United States
                   Environmental Protection
                   Agency
Environmental Monitoring and
Support Laboratory
Cincinnati OH 45268
                   Research and Development
EPA/600/S4-86/001 Jan. 1986
x°/EPA         Project  Summary
                   Evaluation  of  Methods  for
                   Hazardous  Chemicals  Listed  in
                   Appendix D  to 40  CFR  122
                   (Table V)
                   S. V. Lucas, M. Cooke, and T. F. Cole
                     This study involved method develop-
                   ment for several compounds that had
                   not been tested by existing U.S.  EPA
                   Methods: semivolatiles volatiles
                   (6 compounds), purgeables (3 com-
                   pounds), volatile amines (6 com-
                   pounds), and alcohol amines (2 com-
                   pounds). These compounds are on a list
                   of 75 organic compounds in Table V of
                   Appendix D to 40 CFR 122. Of those
                   75 compounds, 24 had not been tested
                   by an existing EPA method for analysis
                   in water and wastewater. The present
                   work reports on efforts to demonstrate
                   the analytical performance of 17 of
                   those 24 compounds plus an additional
                   five compounds not included in Table V
                   of Appendix D by applying existing 600-
                   series methods with appropriate modi-
                   fications. In each case, a test analyte set
                   for a given method/approach consisted
                   of essentially all of the Appendix D
                   Table V compounds belonging to that
                   compound class. The approach was to
                   demonstrate performance separately in
                   the  areas: (1) chromatography -using
                   fused silica capillary columns whenever
                   possible and including the evaluation of
                   cold, on-column injection whenever
                   necessary, (2) modified extraction  and
                   concentration techniques, and (3) mod-
                   ified cleanup techniques. In cases
                   where all of these areas gave appropri-
                   ate  results, an integrated method was
                   tested  for accuracy and precision.
                     For the semivolatile compounds (6 of
                   the  17), two compounds (benzonitrile
                   and quinoline) gave excellent recovery
                   and precision through extraction  and
                   cleanup, three other compounds  (ke-
pone, strychnine and dichlone) gave 50
to 80 percent recovery, and one com-
pound (trichlorfon) was not stable in
aqueous systems at neutral pH.
  For the purgeable compounds (3 of
17), one analyte (propylene oxide) gave
marginally acceptable precision results,
with the observed deficiency appar-
ently due to hydrolysis  during  the
purge-and-trap desorption step.  The
other two analytes gave unacceptable
results but for different reasons: ally!
alcohol was purged with efficiency only
15 percent at 85°C and also gave unac-
ceptable GC peak tailing, resulting in a
relatively high estimated detection
limit of 70 |ig/L. Although methyl mer-
captan also exhibited some tendency
toward decomposition on the trap, the
principal difficulty is its elution early in
the chromatogram where baseline dis-
turbances and methanol elution occur.
A "Hall detector" in the sulfur detection
mode is recommended for analysis of
methyl mercaptan by the room temper-
ature purge-trap-desorb approach.
  For the volatile amines (6 of the 17), a
special GC packing material was pre-
pared and demonstrated to be effec-
tive. However, all  efforts to develop a
purge-trap-desorb sample workup pro-
cedure were unsuccessful. For the alco-
hol amines (2 of the 17), none of the gas
chromatography approaches tried pro-
vided performance adequate to justify
further method development.

  This Project Summary  was devel-
oped by EPA's Environmental Monitor-
ing and Support Laboratory, Cincinnati,

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OH, to announce key findings of the re-
search project that is fully documented
in a separate report of the same title
(see Project Report ordering informa-
tion at back).

