United States
                    Environmental Protection
                    Agency
         Environmental Monitoring and
         Support Laboratory
         Cincinnati OH 45268
                    Research and Development
         EPA/600/S4-85/071  Dec. 1985
4>ER/\         Project Summary
                     -/
                    USEPA  Extraction Method
                    Development  Study for
                    Trace Metals  in Leachate
                    J. Maney and T. Copeland
US. Ef.vwonmentil Protection Agency
Region V,  U&rtry
230 South DearMffn Street
Chicago, Illinois  6060* , ..,x
                      A study was performed to determine
                    the applicability of currently approved
                    analytical methods for conducting the
                    extraction procedure (EP) toxicity test
                    required  by the Hazardous Waste and
                    Consolidated Permit Program. The first
                    phase of the  study was designed to
                    determine the necessity for performing
                    digestion of the EP leachates prior to
                    trace element analysis  and  also to
                    determine the effect, if any, of preser-
                    vation on total metal  concentrations.
                    Four matrices were used for this phase
                    of the study (river sediment, fly ash,
                    low-pH sludge, and oil/water waste)
                    and analyses were performed for 17
                    elements by both atomic absorption
                    spectrophotometry (AAS) and by In-
                    ductively Coupled Argon Plasma Emis-
                    sion Spectrometry (ICP). Digestion of
                    the leachates generally reduced inter-
                    ferences and improved the accuracy of
                    the analyses. For one high sulfur waste,
                    however, digestion introduced a chem-
                    ical interference. Acid preservation of
                    the wastes did not significantly affect
                    the results.
                      The second phase of the study was
                    designed to determine the effect of pH
                    and time on metal concentrations in the
                    leachate  from low-pH sludge. Deter-
                    minations were made for 17 elements
                    in the EP extracts after adjustment of
                    initial pH to levels of 2, 4, 6 and 8.
                    Extractions were performed 0, 2,8 and
                    16 hours following pH adjustment. All
                    wastes exhibited a strong dependence
                    on the initial  pH  of the wastes—the
                    leachate  concentrations were lowered
                    at higher initial pH values. The time
                    between  pH adjustment and initiation
                    of the extraction procedure did not alter
                    the results.
           The third phase of the study was
         designed to determine the efficiency of
         the EP toxicity procedure in extracting
         metal spikes from three standardized
         reference materials (river sediment, fly
         ash,  and  EPA  Municipal Digested
         Sludge). The results of this phase con-
         firmed the strong pH dependence of
         leachate concentrations found in Phase
         2 and demonstrated that under normal
         EP extraction conditions  extraction
         efficiencies for most metals are low.
           A study was also performed to de-
         termine if metal concentrations were
         affected by various matrices encounter-
         ed using the EP procedures (acetic acid
         [0.6%], nitric acid [0.5%], or acetic acid
         [0.6%]/nitric acid [0.5%]). Of all the 17
         elements studied, only selenium exhib-
         ited a matrix effect from  the dilute
         acids. The slopes of the selenium cali-
         bration curves generated by both ICP
         and AAS were enhanced in the presence
         of acetic acid.
           This Project Summary was developed
         by EPA's Environmental Monitoring and
         Support Laboratory, Cincinnati, OH. to
         announce key findings of the research
         project that is fully documented in a
         separate report of the same title (see
         Project Report ordering information at
         back).

         Introduction
           This investigation was conducted in
         three separate phases with each phase
         focusing on specific questions related to
         the applicability  of various  aspects of
         approved methods for conducting the EP
         toxicity tests and subsequent analyses.
         Phase 1 of the study was designed to
         determine  the necessity of performing

