F-86-MWR2-S0010
TECHNICAL STUDIES SUPPORTING THE MINING WASTE
REGULATORY DETERMINATION
FINAL REPORT
Contract No. 68-01-7053
Work Assignment 42
Tasks 1 and 2
Prepared by:
Jay Bernarding, William Nivens
Versar, Inc.
P.O. Box 1549
Springfield, VA 22151
Prepared for:
Angela Wilkes
Office of Solid Waste
Waste Treatment Branch
U.S. Environmental Protection Agency
401 M Street, S.W.
Washington, D.C. 20460
June 30, 1986
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TABLE OF CONTENTS
SECTION PAGE
1. INTRODUCTION 1
2. CONCLUSIONS AND RECOMMENDATIONS 2
2.1 Task 1 Conclusions 2
2.2 Task 2 Conclusions 3
2.3 Recommendations 3
3. DESCRIPTION OF STUDY 4
3.1 Study Design 4
3.2 Materials/Instrumentation 4
3.2.1 Samples 4
3.2.2 Materials 7
3.2.3 Instrumentation 7
3.3 Methods 7
3.3.1 Sample Preparation 7
3.3.2 ICP Analytical Procedures 11
3.3.3 Program Quality Assurance Measures 12
4. RESULTS AND DISCUSSION 15
4.1 Task 1 - Validation of Element Measurements in EP . . 15
4.1.1 Task 1 Results and Quality Control Data .... 15
4.1.2 Task 1 Discussion 20
4.2 Task 2 - Comparisons of Four Extraction Techniques. . 22
4.2.1 Task 2 Results and Quality Control Data .... 22
4.2.2 Task 2 Discussion 24
APPENDIX 1 ICP Analytical Data
APPENDIX 2 Quality Control Data
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TABLE OF FIGURES
PAGE
3-1 Task 1 Extraction and Analysis Scheme 5
3-2 Task 2 Extraction and Analysis Scheme 6
TABLE OF TABLES
3-1 Synthetic Rainwater Contents 10
3-2 Analytical Methods/Reporting Limits 13
3-3 Frequency of Quality Control Measures 14
4-1 Physical Characteristics and Percent Moisture
of Study Samples 16
4-2 Element Concentrations in the 3050, "Total", and EP . . . 17
4-3 EPA EP-Preaward #1 -
Reference Value, Acceptable Ranges, and Observed Value. . 19
4-4 Comparison of Metals Released by 3050 Digestion With
the EP-Toxicity Test 21
4-5 Element Concentrations in the Four Extractions 23
4-6 Other Major Element Concentrations in the Four
Extractions 25
4-7 Initial and Final pH Measurements in Extracts 26
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1. INTRODUCTION
EPA is concerned with the applicability of the EP (Extraction Pro-
cedure) -Toxicity Test when evaluating the RCRA hazardous characteristics
of mining and smelting wastes. The lead and cadmium values generated by
the EP-Toxicity Test for mining and smelting wastes are of particular
concern. Since approximately 11 million metric tons of mine and mill
wastes and more than a million tons of smelting wastes generated
annually, exceed EP-Toxicity maximum contaminant limits, it is important
to understand whether the EP-Toxicity Test for these sample types is
both accurate and realistic. Two laboratory tasks were undertaken:
Task 1: Assess the validity of As, Pb, Cd, Ba, Ag, and Cr
concentrations in EP-Toxicity leachates.
Task 2: Compare the extraction efficiency of four leachate
techniques.
To accomplish Task 1, the samples were processed, in duplicate,
according to three different preparation procedures (EP-Toxicity Test
and two acid digestion procedures). After analysis by ICP, the element
data generated by the acid digestions were compared to the amount of
element extracted by the EP-Toxicity Test. This comparison of the
potentially extractable element content in the acid digestates with the
observed EP levels was used to confirmed the validity of the EP-Toxicity
Test for these sample types.
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In Task 2, four extraction procedures were performed on the mining
waste samples:
1. EP-Toxicity Test;
2. EP-Toxicity Test without pH adjustment;
3. ASTM Extraction Procedure; and
4. Synthetic Rainwater Leach.
The data generated by the four extractions were compared to
determine any differences between methods as well as to provide a better
understanding of factors influencing element release from these sample
types.
2. CONCLUSIONS AND RECOMMENDATIONS
2.1 Task 1 Conclusions
In Task 1, the validity of As, Ba, Cd, Cr, Pb, and Ag concentra-
tions in the EP-Toxicity Test leachates for mining and smelting wastes
was tested. Conclusions that can be made, based on this limited study
of four samples, are as follows:
Total metals analysis data, were found to be greater than
observed EP-extraction data for these mining waste samples.
Concern that the EP-Toxicity Test generates data for mining and
smelting wastes that are higher than the "total" metal content,
appears to be unfounded.
Duplicate sample precision was generally good (RSD <20 percent).
Errors due to nonhomogeneous samples or imprecision in the
preparation or analytical techniques were not a factor in data
evaluation.