Introduction
  The objective of this research was to
evaluate  analytical methods for  haz-
ardous chemicals listed in Appendix D
to 40 CFR 122 (Table V). This listing con-
tains 75 organic chemicals that must be
analyzed if they are expected to be
present in existing discharges. Stand-
ard analytical methods have been de-
veloped and validated  by the EPA for
most  of these 75 Appendix  D/Table V
compounds. The 24 untested com-
pounds are listed in Table 1. Seven of
these  24 untested compounds were of
chemical  classes that were beyond the
scope of this work, and, therefore they
were eliminated by the Project Officer
from method evaluation. Thus, the work
reported here focused on  17 of the
untested compounds thought to be
amenable to gas chromatography (GC).
A major objective of this work was to
provide a minimum number of methods
to cover  a  maximum number of Ap-
pendix D/Table V compounds. This
would minimize the effort required by
the analyst. Accordingly,  the  Ap-
pendix D/Table  V chemicals  were di-
vided  into six chemical classes, each of
which contained at  least one of the
untested  compounds. These  chemical
classes were:  organophosphorous
compounds, neutral nitrogen com-
pounds,  chlorinated pesticides, ex-
tractable semivolatile bases, volatile
compounds, volatile  amines, and alco-
hol amines. The chemical class of each
untested compound is  identified in
Table 1.  In this work, methods  were
evaluated for all or nearly all  of the Ap-
pendix D/Table V compounds of each
class to ensure  that  method modifica-
tions which enhanced performance for
a high-interest analyte did not detract
from the method performance already
in place for the other compounds in the
class. In addition, the volatile  com-
pounds class was augmented by an ad-
ditional five compounds which were not
in the Appendix D/Table V listing but
were of interest to the EPA Project Offi-
cer. These  compounds were acetone,
methyl ethyl ketone, methyl isobutyl ke-
tone, methyl butyl ketone, and dioxane.
This report addresses a total of 22 com-
pounds which are  broadly  sub-
classified into three  sets: semivolatile
(extractable) compounds, volatile
(purgeable) compounds, and amines
(including alcohol amines).

Experimental Design
  The experimental design for each of
the three compound classes incorpo-
rated independent evaluation of four as-
pects  of a method: chromatographic
separation, injection conditions, sample
workup, and cleanup procedures.  A
main  feature of the chromatographic
separation evaluation for semivolatile
compounds was to test both polar and
nonpolar fused silica capillary columns.
Injection  conditions tested for the
semivolatile group were evaporator
cavity (split/splitless) injection  at vari-
ous temperatures for all compound sets
and cold,  on-column  injection for se-
lected compound sets. Sample workup
for semivolatile compounds involved
liquid-liquid extraction and extract con-
centration, while cleanup procedures
emphasized Florisil column techniques
using  solvent systems already in use in
EPA cleanup methods. When reason-
able results were  obtained in each of
these  areas, the precision and accuracy
of the integrated method was tested.
  The purge-and-trap analysis condi-
tions were essentially those of Method
5030  employing  room temperature
purging with the three-component trap
(Tenax, silica gel and activated carbon)
for nonpolar compounds  and  85°C
purging with the all-Tenax trap for polar
compounds. Three GC column packings
were  tested Porapak-QS, 10 percent
Carbowax 20M on Supelcoport, and
1 percent SP1000 on Carbopack B, and
the latter one was selected for the re-
covery and precision studies. Reagent
water  was used as the matrix in all spike
recovery experiments, and  a Tekmar
LSC-2 purge-and-trap apparatus  was
used to generate the data.
  Studies with the amine analyte set
were restricted to the establishment of
an adequate column packing material,
feasibility studies on the purge-and-trap
sample processing  approach, and an in-
vestigation of the applicability of  auto-
mated heated headspace sampling with
capillary chromatography using  a
Perkin-Elmer HS-100  automated
headspace sampling unit.

Results and Discussion

Organophosphorous  Com-
pounds
  Trichlorfon is the only  organophos-
phorous compound listed in Table 1.
Appendix D to 40 CFR 122 (Table V) con-
tains an additional 11 organophospho-
rous  compounds: chlorpyriphos,
coumaphos, diazinon,  disulfoton,
ethion, guthion, malathion, methyl
parathion, mevinphos,  naled, and
parathion. GC studies with all 12 com-
pounds showed that trichlorfon was es-
sentially quantitatively decomposed
upon splitless, evaporator cavity injec-
tion above 250°C. In addition, mevin-
phos  decomposed significantly and
naled decomposed slightly under those
injection conditions. Therefore, cold on-
column injection was used for all subse-
quent work. Studies using separatory
funnel  shakeout,  reverse phase extrac-
tion, and KD concentration with the two
most  labile compounds (mevinphos
and trichlorfon) showed that trichlorfon
decomposed, essentially quantitatively,
in pH 7-buffered reagent water, but that
it survived KD concentration in a variety
of solvents. Once it was shown that the
only Table 1 organophosphorous com-
pound, trichlorfon, was not stable  in
water, experimental work on the re-
maining  11 compounds  was termi-
nated.

