600D80022
Tuesday
December 18, 1979
Part IV



Environmental

Protection  Agency

Guidelines Establishing Test Procedures
for the Analysis of Pollutants; Proposed
Regulations; Correction
                 EPA-600/D-80-022

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75028        Federal Register  /  Vol. 44. No. 244  /  Tuesday. December 18. 1979 / Proposed Rules


ENVIRONMENTAL PROTECTION
AGENCY

40 CFR Part 136

[FRL 1323-D]

Guidelines Establishing Test
Procedures for the Analysis of
Pollutants

Correction
  In FR Doc. 79-36871, appearing at
page 69464 in the issue for Monday,
December 3,1979, Table I—List of
Approved Test Procedures (pages
69568—69573) and Table II--Containers,
Preservation, and Holding  Times (pages
69574—69575), contained numerous
printing errors. Tables I and II should
have read as set forth below:

BILLINO CODE 1S05-01-M

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                Federal Register / Vol. 44, No. 244 / Tuesday, December 18, 1979  / Proposed Rules
                                                                                                                           75029


1MUB I. LIST OF AttWWED TC9T
mxjaiuws

Reference (Page Hoe.)



1.

2.


3.





Parameter and units
Acidity, as CaOOj,
milligrams par liter
Alkanl'jilty, as CaCOj
milligrams per liter

ftmonla (as H) ,
milligrams per liter


1974
H*
Method Methods
Electrometric end point (pH of 8.2) 1
or phenolphthalein end point
Electrometric titration (only to 3
pH 4.5) manual or automated, or 5
equivalent aubomated methods
Manual distillation3 (at pH 9.5)
followd by nesslerlzaticn, titration, 159
electrode, 165
automated phenolate 168
14th Ed. Part 31
Standard 1975
Methods ASM
273 (4d) 116

278 111
-

410
412 237
-
61S
Other
U9G3 , Approved
Methods Methods
40 (607) 2

41 (607) 2
-

-
116 (614) 2
-
"
Bacteria
4.

5.


6.

7.


8.


Ooliform (fecal)4
number per 100 ml
Coliform (fecal)4 in
presence of chlorine.
number per 100 ml
Coliform (total)4,
number per 100 ml
Ooliform (total)4 in
presence of chlorine,
number per 100 ml
Fecal streptococci4.
number per 100 ml

MWi5
membrane filter
MTO;5
membrane filter 5«7

MPt»,5
membrane filter
MPHi5
membrane filter Kith enrlchnant

MPNt5
membrane f liter I
plate count
922
937
922
928,937

916
928
916
933

943
944
947
<130«
(45»* 
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75030
Federal Register  / Vol. 44, No. 244  / Tuesday, December 18, 1979  / Proposed Rules
                                                TNSUS I.  LIST OT MVMWEU TEST MtXUXWS   (Conl.)
    Parameter and cnits
                                            Method
                                                                      1974
                                                                       cm
                                                                     Methods
                                                                          Reference (Page Nog.)
                                                                 14th M.     Part 3l
                                                                 Standard      197S          U9GS
                                                                                                ASM
                                                                                                           Methods
                                                  Other
                                                 Approved
                                                 Methods
13.  Chloride, milligram
     par liter

14.  Chlorinated organic
     compounds  (exoept
     pesticides), milligram
     per liter
15.  Chlorine—total
     residual, milligram
     per liter
16.  color, platlnn cobalt
     uilta or dominant «ava
     length, hue, lualnanos,
     purity
               Silver nitratet
               mercuric nitrate)  or
               automated coloria»tric-ferricyanide
               GM chromabography U
29
31
               lodonetxlc titratlen, amperometrlc or
               •tarch-iodlne end-point)                35
               at) coloriaetrie or
               Tltrimetrlc •athodi Rtaae last two
               are Interim matted* pending labora-
               tory testing.)
               ODlortaetrlci                          36
               •pectrophotcnetrlci or                  39
               AM procedure U
303
304
613
                          267
                          265
(46) W
           1615)'
             318
             322
             332
             329
             64
             66
             278
                                                                                                              82
17.  Cyanide,  total u,
     •llllgram per liter

IB. Cyanide amenable to
     chlorinatitn, mllil-
     grana per liter

19.  Uaaolved oxygen,
     milligram per liter
20,  Fluoride, milligram
     per liter
 21.  Hardness—total,  aa
     CaCo.,, milligram
     par liter
              Distillation followed by  silver nitrate   40
              titratlen or pyridine pyrazolone  (or
              barbituric acid) colorlmetric
                                                                  361
                                                                                             85         (22)'
               Distillation followed by silver nitrate   49         376
               titratlen or pyridine pyrazolone (or
               barbituric acid) colorinetrlc
               MnUer  (Aside modification) or           51         443
               electrode method                         56         450
               Distillation3 followed by                -          389
               ion electrode)                           65         391
               SPAtNEi  or                               59         393
               autonated ooifileonne                     61         614
               EDZA  titratlen)                          68         202
               autcnated ooloriimstrlc) or               70           -
               atomic absorption (BUB of Ca and Hj        -
               aa their reapective carbonates)
                                                                                503
                                                                                503
                          368         126         (609)'
                          307          93
                          305
                                                                                                  161
                                       94        (617)2

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                 Federal Register  /  Vol. 44, No. 244. / Tuesday, December 18, 1979 /  Proposed Rules
                                                                                                 75031
                                               •ML* I.  UST OF APPROVED TOST PROCEDURES   (Cant.)
    Parameter and mite
                                           Method
                                                                                           Reference (Page NOB.)
                                                                      1974        14th ftl.     Part 31
                                                                       EPA        Standard      1975          U9GS .
                                                                     Methods      Method!       ASM        Methods
                                                                                         Other
                                                                                        Approved
                                                                                        Methods
22.  Hydrogen Icn (pH),
     pH unita
23.  Kjeldahl nitrogen  (as-
     N), milligram par
     liter
Electrcmetrlc measurement                239

Digestion and distillation followed      175
by nesslerlzaticn,  tltraticn, or
electrode)                              165
automated dlgeatlon autanted phenolata  182
                                                                                   460
                                                    437
                                                                                                178
                                                                                                             129
                                                                              122
                                                                                                                        (606)'
                                                                                         (612)'
Metal*
24.  Alunintn—total,
     •llllgnn par liter
25.  AlvminuB—dissolved,
     mllligrtms per liber
Digestion14 followed by
atcnic absorption15 or by
oolorinetrlc (Eriochrome Cyanide R)
or by I0>27
0.45 micron filtration16 followed Jy
referenced nthads for total aliadnui
                                         92
152

171
                                                                             (19)
                                                                                 10
26.  Antimony—total,
     milligram per liter
Digestion14  followed by
atsnic absorption U
27.  Antinny—disaolvwS,
     •ilUgnwper liter
28.  Arsenic—total,
     Milligram per liter
29.  Arsenic—dlMolved,
     •illignoa per liter
30.  Baria—total,
     •dlUgrao* par liter
31.  B«rii»—dissolved.
     •UliqraM per liter
32.  Barylllvw—total,
     ndlligran per liter
0.45 micron filtration u followed by
referenced method for total antimony
Digestion followed by
silver diethyldithiocarbaBBtei  or
atomic absorption 1S< a
or by 1O> n
0.45 micron filtration M followed by
                           araenio
referenced method for
Digestion **  followed fay atomic
absorption15  or by KP27
0.45 micron filtration" followed by
referenced method for total Darin
Digestion M  followed by atomic
absorption**  or by oolarimetria
(Alimdnon) or fay TCP27
                                        9
                                       95
                                       97
                                                    285
                                                    283
                                                    159
                                                   152
                                                   .152
                                                   177
                          (31)
                          (37)
10
10
                                                                              52
                                                                              S3

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75032
Federal Register / Vol. 44, No. 244 /  Tuesday, December 18, 1979 /  Proposed Rules
•WBIB1, UST OP ATPncMEO TEST PHXEDWES (Cont.l

33.