Accuracy of the ICP method was measured by bench spiking all
samples. Spike recoveries were generally in acceptable ranges
(80 to 120 percent), indicating that the ICP method did not
significantly bias the results.
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2.2 Task 2 Conclusions
In Task 2, the EP-Toxicity Test was compared with three other
extraction procedures to determine if the EP-Toxicity Test is an approp-
riate method for determining the toxicity of mining and smelting wastes.
The conclusions are as follows:
The extraction pH, and not the affinity of acetic acid (as used
in the EP-Toxicity Test), appears to be the dominant factor in
regulating extracted metal levels. Generally, the lower the
extract pH value (as in the Synthetic Rainwater Leach and EP-
Toxicity Test) the greater the observed metal concentrations.
Conversely when the extract pH values were higher (as in the
ASTM and EP-Toxicity Test without pH control), the observed
metals levels were lower. These are general observations and
were not rigorously tested.
Where pH control was not used, as in the ASTM and EP-Toxicity
Test without pH control, the extraction solid/liquid ratio
probably controls the leachate metal levels.
t The Synthetic Rainwater Leach was a rapid technique. Duplicate
results, however, showed poorer precision than other extraction
methods. Greater quantities of metals were leached out by the
Synthetic Rainwater Leach than any other procedure. This is
understandable, since the pH of the extraction fluid (3.98) was
the lowest used in the study.
2.3 Recommendations
To accurately assess pH control of metal release, a rigorous
statistical study employing several different acids and pH
levels would be necessary.
The Synthetic Rainwater Leach may be a viable alternative to the
EP-Toxicity Test, but a more thorough study would be necessary to
define experimental parameters as well as to determine method
precision.
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3. DESCRIPTION OF STUDY
3.1 Study Design
In Task 1, three preparation procedures were carried out on the four
samples selected for use in the study. A fifth sample provided by EPA
(an EP-QC sludge) was also included. Figure 3-1 provides a schematic
description of the preparation and analysis procedures. All samples in
this task were run in duplicate to determine method precision. Also,
bench spikes of the six study elements (As, Ba, Cr, Cd, Pb, and Ag) were
performed on all samples to investigate ICP accuracy in these matrices.
In Task 2, the EP results on the samples from Task 1 were compared
with the results from three additional extraction procedures carried out
on the same samples. A schematic description of this study is provided
in Figure 3-2. Again, all sample extracts were bench spiked and
reanalyzed to evaluate the accuracy of the ICP method in these sample
matrixes.
3.2 Materials/Instrumentation
3.2.1 Samples
There were five samples used in this study. Four of the samples
were supplied by Bob Hoy of PEI Associates in Cincinnati, Ohio. The fifth
sample was supplied by Florence Richardson, Quality Assurance Officer,
of the EPA's Office of Solid Waste. A list of the samples follows:
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ICP analysis
Sample
(in duplicate)
1
1
1
EP-Toxicity
extraction
i
1
1
1
EP-extract
digestion
1
1
1
1
1
1
1
1
Method 3050
acid digestion
i
I
1
1
ICP analysis *
1
|
j
1
HF:HC104:HN03
acid digestion
i
I
1
1
ICP analysis *
* All samples were bench spiked (after digestion) and reanalyzed.
Figure 3-1 Task 1 Extraction and Analysis Scheme
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Sample
1
1
1
EP-Toxicity EP-Toxicity
extraction extraction
w/o pH
adjustment
' 1
1
i
EP-extract EP-w/o extract
digestion digestion
i i
i
1
i
1
ICP ICP
analysis * analysis *
ASTM SRL
extraction extraction
ASTM extract SRL extract
digestion digestion
1
1
I
ICP ICP
analysis * analysis *
* All samples were bench spiked (after digestion) and reanalyzed.
Figure 3-2 Task 2 Extraction and Analysis Scheme
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3.2.2
Lab
Sample No.
2023
2024
2025
2028
Materials
Acids:
Field
Sample No.
OR 089
OR 950
DR 713
DQ 231
EPA
Pre award 1
PEI Sample
Description
Sn Smelter Slag
Pb/Zn Smelter Slag
Cu Smelter Slag
Pb Smelter Slag
Solid Waste
- Baker Reagent Grade HF
- Baker Instra Analyzed HN03
- Baker Ultrex HC104
- Fisher Glacial Acetic Acid
- Fisher Reagent Grade HC1
Mallinckrodt Reagent Grade 30 percent Hgf^
NBS Aqueous Spectrometric Standard Reference Materials
Diamonite mortar and pestle
Dynalon PTFE Teflon beakers
Pyrex glassware (acid cleaned)
Nalgene pressure filtration apparatus
3.2.3 Instrumentation
Orion Research pH meter model 501
Eberbach horizontal extraction shaker
Sybron/Thermolyne 30400 furnace
Mettler 440 analytical balance
Rotary 6 place EP-extraction box
Labconco Micro Kjeldahl digestion rig
Jarrell-Ash 1150 Inductively Coupled Argon Plasma Spectrometer
3.3 Methods
3.3.1 Sample Preparation
There were two solid digestion procedures and four solid/liquid
extraction procedures used in Tasks 1 and 2. Additionally, a liquid
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digestion procedure was required following the solid/liquid extraction.