Neutral Nitrogen Compounds
  Of 13 neutral nitrogen compounds on
the Table V list of Appendix D 40 CFR
122, benzonitrile was the only untested
(Table  1) compound. The other 12 com-
pounds are: diuron, dichlobenil, carbo-
furan,  mexacarbate, carbaryl, methio-
carb,  and all  isomers  of  nitrotoluene
and dinitrobenzene. The chromato-
graphic performance  of  all  13  com-
pounds was tested using 30 meter SPB-
5 and Carbowax  20M fused silica
capillary columns. The high polarity and
high molecular weight pesticides failed
to elute from the Carbowax 20M
column.  Subsequent  work with the
SPB-5  column using  GC-MS demon-
strated that diuron decomposed quanti-
tatively in the evaporator cavity injector
at temperatures between 250 and
300°C, and that carbofuran, mexacar-
bate, carbaryl and methiocarb partially
decomposed (up to 50 percent at 300°C)
over that range. Since the untested
compound benzonitrile performed well
under these injection conditions, testing
with cold, on-column injection was not
conducted. The extraction  efficiency of
benzonitrile from reagent water aver-
aged 103 ±8 percent using methylene
chloride.  Extraction efficiencies for the
other  12  compounds  were not tested
since they are all listed in  current EPA
methods. A Florisil column cleanup pro-
cedure was evaluated for all  com-

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 pounds except  diuron. Nitrotoluenes
 were recovered in the 20 percent diethyl
 ether in  hexane elution fraction (frac-
 tion 1). Carbofuran and carbaryl were
 recovered in the 15 percent acetone in
 hexane fraction  (fraction 3). The other
 compounds were recovered in  the
 6 percent acetone in hexane fraction
 (fraction  2). Recoveries of all com-
 pounds were 79 percent or greater ex-
 cept for mexacarbate and methiocarb.
 They were recovered at about 35 per-
 cent. Four replicate analyses of reagent
 water spiked at the 25 (tg/L level with
 the  12 compounds (diuron omitted)
 were carried through the extraction,
 concentration, and cleanup sequence.
 They were analyzed using a  nitrogen
 specific detector to generate accuracy
 and precision data. The results showed
 recoveries between 72 and 80 percent
 with relative standard deviation (BSD)
 values between  10 and 15 percent for
 benzonitrile, and three nitrotoluenes, di-
 clobenil and 1,2-dinitrobenzene. The re-
 coveries for 1,3-dinitrobenzene and 1,4-
 dinitrobenzene were 72 ± 23  and
 64 ± 12 percent, respectively. The re-
 covery and precision data obtained for
 carbofuran,  mexacarbate, carbaryl and
 methiocarb  were 120 ± 17, 98 ± 25,
 144 ±20  and 10 ± 7, respectively.  Un-
 doubtedly, the observed splitless injec-
 tion decomposition for these four pesti-
 cides accounts for a large measure of
 the variability in these results. The low
 (10 percent) recovery of methiocarb
 could not be attributed to a specific
 cause.
  In summary, benzonitrile can be de-
 termined using methylene chloride ex-
 traction,  Florisil  column cleanup, and
 fused silica, capillary column GC analy-
 sis with nitrogen-specific detection. The
 overall recoveries  obtained for the ni-
 trotoluenes, dinitrobenzenes  and
 dichlobenil were  generally acceptable
 at 70 to 80 percent, but somewhat er-
 ratic results for  carbofuran, mexacar-
 bate, carbaryl and methiocarb prevent
 making any definitive method perform-
ance conclusions on those four com-
pounds.