34.
35.
36.

37,

38.

39.

40.

41.
42.
43.
44.

Parameter and units
BeryUium— dissolved.
milligram per liter
Boron— total. Milli-
grams per liter
Boron — dissolved,
Milligram per liter
Cadmium— total
milligram per liter

Cadmium— dlsaolwd.
milligram per liter
Calcium— total.
milligram per liter
Calcium— dissolved,
Milligram per liter
Chromium VI, milli-
gram per liter
Chromium VI— dissolved.
milligram per liter
Chromium— total,
mllllaram per liter

Milligram per liter
Cobalt— total.
Milligram per liter

deference (Page NOB.)
1974 14th Bd. Part 31 Other
EPA Standard 1975 U9GS , Approved
Method Methods Methods ASM Methods Methods
0.45 micron filtration1* followed by -
referenced Method tor total beryllium
Colorimetrie (Curcumln), 13 287 - -
or by ICP27 ... -
0.45 micron filtration1* followed by -
referenced method for total boron
Digestion14 followed by 101 148 345 62 (619) 2 (37)'
atomic absorption or by
oolorimetric (Dithiscne) 182
or by ICP27 - -
0.45 micron filtration 1S followed by -
referenced method tor total cedmlu*
Digestion14 followed by 103 148 345 6«
atomic absorptlont or
BDT* titration - 189 - -
or by TCP "
0.45 micron filtration16 followed -
by referenced method for total calcium
Extraction and atomic absorption) 89, 105 76
colorlmetrlc (Dlphanylcarbazide) 192 75
0.45 micron filtration16 followed by -
referenced Method for chromium VI
Digestion" followed by 105 148 345 78 (619) 2
atomic absorption or by
oolorimetric (Diphenyloarbazide) - 192 286 77
or by KP27 ...
0.45 Micron filtration16 followed by
referenced method fair total otumium
Digestion 1* followed by 107 148 345 80 (37)
or by KP27 ... -

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                 Federal Register /  Vol. 44. No. 244 /  Tuesday, December 18, 1979  /  Proposed Rules
                                                                                                 75033
                                               TTIBLB I.  UST or AITIOVED TEST PWXHWBE8   (cont.)

45.
46.
Psrareter and wiita
Cobalt — dissolved,
milligram per liter
Copper — total,
milligram per liter
1974
EPA
Method Methods
0.45 micron filtration16 followed by
referenced method for total cobalt
Digestion 14 followed by 108
atonic absorption or by
colorimetric (Neocuproine) »
14th td.
HeShrds
148
196
Rpferenre \fz 27
                                                     16
0.45 micron  filtration    followed by
referenced method for total copper
Digestion 14 followed by
atonic absorption 18
49.  Iridium—total, milli-
     grams per liter
Digestion
                                        14
            followed by
atonic absorption 19
50.  Iron—total, milli-
     grams per liter
Digestion U followed by
atonic absorption    or by
colorimetric  (Phsnanthrollne)
or by ICP 27
                                                                      110
                                                    148

                                                    206
               345

               326
                                                                                                             102        (619)"
51.   Iron—dissolved,
     milligram per liter
52.   lead—total, milli-
     grams per liter
53.  Lead—dissolved,
     milligram per liter
54.  Magnesia*—total,
     milligram per liter
55.  Itegnesiin-dlsaolved,
     milligram per liter
56.  Manganese  total,
     milligram par liter
0.45 micron filtration16 followed by
referenced method for total iron
Digestion 14 followed by
atonic absorption    or by
colorinetric (Dithizcne)
or by ICP27
0.45 micron filtration16 followed by
referenced method for total lead
Digestion14 followed by
atonic absorption) or
9raviinetrlc
or by ICP27
0.45 micron filtration 1S followed by
referenced method for total mognesiun
Digestion   followed by
atonic absorption    or by
colorimetrlo (Feraulfate or perlodate)
or by Id 2*
                                        112
                                        114
                                        116
  148

  215




  148

  221




  148

225, 227
                                                                345
                                                                              105
                                                                                           (619)'
                                                                345
                                                                             109
                                                                                          (619)'
                                                                345
                                                                             111
(619)'

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75034
Federal Register  /  Vol. 44, No. 244  / Tuesday, December 18, 1979  /  Proposed Rules
TOBLE I. LIST or WT1WEO TEST PKXETWraS (Cont.)

57 .

58.

59.

60.


SI.

62.



61.

64.

Parameter and units
}tai JIJ^M nj-jc dissolved .
milligram per liter
ttercury— total.
milligram per liter
Mercury — dissolved,
milligrams per liter
jfclybJenu*— total,
milligrams per liter

MDlytdenim— dissolved.
milligram per liter
Nickel—total,
milligrams par liter


Nickel— dissolved,
milligram per liter
CWniun— total,
milligram per liter
Reference (Page Mne.)
1974 14th Ed. Part 31 Other
B* Standard 1975 UBG8 . Approved
Method Methods Methods ASTM MeUwds Methods
0.45 micron filtration followed by -
referaiced method for total aainjarieua
Flawless atrmio absorptim 118 156 338 (51) 10

0. 45 micron filtration16 followed by -
referenced method for total mercury
Digestion M followed by 139 - 350 - -
atomic absorption 15
or by 10>27 -
0.45 micron filtration16 followed by - -
referenced method for total molybdenui
Digestion M followsd by 141 148 345 115
atomic absorption or by
colorlmetrlc (Heptadire) _ 232 ...
orbylCP27
0.45 micrcn filtration16 followed by -
referenced method for total nickel
Digestion U followed by -
atomic absorption
 65.  Palladitm—total,
     milligram per liter
               Digestion14 followed by
               atomic absorption U
 66.  Platintn—total,
     milligram per liter
               Digestion
                                        14
            followed by
atomic absorption 18
 67.  Potassium—total,
 ^  milligrams per liter
               Digestion U  follownd by
               atomic absorption,
               coloriaetric  (Oobaltinitrite), or by
               flame photometric
               or by ICP 2'
                                                                    143
                                                                                                        134
                                                                                     (620)'
                                                                                235
                                                                                234
                                                                                            403

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Federal Register / Vol. 44, No. 244 / Tuesday, December 18, 1979 /  Proposed Rules
75035
ireus i. LIST or MHWED it&r faoaauaa (ooot.)

68.

69.
70.
71.
72.

73.

74.


75.

76.



77.