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leachate digestion after the EP toxicity
test a nd to determ i ne the effect of preser-
vation on metal concentrations.  Four
materials were tested—river sediment,
fly ash, a low-pH sludge,  and oil/water
waste. For the oil/water waste, a separate
extraction and analysis was performed on
the oil phase. For all extractions, analyses
were performed in triplicate using atomic
absorption spectrophotometry (AAS) and
inductively coupled argon plasma emis-
sion spectroscopy (ICP).
  The  second  phase was designed to
determine the  effect of pH and time on
leachate metal concentrations from the
low-pH sludge. The waste was extracted
at 0, 2, 8 and 16 hours after pH adjust-
ment, with the pH  adjustments  being
made at levels of 2,4,6 and 8 with 1.0 M
sodium hydroxide. Analyses were per-
formed in triplicate using  both AAS and
ICP.
  The  third  phase  of  the study was
designed to determine recovery of metal
spikes from three standardized reference
materials. The  three standardized refer-
ence materials (river sediment, fly ash,
and EPA Municipal Digested Sludge) were
spiked in triplicate at three levels, ex-
tracted according to the EP toxicity test
procedures, and analyzed using AAS and
ICP.
  Preliminary to all three phases, a
calibration study was performed to de-
termine the effect,  if any,  of the acid
matrix (0.6% acetic, 0.5% nitric or 0.6%
acetic andO.5% nitric) on the slopes of the
calibration curves.

Procedure

Calibration Study
  Standards for the calibration  study
were prepared by dilution of 1000 ppm
Fisher or Ventron certified reference
standards with the  appropriate matrix.
Ultrex acetic and nitric acids were used
for preparation of the standard matrices
(0.6% acetic acid, 0.5% nitric acid, and
0.6% acetic acid/0.5% nitric acid).  Mixed
standards were  used for all elements
except As, Hg, Se and Ag which  were
prepared individually and were prepared
daily to minimize losses.

Phase 1 Analyses
  Phase 1 analyses  were performed on
samples of river sediment, fly ash, low-pH
sludge, and oil/water waste. The Phase 1
procedures consisted of  the following
general analytical schemes:
Scheme 1—EP test with leachate  diges-
           tion
Scheme 2—EP test without  leachate
           digestion
Scheme 3—Digestion according to EPA
           procedures with sample
           stored at room temperature
Scheme 4—Digestion according to EPA
           procedures with sample pre-
           served  by addition of nitric
           acid (HN03) to pH <2

Analytical results from Schemes 1 and 2
were used to evaluate the requirement to
digest leachates resulting  from the  EP
test. Results for Schemes 3 and 4 were
used to evaluate sample storage require-
ments.
  Modified  procedures were utilized  for
the following elements: As and Se—EPA
Methods 206.2 and 270.2, Hg—Method
245.1; and Sb—Method 204.2. Analyses
were  performed by AAS  according to
methods specified  by EPA and  Perkin-
Elmer. Graphite furnace AAS  was  used
for atomic absorption determination of As
and Se and  cold-vapor AAS was used for
determination of Hg. All other  elements
were  determined  by flame  methods.
Analyses were  also performed by ICP
according to methods specified  by EPA
and Jarrell-Ash. Extractions and analyses
were performed in triplicate.
  The sequence of events  occurring  for
each Scheme of Phase 1 of the project are
summarized below:

Scheme 1—Divide  sample aliquot into
           triplicates, perform  EP extrac-
           tion, digest the extract (sepa-
           rate digestions for Ag,  Hg
           and Sb), analyze, spike, wait
           two weeks, analyze by AA.
Scheme 2—Divide  sample aliquot into
           triplicates, perform  EP extrac-
           tion, analyze, spike, wait two
           weeks,  analyze by AA.
Scheme 3—Divide  sample aliquot into
           triplicates, digest  the tripli-
           cates (separate digestions for
           Ag,  Hg and Sb),  analyze,
           spike, wait two weeks, ana-
           lyze by AA.
Scheme 4—Exactly as in Scheme 3 only
           use the acid preserved
           sample aliquot.