Chlorinated Pesticides
  The two untested Table 1 compounds
in this group were diclone and kepone.
Methoxychlor and captan, which  are
also in Table V of Appendix D/40 CFR
 122, were also included in the study. Of
the four compounds,  only  diclone
eluted from  the  Carbowax 20M fused
silica capillary column. Excellent chro-
matographic performance was ob-
 Table 1.    Untested Compounds from Table V of Appendix D to 40 CFR 722
       Compound
                 Chemical Class
Allyl alcohol
Bemonitrile
Butylamine
Dichlone
2,2-Dichloropropionic acid
Diethylamine
Diquat
Ethanolamine
Isopropanolamine
Kepone
Methyl mercaptan
Ethylamine
Methylamine
Naphthenic acid
Phenol sulfonate
Phosgene
Propargite
Propylene oxide
Pyrethrins
Quinoline
Strychnine
Trichlorfon
Trimethylamine
Triethylamine
          Volatile compound
          Neutral nitrogen compound
          Amine
          Chlorinated pesticide
          (Eliminated)
          Amine
          lEIiminated)
          Amine
          Amine
          Chlorinated pesticide
          Volatile compound
          Amine
          Amine
          (Eliminated)
          (Eliminated)
          (Eliminated)
          (Eliminated)
          Volatile compound
          (Eliminated)
          Extractable semivolatile base
          Extractable semivolatile base
          Organophosphorous compound
          Amine
          Amine
 tained for all four compounds using the
 SPB-5 nonpolar  fused silica capillary
 column. Captan, however, apparently
 decomposed in the 300°C evaporator
 cavity, splitless injector. Since captan
 was not a high-priority. Table 1 analyte,
 and since this partial decomposition did
 not seem to have any effect on analysis
 precision, cold,  on-column  injection
 was not tested for this analyte set.
  Neutral  pH extraction of aqueous
 spiked samples with methylene  chlo-
 ride was shown to  be an effective ex-
 traction approach with recovery rang-
 ing from 76 to 92 percent and precision
 ranging from 7 to 12% BSD. The elution
 scheme using Florisil column cleanup
 was modified by the addition of 100 per-
 cent ethyl ether and 6 percent acetone
 in ethyl ether elutions to provide recov-
 eries of the four analytes.
  The integrated method including
 methylene chloride  extraction, KD con-
 centration, Florisil column cleanup and
 GC-ECD analysis using  a nonpolar
fused silica capillary column was tested
with four 1-L reagent water replicates
spiked with 25  \t.g of each of the four
analytes. All applicable Florisil column
eluates were pooled  before  analysis.
The average percent recoveries, and
standard deviations obtained were di-
clone,  48 ± 7 percent,  captan 71  ± 13
percent,  kepone  74 ± 5 percent, and
methoxychlor 92 ± 7 percent. The  poor
recovery for diclone is probably due to
losses at the Florisil column cleanup
step and/or KD  distillation of  the ethyl
ether-containing Florisil elution solvent.
Except for dichlone, which is an
untested Table 1 compound,  analysis
method  performance for the chlori-
nated  pesticides was judged accept-
able.

Extractable Semivolatile  Bases
  This group of three compounds con-
sisted  of two high-interest compounds
from Table 1 (quinoline and strychnine)
plus aniline.  Since  strychnine did not
elute from the polar, Carbowax 20M
column the SPB-5 (Supelco) nonpolar
fused silica capillary column was  used
for all  of the studies performed on this
group. Aqueous extraction studies with
methylene chloride at both neutral and
basic pH, both with and without acidic
pre-extraction and/or salting out
(sodium chloride at 200 g/L), gave quan-
titative recovery of aniline and quino-
line but only 46 to 58 percent recovery
of strychnine. Extraction using  two sol-
vent systems, 15 percent hexane  in
methylene chloride, and methyl t-butyl
ether,  gave similar  results except that
the strychnine recoveries were 38 and
10 percent, respectively. A check of the
KD concentration procedure indicated
that for methylene  chloride, the  poor
strychnine extraction recovery  was
probably due  to losses at that stage.
Similar results were obtained for diethyl
ether,  but essentially quantitative KD
concentration  recovery  was obtained
for strychnine with methyl t-butyl ether
solvent. Quantitative recovery  through

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the K-D step was also obtained for ani-
line and quinoline with both solvents.
Since suitable  extraction conditions
could not  be identified for strychnine,
further work to test cleanup procedures
and an integrated method for the  ex-
tractable semivolatile bases was  not
conducted.

