178/188
Benzidine........................................ d8 184/192
Benzo(a)anthracene............................... d12 228/240
Benzo(b)fluoranthene............................. d12 252/264
Benzo(k)fluoranthene............................. d12 252/264
Benzo(a)pyrene................................... d12 252/264
Benzo(ghi)perylene............................... d12 276/288
Biphenyl......................................... d10 154/164
Bis(2-chloroethyl) ether......................... d8 93/101
Bis(2-chloroethoxy)methane....................... ......... 93
Bis(2-chloroisopropyl) ether..................... d12 121/131
Bis(2-ethylhexyl) phthalate...................... d4 149/153
4-bromophenyl phenyl ether....................... ......... 248
Butyl benzyl phthalate........................... ......... 149
n-C10............................................ d22 55/66
n-C12............................................ d26 55/66
n-C14............................................ ......... 55
n-C16............................................ d34 55/66
n-C18............................................ ......... 55
n-C20............................................ d42 55/66
n-C22............................................ ......... 55
n-C24............................................ d50 55/66
n-C26............................................ ......... 55
n-C28............................................ ......... 55
n-C30............................................ d62 55/66
Carbazole........................................ d8 167/175
2-chloronaphthalene.............................. d7 162/169
4-chlorophenyl phenyl ether...................... d5 204/209
Chrysene......................................... d12 228/240
p-cymene......................................... d14 114/130
Dibenzo(a,h)anthracene........................... ......... 278
Dibenzofuran..................................... d8 168/176
Dibenzothiophene................................. d8 184/192
Di-n-butyl phthalate............................. d4 149/153
1,2-dichlorobenzene.............................. d4 146/152
1,3-dichlorobenzene.............................. d4 146/152
1,4-dichlorobenzene.............................. d4 146/152
3,3[prime]-dichlorobenzidine..................... d6 252/258
Diethyl phthalate................................ d4 149/153
2,4-dimethylphenol............................... d3 122/125
Dimethyl phthalate............................... d4 163/167
2,4-dinitrotoluene............................... d3 164/168
2,6-dinitrotoluene............................... d3 165/167
Di-n-octyl phthalate............................. d4 149/153
Diphenylamine.................................... d10 169/179
Diphenyl ether................................... d10 170/180
1,2-diphenylhydrazine \1\........................ d10 77/82
Fluoranthene..................................... d10 202/212
Fluorene......................................... d10 166/176
Hexachlorobenzene................................ 13C6 284/292
Hexachlorobutadiene.............................. 13C4 225/231
Hexachloroethane................................. 13C 201/204
Hexachlorocyclopentadiene........................ 13C4 237/241
Ideno(1,2,3-cd)pyrene............................ ......... 276
Isophorone....................................... d8 82/88
Naphthalene...................................... d8 128/136
B-naphthylamine.................................. d7 143/150
Nitrobenzene..................................... d5 123/128
N-nitrosodimethylamine........................... ......... 74
N-nitrosodi-n-propylamine........................ ......... 70
N-nitrosodiphenylamile \2\....................... d6 169/175
Phenanthrene..................................... d10 178/188
Phenol........................................... d5 94/71
a-picoline....................................... d7 93/100
Pyrene........................................... d10 202/212
Styrene.......................................... d5 104/109
a-terpineol...................................... d3 59/62
1,2,3-trichlorobenzene........................... d3 180/183
1,2,4-trichlorobenzene........................... d3 180/183
------------------------------------------------------------------------
\1\ Detected as azobenzene.
\2\ Detected as diphenylamine.




Table 77_Acid Extractable Compound Characteristic Masses
------------------------------------------------------------------------
Labeled Primary m/
Compound analog z
------------------------------------------------------------------------
4-chloro-3-methylphenol.......................... d2 107/109
2-chlorophenol................................... d4 128/132
2,4-dichlorophenol............................... d3 162/167
2,4-dinitrophenol................................ d3 184/187
2-methyl-4,6-dinitrophenol....................... d2 198/200
2-nitrophenol.................................... d4 139/143
4-nitrophenol.................................... d4 139/143
Pentachlorophenol................................ 13C6 266/272
2,3,6-trichlorophenol............................ d2 196/200
2,4,5-trichlorophenol............................ d2 196/200
2,4,6-trichlorophenol............................ d2 196/200
------------------------------------------------------------------------




