United States
Environmental Protection
Agency
Environmental Monitoring Systems
Laboratory
Las Vegas NV 89114
Research and Development
EPA-600/S4-81-027 Aug. 1981
Project Summary
Evaluation  of the
Procedures for  Identification
of  Hazardous Wastes:
Part  1.  Sampling, Extraction, and
Inorganic Analytical  Procedures
L. R. Williams, E. P. Meier, T. A. Hinners, E. A. Yfantis, W. F. Beckert, and
T. E. Gran
  A study was performed to evaluate
the sampling, extraction, and analytical
procedures (inorganic) proposed in
the RCRA regulations for identifying
wastes as  hazardous by the toxicity
characteristic. Twenty-seven different
wastes were sampled and analyzed in
accordance with the RCRA regulations.
The high degree of heterogeneity
found in many wastes underscores the
need for a carefully designed sampling
protocol to reproducibly obtain repre-
sentative samples from each waste
source. A protocol was developed and
tested for obtaining composite samples
from waste ponds or lagoons. Sam-
plers tested, the pond sampler and the
COLIWASA (composite liquid waste
sampler), were found to be acceptable
for sampling hazardous waste, when
used  in a well-designed  sampling
protocol. Reliability and reproducibility
of the EP (extraction procedure) were
evaluated (RSD <15%). The blade-
type rotary extractor (as cited in the
proposed regulations), a tumbling-
type extractor, and a wrist-arm-type
shaker were compared and found to
yield similar EP extracts. The support-
ing analytical methods (atomic absorp-
tion spectrometry) were found to be
highly reproducible for Cr and Pb. and
somewhat less for Ba (RSDs <3.1%;
4.6%; and 16.4%, respectively). Inde-
pendent analyses of the same waste
extracts by two laboratories were
highly reproducible, i.e., the variance
from analyses was negligible. How-
ever, differences in the EP extracts
produced by the two laboratories
show the need for a detailed and
concise protocol for conducting the
EP. Problems with sample contamina-
tion from the blade-type extractor
(chromium) and the filtration apparatus
(barium) were identified.
  This Project Summary was devel-
oped by EPA's Environmental Moni-
toring Systems Laboratory, Las Vegas,
NV. to announce key findings of the
research project that is fully docu-
mented in a separate report of the
same title (see Project Report ordering
information at back).

Introduction
  The rapid  technological advances
over the past several decades have
significantly improved the American
economy and lifestyle. However, im-
proper disposal of hazardous wastes
generated by industry as a result of
these advances has created a hazard to
both human health and the environ-

-------
ment. The identification of those wastes
and wastestreams which require special
management because of their present
or potential hazard is a high priority of
regional, state, and federal interests.
  Background of the study. This study
was conducted in support of the EPA's
Office of Solid Waste (OSW). The results
are to be used by OSW to better define
the reliability and reproducibility of
sampling, extraction, and analytical
procedures in regulations proposed (FR
Dec. 18, 1978) and published (FR  May
19, 1980) under Section 3001 of the
Resource Conservation and Recovery
Act (RCRA) of 1976 (and its  amend-
ments).
  The problem.  Previous studies (in
some cases with wastes of unknown
history) have demonstrated the utility
and validity of the proposed methods.
However, the EPA felt that additional
studies (with wastes from known in-
dustrial sources) were warranted to
confirm that valid and defensible data to
support the regulatory requirements
can be provided using these methods.
  Purposes of the study. The purposes
of the study were to 1) evaluate the
reproducibility of the sampling and
extraction procedures and the accuracy
and precision of the analytical proce-
dures described in the proposed regula-
tions; 2) compare candidate extractor
types for use with the proposed extrac-
tion procedure; and 3)evaluate the
application of the proposed extraction
procedure (and  associated analytical
procedures) to municipal sewage sludge
samples. In addition, special studies
were performed to identify sources of
specific  problems (i.e., barium and
chromium contamination  of  extracts
from extraction and filtration apparatus;
high variability in flame atomic absorp-
tion analyses for barium; low  mercury
levels in extracts of samples known to
be high in mercury;  and low analytical
recoveries for  certain metals  in some
extract  media). Interim findings  from
these studies were submitted to OSW
and are reflected in the methods pub-
lished  in SW-846, "Test Methods for
Evaluating Solid Waste -  Physical/
Chemical Methods" (1980).