Volatile Compounds
  Of 17 volatile compounds tested, only
three  are  high-interest. Table 1 com-
pounds: methyl mercaptan, propylene
oxide and  allyl alcohol. Fourteen other
compounds  were  included  in the
volatile set. Of  those  14  compounds,
9 compounds were from Table V of Ap-
pendix D 40 CFR 122, and 6 compounds
were specified by EPA. This  17-
compound analyte set was divided into
polar  and  nonpolar sets for which an
85°C and ambient temperature, respec-
tively, purge-trap-desorb approach was
employed. These analyte  sets are
shown in Table 2. The traps used were
those of Methods 8030 (85°C purge) and
8010 (ambient temperature purge) with
the purge-trap-desorb conditions as
specified in Method  5030. A Tekmar
LSC-2 liquid sample concentrator inter-
faced  to a  GC with flame ionization  de-
tector was used for all sample analyses.
  Three GC column  packings were
tested in this work: Porapak OS, 10 per-
cent Carbowax 20M on Supelcoport 80/
100, and 1 percent SP1000 on Carbo-
pack B 60/80. The latter packing, in a
6 foot, 2 mm I.D. glass column, pro-
vided the  best  performance for all
analytes and was used to produce  the
data reported here. Neither of the other
two columns performed adequately for
recommendation as a backup column in
these analyses.
  The most volatile analytes  were
checked for trap breakthrough. As ex-
pected, none of the nonpolar analyte
broke through the Method 8010 trap at
less than 1600 mL purge volume. For
the polar analytes, only acetone and
propylene oxide, with  breakthrough
volumes of 560  and 400 ml, respec-
tively, for 1.0 |xg trap loadings, ap-
proached the 300 ml purge volume of
Method 5030.
  Purging  and desorption efficiencies
were separately determined.  For the
nonpolar analytes, all but methyl  mer-
captan and propylene oxide were quan-
titatively purged  and desorbed. Propy-
lene oxide purged with only about
25 percent efficiency, and about two
thirds of the purged amount apparently
decomposed during desorption giving
an overall recovery of 9 percent. For
methyl  mercaptan, 70 percent  purging
efficiency was found, but a 50 percent
loss on desorption gave a 35 percent
overall recovery. For the polar analytes,
only the ketones approached quantita-
tive purge/desorb recoveries (87 to 100
percent). Lower overall  recoveries for
the acetates was entirely attributable to
desorption losses of 50, 20 and 35 per-
cent for the  vinyl, butyl  and amyl ac-
etates, respectively. Epichlorohydrin
was also found to purge essentially
quantitatively but experienced about
80 percent loss on desorption. The two
remaining analytes, allyl alcohol and
dioxane, were  desorbed with about
90 percent recovery but  were purged
with only about 15 percent efficiency.
  Replicate analyses of low-level spiked
reagent water samples were performed
to estimate the  detection limits for all
analytes except methyl mercaptan, and
the results are shown in Table 2. Some
Table 2.    Estimated Detection Limits for Volatile Analyte Sets
Polar Compounds
(85°C Purge)
allyl alcohol1*'
propylene oxide1*1
epichlorohydrin
vinyl acetate
butyl acetate
amyl acetate
acetonelc>
methyl ethyl ketonelc>
methyl isobutyl ketone<0>
methyl butyl ketonelc>
dioxanelcl
Estimated
Detection
Limit,
W/L
70
5
10
2
1
2
4
0.3
0.3
0.6
10
Nonpolar Compounds
(Room Temperature Purge)
methyl mercaptanla>
propylene oxide1"1
allyl chloride
isoprene
cyclohexane
o-xylene
ethyl etherA high-interest. Table 1 compound. Note that propylene oxide is included in both analyte
  sets.
"''Not determined, see discussion in text.
M Compound not listed in Table V of Appendix D to 40 CFR 122.

                                  4
analytical problems were encountered
with all three of the high-interest ana-
lytes, propylene oxide, methyl mercap-
tan and allyl alcohol. Propylene oxide
can be analyzed by either the room tem-
perature or 85°C purge-and-trap ap-
proach. However, the propylene oxide
data clearly indicate that this compound
partially decomposes during  trap de-
sorption, and the result is that variable
precision and  accuracy might be ex-
pected  without further  method im-
provements. Indeed, most of the prob-
lems  associated  with  the
purge-and-trap analyte sets were
shown  to be associated  with decompo-
sition,  probably by hydrolysis, during
trap desorption. Two additional prob-
lems were encountered  with methyl
mercaptan: (1) FID  sensitivity was low,
as expected, and (2) near coelution with
methanol,  significantly  reduced its re-
producibility. Both  of these problems
could  be  eliminated with a sulfur-
specific detector. In the case of allyl
alcohol, the estimated detection limit of
70 n-g/L was due partially to the very low
purging efficiency (about 15 percent) at
85°C but primarily  to the extreme GC
peak tailing on the 1 percent  SP1000/
Carbopack B column.