Phase  2 Analyses
  For the Phase 2 analyses of the low-pH
sludge,  16  separate aliquots  were  re-
moved,  subsampled in  triplicate, and
adjusted to pH levels of 2, 4, 6 and 8 by
addition of 1 M sodium hydroxide(NaOH).
At times of 0,2, Sand 16 hours following
pH adjustment, one triplicate subsample
from each pH level was extracted using
the EP toxicity test procedure and ana-
lyzed for  17 trace metals. Details of
extraction and analysis were identical to
those described in the section  entitled
"Phase 1 Analyses," for Scheme 2.

Phase 3 Analyses
  These standardized reference materials
were prepared  by drying, grinding, and
homogenizationof river sediment, fly ash,
and EPA Municipal Digested Sludge (the
latter material required only homogeniza-
tion). After the determination of total
metal concentrations,  each  sample was
divided into 10 aliquots and  prepared for
extraction according to procedures speci-
fied for the EP toxicity test. After addition
of distilled water, each  material was
spiked in triplicate at levels approximating
50, 100  and 150% of the total metal
concentration using Fisher certified ref-
erence standards. An  unspiked  sample
was subjected to the EP test as a control
and to allow correction for the background
metal concentration  in the leachate.
During addition of the standard  spiking
solutions, pH was either  allowed to
change or was  maintained  at its initial
level by concurrent titration with 0.25 N
sodium carbonate (Na2C03). After spike
addition, samples  were extracted  and
analyzed using methods identical to those
presented in Phase 1, Scheme 2.
Results and Discussion

Calibration Study
  For each of 17 elements, the slope,
intercept, and correlation coefficient for
the calibration  curve are presented.
Actual calibration curves are also  pre-
sented.
  For all elements except Se, the slopes
of the calibration curves for standards
prepared in 0.6% acetic acid and 0.6%
acetic acid/0.5% nitric acid were within
±5%  of the  slopes of the reference
standards prepared in 0.5% nitric acid. In
the case of Se, the slope of the calibration
curve in the 0.6% acetic acid was  14%
greater than the slope of the calibration
curve in 0.5% nitric acid.

River Sediment
  For nine elements (Al, Ba, Be, Cd, Fe,
Pb, Mn, Ni and Zn) no statistically signif-
icant differences were observed between
digested and undigested leachates.
  Recoveries of spikes from the analyte
solutions determined  by AAS are  pre-
sented. Recoveries were within the range

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of 80-120% except for As, Hg, Ag and Zn,
which had recoveries of 109-141%, 66-
99%, 73-108% and 47-85%, respectively.
   No significant differences were found
between the digested and undigested EP
leachates for any elements present above
the detection limits for the river sediment
sample. Significant differences between
Schemes 3 and  4 (unpreserved and
preserved sample aliquots, respectively)
were found by AAS for As, Fe and Ag.
However, none of these differences were
statistically significant when analyzed by
ICP. For  all three elements, concentra-
tions as determined by AAS were higher
in the unpreserved sample.
   Recoveries of spikes for all  four
schemes analyzed by AAS were between
80-120% except for As, Hg, Ag and Zn.
Zinc recoveries were  consistently  low
(47-85%), As recoveries consistently high
(109-141%). Silver and Hg  recoveries
were low only for the nitric acid preserved
(Scheme 4)  samples.  The Zn and As
recoveries from the fly ash samples also
followed these trends indicating a positive
interference for As and a loss of Zn to the
residual solids or to the glassware.
   Recoveries of spikes of 11 elements (Al,
Sb, Be, Cd, Cu, Fe, Mn, Hg, Ni, Ag andTI)
were in the range of 80-120%. Recoveries
for the remaining six elements were as
follows: As, 116-143%; Ba, 0-108%; Cr,
108-128%; Pb, 70-101%; Se, 30-95%;
and Zn, 70-88%.
   Significant differences for fly ash EP
leachates were found for Cu, N i and Se by
AAS  and for  Ba,  Cd  and  Cr by ICP.
Differences  for Cu and Ni  were  not
significant by ICP and Se was below the
ICP detection limit. Cu and Ni by AA are
affected by Fe and other transition metals.
The difference in Ba concentrations be-
tween the digested and undigested leach-
ates is over an order of magnitude (the
undigested value higher).
  As with the river sediment samples, Zn
recoveries were consistently low. As
recoveries consistently high. In addition,
Cr recoveries were somewhat high par-
ticularly  for the  completely  digested
(Scheme 3) sample supporting the possi-
bility of contamination during digestion.
  Recoveries of Ba, Pb,  Se and Ag were
low for the digested EP leachate (Scheme
1). The  fly ash sample was  generated
from fuel containing significant levels of
sulfur and the possibility of sulfate forma-
tion during digestion with subsequent
precipitation of insoluble sulfatesfBa, Pb,
Ag) is highly likely. The low Se recovery
cannot be explained by sulfate precipita-
tion but may be due to the formation of
nickel sulfides rather than nickel sele-
nides in the graphite furnace with sub-
sequent loss of SeC>2