Procedure
   Theoretical assumptions underlying
the study. The extraction procedure
(EP) is intended to identify the potential
for migration—from waste to the  envi-
ronment—of toxic constituents in an
improperly managed waste.  For pur-
poses of regulation, a waste may be
considered hazardous, by the toxicity
characteristic, if levels of specific toxic
chemicals, in EP extracts of that waste,
meet or exceed the stated limits. To test
the procedures associated with the EP,
test materials (waste samples) should
be selected that are representative of
the most difficult waste types to sample,
extract and analyze. In this way, con-
servative estimates of the precision and
accuracy of the procedures can be
developed.

  Selection and sampling of wastes.
Waste and sites to be sampled were
selected with the  active  assistance of
industrial and government facilities that
generate or dispose  of a variety of
hazardous and non-hazardous wastes.
Eleven sites were visited and 27 dif-
ferent wastes were collected, by a
variety of sampling methods, from pits,
ponds, drums, tank trucks, waste piles,
dumpsters, and process stream taps.
Samples were shipped to the Laboratory
under chain-of-custody and in conform-
ance with Department of Transportation
regulations.

  Procedures for evaluating samplers.
The pond sampler and COLIWASA
(composite liquid waste sampler), used
in accordance with published protocols
(deVera et al., EPA-600/2-80-018,
1980), were the only sampling methods
evaluated. The initial experimental
design for testing  the pond sampler (a
one-sided parametric test)  called for
collection  of 39  samples per pond.
Subsequently, the design was modified
to a hierarchical (nested) analysis of
variance (ANOVA) to define  the major
sources of sampling and analytical
variability. Samples were collected with
the pond sampler from five different
waste sources at two sites. Uniformity
of samples with respect to pH and per-
cent solids (Non-filterable Residue
Method 160.2, "Methods for  Chemical
Analysis of Water and Wastes", EPA
1979) was used to estimate  the repro-
ducibility of the sampling procedure.
Wet weights of sample solids—routinely
measured in the EP to determine whether
a minimum percent solids level is ex-
ceeded—were not considered precise
enough to use in  determining sample
uniformity. A sampling plan was devel-
oped for collecting composites of random
samples from accessible areas and was
tested on Ponds 0 and 12.
  The COLIWASA was used to sample
five different drummed wastes at three
sites. Uniformity of the samples with
respect to percent solids and to the oil/
water ratio (for biphasic wastes) wad
used to estimate sampling reproduci-
bility.
  Procedure for evaluating the EP. The
EP was used in essential agreement
with the proposed  regulations. Waste
samples from three different ponds
were used in initial tests of the EP with
blade-type extractors. The resulting
extracts were then analyzed by atomic
absorption spec'troscopy methods to
determine how uniform the extracts
were with respect to selected metals.
  A hierarchical testing design was
used to compare the blade-type extrac-
tor, a tumbling-type extractor, and a
laboratory wrist-arm shaker. The test
yielded 108 separate EP extracts from
each of three waste sample types. Each
extract was analyzed for barium, chro-
mium, and lead. The data were subjected
to analysis of variance to determine the
sampling, extraction, and analytical
variability with each waste type.
  Procedure for evaluating analytical
methods. The atomic absorption spec-
troscopy (AAS) methods evaluated are
standard methods (EPA 1979) for anal-
ysis of water, wastewater, or industrial
effluents. However, they had not previ-
ously undergone extensive testing with.
solid wastes or their extracts.        I
  Extracts of the various types of sam-
ples collected were first screened using
ICP (inductively coupled plasma emis-
sion spectroscopy) methods for  a quick
and "semi-quantitative" look at the
metals of interest  contained in each.
Next, selected extracts—with and with-
out "spikes" of metals in known con-
centration—were analyzed by  AAS
methods. Recovery (an indicator of
accuracy) and reproducibility (precision)
were determined  from the data for
arsenic, barium, cadmium, chromium,
lead, mercury, selenium, and silver.
Recovery of known concentrations of
metals from acetate buffer and  from
selected waste extracts was compared
with that from "standards" in nitric acid
using linear regression analysis.
  When the standard deviations for
analyses of percent solids and for mean
percent solids content by locations
(based  on these analyses) were com-
pared, imprecision of the analyses was
found to account for a large portion of
the location-to-location differences
noted.  It is difficult to obtain uniform
weights among waste samples dried
under similar conditions, and small
weight differences  contributed  heavily
to the  variability  among  low-solidS|
samples.                          m