78.
Parameter and imits
Potaaaiun— dissolved,
milligrams per liter
Rndlm— total,
milligrams per liter
Ititheniun— total,
milligrams per liter
Seleniu*— total,
milligrams per liter
Selenlin— dissolved.
milligrams per liter
Silica— dissolved.
miligram per liter
Silver-total M
ftfiijji ffff per liter


Silver-dissolved ls.
milligrams per liter
Sodlm— total,
milligrams per liter


Sodivin— -dissolved.
milligram!! per liter
Tnslliun— total,
milligram per liter
Reference (Page (fee.)
1974 14th Bd. Part 31 Other
B* Standard 1975 USGS . Approved
Method Methods Methods ASTM Methods Methods
0.45 micron filtration 16 followed by -
ref erenoed method for total potoasiun
Digestion M followed by -
atonic absorption lg
Digestion M followed by -
atonic absorption
Digeatlon M followed by 145 159 -
atcmic absorption "• 1B
orbyld>27
0.45 micron filtration 1S followed by -
reference method for total seleniun
0.45 micron filtration l6 followed by 274 <• 398 139
colorinetrlc Qtolybdoeilicate) 497
or by 1CP27 .....
Digestion M followed by 146 148 - 142 (619) 2 (37)9
atomic absorption or by
colorjnetric (Dithixone) 243 - -
orbyHT27
0.45 micron filtration 1S followed by -
ref erenoed method for total silver
Digestion M followed by 147 143 (621) 2
atonic absorption or by
flans photometric * 250 403
orbyltT27
0.45 micron filtration 1S followed by -
referenced nothod fot tPtJil sodltn
Digestion 14 followed by 149
atonic absorption 15

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75036
Federal Register /  Vol. 44, No. 244  / Tuesday, December 18,  1979  /  Proposed Rules
                                               TflBUB I.  LIST 07 APPRWED TEST PROCEDURES   (Cont.)
    Parameter and units
                                           Method
                                                                                           Beference (Page NOB.)
                                                                      1974        14th W.     tart 31                   Other
                                                                       em        Standard      197S         U9GS .     Approved
                                                                     Methods      Methods       WSTM       Methods1     Methods
79.  Thallim-dissolved,
     milligram per liter
60.  Tin—total, milli-
     grams per liter
                0.45 micron filtration16 followed by
                referenoed method for total thallium
                Digestion 14 followed by
                                 atonic absorption
                                 15
                                      150
                                                                            (65)
                                                                               10
01.  Tin—dissolved, milli-
     gram per liter
82.  Titenlin—total,
     milligrams per liter
0.45 micron filtration U followed by
referenced method for total tin
Digestion M followed by
atomic absorption
                                                      151
83.  Titanius-dissolved,
     milligrams per liter
84.  Vanadium—total,
     milligram per liber
0.45 micron filtration 1S followed by
referenced method for total titanium
Digestion M followed by
atonic absorption    or by
oolceimetric (Gallic add)
or by KT n
                                                      153
                                                                  152

                                                                  260
                                                                                                Ml
                                                                                                            W?)
                                                                                                                10
 85.  Vanadiun—dissolved
     milligram per liter
 86.  Zinc—total, milli-
     grams per liter
 87.  tine—dissolved,
     milligram par liber
                0.45 micron filtration16 followed by
                referenoed method for total vanadltm
                Digestion14 followed by
                atomic absorption   or by
                colorimetric (Dithlione)
                or by OT27
                0.45 micron filtration16 followed by
                          mefchod Cor totflJL sine
                                      155
                                                   148
                                                               345
                                                                            159
                         (619)2(J7)9
 88.  Nitrate (as Nt, milli-
     grams per liter
 89.  Nitrite (as N), milli-
     grams per liter
 90.  CHI and grease, milli-
     gram per liter
                Cadmiu* reduction                     201
                brucine sulfatel                      197
                automated cadMin or hydrazine reduc-  207
                tien20
                Manual  or autcmted colcriTOtric       215
                (Dlaxotizatlon)
                Liquid-liquid extraction with tri-     229
               chlorotrmuoroethane-gravinetric
                                                   423
                                                   427
                                                   620

                                                   434

                                                   SIS
358
            119
                                                                                                            121
                         (614)2  (28)'

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                  Federal Register  / Vol. 44, No. 244  / Tuesday, December 18, 1979 /  Proposed Rules
                                                                                                75037
                                                 TtBLE 1.  UST OP ATPflWED 1BOT PROCEDURES   (Cont.)
     Parameter and units
                                             Method
                                                                                            Reference (Page Nos.)
                                                                       1974        14th W.     Part 31                   Other
                                                                        Hf»        Standard      1975          UBGS .     Approved
                                                                      Methods      Methods       ASM        Methods     Methods
  91.  Organic carbon)  total
      (TOC), milligram per
      liter
  92.  Organic nitrogen
      (as N), mllligrms
      per liter
Confcustlon— Infrared netted2           236          532
  KJeldahl nitrogen ndnm amonia       175,159      43V
  nitrogen
                                                               467
                                                                           ( 4)
                                                                            122
                                                                                                                 22
(612,614)'
 Qrauiic
 93.  Acenaphthene,
      microgra™ per liber
 94.  Acenaphthylane,
      nicrogranv per liter
 95.  Acroleln,
      mlcrogrwiB par liter
 96.  ftcrylonitrile,
      •dcxogranB par liter
  OC or HPIC method (610)
  OVM3 i»sthod(625) 26
  GC or HPI£ method (610)38
  GO/MS mettod(625) M
  OC method (603)31
        BBthDd(524) M
                31
 OC method (603)
        method (624)
                    K
 97.  Aldrln,
      nicrogramg per liter
 98.  Anthracene,
      nicrograma par liter
 99.  Benzene,
      micrognro par liter
100.  Benzldlnei
      mllllgron per liter
      nicrograna par liter
101.  Benzo(a)anthracenB,
      nicrograno per liter
102.  Benzo(a)pyrena,
      mictograms per liter
103.  Benzo(b)fluoranthena
      Bd.crujj.MTiB per liter
104.  Benxo(g,h,l)peryl0na,
      microgranv per liter
GC method (608)
GC/MS, method
                                                 36
                    26
                  ,26
OC or VPIC method (610)
OC/IB method (62S)26
OC method (602)
GC/MS method (62'4)'
HPIC method (60S)33
Oxldatlon-oolormetrlc*
GC/MS method(625)  26
OC or HPIC method (610)
GC/MS, method (625)26
OC or HPIC method (610)
       ethod
                       38
                       38
                       38-
 OC or W1C method  (610)
 OC/HB method ( 625 )26
 OC or HPIC method  (610)
       method (625) 26
                       38
                      38

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75038
Federal Register / Vol. 44, No. 244 / Tuesday, December 18, 1979 / Proposed Rules
17IBt£ I. LIST OF APPRWED TEST PHUCHJUHtS (Cent.)

105.

106.
107.
108.
109,
110.
111.
112.
113.
114.

115.
116.
117.
118.
119.
120.