Volatile Amines and Alcohol
Amines
  Five of the six amines tested are high-
interest, Table  1 compounds: trimethy-
lamine, ethylamine, diethylamine, tri-
ethylamine, and butylamine. The  sixth
amine in the set was methylamine. The
two alcohol  amines tested were
ethanolamine  and  isopropanolamine,
also high-interest. Table 1 compounds.
  Chromatographic characteristics of
the amines were  investigated using
commercially available fused silica cap-
illary columns, Carbowax 20M and DB-
5, and  column packings, Porapak QS
and 1 percent SPIOOO/Carbopack B, plus
a custom-made packing based on Car-
bopack B treated with KOH (0.3 percent)
and  then coated with 4.8 percent Car-
bowax 20M. The later column was the
only one which gave adequate perform-
ance for all six amines.
  Volatile amine sample workup stud-
ies were limited to feasibility investiga-
tions of purge-and-trap-based and
heated headspace sampling  ap-
proaches. None of the three traps tested
performed adequately. The  Method
8010 trap and an activated carbon trap
prevented breakthrough but gave poor
or  no  desorption recoveries. The
Method 8030 trap gave good desorption

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 recoveries but exhibited breakthrough
 for methylamine, ethylamine,  and
 trimethylamine. Since an adequate trap
 was not available, purging efficiency
 studies were not performed. Automated
 heated headspace sampling performed
 well for tertiary amines but very poorly
 for primary amines, apparently due to
 adsorptive problems with metallic com-
 ponents of the autosampler. For the al-
 cohol amines, none of the chromato-
 graphic approaches  tested gave
 adequate chromatographic perform-
 ance, and, without a determinative tech-
 nique for these compounds, no further
 work was possible.

 Conclusions and Recommenda-
 tions
  The  low  method development  suc-
 cess rate for the 17 untested, Table 1
 compounds tested reflects the multi-
 plicity  of their chemical  characteristics
 which  prevent analysis using ordinary
 approaches. Only six of the 17 untested
 Table  1 compounds  (benzonitrile,
 quinoline, kepone, strychnine, dichlone
 and propylene oxide) gave acceptable
 or marginally acceptable results.  One
 compound, trichlorfon,  is not stable in
 water,  and no further method develop-
 ment work for aqueous matrices should
 be pursued. Further method develop-
 ment for methyl mercaptan should in-
 clude a purge-and-trap approach with
 Hall electrolytic  conductivity/sulfur
 mode detection. If the chromatographic
 tailing problem can be solved, ally! alco-
 hol may be effectively analyzed with an
 85°C purge-and-trap approach even
though it has only a 15 percent purging
 efficiency. In general, loss of labile ana-
 lytes during  trap desorption is a prob-
 lem that should be addressed to  im-
 prove the performance of many of the
volatile analytes. Although good chro-
 matography was achieved  for  the
volatile amines, the method currently is
 limited to direct aqueous injection.  Fur-
ther work on the six volatile amines
should include pre-analysis concentra-
tion method development and investi-
gation  of alternate  determinative tech-
niques such as ion chromatography,
especially for the alcohol amines (2 of
the 17 high-interest compounds).
S. V. Lucas. M. Cooke, and T. F. Cole are with Battelle Laboratories, Columbus
  Division. Columbus. OH 43201 -2693.
James Longbottom is the EPA Project Officer (see below).
The complete report, entitled "Evaluation of Methods for Hazardous Chemicals
  Listed in Appendix D to 40 CFR 122 (Table V)," (Order No. PB 86-136 520/A S;
  Cost: $16.95, subject to change) will be available only from:
       National Technical Information Service
       5285 Port Royal Road
       Springfield, VA22161
       Telephone: 703-487-4650
The EPA Project Officer can be contacted at:
       Environmental Monitoring and Support Laboratory
       U.S. Environmental Protection Agency
       Cincinnati, OH 45268
                                                                             U. S. GOVERNMENT PRINTING OFFICE:1986/646-l 16/20758

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Agency
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Information
Cincinnati OH 45268
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