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   Analysis of variance of Pond 0 solids
rdata revealed significant differences (at
 the 5% level) between successive sam-
 ples at the same location, while dif-
 ferences between locations were not
 significant. Pond 13 percent solids data
 also showed significant differences
 between  successive samples,  but sig-
 nificant differences were detected be-
 tween locations (by analyses of both pH
 and percent solids data). The location-
 to-location differences noted indicate
 the highly heterogeneous nature  of
 Pond 13.
   When the mean values for each field
 sample were treated as single results,
 the average percent solids for Pond 0
 and 13 were 1.45 ± 0.27 (n=8) and 4.47
 ± 1.38(n=10), respectively. The average
 pH for Pond 13 was 5.31 ±1.85(n=10).
 Even with very heterogeneous wastes,
 the pond samples were reproducible
 (within ±35%) by either pH or percent
 solids analyses. The largest overall
 source of variability appears to be be-
 tween locations on the ponds.
   If the two samples collected at each
 location on Ponds 0 and 13 are treated
 as independent samples, two duplicate
 sets of data can be identified for each
L pond (i.e., set of first samples vs. set of
'second samples). The average values
 (pH and percent solids) for each set of
 data then provide mathematical com-
 posites of the samples for that set.
 Comparison of these average values
 demonstrates the high degree of overall
 reproducibility for the pond sampler.
 Average  relative  standard deviations
 (RSDs) were 1.1 % and 2.3% respectively,
 by pH and percent solids.
   Analyses (for percent solids) of 216
 aliquots [9 aliquots from  each  12 one-
 gallon composite samples, from each of
 2 ponds (Ponds 0 and 12)] indicate that
 sample-to-sample variability remains
 the greatest source of error in waste
 analysis. The cumulative  RSD for Pond
 12 composite samples (20.3%) is lower
 than previously  noted with discreet
 pond sample  comparisons. However,
 Pond 0 was found to be more heteroge-
 neous (RSD of composite samples =
 53.3%) than when it had been sampled
 five months previously.
   Reproducibility of triplicate samples
 collected with the COLIWASA from
 each of 15 drums of API separator waste
 (as measured  by average percent total
 solids) was very good (RSD = 1.1 %). In a
 more rigorous test of the COLIWASA's
 ability to handle complex waste mixtures,
 an oil/water biphasic waste was sam-
Table 1.    Average Means, Standard Deviations, and RSDs for AAS Analyses*
           of EP Extracts of Wastes from Ponds 0 and P
Barium (mg/l)
Sample Extracted x
PondO
PondP
2A
2B
2A
2B
1.65
1.34
29.9
27.8
s
0.17
0.05
4.9
3.7
RSD
10.3
3.7
16.4
13.3
Chromium (mg/l) Lead (mg/l)
X
1040
943
77.6
82.5
s
17
21
2.4
2.0
RSD
\ /Of X S
i.
2.
3.
2.
6 45.7 0.5
2 43.5 2.0
1 — ' —
4 — —
RSD
1.1
4.6
—
*Flame atomic absorption spectrophotometric analyses performed in triplicate on
 each of three aliquots of sample extracts.
 RSD = Relative Standard Deviation
Table 2,    Relative Standard Deviations (RSD) of Extractions and Analyses for
           Selected Metals
          Analysis          	
 (Sample source: Ponds 0 andP)    Barium
                                               RSD (%)
       Chromium
Lead
 Differences between replicate
  determinations on a given
  EP extract                       14.9

 Differences between replicate
  extractions on a given sample
  of waste                         11.0
          1.3
          1.8
 2.0
 3.0
pled. The high reproducibility of triplicate
samples  from each of three drums
(average RSD = 12.2%) allowed detection
of significant drum-to-drum differences
in oil/water ratio.