Outlines of these methods follow with method references provided at the
end of the section.
HF:HC104:HN03 Sample Digestion1 - ("Total")
Sample is pulverized using a mortar and pestle;
Sample is dried at 60° C;
A 0.5 gram sample is weighed into a Teflon beaker;
Five mis of 48 percent HF are added;
Sample is brought to dryness on a steambath;
The residue is transferred to a 100 ml Kjeldahl flask;
Ten ml of a 5:3 HN03:HC104 solution are added;
Sample is heated in a Kjeldahl digestion rig until the
evolution of HC104 fumes;
0 Five ml of HC1 are added and the sample is heated for one
hour; and
The sample is cooled, filtered (if necessary), and brought
to a final volume of 100 ml.
Acid Digestion of Sludges2 - (3050)
One gram of dried sample is weighed into a 150 ml beaker;
t Ten mis of 1:1 HN03 are added and the sample is refluxed for
ten minutes;
Five mis of HNO-j are added and the sample is refluxed for
another 30 minutes;
The sample is cooled and two mis of DI and three mis of
^2 are added;
The sample is heated to promote the peroxide reaction;
Additional H202 is added as needed (10 mis maximum);
The sample is cooled; five mis of 1:1 HC1 and ten mis of
01 are added; the beaker is warmed; and
t The sample is filtered (Whatman No. 41) and brought up to
a final volume of 100 mis.
EP-Toxicitv Test2 - (££)
A 100 g of sample is weighed out and separated into its
component phases by pressure filtration.
The filtrate is stored; the solid portion is placed in
an extraction bottle and 16 times its weight in DI is added.
The sample is extracted over a period of 24 hours in a
rotary extractor; the pH of the extraction fluid is controlled
to a pH of 5.0 with 0.5 N acetic acid. No more than four
mis of extraction fluid per gram of sample is added to the
sample.
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t At the conclusion of the 24 hour period the final volume is
adjusted to 20 times the sample weight.
0 The solid and liquid phases are separated by pressure
filtration and the filtrate is combined with the initial
liquid phase as the EP-leachate.
The sample is now ready for a 6010 digestion and analysis.
EP-Toxicitv Test Without oH Adjustment2 - (EP-w/o)
0 Same procedure as in the previous EP-Toxicity Test without
the addition of the acetic acid for pH adjustment.
ASTM Extraction Procedure3 - (ASJM)
0 350 grams of sample are weighed into an extraction bottle.
0 DI is added at a ratio of 4:1 (1400 mis).
0 The container is closed and inverted at a rate of
25 times/minute for three minutes.
0 The sample is placed on a horizontal extraction shaker and
extracted for 48 hours at 60 to 70 cycles/minute.
0 The solid and liquid phases are separated by pressure
filtration.
0 The sample is now ready for 6010 digestion and analysis.
Synthetic Rainwater Leach - (SRL)
0 Ten grams of sample are weighed out into a plastic
container.
0 Two hundred mis of Synthetic Rainwater (similar to NBS SRM
2694-1) are added. This solution can be purchased :r prepared
as specified in reference 4. The chemicals used to make up this
solution are listed in Table 3-1.
0 The container is closed and placed on a wrist action
shaker for one hour.
0 The sample is centrifuged and filtered.
0 The extract is now ready for 6010 digestion and analysis.
Method 6010 ICP Digestion for Aqueous Samples, oar. 7.32
0 Fifty mis of sample are transferred to a beaker.
0 Three mis of HN03 are added and the sample is evaporated to
near dryness.
0 The sample is cooled and an additional three mis of HN03
are added.
0 The sample are refluxed for one hour.
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10
Table 3-1 Synthetic Rainwater Contents
Concentration in SRL *
Compound (in mg salt/liter)
NaN03 0.491 mg
KN03 0.130 mg
CaCl2 x 2H20 0.057 mg
MgS04 x 7H20 0.205 mg
NH4C1 0.300 mg
H2S04 0.025 mmol
HN03 0.050 mmol
NaF 0.117 mg
* Based on NBS SRM 2694-1. Koch, W.F., Marimenko, G., and Paule,
R.C. 1986 (in publication). Development of a standard reference
material for rainwater analysis. J.Res. NBS (draft) 91(1): .
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11
t Five mis of 1:1 HC1 and ten mis of DI are added and the
beaker Is warmed.
The sample is cooled, filtered if necessary, and brought up
to a final volume of 50 mis.
References:
1. Procedures for handling and chemical analysis of sediment and
water samples. May 1981. Technical Report EPA/COE, CE-81-1.
2. Test methods for evaluating solid wastes, physical/chemical
methods. SW 846, U.S. Environmental Protection Agency, 1982.
3. Shake Extraction of Solid Waste with Water. ASTM Method D 3987-
81.
4. Development of a standard reference material for rainwater
analysis. Koch, W.F., et al. 1986. Journal of Research of the
National Bureau of Standards. Vol. 91, No. 1 (in publication).