Parameter and units
DenzoOc) CluoranthenBf
RilcLuyiauB per liter
B-BHC,
ntlczogran per liter
b-BHC,
mlcrograme per liter
d-BHC,
nicrognn per liter
g-BIC
microgranB per liter
Bis(2-chloroethyl) ether
•ticxocfraRB per liter
Bis(2-chloroethoKy) methane
raicrogra™ par liter
Bl»(2-chlorolaopropyl) ether
microgranB per liter
BU(2-ethylhexyl) phthalate,
micrograms per liter
Brarodichloromethane,
microgranB per liter
micrograms per liter
BromofflethanB,
mlcrograma per liter
4-Bronophenylphenyl ether,
nicrograRB per liter
Butyltenzyl phthalate,
micrograne per liter
Carbon te trichloride,
micrograme per liter
Chlordane,
micrograRis per liter
Reference (Page Nos.)
1974 14th M. Part 31
EPA Standard 1975 USGS ,
Method Methods Methods ASW Methods
OC or HPIC method (610)38 ....
OC/MS method, U25)2* .
OC method (60S)36 -
OC/MS method (62S)26 -
OC method (60S)36 -
OC/MS method (6J5)26 ....
OC method (60S)36 -
GC/MS method (625) X -
OC method (60S)36 -
OC/MB method (625) M ....
GC method (611)39 ....
OC/MS method (625) M -
GC method (611)39 ....
OC/MS method (625) 26 -
OC method I611)39 -
OC/MS method (625) x -
OC method (606)34 -
OC/MS method (62B)26 -
OC method (601)29 -
OC/MS method (SZ^)2* -
GC method (601) W ....
GC/MS method (624)* -
OC method (601)29 ....
GC/MS method (6Z4)26 -
GC method (fill)39 -
OC/MS method (82S)26 ....
GC method (606)34 -
OC/MS method (62S)26 -
OC method (601)29 ....
OC/MS method (624)26 -
OC method (60S)36 ....
GC/MS method (6i5) -
Other
Methods
_
.
-
-
-
;
-
:
:
-
.
-
-
-
-
:
-
.
-

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Federal Reeister / Vol. 44, No. 244 /  Tuesday, December 18, 1979 / Proposed Rules
75039
TOW* 1. LIST OF APPBCWED TEST PWXECU3S (Oont.)

121.

122.

123.

124.

125.

126.

127.

128.

129.

130.

131.

132.

133.

134.

135.

136.

Parameter and wits
4-Chloro-3-methylphenol
nlcrocfFBnB per liter
OilorobenxenB/
ntcrognro per liter
Odoroe thane,
mlcrogrwna per liter
2-Chloroettrylviiyl fetter
nicroijiflns per liter
ChlorofoOT,
inicxuyiflsTB per liter
ChloconethBnBf
•dciugiaia per liter
2LC method (610)38 -
OC/MS method (eWfl26 -
OC method (608)3* -
OC/MS method (625) X -
OC mettnd (60S)36 -
OC/MS method (625) 2S -
OC method (60S)36 -
OC/MS method (625) * -
OC or BPLC method (610)38 -
OC/MS method(625) 26 _ - - -
OC method (601)29 -
OC/MS method (624J26 -
OC methods (601)M (602) 30 (612) 40 -
OC/MS method (62J)26 _ - - -
Other
flpprowed
Methods
-
•
-

-
-
-
-
-
-
-
-
-
-
-
-
-
—
-
™
-
-
-
-
-
-
-
-
-
-
-
-

-------
75040
Federal Register / Vol. 44, No. 244 / Tuesday, December 18, 1979 / Proposed Rules
TRBUS I. UST OF AOTWED TEST PI»?EDUHES (Cont.)






Parameter and units
137.

138.

139.

140.

141.

142.

143.

144.

145.

146.

147.

148.

149.

150.

151.

152.

1 , 3-Oichlorobenzene
micrograms per liter
1, 4-Oichlorobenzene,
micrograms per liter
3 , 3 ' -Dichlorcfcenzidine ,
micrograms per liter
Dichlorodifluorone thane
micrograms per liter
1,1- Dichloroethana
ntLcrogrsms per liber
1, 2-Dichloroethana,
raicrogra™ per liter
1,1-Oichloroethane
micrograms per liter
trano-l, 2-OidiloeDeth»nB,
miciuyiswB per liter
2, 4-Oichlorophenol,
microgranB per liter


fnl 'ii un JMIM r^r 1 4 titr
ci8-l,3-Dichlaropropene
microgramB per liter
trans-1, 3-Dichloropropaie
mjuimjt MM per ULber
Dieldrin,
micrograms per liter
Diethyl phthalabs,
microgrjro pel liter
2, 4-DtnethylphenDl,
nicrograms per liter
Dimethyl phthalabs.
microgramB per liter
Reference (Page Nos.)
1974 14th Ed. Part Jl
EEft Standard 1975 U9GS ,
Method (tethods Methods ASTM Methods
GC methods (601) M (602) X (612) 40 -
GC/ttS method (62S)26 -
OC methods (601) 29 (602) M (612) 40 -
QC/HS method (S25)26 ....
One method (60S)33 -
OC/MS method (6ZS}26 -
OC method (601)29 - -

OC method (601) ** -
OC/»B method (624) K -
OC method (601)29 -
OC/HS method (624) 2* - _ _ -
OC method (601)29 -
OC/MS method (624) 2S -
OC method (601)29 -
OC/M5 method (624) * -
OC method (604)32 -
OC/MS method (625)26 -
OC method (601)29 -
OC/MS method (624)26 -
OC method (601)29 -
OC/«S BBthod(624)26 -
OC method (601)29 -
GC/VB netted (62O26 -
OC method (60S)36 -
OC/MS method (625) * -
OC method (606)34 ....
OC/MB method (62Sf 28 -
OC method (604)32 -
OC/MB method (625) M -
OC method (606)34 -
OC/MS method (625) 26 -

Other
Approved
Methods
-
-
-
-
-
-
-

-
-
.
-
-
-
-
-
-
-
-
-
-
-
-
-
-
*
-
*
-
-
'-
"

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          Federal Register / Vol. 44, No. 244 / Tuesday, December 18, 1979 / Proposed Rules
75041
tfBlX I. LIST OP APVRM9J TE3T PRXEDWES (Cont.)

153.
154.
155.
156.
157.
158.
159.
160.

161.
162.
163.
164.
165.
166.
167.
168.
Parameter and units
Di-n-butyl phthalat*,
micrograms per liter
Di-n-octyl phthalabe,
itdcrograms per liter
4 , 6-Dini tro- 2-methylph»-
nol, micrograms per liter
2,4-Dinitrophenol,
micrograms per liter
2,4-Dlnitrotoluane,
micrograms per liter
2, 6-Dini trotoluene,
micrograms per liter
1,2-Dlfhenylhydraslne,
nd-crograBiB por liter
Endoeulfan I,
ndcrograrae per liter
Enfeeulfen II,
miuiuyrsMi per liter
Endoeulfen eullafae,
micrograws per liter
Endrin,
BdcrograM per liter
Endrin aldehyde,
•dcrograMs per liter
Bthylbamene,
nicrograms per liter
Fluoranthene,
micrograns per liter
Pluorene,
mtciMiii.au) per liter
fteptechlor.
Reference (Page NOB.)
1974 14th Bd. Part 31
EPA Standard 1975 USGS .
Method Methods Methods WIM Methods
OC method <606) 34 -
OC/MS method (625)26 -
OC method (606)3* -
GC/MS method (625) 26 -
OC method (604)32 -
GC/MS method (625) 26 -
OC method (604)32 -
OC/MS method (6Z5)26 -
OCiBBtnod (609)37 -
OC/MB method (625)2S -
OC method (609)37 ....
OC/HS method (62S)26 -
OC/HB method (6Z5)26 -
OCBsthod (608)36 -
OC/MS method (62S)26 ....
OC method (608)36 - ...
OC/HS method (625) M -
OC method itm}36 .
DC/to method (625) * - ...
OC method (60S)36 - ...
OC/MS method (625) W - ...
OC method (608)36 -
OC/HB method (625) K -
OC method (602)30 - ...
OCAB method (624) ^ - ...
OCor me method (610) M -
OVHB method (62S) * -
OC or HPIC method (610)38 - . .
OCVHB method (62S>26 - ...
OC method (6O8)36 -
Other
Approved
Methods
-
-
-
-
-
:

_
_
-
-
-
-
-

mlcrogrtpB per liter
                        OC/HB method (625)
                                      **

-------
75042
Federal Register /  Vol. 44, No. 244 / Tuesday, December 18,1979 / Proposed Rules
TffUE 1. LIST OF KfPKNED TEST MUEUUWS (Cnnt.)
Parameter and unlta
169.
170.
171.

172.
173.

174.
175.
176.
177.
178.
179.
180.
181.
182.
Heptachlor epoxide,
ralcrrxfranw per liter
Itexachlorcfoenssens,
mlcrogrwiB per liter
tfexachlorobutadlwe,
ndcrogra™ per litar
itexachlarocjclopentacUsne,
mtcrogrsw par liter
ttexadhloroethane.
micrograna per liber
micrograms per liter
Isophorone,
microgrsiB per liter
Methylene chloride,
micrograne per liter
Nitrobenzene,
micrograniB per liter
2-Hitrophenol,
4-Hitrophenol,
micro^nvrB per liter
^^^^l^ t^ » >E'«HI"»I ^ylf11^ y^i

H^troBodipropylaidnB,
Befermra (Page »«.)
1974 l4th «. ParFTT
K>thod Methods Methods ASflH Methods
OC method (60S)3* -
OV^E method (625)26 - -
GC method (612) 40 -
OC/MS method (625)2S -
OC meOcd <6ia)40 -
OC/MS method (625J26 -
OC emthod (612)40 -
OC/»« method (625) 2fr -
QC nethod (612) 40 -
OC/MS method (625) 26 -
OC or OPIC method (610)38 -
OC/MS method (625) ^ -
OC method (609)37 -
OCAB method (62S)26 -
QC method (601)29 -
OCABmBewd (624)26
OC or HPUC method (610)38 -
OCAB mthod (625)26 -
OC nethod (609)37 -
OCAB method (625)26 -
0= method (604)32 -
OCAB method (625)2S - - - -
OC nethod (604)32 -
OCAB method (625)26 -
OC method (607)35 -
OCAB method (625) * -
OC netted (607)35 -
OtSier
Mettxris
-
-
-
-
-
„
-
:
-
-
-
_
_
_
.
-
                                               26
 183.  H-NitrooodiphenylaBdne,
      nticxo^rafflB per liter
 184.  PCB-1016,
               per liter
                 OC/MS method (625)
                 OC method (607) 35
                 OCAS method (625)
                 OC method (60S)
                 OC/HB method (625)26
26

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                Federal Register  / Vol. 44, No. 244 /  Tuesday, December 18, 1979 /  Proposed Rules
                                                                                          75043
- —
185.

186.
187.

188.
189.
190.
191.
192.

Parameter en) unlU
POB-1221,
microgr&Kj P&f liter
PCB-12J2,
ndcrograms per liter
PCB-1242,
*B| r^W^ur >U.-1 f»f 1 ^ ^"OT
PCB-1248,
mlcro^frafno per Xlber
PCB-1254,
• n •!!• r*»T 1 1 t^V
PCB-1260,
PentacMorophenol,
mlcrogrow per liter
Phenanthrene,
T«BU! I. UST OF APPKNED TEST PWXEDOiaS (Cont.)
Reference (Page_NoB . )
1974 14th ta. Pwt "11
EPA Standard 1975 USGS j
Methtid Methods Methods ."OTM Mctficds
OC method (60S)36 -
OVMS method ($2S) 26 -
a.' metiiod (60S)36 -
GC/MS method (626) 2* -
GC method (60S)3* -
OVMS methtxl(625)M -
OC mathod (60S)36 -
OC/>6 method (S?5)2S - - - -
OC method (608) X -
OCAB method (6Z5) 26 -
OC m-ttiod (60S)36 -
OC/tE method (625) 26 -
GC netiiod (60S) - -
GC/MS matiod (625) 26 _ - - -
GC or MPIC method (610) M -

Otlier
Approved
Methods
-
~
-
-
-
-
-
-
-
-
193.  Pherol,
     ndcxogram per liter
194.  Pyrene,
     ndcrogrnB per liter
195.  2,3,7,9-ttetrarfdoto-
     dlbenzo-p-dioBtln
     mlcrogmiB per liter
196.  1,1,2,2-TetrachlDeoB-
     thnno,
               per liter
197.  Tetrachlaroethene,
                sr liter
198.  Tbluene,
     micro9mno per liter
199.  Ttaxaphene,
                                  OC/MS mettod (625) 26
                                  GC netted (604)
                                               32
                 26
OC/MS method (6?S)
GC or HPIC method (610)
GC/MS metiwd (623\26
                     38
      irethods (613)41  (6S5)2'
OC method  (601)
              29
                 26
                 26
               psr liter
GC/»B method (62«)
OC method  (601)29
OC/W method (624)
OC method  (602)M
DC/MS method (624).26
OC method  (609)36
GC/MS method (GZ5)26

-------
75044
Federal Register  /  Vcl. 44, i\'o.  244  / Tuesday, December 18, 1979 /  Proposed Rules
                                               TBBIE I.  UST Of APFRWED TEST PHOCEDUPES   (Goflt.)
    Parameter and initn
200.   l,2,4-Trlc^oroben»es*,
      inicmyi <_HKI pc_r li^jsr
201.   1,1,1-Triohloroethai*,
      wiu JL uy i w w per ii bsx"
202.   1,1,2-Trichloroethane,
      mictogiavM per liter
203.   TrichlDroethene,
      ndcrogme per liter
204.   TriehlegoflueaoneUianB,
      mlcrogramB per liter
205.   2,4,6-TricMQrophe«>l,
      niicrograms per liter
206.   Vinyl Chloride,
      micrograms per liter

207.   Qrthophosphate  (as P),
      milligrams per liber
208.   •Pesticides, milligram
      per liter
209.   Phenols, milligram
      per liter
210.   Phosphorus  (elemental),
      milligrams per  liter
211.   Phosphorus) total (as
      P), milligrams per
                                                 *°
                  QC nethod (612)
                  OC/MS i~rthod(625)
                  OC msthod (601)29
                  QC/fB i
                                                    26
                                   QC method (601)
                                   OC/MS nethod(624)
                                   OC method (601)W
                                   OC/MS method(62«)
                                   OC method (601)W
                                   OC/MS method (624)
                                   OC method (604)32
                                                  29
                                   OC meUwd (601)
                                         TOthod(624)
                                                    26
                                                                                  14th BH.
                                                                            "tar OF
                                                                              1975
                                                                                                                         OtJ>er
                                   Manual car                            249
                                   automated ascorbic acid reduction     256
                                                    .10
                                   Gaa chxtmtography'
                                   Oolorlimtrlc, (4AAP)
                                                     22
                                                                        241
                                                                    481
                                                                    624
                                                                    555
                                                                                     582
                                                                                                  384
                                                                                                 529
                                                                                                 545
131         (621)"