  Extraction procedure (EP). Data in
Tables 1 and  2  indicate the level of
extraction reproducibility observed with
waste samples from Ponds 0 and P. The
high reproducibility  of replicate extrac-
tions, with chromium and lead concen-
trations as indicators, closely approaches
the analytical precision for these metals.
Problems with barium contamination
from  prefilters and flame disturbances
in the AAS analysis for barium—both of
which were subsequently identified and
largely resolved—resulted in lower
precision of estimates based  on  this
element.
  Intralaboratory  reproducibility of  the
EP with  seven sewage sludges was
rather good (RSD = 33% for average
combined extraction and analytical
reproducibility) considering the hetero-
geneous nature of such samples. Inde-
pendent extraction of sludge samples
and  analysis of extract splits by the
Municipal  Environmental  Research
Laboratory, Cincinnati, yielded excellent
agreement on extract analyses but
revealed procedural differences in the
conduct of the EP.
  A  study was performed which  com-
pared the blade-type extractor with a
tumbling-action extractor and a wrist-
arm  shaker using Pond 0, Pond 12, and
biosolids samples. The average concen-
trations and standard deviations for
each of three metals analyzed from the
resulting EP extracts are shown in Table
3. The Student-Newman-Keuls multiple
comparison test did not demonstrate
one  extraction technique to be "better"
than another. The relative percent of
total variance contributed by sample
(63%),  aliquots (20%), extraction tech-
niques  (10%) and analyses (7%) was
estimated.
  The similar performance of the three
extractors is perhaps best summarized
by comparing the RSDs for each extrac-
tor (overall RSD including the variability
components associated with sampling,
aliquoting and analysis):

-------
                                     Overall RDS (as percent}
    Extractor

Blade-type (rotary)
NBS tumbling-type
Wrist-arm shaker
Pond 0

 10.8
 10.0
 12.3
  Some of the  EP extracts, especially
those with high concentrations of in-
organic and organic materials, formed
precipitates over a period of several
days. Even acidification to pH <2 was
not sufficient to totally prevent pre-
cipitation in the most concentrated
samples.  Prompt analysis is recom-
mended to minimize this problem.
  Low-level  chromium and barium
contamination  was detected in 0.1N
acetic acid blanks run through the EP
apparatus (filters and blade-type ex-
tractor) following extraction of a waste
sample and routine cleaning. Chromium
levels in the blanks generally paralleled
those in the preceding sample. A more
rigorous post-extraction cleanup proce-
dure was  adopted and distilled water
blanks were replaced by acidic blanks
for  routine monitoring of the EP ap-
paratus.
  To determine  if abrasion/dissolution
of stainless steel components was con-
tributing to the  chromium contamina-
tion of EP extracts, a rigorous extraction
of abrasive material (fine sand) with
aggressive (dilute nitric acid) and less
aggressive (dilute acetic acid) extract ants
was carried out  in blade-type extractors
(with polyethylene tumbling-type ex-
tractors as controls). Chromium levels
up to 0.18 mg/l were found in unfiltered
nitric acid  extracts from the blade-type
extractors. No  detectable chromium
was leached from  the sand or the
tumbling-type extractor. One of the two
unfiltered  acetic acid extracts showed
detectable (>0.01 mg/l) chromium
Pond 12