Low pH Sludge
  For the Scheme 1  and 2 data, concen-
trations of seven elements (Sb, Ba, Be,
Hg, Se, Ag and Tl) were below the limit of
detection of the analytical methods and
no statistical comparisons could be per-
formed. For six elements (Al, Cr, Cu, Fe,
Pb  and Mn),  no significant differences
were detected. For four elements (As, Cd,
Ni and Zn), significant differences were
detected using AAS results. For Cd, Ni
and Zn, differences were not significant
using ICP data. For the Scheme 3 and 4
data, which compared preserved and
unpreserved sample aliquots, five ele-
ments (Sb, Be, Se, Ag and Tl) were below
the  limits  of detection. By AAS, no
significant differences were detected for
Al,  As, Ba, Cd, Cu, Pb, Mn and  Zn.
Significant differences were detected for
Cd, Fe, Mn and Ni by AAS and for Cu, Fe,
Pb, Mn and Ni by ICP.
  Recoveries of spikes for 11 elements
(Al, Sb, Be, Cd, Cr, Cu, Fe, Mn, Hg, Ni and
Tl), were in  the range  of 80-120%.
Recoveries for the remaining elements
were as follows: As, 56-92%; Ba, 0%; Pb,
41 -89%; Se, 78-98%; Ag, 7-24%; and Zn,
86-128%.
  The AAS data for Schemes 1  and 2
indicate significant differences for As, Cd,
Ni and Zn. Arsenic levels were below ICP
detection limits while the ICP data for Cd,
Ni and Zn showed no differences. The As
values for the undigested leachate  are
higher than for the digested sample. Two
possible causes are that As is lost during
digestion  or  that there  is a  spectral
interference in the  undigested sample.
Spike  recoveries for  the  undigested
sample averaged 56% and for the digested
sample 84%, supporting the likelihood of
an interference in the undigested sample.
  The practical significance of the AAS
Cd  data is suspect.  The  high precision
allows 0.23 and 0.24 mg/L to be statis-
tically different.
  The nickel data for the digested leachate
are higher (by both AAS and ICP although
not significant by ICP). Since the differ-
ence is  small, contamination  during
digestion or slight nonhomogeneities in
the sample aliquots are the likely causes.
An enhancement of flame AAS analyses
for  Ni by large  excesses  of Fe is well
known.
  In the comparison of Schemes 3 and 4,
the AAS data are significantly different
for Cd but the ICP data are not. For Cu, the
ICP data are significantly different while
the AAS data are not. An examination of
the raw data again suggests that these
results  are  the mathematical  conse-
quence of high precision rather than of a
practical difference. The Pb data for ICP
Scheme 3 (unpreserved) are higher than
for the preserved sample while the AAS
data show no difference. Both the Scheme
3 and Scheme 4 ICP values are higher
than the AA results. The  most likely
explanation of this is that it is a conse-
quence  of a spectral interference from
the extremely high levels of Fe, Mn or Ni
present  in this sample. If the difference
were due to a true chemical change in the
unpreserved sample  or a sample non-
homogeneity, the AAS results should
also reflect the increased concentration.
  Recoveries of spikes from  this waste
were generally high with two exceptions:
As and Se recoveries from the undigested
EP leachate were low and elements
forming insoluble sulfates had universally
poor recoveries (Ba, Pb and Ag).