(24)U
                                   Gas chrcnatography'

                                   Persulfate digestion followed by manual 249
                                   or autonted ascotblc acid reduction   256
                                                                    476,481
                                                                    624          384
                                                                                             133
                                                                                                          (621)''

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                  Federal Register /  Vol. 44, No. 244 /  Tuesday, December 18, 1979  / Proposed Rules
                                                                                              75045
                                                      I.  LIST OF APPROVED TEST PROCEDURES   (Cont.)
    Parameter aid units
                                            Method
                                                                       1974
                                                                       EPA
                                                                     Methods
                                                         Reference (Page NOB.)
                                               14th W.     Part 31
                                               Standard      1975         U9GS
                                                                                                                         Otter
                                                                                  Methods
                                                                                                           Methods      Methods
Radiological
212.  Alpha—total, pCi per
      liter
213.  Alpha—countin} error,
      pCi per liter
214.  Beta—total, pCi par
      liter
215,  Beta—oounting error,
      pCi per liter
216.  a) tediim—total, pd
         per liter
      b) 22«n», pCi per
         liter

Residue
217.  Total, milligrams per
      liter
218.  Total dissolved (fil-
      terable) , milligram
      per liter
219.  Total suspended (non-
      filterable), milli-
      gram per liter
220.  Settleable, mllU-
      llters per liter or
      milligram per liter
221.  Total volatile, •dill-'
      grans per liter
 Proportional or scintillation

 Proportional or scintillation
 counter
 Proportional counter

 Proportional counter

 Proportional counter

 Scintillation counter
Gravimetric,  103 to 105"C
                                     270
Glass fiber filtration, 180*C         266
Glass fiber filtration, 103 to 105*0   268
Vblunetric or gravimetric
Gravimetric,  550*C
                                    272
648

648

648

648


661

667



91

92


94



95



95
                                                               591       (75)10 (78)2*
594
606
661
             (79)
                10
601       {75)10  (78)2t
             (79)
                10
                                                                           (81)
                10
                        (537)
                                                                                           26

-------
75046
Federal Register / Vol. 44, No. 244 / Tuesday, December 18, 1979 / Proposed Rules
TABLE I. UCT CT MTBCNED TEST PH3OMJWS (Cont.)
Parameter and units
222.


223.


224.


225.
226.

227.

228.
Specific conductance,
mlciuiif m6 per centi~ '
meter at 25*C
Sulfate (as SOj)
milligram per liter


Sulflde (as S), Milli-
grams per liter

Sulfite (as S03),
milligrams per liter
Surfactants, milli-
grams per liter
Tenperature, degrees C

Turbidity, NIU
1974
EPA
Method Methods
ftieatstone bridge conaucUnetry 275


Gravimetric;
turbidinetrici or 277
automted colocimetric (barton 279
chloranilata)
tttrlmetric— iodine for levels greater 284
than 1 mg per liter)
Methylene blue photometric
TltrlnBtric, lodlne-iodate 285
ODlorinetric (Methylene blue) 157

Calibrated glass or electromatric 286
thsuiuiieter
Hephelcnetrlc 295
Reference (Page Noe.)
14th Hi. Part 31 Other
Standard 1975 USGS . approved
Methods ASW Methods Methods
71 120 148 (606)2


493 424 - (624 ?
496 425 - (623) 2
- - - -

505 - 154

503
508 435
600 494 (ID22

125 - (3D25

132 223 156

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	      Federal Register / Vol. 44. No. 244  /  Tuesday, December 18. 1979 / Proposed Rules	75047


Footnotes:

1.     All page references for USGS methods unless otherwise noted are to Brown, E., Skougstad, N.W.,
       and Fishman, M.J., "Methods for Collection and Analysis of Water Sanples for Dissolved Minerals
       and Gases, "U.S. Geological Survey Techniques of Water-Resources Inv., book 5 ch. Al,  (1970)."

2.     EPA comparable method may be found on indicated page of "Official Methods of Analysis of the
       Association of Official Analytical Chemists" methods manual, 12th ed. (1975).

3.     Manual distillation is not required if comparability data on representative effluent samples
       are on coipany file to show that this preliminary distillation step is not necessary; however,
       manual distillation will be required to resolve any controversies.

4.     The method used must be specified.

5.     The 5 tube MPN is used.

6.     Slack, K.V. and others, "Methods for Collection and Analysis of Aquatic Biological and Micro-
       biological Samples "U.S. Geological Survey Techniques of Water-Resource Inv., book 5, ch A4 (1973)."

7.     Since the membrane filter technique usually yields low and variable recovery from chlorinated
       wastewaters, the MPN method will be required to resolve any controversies.

8.     The_chloromine-T oxidation-colorraetric procedure for benzidine is available from the Environmental
       Monitoring and Support Laboratory, U.S.  Environmental Protection Agency, Cincinnati.Ohio 45268
9.     American National Standard on Photographic Processing Effluents, Apr. 2, 1975.  Available
       from ANSI, 1430 Broadway, New York, N.Y.  10018.

10.    Fishman,  M.J.  and Brown, Eugene,  "Selected Methods of the U.S.  Geological Survey for Analysis
       of Wastewaters," (1976)  open-file report  76-177.

11.    Procedures for pentachlorophenol, chlorinated organic compounds,  and pesticides  can be obtained
       from the Environmental Monitoring and Support Laboratory,  U.S.  Environmental Protection Agency,
       Cincinnati, Ohio 45268.

12.    Color method (ADMI procedure)  available fron Environmental Monitoring and Support Laboratory, U.S.
       Environmental  Protection Agency,  Cincinnati,  Ohio  45268.

13.    For samples suspected of having thiocyanate interference,  magnesium chloride is  used as the
       digestion catalyst.  In the approved test procedure for cyanides,  the recommended catalysts are
       replaced with  20 ml of a solution of 510  g/1 magnesium chloride (MgCl_•6H 0).  This substitution
       will eliminate thiocyanate interference for both total cyanide  and cyanide  amenable to chlori-
       nation measurements.

14.    For the determination of total metals the sample is not filtered before  processinq.  Because
       vigorous  digestion procedures may result  in a loss of certain metals through precipation, a
       less vigorous  treatment is recommended as given on p.  83 (4.1.4)  of "Methods for Chemical
       Analysis  of Water and Wastes"  (1974). In those instances  where a more vigorous  digestion
       is desired the procedure on p.  82 (4.1.3) should be followed.   For the measurement of the
       noble metal series  (gold,  iridium,  osmium,  palladium,  platinum,  rhodium  and ruthenium),  an
       aqua regia digestion  is  to be substituted as  follows:   Transfer a representative aliquot
       of the well-mixed sample to a Griffin beaker  and add 3 ml  of  concentrated redistilled HNO  .
       Place the beaker on a steam bath  and evaporate to dryness.  Cool the beaker and  cautiously
       add  a 5 ml portion  of aqua regia.   (Aqua  regia is prepared immediately before  use by carefully
       adding 3  volumes of concentrated  HC1 to one volume of concentrated HNO,.)   Cover the beaker
       with a watch glass  and return to  the steam  bath.   Continue heating the covered beaker for
       50 rain.   Remove cover and evaporate to dryness.   Cool and  take  up the residue  in a small
       quantity  of 1:1 HC1.   Wash down the beaker  walls  and watch glass with distilled  water and
       filter the sample to  remove silicates and other insoluble material that  could  clog the
       atomizer.   Adjust the volume to some predetermined value based  on the expected metal
       concentration.   The sample is now ready for analysis.