 226.4
 129.7
 143.9
Biosolids

  12.8
  10.8
  10.5
           levels. The data suggest that the use of
           stainless steel extractors for testing
           strongly acidic, abrasive wastes may
           result in contamination of the extracts
           and should be avoided.
            To investigate the source(s) of barium
           found in filtered acidic blanks, Nuclepore®
           and Millipore® glass-fiber prefilter pads
           and Nuclepore® polycarbonate filters
           were leached for 1 -2 hours in dilute acid
           solutions. Barium (up to4 mg/l) leached
           from the prefilter pads, but not from the
           filters.
            Analytical  procedures.  Precision of
           the AAS analyses for barium, chromium,
           and lead  in EP extracts are shown in
           Tables 1 and 2 (for Pond 0 and P samples)
           and Table 4 (for 11  other waste samples).
           For Pond 0 and P samples, the highest
           RSDs were 16.4% for  barium, 3.1% for
           chromium, and 4.6% for lead. With
           other waste samples the average RSDs
           ranged from 11 -66% for barium, <1 -
           11 % for chromium, and 5-140% for lead
           (average RSD <14% for extracts with
           >0.2  mg/l lead). Precision of AAS
           analyses of sludge digests averaged
           11.1% (RSD) for barium, chromium,
           lead,  arsenic, cadmium, and selenium.
            Precision of the AAS analyses to
           determine spike recovery of eight ele-
           ments of interest (As, Ba, Cd, Cr, Pb, Hg,
           Ag, and Se,  in a variety of sample
           matrices) was quite high, with the
           exception of barium (Table 5).
            When recovery of elements added
           (spiked) to sample extracts approaches
           100%, it is an indication (but no guaran-
           tee) of accuracy. Table 5 shows average
recoveries near 100 percent from ex- {
tracts of many waste samples. Low
recovery (52%) of lead in an undiluted
EP extract was corrected to 100% re-
covery with calibration by the method of
standard additions and also by simple
diIution of the extract. These techniques
provide  the necessary detection/cor-
rection for most suppression. Evidence
for instrumental response enhancement
was found (e.g., chromium, 144%, and
selenium, 160%, Table 5).
  Standards prepared in 0.2 M acetate
buffer and EP extracts compared well
with corresponding standards in nitric
acid. Values for As, Ba, Cd, Cr, Hg, and
Se were within 8% of the regression
slope with the buffer and 10% with EP
extracts. Lead was 13% low in the
acetate  buffer and mercury was 15%
low in waste extracts (when the highest
Hg value was deleted).

Discussion
  Sampling results emphasize the fact
that  waste from sources such as dis-
posal ponds may be very heterogeneous
and  that a number of samples from
different locations on  the pond are
required to properly represent a waste
for identification as hazardous or non- t
hazardous. Existing information on "
waste sources to be sampled,  or better
still,  preliminary sampling data should
be factored into any sampling design to
assure that representative samples are
obtained on a waste-by-waste basis.
"Mathematical composites" of sample
data  indicate  that  a composite of five
samples from different locations on  a
pond should provide a more reproducible
indication of  the pond's composition
than is possible with a single, discreet
sample.
  Sampling precision, as indicated  by
RSDs of percent solids data, is influenced
Table 3.    Extractor Comparison—Mean and Standard Deviation of Concentrations of Metals Extracted with the Three
           Extractor Types
Ba
W N R
PondO x=6.21 x=5.40 x=3.72
s=1.25 s=0.72 s=0.84
Pond 12
NO ANALYSES PERFORMED
Biosolids x=1.56 ~x=1,38 x=1.22
s=0.48 s=0.41 s=0.50

W
x=917
5=113
x=0.66
s=0.9S
x=0.31
s=0. 13
Cr
N
x=948
s=94.6
x=0.37
s=0.48
x=0.23
s=0.06

R
x=907
S=94.6
x=0.53
s=1.20
x=0.17
s=0.06

W
x=36.70
5=3.96
x=0.58
s=0.51
x=0.38
s=0.04
Pb
N
x=36.95
s=4.37
x=0.48
s=0.34
x=0.37
s=0.04

R
x=36.50
s=4.56
x=0.67
s=0.84
x=0.39
s=0.05
 W= Wrist-Arm Shaker
 N = NBS Tumbling- Type Extractor
 R = Blade-Type Extractor