3.3.2 ICP Analytical Procedures
Samples are run on a direct reading Jarrell-Ash 1150 Inductively
Coupled Argon Plasma Spectrometer (ICP). The instrument is outfitted
with a sophisticated, computer-controlled (DEC POP 11-23), background
correction and data management system. The spectrometer is currently
configured for simultaneous analysis of 32 elements.
A two-point standard calibration process is followed employing a 3
percent HNC^ blank solution and a standard solution at one or ten mg/L
(depending on the element). Computer-fitted linear regression curves
are calculated for comparison with unknowns.
Samples from each of the six preparation schemes were run in the
following manner. The sample was run straight (IX) and then diluted (if
necessary) and rerun. A dilution on a sample was deemed necessary if
the concentration of any of the six required elements (As, Ba, Cd, Cr,
pb, Ag) were outside their linear range. Dilutions were also performed
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12
when high concentrations of other elements were suspected to interfere
in element quantification. Additionally, samples were spiked with each
with the six elements and were reanalyzed to evaluate the accuracy of
the ICP method on those sample types. Reporting limits for the six
elements can be found in Table 3-2. These limits changed for some
samples when dilution was necessary.
3.3.3 Program Quality Assurance Measures
(1) Task 1. Laboratory quality assurance measures included
preparation blanks, duplicates, and spikes, the frequency of which is
reported in Table 3-3. To obtain the best information on biases due to
sample heterogeneity and preparation/analysis errors, every sample in
the three preparation procedures ("Total", 3050, and EP) was duplicated.
As mentioned previously, all samples were bench spiked to investigate
the accuracy of the ICP method in the study matrices. To check for
instrumental drift and standard accuracy, EPA reference vials were
analyzed prior to each analysis and at a frequency of five percent. If
concentrations of the six elements fell outside of control limits for
the EPA solutions, the analysis was terminated, the problem corrected,
and any samples analyzed up to the failed check sample were reanalyzed.
To assist in verifying the accuracy of the EP-Toxicity Test a QC
sludge sample (EPA Preaward Sample #1) provided by EPA was analyzed. The
sample was prepared and analyzed according to all three procedures.
(2) Task 2. QC frequency for Task 2 is also provided in Table 3-3.
Only one duplicate was analyzed in the EP-w/o, ASTM, and SRL preparation
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13
TABLE 3-2 ANALYTICAL METHODS/REPORTING LIMITS
Element
Arsenic
Barium
Cadmium
Chromium
Lead
Silver
Method
6010 ICP
6010 ICP
6010 ICP
6010 ICP
6010 ICP
6010 ICP
Reporting Limit
mg/1
0.05
0.003
0.004
0.004
0.05
0.01
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14
Table 3-3 Frequency of Quality Control Measures
Preparation
procedure
"3050"
"Total"
EP
EP w/o
ASTM
SRL
Task
1
1
1,2
2
2
2
Number of QC Measurements
Preparation Matrix * Bench **
blanks Duplicates spikes spikes
1
1
1
1
1
1
All samples
All samples
All samples
1
1
1
1
1
0
0
0
0
All
All
All
All
All
All
samples
samples
samples
samples
samples"
samples
* Matrix Spikes - Spikes made into the sample prior to and carried
through preparation procedure.
** Bench Spikes
Spikes made after sample preparation, but prior to
instrumental analysis.
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15
schemes; however, the same frequency of blanks and bench spikes were
analyzed as in Task 1.
4. RESULTS AND DISCUSSION
4.1 Task 1 - Validation of Element Measurements in EP
4.1.1 Task 1 Results and Quality Control Data
Four smelter slag samples and an EPA QC-sludge sample were used in
the study. The slag samples were previously homogenized by PEI and
contained little water. The EPA material was a mud and contained more
than 50 percent water. A physical description of these samples and
their percentage of solid content are provided in Table 4-1.
The analytical data for the "Total", 3050, and EP extracts are
displayed in Table 4-2. In Appendix 1, the final reported value of each
sample is provided, along with the raw unadjusted concentration in the
digestate, dilution factors, and bench spike data.
Preparation blank values were insignificant compared to sample data
and in almost all cases were below detectable limits. Duplicate RPD
values were <20 percent, except for some elements when they were near
the detection limit, and in two cases for Ba in the EP-extract. Matrix
spike recoveries were in the acceptable range of 80 to 120 percent in
the two acid digestion procedures with the following exceptions:
1. Silver recoveries were low and could be due to AgCl precipi-
tation during sample preparation. Additionally, adsorption of
silver to digestate container walls is possible.
2. The Cr spike in the "Total" digestate was high. This was
probably because of the relatively high quantities of Cr in the
sample compared to the spike level.