Oil/ Water Waste
  For data from Schemes 1  and 2, only
two elements (Fe and Mn) were present
at concentrations  above the  limit of
detection and no significant differences
were evident. For data from Schemes 3
and 4, all elements except Sb, As, Se, Ag
and Tl  were present at concentrations
above the limit of detection and no signif-
icant differences were detected.
  Oil phase analyses indicated measur-
able amounts of Al, Ba, Cu, Fe, Pb, Mn
and Ni in the leachates. For  purposes of
comparison,  concentrations were calcu-
lated on the  same basis as the previous
phase leachate. The fractions of the total
metal contained in the oil phase were as
follows:  Al, 32-57%; Ba, 9-12%; Fe, 26-
29%; Mn, 17-24%; and Ni, 44%.
  For 15 elements (Sb, As, Ba, Be, Cd, Cr,
Cu, Fe, Pb, Mn, Ni, Se, Ag, Tl and Zn),
recoveries were in the range of 80-120%.
Recoveries of the remaining elements
were as follows: Al, 96-124%;  and Hg,
15-104%.

Phase  2 Analyses
  Aliquots of the sludge were adjusted to
pH 2, 4, 6 and 8 with 1 M NaOH and then
extracted at  time intervals (post-pH ad-
justment) of  0, 2, 8 and 16 hours. Of the
17 elements in this study, 10 were
present in the pH 2 samples at concentra-
tions above the analytical detection limits
(Al, As, Cd, Cr, Cu, Fe, Pb, Mn, Ni andZn).
  None of the metals exhibited a strong
leachate  concentration dependence on
the time interval between pH adjustment
and extraction.  However, 9  of the 10
elements present (As being  the single

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 exception) exhibited strong concentration
 dependence on pH during the EP leachate
 generation.  It should be  noted that the
 aliquots of sludge which were adjusted to
 pH 6 or 8 were (at the appropriate time
 interval) adjusted to pH 5 as would be
 required by the EP test. The extracts were
 analyzed without digestion, that is, by
 procedures analogous to Phase 1,
 Scheme 2.


 Phase 3 Analyses
   The purpose of Phase 3 was to deter-
 mine the efficiency of the EP in extracting
 metal spikes  from standard reference
 materials. The materials chosen were fly
 ash, river sediment, and EPA Municipal
 Digested Sludge. The fly ash and river
 sediment were dried, ground, and ho-
 mogenized prior to use. The samples of
 dried municipal sludge were composited
 to obtain a sufficient quantity of homog-
 enous material for the study.
   Aliquots of all three materials were
 digested and analyzed in triplicate by AAS
 to provide the total bulk concentrations of
 the 17 metals in the reference materials.
 The results obtained  by ERGO were
 confirmed by an outside laboratory.
   Each sample was prepared for the EP
 extraction according to the EPA specified
 methods. After addition of distilled water
 to the dried ash, sediment and sludge, the
 samples were spiked (in triplicate) at
 three different concentration levels  rep-
 resenting 150%, 100%, and 50% of the
 total metal content or 20,10, and 5 times
 the detection limit for those elements
 which were not detected  in the bulk
 analyses of the materials.  Due to the acid
 content of the spiking solutions, the pH of
 the spiked sample/distilled water mat-
 rices ranged from 1.39 to 3.28. This pH
 range is low for EP extractions where the
 pH of neutral or basic sludges are typically
 adjusted to pH 5.0 ± 0.2 with acetic acid.
   For a second series, the sample pH was
 maintained at its initial level during spike
 addition by concurrent titration with 0.25
 H. NaaCOa.  These samples were then
 adjusted to pH 5 and extracted according
 to the EP test procedure.
   Blank spike recoveries at the  150%,
 100%, and  50% levels  for the pH 5
 samples and at the 100% spike level for
 the low-pH  samples are  also included.
. Recoveries for most metals in the blank
 spikes were in the range 85% to 115%
 with the certain exceptions.
   For the pH 5 adjusted  river sediment
 samples, recoveries ranged from <1 % to
 169%; for the low-pH samples, the re-
 coveries ranged from 1% to 323%. In
general, recoveries of the  high (150%)
spikes were higher thanfor the low(50%)
spikes. The most  obvious difference is
that the recoveries for the low-pH samples
are much higher  and much  closer to
100% than the pH  5 recoveries.
  The recoveries of Se, Sb and As were
poor for both low-pH and pH 5 extracts.
These elements would most  likely  be
present as oxyanions and would  not
precipitate as hydroxides. The most likely
mechanisms of  loss of those would be
adsorption or co-precipitation.