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 greatly by small differences in mean
 percent solids (the denominator in cal-
 culating the RSD), especially in samples
 with low solids. In general, RSDs based
 on percent solids are lower (better
 precision) with samples higher in solids
 (e.g., >5%). At the same time, for a given
 sample type, the lower the solids content,
 the less influence small changes are
 likely to have on the composition of the
 resulting extracts.
   Specifications and design advantages
 for the DAT (drum and tank) sampler
 developed at this  Laboratory can be
 found in  the  report from which this
 summary was written.
   The blade-type extractor tended to
 yield lower extract concentrations of the
 metals measured than the other two
 types tested, especially for samples with
 low solids (Pond 0). Of the three extractor
 types, the blade-type agitates the sam-
 ples least and appears most dependent
 upon a minimum solids content in the
 sample for effective extraction.
   Clogging of the nitrous oxide-acetylene
 burner, by extracts high in dissolved
 solids, was found to be a major reason
 for poor precision in the analyses of EP
 extracts for barium. Sample dilution or
I use of furnace AAS techniques should
' be used to avoid this problem.

Table 4.    Atomic Absorption Analyses*
           Standard Deviations
      Table 5.    Spike Recoveries of Selected Elements from Various Sample Matrices
                                         Spike Recovery (%)
                                       Analyses
         Element   No. of Samples     Average
                         Range     Average RSD (%)
Lead
Mercury
Silver
Arsenic
Cadmium
Selenium
Barium
Chromium
18
3
7
7
7
7
19
18
107.1
87.0
96.0
109.6
99.1
105.1
95.3
105.5
64-120
78-97
94-98
102-122
95-1O4
38-160
33-120
89-144
2.8
0.3
0.0
3.0
1.1
4.9
10.1
3.9
        Low mercury responses in waste
      extracts  appear to have resulted from
      instrumental suppression by some
      waste component since good agreement
      was observed between Hg standards
      prepared in acetate buffer and nitric
      acid.  Calibration by the standard addi-
      tions method should compensate for
      such suppression. Inadequate oxidation
      of EP extracts in the digestion step could
      explain  low mercury recoveries  and
      should be investigated.
        "Memory effect", false high readings
      resulting from inadequate cleanout of
      the AAS nebulizer and burner system
      between solutions, was largely elimi-
      nate by appropriately scheduled rinses
      and prolonging the solution uptake prior
      to measurement.
                Conclusions and
                Recommendations

                  The following conclusions and recom-
                mendations are based upon data pre-
                sented and observations made during
                the study period:
                  • The method developed and stan-
                    dardized for sampling ponded
                    wastes provided representative
                    composite samples of the ponded
                    wastes tested. It is recommended
                    that background information, in-
                    cluding preliminary sampling data,
                    be obtained and factored into the
                    sampling design on a waste-by-
                    waste basis to assure that samples
                    obtained are representative of the
                    waste site sampled.
    of EP Extracts for Barium, Chromium, and Lead: Mean Values (mg/l) and Relative
Barium
x RSD (%)
Sulfonation Tars
Paint Sludge
(collected 4-1 9-79)
(collected 6-1 3-79)
Pesticide Waste
API Oil Separator Inlet
Chromate Oxidation Paste
n.d.
9.8
13. 1(2)
0.9
n.d.
n.d.
—
15
10
11
—
—
Chromium
x RSD (%)
n.d. —
4.1 2
1.5(2) 1 1
n.d. —
3.8(3) <1
4.7(2) 5
Lead
x RSD (%)
0.3(2)
0.1
0.08
n.d.
0.1(3)
n.d.
33
100
125
—
140
—
 Electric Furnace
  Baghouse Dust

 Blast Furnace Scrubber
  Filter Cake

 Mill Scale, Water
  Treatment Plant

 Filter Cake, Chlorine/
  Hg Process  Stream

 Chlorine Process Sludge
0.9(3)    14


0.87(3)   11


0.3(6)    11


0.18(3)  32

0.62(3)  66
n.d.      —


n.d.      —


n.d.      —


n.d.      —

n.d.      —
 0.13(3)   28


13.8(3)     5


 n.d.      —


 0.1      60

 0.46(3)    9
 *Flame atomic absorption analyses performed in triplicate
 n.d. Not detected
if J Average means (and corresponding average RSDs) based upon number of extracts indicated in parentheses.