-------
75048	Federal Register / Vol. 44. No. 244  / Tuesday, December 18. 1979  /  Proposed Rules	


15.    As the various  furnace devices  (flameless AA)  are essentially atonic absorption techniques,
       they are considered to be approved test methods.    Methods of standard addition are to be
       followed as  noted in p. 78 of "Methods for Chemical Analysis  of Water and Wastes."  1974

16.    Dissolved metals are defined as those constLtutuents  which will pass through a 0.45 jsn
       membrane filter.  A prefiltration is permissible bo free the  sample from larger suspended
       solids.   Filter the sample as scon as practical after collection  using the first 50 to 100 ml
       to rinse the filter flask.   (Glass or plastic filtering apparatus are reccrnnended to avoid
       possible contamination.)  Discard the portion used to rinse the  flask and collect the required
       volume of filtrate.  Acidify the filtrate with 1:1 redistilled UNO, to a pH or 2.  Normally,
       3 ml of  (1:1) acid per liter should be sufficient to  preserve the samples.

17.    See "Atonic  Absorption Newsletter," vol. 13, 75 (1974).  Available from  Perkin-Elmer Corp.,
       MainAve., Norwalk, Conn.  06852

18.    Method available from Environmental Monitoring and Support laboratory, U.S. Environmental
       Protection Agency, Cincinnati, Ohio  45263

19.    Recfrntvended  methods for the analysis of silver in industrial  wastewaters at concentrations
       of 1 mg/1 and above are inadequate where silver exists as an  inorganic halide.  Silver halides
       such as  the  brotd.de and chloride are relatively insoluble in  reagents  such as nitric acid
       but are  readily soluble in an aqueous buffer of sodium thiosulfate and sodium hydroxide to a
       pH of 12. Therefore, for levels of silver above 1 mg/1 20 ml of sample  should be diluted
       to 100 ml by adding 40 ml each of 2M Na 5,0., and 2M NaOH. Standards should be prepared in the
       same manner. For levels of silver below I ffig/1 the recomended method is satisfactory.

20.    An automated hydrazine reduction method is available  fron the Environmental Monitoring and
       Support Laboratory, U.S. Environmental Protection Agency, Cincinnati,  Ohio 45268.

21.    A number of  such systems manufactured by various cotpanies are considered to be comparable
       in their performance.  In addition, another technique, based  on  conbustion-methane detection
       is also acceptable.

22.    Goerlitz, D.,  Brown, E., "Methods  for Analysis of Organic  Substances  in Water"!  U.S.
       Geological  Survey Techniques of Water-Resources Inb., book 5,  ch. A3  (1972)

23,    R.F, Addison and E.G. Ackman,  "Direct Determination of Elemental Phosphorus by Gas-Liquid
       Chranatography," "Journal of Chromatography," vol.  47, No.  3,  pp. 421-426, 1970.

24.    The method  found on p. 75 measures only the dissolved portion while the method on p. 78
       measures only  suspended.  Therefore,  the 2 results  must be added together to obtain "total".

25.    Stevens, H.H., Fick, J.F.,  and Snoot, G.F., "Water  Temperature - Influential Factors, Field
       Measurement and Data Presentation;  U.S. Geological Survey Techniques of Water Resources
       Inv., book  1 (1975)."

26.    EPA interim methods for analysis of organics in municipal and industrial wastewater by GC/MS
       purge and trap (Method 624   and methylene  chloride extraction  (Method 625) procedures are
       available from the Enyironnental Monitoring and Support Laboratory, O.S.E.P.A., Cincinnati,
       Ohio, 45268.  Direct Aqueous injection is to be used in these GC/MS procedures  for all compounds
       that exceed 1000 micrograms per liter.  Dichlorodifluoronethane should be analyzed  by the
       interim gas chranatographic method 601. For differentiation between  iscmeric pairs anthracene
       and phenanthrene, chrysena and benzo(a)anthracene,    and benzo (b) fluoranthene and benzo
        (k)  fluoranthene use method 610 of polynuclear aromatic hydrocarbons. "Interim Method  for
       Benzidine and its Salts in Wastewater" is available frou the Environmental Monitoring and
       Support Laboratory, U.S.E.P.A., Cincinnati, Ohio,  45268 (EMSL-CI).

27.    The Inductively Coupled plasma Optical Emission Spectronetric Method  (ICP) is  available from
       the Environmental Monitoring and  Support Laboratory, IJ.S-E.P.A. Cincinnati, Ohio 45268
        (EMSL-CI),

28.    Method  507  for Carbonaceous Biochemical Oxygen Demand  (BOD carbonaceous) is available  fron
       the Environmental Monitoring and  Support Laboratory, U.S.E.P.A. Cincinnati, Ohio 45268
        (EM3L-CI),

-------
              Federal Register / Vol. 44, No. 244 /  Tuesday. December 18. 1979 / Proposed Rules	75049


29.    Inert gas purge, followed by gas chromatography with halide specific detection
       (interim method 601), available from EMSL-CI.

30.    Inert gas purge followed by gas chronatography and photoionization detection
       (interim method 602), available from EMSL-CI.

31.    Inert gas purge followed by gas chrctnatographic separation and detection with flame
       ionization detector (interim method 603), available from EMSL-CI.

32.    Methylene chloride extraction,  followed by gas chromatography with flame ionization or
       electron capture detection (interim method 604), available from EMSL-CI.

33.    Chloroform extraction followed by concentration and high performance liquid chromatography
       (HPLC)  with electrochemical detection (interim method 605), available from EMSL-CI.

34.    Methylene chloride extraction followed by gas chronatography with flame ionization or
       electron capture detection (interim method 606), available from EMSL-CI.

35.    Methylene chloride extraction followed by gas chronatography with nitrogen-phosphorous or
       reductive Hall detectors (interim method 607), available from EMSL-CI.

36.    Methylene chloride extraction followed by gas chronatography with electron capture or
       halogen specific detection (interim method 608), available fron EMSL-CI.

37.    Methylene chloride extraction followed by exchange to toluene, gas chromatography with
       flame ionization detection (interim method 609), available fron EMSL-CI.

38.    Methylene chloride extraction followed by HPIC with fluoresence or UV detection; or gas
       chronatography (interim method 610), available from EMSL-CI.

39.    Methylene chloride extraction followed by gas chromatography with halogen-specific
       detector (interim method 611),  available froti EMSL-CI.

40.    Methylene chloride extraction followed by concentration,  gas chromatography with electron
       capture detection (interim method 612),  available from EMSL-CI.

41.    Methylene chloride extraction followed by transfer to hexane and capillary column gas
       chromatography/faass spectonetry with electron impact ionization (interim method 613),
       available from EMSL-CI.