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16
TABLE 4-1 -Physical Characteristics and Percent Moisture of Study Samples
Sample Physical Characteristics Percent Solids
Sn Smelter Slag Dark grey, dense, equal mixture 99.8
of fine powder and gravel
Pb/Zn Smelter Slag Dark grey to black, porous,gravel 99.9
Cu Smelter Slag Reddish brown, porous, gravel 99.9
Pb Smelter Slag Black, porous, sand to gravel 98.5
EPA Preaward #1 Brownish, silty clay 47.4
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Table 4-2 Element Concentrations in the 3050. "Total", and EP
(Concentrat i on- mg/L)
Arsenic
Barium
Cadmium
Chromium
Lead
Silver
Sample ID
Sn Smelter
Slag
Pb/Zn Smelter
Stag
Cu Smelter
Slag
Pb Smelter
Slag
EPA
Preaward #1
3050 "Total" EP
<50* <200* <0.05
288 144 <0.05
<5 <200* <0.05
<50* <200* <0.05
13700 12800 1.56
3050 "Total" EP
810 912 0.435
3060 3440 2.84
5.1 376 0.075
190 260 0.041
13200 13240 0.62
3050 "Total" EP
<4* 1.00.006
26 20.4 0.035
<0.4 3.2 0.004
70 72 2.34
26400 25200 556
I
3050 "Total" EP | 3050 "Total" EP
I
109 1170 0.005 | 144 144 0.071
1
I
1
<8* 112 <0.004| 17600 18500 35.7
1
|
1
4.2 276 <0.004| <5 26.4 <0.05
1
1
36 412 <0.004| 31400 29000 352
1
1
11000 11000 0.48 (113000 92000 15.5
1
1
1
3050 "Total" EP
1
!<10* <40* <0.01
<20* <40* <0.01
<1 <40* <0.01
<20* <40* <0.01
83 17.6 0.061
EP Toxicity HCL 5.0
100
1.0
5.0
5.0
5.0
'Sample was diluted, which resulted in increased detection limit.
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18
3. Arsenic recovery was low in the "Total" digestate. A loss of As
in the preparation procedure, due to its volatility, is
suspected.
Duplicate results were generally quite good (less than 20 percent
RPD). There were a few exceptions, the most notable of which was the 89
percent RPD for lead in Sn slag after the 3050 digestion. This varia-
tion may be due to a non-homogeneous sample, or contamination during
sample preparation.
QC data are provided in detail in Appendix 2.
All samples were bench spiked to determine the accuracy of the ICP
method on these sample types (see Appendix 1). As can be seen in
Appendix 1, 57 of 64 spike recoveries for the EP, 64 of 72 for the
"Total," and 67 of 72 for the 3050 were in the 80 to 120 percent
recovery range. This indicates that the ICP method is providing an
acceptable data base without any inherent biases for these sample types.
To supplement the quality control procedures used in the method, an
EPA- EP-QC Sludge (Preaward Sample # 1) was obtained and analyzed by all
the preparation schemes. Table 4-3 compares the EPA-EP acceptable
ranges to the observed EP-values for this sample. As can be seen in
the table, several elements fell outside the "Acceptance Range".
EPA has not "certified" these elements, however, and is investigating
the differences between the "true" and observed levels (communication
with Ms. Florence Richardson, EPA-OSW).
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19
Table 4-3 EPA EP-Preaward #1 -
Reference Value, Acceptable Ranges, and Observed Value
Element
Ag*
As*
Ba*
Ca
Cd
Cr*
Hg*
K
Mg
Na
Ni
Pb*
Se
Zn
Observed
value
0.061
1.56
0.62
76.6
556.0
0.48
732.0
86.0
532.0
69.0
15.5
320.0
Reference
value
0.12
12.8
2.4
83.2
717.5
0.16
128.0
827.0
99.7
560.0
78.4
69.2
2.4
362.0
Acceptance range
0.06 -
6.4 -
1.2 -
41.6 -
358.8 -
0.08 -
64.0 -
413.5 -
49.8 -
280.0 -
39.2 -
34.6 -
1.2 -
181.0 -
0.24
25.6
4.8
166.4
1435.0
0.32
256.0
1654.0
199.4
1120.0
156.8
138.4
4.8
724.0
Values for these elements are not "certified." EPA, according to
Ms. Florence Richardson, is investigating difficulties between the
"true" and observed levels of these elements.
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20
4.1.2 Task 1 Discussion
Method 3050 does not totally digest a solid sample, but is really
an acid leaching procedure. Visible solids remained after the
digestion, as well as what appeared to be a gelatinous layer in the four
mining waste samples. Repeating the digestion of one sample using less
sample weight but the same quantities of acids was undertaken to see if
a more thorough digestion of the gelatinous material was possible.
Results indicated that as the sample weight was decreased in the
digestion, slightly higher metal concentrations were observed.
For comparison with the 3050 digestion, a "Total" metals digestion
was carried out with HF:HN03:HC104 acids. No visible solids remained
after this digestion, thus indicating that this was a complete digestion.
In general, for the six elements of interest, the data were roughly
equivalent between the two acid digestions. Chromium was an exception,
where considerably higher concentrations were observed in the "Total"
digestate. This seems to indicate that five of the six elements were
bound in more easily released phases in these samples.