-------
 The Composite Liquid Waste Sam-
 pler (COLIWASA) provided repro-
 ducible samples from drums of the
 liquid wastes tested. Present de-
 sign of the COLIWASA prevents
 adequate sampling of the bottom-
 most layer in drums or tanks. The
 alternative sampler design proposed
 (DAT Sampler) should be evaluated
 with liquid wastes in drums, tanks,
 or vacuum trucks.
 In intralaboratory studies, the pro-
 posed Extraction Procedure was
 found to be reproducible (RSD < ±
 15% for the waste types sampled).
 However, interlaboratory studies
 indicate that adherence to clear,
 detailed,  step-by-step protocols is
 needed to eliminate misinterpreta-
 tion or substitution of non-equiva-
 lent procedural elements. The  EP
 should be evaluated to determine
 its applicability to oily or solvent-
 containing waste samples.
> A problem with  contamination of
 acidified extracts by barium leached
 from  glass-fiber prefilters was
 identified. Until prefilters are iden-
 tified which do not contribute barium
 to the filtrate, it is recommended
 that a 100-ml portion of 0.1N acetic
 acid precede each waste sample
 through the pref liter and be stored
 for possible future use in determin-
 ing blank correction for the sample.
 It is anticipated that such blank
 correction would only be used in
 the event that the barium levels in
 the samples exceed the criteria
 level for hazardous waste identifi-
 cation by the toxicity characteristic.
i Intra- and interlaboratory studies
 indicate that atomic absorption
 spectroscopy is an accurate and
 highly reproducible method  for
 analysis of most inorganic compo-
 nents of waste extracts.
i Some problems in the analyses of
 barium and  mercury remain to be
 resolved. The method of additions
 is recommended to provide inter-
 ference correction. Extracts very
 high in dissolved solids concentra-
 tions may cause build-ups of mate-
 rial which alter the flame charac-
 teristics  of the atomic absorption
 spectrometer. Such samples should
 be  diluted  prior to analysis or
 analyzed by furnace procedures.
» The three extractor types compared
 (i.e., the blade-type, NBS tumbler-
 type, and the wrist-arm shaker)
 provide comparable waste extracts
 when used in the proposed EP.
  When possible, EP extracts should
  be analyzed immediately, as some
  waste extracts are not stable over a
  period of hours or days.
  Applicability of the EP toxicity
  criterion for mercury should be re-
  evaluated, as low EP recoveries
  may be misleading with respect to
  the toxicity hazard presented by
  wastes containing high levels of Hg
  in temporarily insoluble forms.
  Inadequate oxidation of mercury-
  containing EP extracts should be
  investigated to explain low mercury
  recoveries.
The EPA authors L R. Williams. E. P. Meier. T. A. Hinners. E. A. Yfantis. and
  W. F. Beckert are with the Environmental Monitoring Systems Laboratory,
  Las Vegas. NV; and T. E. Gran is with Northrop Services, Inc.. Las Vegas. NV.
L R. Williams is the EPA Project Officer (see below).
The complete report, entitled "Evaluation of the Procedures for Identification
  of Hazardous Wastes: Part 1. Sampling, Extraction, and Inorganic Analytical
  Procedures," (Order No. PB 81 -203 804; Cost: $9.50. subject to change) will be
  available only from:
       National Technical Information Service
       5285 Port Royal Road
       Springfield, VA 22161
        Telephone: 703-487-4650
The EPA Project Officer can be  contacted at:
       Environmental Monitoring Systems Laboratory
       U.S. Environmental Protection Agency
       P.O. Box 15027
       Las Vegas, NV89114
                                                                                ft UA GOVERNMENT PNNTWQ OFFICE 1«1 -757-012/7262

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