42.    Microbiological Methods for Monitoring the Environment (December 1978) available for the
       Environmental Monitoring and Support Laboratory U.S. E.P.A. Cincinnati, Ohio 45268.

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75050
Federal Register / Vol. 44,'No. 244 / Tuesday, December 18, 1979 /  Proposed Rules

TABLE
Measurement
1
2
3


4-7

8

9
10

11
12

13
14
15

16
17-18


19

20
21
22
23&92

40-41
Acidity
Alkalinity
Armenia

BACTERIA
Coliform, fecal
and total
Fecal streptococci

Biochemical oxygen demand
Biochemical oxygen
demand Carbonaceous
Bromide
Chemical oxygen
demand
Chloride
Chlorinated organic
compounds
Chlorine, total
residual
Color
Cyanide, total and
amenable to chlorination

Dissolved oxygen
Probe
Winkler
Fluoride
Hardness
Hydrogen ion (pH)
Kjeldahl and organic nitrogen

hETAIS6
Chromium VI
II. CCNBUNEPS, PRESETOATICN,
Container
P.G
P.G
P.G


P,G

P.G

P,G
R,G

P.G
P.G

P,G
G, teflon-lined
cap
P.G

P.G
P.G
P.G

G bottle I top
G bottle & top
P
P.G
P.G
P.G

P.G
Atd HOUMJG TIMES
Preservative
Cool, 4"C
Cool, 4°C
Cool, 4°C
H-9O. to pH<2

Cool, 4'C h
0.008% Ha^SjO,
Cool, 4°C .
0.008% MajSjOj
Cool, 4'C
Cool, 4°C

None required
Cool, 4*C
HjSO^ to pH<2
None Required
Cool, 4°C h
0.008% NajSjO,
Determined on-site

Cool, 4°C
Cool, 4°C
NaOH to PIM2,,
0.008% Na2S20^
Determine on site
Fix on site
None Required
HN03 to pH<2
Determine on site
Cool, 4°C
H-SO. to pH<2
Cool, 4°C

Maximum ,
Holding Time
14 days
14 days
28 days


6 hours

6 hours

48 hours
48 hours

28 days
28 days

28 days
7 days (until extraction)
30 days (after extraction)
2 hours

48 hours
14 days


1 hour
8 hours
28 days
6 months
2 hours
28 days

48 hours

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Federal Register / Vol. 44, No. 244 /  Tuesday, December 18, 1979  / Proposed Rules
75051
TABLE II. COtnWNERS, PRESERVATION, AMD BODING TIMES (cont.)
Measurement3 Container
58-59
24-87
88
88 (a)1
89
90
91
93-206
Mercury
Mstals
except above
Nitrate
Nitrate-nitrite
Nitrite
Oil and Grease
Organic Carbon
ORWNIC COMPOUNDSf
P,G
P,G
P,C
P,G
P.G
G
P.G

Extractables (including G, teflon-lined
phtha2at.es, nitrosamines cap
organochlorine pesticides,
PCB's, nitroaromatics,
isophorone, polynuclear aromatic
hydrocarbons, haloethers,
chlorijiated hydrocarbons and TCDD)



207
208
209
210
211
Extractables (phenols)
Purgeables (Halocarbons and
Aroma tics)
Purgeables (Acrolein and
Acrylonitrite)
Orthqphosphate
Pesticides
Phenols
Phosphorus (elemental)
Phos^.iorus, total
G, teflon-lined
cap
G, teflon-lined
septum
G, teflon-lined
septum
P,G
G, teflon-lined
cap
P,G
G
P,G
Preservative
HNOjto pH<2
0.05% K2Cr207
HNOj to pH-'2
Cool, 4°c
Cool, 4°C
Cool, 4°C
Cool, 4°C
H.SO. to pH'2
Cool, 4°C
H SO to pfl<-2
Cool, 4°C h
0.008% Na-^Oj
Cool, 4°C
HjSO .to pH<2
0.008% Na2S2Oj
Cool, 4°C .
0.008% NajS-jOj
Cool, 4°C .
0.008% Na2S20;J
Filter on site
Cool, 4»C
Cool, 4°C .
0.008% Na2S2Oj
Cool, 4°C
H S<^ to pli<2
Cool, 4"C
Cool, 4«C
Maximvn .
Holding Time
28 days
6 months
48 hours
28 dayg
48 hours
28 days
28 days
7 days (until
30 days (after
7 days (until
JO days (after
14 days
3 days
48 hours
7 days (until
30 days (after
28 days
48 hours
28 days





extraction)
extr-.i--j.on)
extraction)
extrai-t-ion)

extraction)
extraction)

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75052
Federal Register /  Vol. 44, No. 244 /  Tuesday, December 18,  1979  / Proposed Rules

TABLE
Measttreinent
212-216
217
218
219
220
221
73
222
223
224
225
226
227
228
RADIOUOGICAL
Alpha, Beta and radiiin
Residue, total
Residue, Filterable
Residue, nonfilterable
Residue, settleable
Residue, volatile
Silica
Specific conductance
Sulfate
Sulfide
Sulfibe
Surfactants
Temperature
Turbidity
11. CONTAINERS,
Container
P,G
P,G
P,G
P,G
P,G
P,G
P
P,G
P,G
P,G
P,G
P,G
P,G
P,G
PRESERVATION, AND HOU)IH3 TIMES (oont.)
Preservative
HNO3 to pH<2
Cool, 4°C
Cool, 4°C
Cool, 4°C
Cool, 4°C
Cool, 4°C
Cool, 4°C
Cool, 4°C
Cool, 4°C
Cool, 4°C
Zinc flcetate
Cool, 4°C
Cool, 4°c
Determine on site
Cool, 4°C

Maximum -,
Holding Time
6 months
14 days
14 days
7 days
7 days
7 days
28 days
28 days
28 days
28 days
48 hours
48 hours
imnediately
48 hours
a  Parameter numbers refer to Table I.
b  Polyethylene  (P) or Glaes (G).
c  Sample preservation should be performed immediately upon sample
   collection.  For composite samples each aliquot should be preserved
   at the time of collection.  When  use of an automatic  sampler makes
   impossible  to preserve each  aliquot, then samples may  be
   preserved by  maintaining at  4°C  until compositing and
   sample  splitting  is completed.
d  Samples  should be analyzed as soon as possible after collection.
   •n» times listed are the maximum tines that samples may be held
   before analysis and still considered valid.  Samples may be held
   for longer periods only if the  permittee, or monitoring laboratory,
   has data on file to show that the specific types of samples under
   study are stable for the longer time.

   Some samples may not be stable  for the maximum time period given in
   the table.  A permittee, or monitoring laboratory, is obligated to
   hold the sample for a shorter time if knowledge exists to show this
   is necessary  to maintain sample stability.

e  Samples should be filtered immediately en-site before adding preser-
   vative for dissolved metals.
f  Guidance applies to  samples to be analyzed by GC, 1C, or GC/MS for
   specific organic compounds.
g  This parameter not listed in Table I.
h  Should only be uaed  In the presence of residual chlorine,
i  Not available in Table  I.

BILLING CODE 15O5-01-C
                                                                                             i US GOVERNMENT PRINTING OFFICE 1981 -757-064/0214

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