The objective of Task 1 was to compare EP-leachate metal values for
mining and smelting wastes relative to total values. The comparison
showed that, for all six metals, there was a sufficient quantity of
metal in each sample to account for the EP results. This can be seen
for Pb and Cd in Table 4-4, which compares data in the EP-leachate with
the amount that could be potentially extracted from the sample based on
the 3050 digestate levels. The data base, however, is limited and there-
fore may not be indicative of all mining and smelting waste samples.
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21
Table 4-4 Comparison of Metals Released by 3050
Digestion With the EP-Toxicity Test
3050
mg/kg
Sn smelter
slag <5.
Pb/Zn smelter
slag 26
Cu smelter
slag <5.
Pb smelter
slag 70
EPA preaward
#1 26,400
Cadmium
Potential*
EP
mg/1
<0.25
1.3
<0.25
3.4
626
EP
mg/1
<0,05
<0.05
<0.05
2.34
556
3050
mg/1
144
17,600
<5
31,400
113,000
Lead
Potential*
EP
mg/1
7.2
880
<0.25
1,550
2,680
EP
mg/1
0.071
35.7
<0.05
352
15.5
* The Potential EP is the concentration expected in an EP, if all the
metal were released: 3050 value (mg/kg) x percent solids (see Table
4-1) x 0.1 kg total / EP-extract volume (2 L for all samples except
EPA sample, which was 1.809 L).
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22
4.2 Task 2 - Comparisons of Four Extraction Techniques
4.2.1 Task 2 Results and Quality Control Data
The data for samples in the SRL, EP-w/o, and ASTM extractions (EP
results were discussed in the previous section and are also included in
Appendix I) including bench spike, duplicate, and blank results can be
found in Appendix 1. Most bench spike recoveries were within the 80 to
120 percent range, indicating accurate analyte quantitation. Exceptions
outside of this range are as follows:
Extraction
EP-w/o
SRL
SRL
ASTM
ASTM
Samole ID
Pb/Zn Slag
Cu Slag
EPA Preaward 1
Pb/Zn Slag
EPA Preaward 1
Metal (s)
As,
Pb
Ba
As
Ba,
Cr
Cd
Other QC data on calibration blank values, calibration check
standard results, and duplicate RSD are reported in Appendix 2. Of note
here is the relatively poor precision found for duplicates in the SRL.
More detailed study of this new procedure would be necessary to determine
whether the poor precision is inherent in the method or a result of
these particular samples.
Table 4-5 compares data on the five samples by element and extrac-
tion procedure. EP-maximum contaminant levels (MCL) are also provided
in this table. The EPA Preaward #1 and Pb Smelter Slag exceeded MCLs
for both Cd and Pb, and sample Pb/Zn Smelter Slag exceeded the MCL for
-------
Table 4-5 Element Concentrations in the Four Extractions
(Concentration- mg/L)
Arsenic Barium Cadmium
23
Sample ID
EP
EP w/o ASTM SRL
EP
EP w/O ASTM SRL
EP
EP w/o ASTM SRL
Sn Smelter
Slag
Pb/Zn Smelter
Slag
Cu Smelter
Slag
Pb Smelter
Slag
EPA
Preauard #1
<0.05 <0.05 <0.05 <0.05
<0.05 <0.05 <0.05 <0.5 *
(0.05 <0.05 <0.05 <0.05
-------
24
Pb only. N& other MCLs were exceeded by these samples for the six
elements of interest.
4.2.2 Task 2 Discussion
For most elements, the SRL data was greater than or equal to EP
data. The data for these two extractions were generally much greater
than the ASTM and EP-w/o data. The ASTM had levels slightly greater
than those found in the EP-w/o. There were exceptions (As, Ag, Cr)
whera insufficient data (i.e., metal levels less than detection limits)
inhibited an accurate portrayal of these trends. This relationship was
more obvious in comparison of some of the major elements (Fe, Ca, Mg,
Na, Zn) that were quantitated concurrently by the ICP method. The data
for these elements are provided in Table 4-6.