Table 8_Acceptance Criteria for Performance Tests
----------------------------------------------------------------------------------------------------------------
Acceptance criteria
-----------------------------------------------------------------
Initial precision and Labeled Calibration On-going
EGD Compound accuracy section compound verification accuracy
No. 1 8.2.3 (µg/L) recovery sec. sec. 12.5 sec. 11.6 R
----------------------- 8.3 and 14.2 P (µg/ (µg/
s X (percent) mL) L)
----------------------------------------------------------------------------------------------------------------
301 Acenaphthene.......................... 21 79-134 .............. 80-125 72-144
201 Acenaphthene-d10...................... 38 38-147 20-270 71-141 30-180
377 Acenaphtylene......................... 38 69-186 .............. 60-166 61-207
277 Acenaphthylene-d8..................... 31 38-146 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 ns-ns ns-ns ns-ns ns-ns
372 Benzo(a)anthracene.................... 20 65-168 .............. 70-142 62-176
272 Benzo(a)anthracene-d12................ 41 25-298 12-605 28-357 22-329
374 Benzo(b)fluoranthene.................. 183 32-545 .............. 61-164 20-ns
274 Benzo(b)fluoranthene-d12.............. 168 11-577 ns-ns 14-ns ns-ns
375 Benzo(k)fluoranthene.................. 26 59-143 .............. 13-ns 53-155
275 Benzo(k)fluoranthene-d12.............. 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)perylene-d12................ 45 29-268 14-529 13-ns 25-303
712 Biphenyl (Appendix C)................. 41 75-148 .............. 58-171 62-176
612 Biphenyl-d12.......................... 43 28-165 ns-ns 52-192 17-267
318 Bis(2-chloroethyl) ether.............. 34 55-196 .............. 61-164 50-213
218 Bis(2-chloroethyl) ether-d8........... 33 29-196 15-372 52-194 25-222
043 Bis(2-chloroethoxy)methane*........... 27 43-153 .............. 44-228 39-166
342 Bis(2-chloroisopropyl) ether.......... 17 81-138 .............. 67-148 77-145
242 Bis(2-chloroisopropyl)ether-d12....... 27 35-149 20-260 44-229 30-169
366 Bis(2-ethylhexyl) phthalate........... 31 69-220 .............. 76-131 64-232
266 Bis(2-ethylhexyl) phthalate-d4........ 29 32-205 18-364 43-232 28-224
041 4-bromophenyl phenyl ether*........... 44 44-140 .............. 52-193 35-172
067 Butyl benzyl phthalate*............... 31 19-233 .............. 22-450 35-170
717 n-C10 (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)*................... 109 ns-985 .............. 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)*................... 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)*................... 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)*................... 35 35-193 .............. 26-392 31-212
525 n-C28 (Appendix C)*................... 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
528 Carbazole (4c)*....................... 38 36-165 .............. 44-227 31-188
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 ether........... 42 75-166 .............. 71-142 63-194
240 4-chlorophenyl phenyl ether-d5........ 52 40-161 19-325 57-175 29-212
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
082 Dibenzo(a,h)anthracene*............... 55 23-299 .............. 13-761 19-340
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 1,3-dichlorobenzene-d4................ 48 13-203 ns-550 52-192 ns-260
327 1,4-dichlorobenzene................... 42 61-194 .............. 62-161 53-219
227 1,4-dichlorobenzene-d4................ 48 15-193 ns-474 65-153 11-245
328 3,3[prime]-dichlorobenzidine.......... 26 68-174 .............. 77-130 64-185
228 3,3[prime]-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 C)............ 45 58-205 .............. 57-176 51-231
607 Diphenylamine-d10..................... 42 27-206 11-488 59-169 21-249
708 Diphenyl ether (Appendix C)........... 19 82-136 .............. 83-120 77-144
608 Diphenyl ether-d10.................... 37 36-155 19-281 77-129 29-186
337 1,2-diphenylhydrazine................. 73 49-308 .............. 75-134 40-360
237 1,2-diphenylhydrazine-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-13C1................. 77 ns-400 ns-ns 47-212 ns-563
353 hexachlorocyclopentadiene............. 15 69-144 .............. 77-129 67-148
253 hexachlorocyclopentadiene-13C4........ 60 ns-ns ns-ns 47-211 ns-ns
083 ideno(1,2,3-cd)pyrene*................ 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-d2......... 64 36-247 16-527 56-177 28-307
355 naphthalene........................... 20 80-139 .............. 73-137 75-149
255 naphthalene-d8........................ 39 28-157 14-305 71-141 22-192
702 B-naphthylamine (Appendix C).......... 49 10-ns .............. 39-256 ns-ns
602 B-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
061 N-nitrosodimethylamile*............... 198 21-472 .............. 40-249 12-807
063 N-nitrosodi-n-proplyamine*............ 198 21-472 .............. 40-249 12-807
362 N-nitrosodiphenylamine................ 45 65-142 .............. 68-148 53-173
262 N-nitrosodiphenylamine-d6............. 37 54-126 26-256 59-170 40-166
364 pentachlorophenol..................... 21 76-140 .............. 77-130 71-150
264 pentachlorophenol-13C6................ 49 37-212 18-412 42-237 29-254
381 phenanthrene.......................... 13 93-119 .............. 75-133 87-126
281 phenanthrene-d10...................... 40 45-130 24-241 67-149 34-168
365 phenol................................ 36 77-127 .............. 65-155 62-154
265 phenol-d5............................. 161 21-210 ns-ns 48-208 ns-ns
703 a-picoline (Synfuel).................. 38 59-149 .............. 60-165 50-174
603 a-picoline-d7......................... 138 11-380 ns-ns 31-324 ns-608
384 pyrene................................ 19 76-152 .............. 76-132 72-159
284 pyrene-d10............................ 29 32-176 18-303 48-210 28-196
710 styrene (Appendix C).................. 42 53-221 .............. 65-153 48-244
610 styrene-d5............................ 49 ns-281 ns-ns 44-228 ns-348
709 a-terpineol (Appendix C).............. 44 42-234 .............. 54-186 38-258
609 a-terpineol-d3........................ 48 22-292 ns-672 20-502 18-339
529 1,2,3-trichlorobenzene (4c)*.......... 69 15-229 .............. 60-167 11-297
308 1,2,4-trichlorobenzene................ 19 82-136 .............. 78-128 77-144
208 1,2,4-trichlorobenzene-d3............. 57 15-212 ns-592 61-163 10-282
530 2,3,6-trichlorophenol (4c)*........... 30 58-137 .............. 56-180 51-153
531 2,4,5-trichlorophenol (4c)*........... 30 58-137 .............. 56-180 51-153
321 2,4,6-trichlorophenol................. 57 59-205 .............. 81-123 48-244
221 2,4,6-trichlorophenol-d2.............. 47 43-183 21-363 69-144 34-226
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\1\ 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.
* Measured by internal standard; specification derived from related compound.
ns=no specification; limit is outside the range that can be measured reliably.