Fly Ash
  The fly ash samples were dried, ground,
and  homogenized prior to bulk analysis
and Phase 3 extractions. Bulk concentra-
tions of the elements of interest were
determined by ERCO  and verified by an
outside laboratory.
  Mean recoveries of 17 elements were
calculated by averaging results for both
AAS and ICP and correcting (where
possible) for the concentration of each
element determined from an unspiked EP
for each material. The concentration of
element recovered was then compared to
the original concentration added to de-
termine the percent recovery.
  As with the river sediment samples,
recoveries from the low-pH extracts were
consistently better than from  the pH 5
extracts and the recoveries of the anionic
species (As, Sb, Se) were low at both pH
values; Ni, again exhibited high recoveries
(particularly by AAS) due to Fe interfer-
ence. In  addition, the fly ash samples
exhibited low recoveries for those  ele-
ments with insoluble sulfates (Ba, Pb) as
didthe fly ash samples utilized in Phase 1.

EPA Municipal Digested Sludge
  Each sample was prepared for the EP
extraction according to methods outlined
by  EPA and  in the  manner  that was
employed for the fly ash and river sedi-
ment samples.  Mean recoveries were
calculated by averaging results for both
AAS  and ICP  and correcting (where
possible) for the concentration of each
element determined from the appropriate
unspiked EP for each material. The con-
centration of element recovered was then
compared to the original concentration
added to determine the percent recovery.
  Recoveries  of the metals in  the blank
spikes were all between 90% and 110%
with the exception  of Ag which is unstable
in the mixed standards and Hg which was
spiked at low levels.
  Recoveries of the metals in the extracts
were extremely poor.  For the pH 5 ex-
tracts, no element exhibited recoveries in
the 80% to 120% range. For the low-pH
extracts only four of the 51  recoveries
were in the 80% to 120% range.  Re-
coveries in the pH 5 extracts were all
extremely low (except Hg) while the low-
pH recoveries were highly erratic. For the
low-pH extracts, Sb, Pb, Ba, Se and Ag
exhibited low recoveries. The Ag was
expected to be low since the spike solution
contains chloride and precipitates the Ag.
The digested sludge apparently contains
sulfate which would selectively precipi-
tate Pb and Ba. The Sb and Se recoveries,
as with the fly ash and river sediment,
were low for both the low-pH and pH 5
extracts.

Comparison of AAS and
ICP Recoveries
  While the intent of Phase 3  was to
determine the ability of the  EP test to
leach  spikes from standard reference
materials,  the data  are also useful in
observing the comparative performance
of AA  and ICP.  Both techniques were
used to analyze the same undigested EP
leachates with the same spike levels and
consequently comparison of their  per-
formance was straightforward.


Conclusions and
Recommendations
  The EP toxicity test was designed to
indicate the concentrations of eight
metals (As, Ag, Ba, Cd, Cr, Hg, Pb and Se)
present in a waste in forms which would
allowthem to become mobile(solubilized)
in a mildly acidic (pH 5 acetic acid)
medium.  Analyses  of the  generated
leachates are performed by atomic absorp-
tion spectrophotometry (AAS).
  The conclusions which may be drawn
from this  study  and recommendations
based upon the conclusions are sum-
marized below.