The higher level of elements in the ASTM extract over the EP-w/o
would be expected because of the larger solid to water ratio (i.e., ASTM
was 1:4 solid:water; EP-w/o was 1:20). The larger values in the other
two extractions are not as easily understood, but may be related to the
pH of the extraction fluid. As the pH decreases sample dissolution (e.g.,
metal sulfides and carbonates, colloidal material) or possibly organic
matter destruction could occur, with resultant leachate metal concen-
tration increases. Additionally, cation replacement on surface exchange
sites by H+ would increase as the pH decreases. Table 4-7 reports
initial and final pH values in the four extracts. As can be seen by
comparing the pH data with the metals data in the extracts, the lowest
pH values were in the SRL (pH of extraction fluid 3.98) where the
-------
25
Sample ID
Table 4-6 Other Major Element Concentrations in the Four Extractions
(Conce. ntration- mg/L)
Calcium iron Magnesium
EP
EP w/o ASTM SRL
EP
EP w/O ASTM SRL
EP
EP W/O ASTM SRL
Sn Smelter
Slag
Pb/Zn Smelter
Slag
Cu Smelter
Slag
Pb Smelter
Slag
EPA
Preaward #1
59.3 6.21 22.1 82.1
UO 4.85 3.57 268
1.43 1.08 5.14 2.16
24.8 13 57.8 181
67.9 33.7 106 54.8
28.2 0.13 0.225 59.9
13 0.024 1.05 171
2.39 0.181 0.189 27.9
1.59 0.022 0.239 386
0.143 0.042 0.398 20.5
18.3 2.46 7.15 13.7
6.64 0.266 0.224 16.9
0.374 0.256 1.77 0.818
5.48 1.44 4.29 53
86.2 50.5 236 67.8
Sodium
Sample ID
EP
EP
w/o
ASTM SRL
Zinc
EP
EP w/O ASTM SRL
Sn Smelter
Slag
Pb/Zn Smelter
Slag
Cu Smelter
Slag
Pb Smelter
Slag
EPA
Preaward #1
14 12.6 65.4 19.6
4.1 0.947 2.04 12.1
1.2 1.44 8.34 5.17
2.4 0.946 3.67 22.1
532 326 1620 404
5.62 0.041 0.049 6.65
102 0.026 6.36 324
0.112 0.027 0.034 0.532
159 11.3 8.5 264
312 7.36 12.6 458
-------
26
Table 4-7 Initial and Final pH Measurements in Extracts
EP
Sample no. Initial Final
pH Measurements
EP-w/o ASTM
Initial Final j Initial Final
SRL
Initial Final
EPA pre-
award #1
2023
2024
2025
2028
7.51*
8.72*
6.48*
6.55*
6.52*
4.94
4.90
4.81
5.18
5.10
7.51
8.78
6.51
6.56
6.53
7.15
9.76
9.93
8.73
6.31
7.51
8.80
6.40
6.56
6.53
7.14
8.49
6.75
8.78
6.24
-** 7.05
-** 5.67
-** 5.18
-** 4.92
-** 5.63
* pH adjusted to 5.0 with 0.5 N acetic acid.
** Initial pH was not measured; however, pH of the extraction fluid was 3.98.
-------
27
highest metal concentrations were found. The EP pH values were higher,
as were respective metal concentrations. Conversely, where the highest
pHs were found, the lowest metal values were observed (EP-w/o and the
ASTM). This indicates that the pH of the extraction fluid is a
controlling factor in metal leaching from samples, and not the suspected
affinity of acetic acid for metals such as Pb and Cd.
It is difficult to ascertain whether a laboratory technique can
realistically predict the release of these metals in situ. It would
appear that the acidity of the rainfall at a dumpsite could control the
release of metals from wastes. Since rainfall acidity varies geograph-
ically, it may be impossible to design an absolute test for use in every
situation. The EP-Toxicity Test will continue to serve as a useful
screening procedure for identifying wastes which are potentially
hazardous when disposed of in certain environments. However, the Agency
should develop additional screening tests and procedures, including one
that simulates the effect of acid precipitation on mine and smelter
wastes.
-------
APPENDIX 1
ICP ANALYTICAL DATA
-------
KEY PHRASES FOR APPENDIX 1 TABLES
KEY:
Digestion DF = Dilution factor in acid digestions.
Unadj. Cone. = Unadjusted Concentration readout from ICP.
Dilution Factor = Extract dilution factor prior to ICP quantitation.
Reported Value = Final reported value with dilution factors applied.
Spike Added = Bench spike added prior to ICP analysis.
Obs. Spk. Value = Observed ICP value of bench spiked sample.
% Recovery = Bench spike recovery.
-------
Preparation Procedure: Method 3050
Date: 29-May-86
Page: 1 of 3
CONCENTRATION
Sample
No.
Blank
Sn Smel
Sn Smel
Pb/Zn i
*Digestion DF = 1
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
ter Slag
*Digestion DF =100
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
ter Slag duplicate
*Digestion DF =100
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
smelter Slag
*0igestion DF = 100
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
As
<0.05 <(
1
<0.05 <
0.2
0.178
89%
<0.05
10
<50
200
184
92%
<0.05
10
<50
100
137
137%
1
0.144
20
288
10000
11400
111%
Ba C
D.003 <0.
1
3.003 <0.
0.1
0.1 0.
100%
0.81 <0.
10
810
1500
2120
87%
0.718 <0
10
718
15000
16600
106%
1.53 0
20
3060
100000
118000
115%
d
004 <0
1
004 <0
0.1
092 0.
92%
004 ]
10
<4
200
204
102%
.004 0
10
<4
100
100
100%
.013 <
20
26
1000
1050
102%
Cr
.004
1
.004
0.1
099
99%
.09
1
109
200
283
87%
.119
10
119
2000
2240
106%
0.004
20
<8
200
198
99%
Pb
<0.05 <0
<0.05 <0
0.2
0.21 0.
105%
1.44
-------
Preparation Procedure: Method 3050
Date:
29-May-86
Page: 2 of 3
CONCENTRATION
Sampl
No.