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Attachment 1 to Method 1625

Introduction

To support measurement of several semivolatile pollutants, EPA has developed this attachment to EPA Method 1625B. 1 The modifications listed in this attachment are approved only for monitoring wastestreams from the Centralized Waste Treatment Point Source Category (40 CFR Part 437) and the Landfills Point Source Category (40 CFR Part 445). EPA Method 1625B (the Method) employs sample extraction with methylene chloride followed by analysis of the extract using capillary column gas chromatography-mass spectrometry (GC/MS). This attachment addresses the addition of the semivolatile pollutants listed in Tables 1 and 2 to all applicable standard, stock, and spiking solutions utilized for the determination of semivolatile organic compounds by EPA Method 1625B.

1 EPA Method 1625 Revision B, Semivolatile Organic Compounds by Isotope Dilution GC/MS, 40 CFR Part 136, Appendix A.

1.0 EPA METHOD 1625 REVISION B MODIFICATION SUMMARY

The additional semivolatile organic compounds listed in Tables 1 and 2 are added to all applicable calibration, spiking, and other solutions utilized in the determination of semivolatile compounds by EPA Method 1625. The instrument is to be calibrated with these compounds, and all procedures and quality control tests described in the Method must be performed.

2.0 SECTION MODIFICATIONS

Note: All section and figure numbers in this Attachment reference section and figure numbers in EPA Method 1625 Revision B unless noted otherwise. Sections not listed here remain unchanged.

Section 6.7 The stock standard solutions described in this section are modified such that the analytes in Tables 1 and 2 of this attachment are required in addition to those specified in the Method.

Section 6.8 The labeled compound spiking solution in this section is modified to include the labeled compounds listed in Tables 5 and 6 of this attachment.

Section 6.9 The secondary standard is modified to include the additional analytes listed in Tables 1 and 2 of this attachment.

Section 6.12 The solutions for obtaining authentic mass spectra are to include all additional analytes listed in Tables 1 and 2 of this attachment.

Section 6.13 The calibration solutions are modified to include the analytes listed in Tables 1 and 2 and the labeled compounds listed in Tables 5 and 6 of this attachment.

Section 6.14 The precision and recovery standard is modified to include the analytes listed in Tables 1 and 2 and the labeled compounds listed in Tables 5 and 6 of this attachment.

Section 6.15 The solutions containing the additional analytes listed in Tables 1 and 2 of this attachment are to beanalyzed for stability. (continued)