Calibration Study
• For 16 of the 17  metals studied, the
   dilute nitric acid or dilute acetic acid
   matrices used for the EP toxicity  test
   had  no effect on the slopes of  the
   calibration curves.  The acetic acid
   matrix enhanced the Se signal by both
   AAS and ICP. Since enhancements of
   almost 10% were found for both AAS
   and  ICP, it is recommended that the
   method of standard additions be used
   for Se analyses or at least that a test be
   performed to ensure that standard
   additions are not needed for every EP
   leachate.

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Phase 1 (AcidPreservation and
Digestion Study)
 • Digestion of the EP leachates removes
   several interferences and is generally
   recommended prior to  analysis by
   either AAS or ICP. However, digestion
   may cause losses from certain samples
   such as the high sulfur containing fly
   ash studied here.  Digestion caused
   formation  of sulfate and subsequent
   precipitation of Ba, Ag and Pb.
 • Acid preservation of the samples used
   in this study caused little difference in
   analytical results.
 • The ICP analyses of undigested leach-
   ates were  less subject to interference
   than were AAS analyses.
 • Even though the leachate digestion of
   the fly ash resulted in losses of Ba, Ag
   and Pb for this sample,  it is recom-
   mended that the digestion  be  per-
   formed. Several matrix interferences
   in all the wastes were eliminated by
   the digestion procedure which other-
   wise would  have required time-con-
   suming techniques such as standard
   additions.
Phase 3 (Extraction
Efficiency Study)
• The pH 5 dilute acetic acid matrix used
   for the leachate generation in the EP
   toxicity test is not capable of leaching
   many metals from a solid waste and is
   incapable of preventing precipitation
   or adsorption of metal ions spiked into
   the solution. In fact, a river sediment
   containing 5,700 yug/g Al and 9,200
   jug/g Fe was leached with an acetic
   acid pH  5 solution containing 42.5
   mg/L  Al (and 68.5 mg/L Fe) with
   recoveries of the metals in solution
   being less than 3%.
• As in  Phase 1, the ICP analysis of
   undigested leachates was less subject
   to  interference  (as measured by %
   recoveries) than was AAS.
Phase 2 fpH and Storage
Time Study)
• The time that a sample is stored (0 to
   16 hours) prior to the initiation of the
   EP leachate generation had no effect
   on the metal concentrations in the
   leachate.
• The  pH of  the  sample prior to the
   initiation of the EP leachate generation
   is extremely important. This may be
   true only for selected wastes such as
   the ones used in this study, i.e., one
   with a high Fe  content which  may
   precipitate at pH 5 or one with a high
   sulfate concentration which may also
   cause precipitation. It would be useful
   to perform Phase 2 on wastes where
   hydroxide or sulfate precipitation were
   less likely.
  The fact that the leachate concentra-
tions are pH dependent was further
confirmed by the Phase 3 data. Due to this
variability in recovery (extraction  effi-
ciency) it is recommended that the intent
of the EP toxicity test be emphasized, i.e.,
that it is an indicator of the concentration
of  mobile  metal species  not  a  total
extraction procedure.
                                                                               U. S. GOVERNMENT PRINTING OFFICE:1986/646-l 16/20729

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     J. Maneyand T. Copelandare withERCO/A Division ofENSECO, Cambridge. MA
       02140.
     John D. Pfaff is the EPA Project Officer (see below).
     The complete report, entitled "US EPA Extraction Method Development Study for
       Trace Metals in Leachate." (Order No. PB 86-118 981/AS; Cost:  $16.95.
       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 and Support Laboratory
            U.S. Environmental Protection Agency
            Cincinnati, OH 45268
United States
Environmental Protection
Agency
Center for Environmental Research
Information
Cincinnati OH 45268
Official Business
Penalty for Private Use $300
EPA/600/S4-85/071
         0000329    PS
                                         AGENCr

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