Pb/Zn
Pb/Zn
e
As
Smelter Slag duplicate
*Digestion DF =100
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
Smelter Slag spike
*Digestion DF =100
Unadj. Cone.
Dilution Facto**
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
Cu Smelter Slag
*Digestion DF =100
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
Cu Smelter Slag duplicate
*Digestion DF "100
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
0.158
20
316
10000
11500
112%
0.207
20
414
14000
16000
111%
<0.05
1
<5
Ba Cd
1.49 0
20
2980
100000
123000
120%
2.52 0
20
5040
200000
204000
99%
0.051 <0
1
5.1
400 400
412 412
103% 102%
<0.05
20
<50
Cr
.014 <0.004
20 1
28 <0.4
1000
980
95%
.021 0
20
42
1500
1540
100%
.004 0
20
<0.4
200
216
108%
0.065 <0.004 0
1 20
6.5 <8
400 400
408 408
102% 100%
200
226
113%
200
208
104%
.005
20
10
300
360
117%
.042
1
4.2
400
416
103%
.073
1
7.3
Pb Ag units
7.66 <0
20
15300
600000
752000
123%
12.3 <0
20
24600
1000000
1190000
117%
<0.05 <0
1
<5
400
396
99%
.01 mg/L
1
<1 mg/kg
400 mg/kg
350 mg/kg
88%
.01 mg/L
20
<20 mg/kg
400 mg/kg
354 mg/kg
89%
.01 mg/L
1
<1 mg/kg
400 mg/kg
372 mg/kg
93%
<0.05 <0.01 mg/L
20 20
<100 <20 mg/kg
400 400
414 400
102% 100%
400 mg/kg
348 mg/kg
87%
* Digestion Dilution Factor » l.Ogm/lOOmL
-------
Preparation Procedure: Method 3050
Date:
29-May-86
Page: 3 of 3
CONCENTRATIO
Sample
No.
Pb Smelter Slag
*0igestion DF =100
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
Pb Smelter Slag duplicate
*Digestion DF =100
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
EPA Preaward #1
*Digestion DF -100
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
EPA Preaward #1 duplicate
*D1gestion DF -100
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
As Ba Cd Cr Pb Ag units
<0.05 0.095 0.035 0.018 15.7 <0.01 mg/L
20 20 20 20 20 20
<50 190 70 36 31400 <20 mg/kg
400 7000 2400 1200 1200000 400 mg/kg
586 7500 2700 1280 1620000 382 mg/kg
147% 104% 110% 104% 132% 96%
<0.05 0.098 0.041 0.02 16.9 <0.01 mg/L
20 20 20 20 20 20
<50 196 82 40 33800 <20 mg/kg
400 7000 2400 1200 1200000 400 mg/kg
572 7320 2740 1280 1460000 364 mg/kg
143% 102% 111% 103% 119% 91%
13.7 13.2 26.4 11 56.6 0.083 mg/L
10 10 10 10 20 10
13700 13200 26400 11000 113000 83 mg/kg
25000 25000 50000 25000 4400000 1600 mg/kg
36400 36900 72400 34600 4860000 1370 mg/kg
91% 95% 92% 94% 108% 80%
7.21 7 13.8 5.94 58.6 0.042 mg/L
20 20 20 20 20 20
14400 14000 27600 11900 117000 84 mg/kg
50000 50000 100000 50000 4120000 3400 mg/kg
66000 62400 123000 59800 4760000 2660 mg/kg
103% 97% 95% 96% 113% 76%
Digestion Dilution Factor - l.Ogm/lOOmL
-------
Preparation Procedure: Total Digestion
Date: 28-May-86
CONCENTRATION
Page: 1 of 3
Sample
No.
Blank
Sn Smel
Sn Smel
As
*Digestion DF = 1
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
ter Slag
*Digestion DF = 200
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
ter Slag duplicate
*Digestion DF =200
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
Pb/Zn Smelter Slag
*Digestion DF =200
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
<0.05
1
<0.05
0.1
0.091
91%
<0.05
20
<200
800
856
107%
<0.05
20
<200
800
812
102%
<0.05
20
<200
6000
6920
115%
Ba
0.122 <0
1
0.122 <0
0.25
0.37 0
99%
0.228 0
20
912
36000
38000
103%
0.23 0
20
920
36000
38800
105%
0.86 0
20
3440
128000
144000
110%
Cd
.004
1
.004
Cr
0.005
1
0.005
0.1 0.1
.102 0.105
102% 100%
.005
1
1
0.292
20
1170
400 40000
436 42800
109% 104%
.009
1
1.80
0.285
20
1140
400 40000
428 44000
107% 107%
.102
1
20.4
800
880
107%
0.028
20
112
4000
4720
115%
Pb
0.057
1
0.057
Ag
<0.01
1
<0.01
units
mg/L
mg/L
0.2 0.2 mg/L
0.238 0.178 mg/L
91% 89%
0.722
1
144
<0.01
20
<40
mg/L
mg/kg
6000 800 mg/kg
6360 644 mg/kg
104% 81%
0.748
1
150
<0.01
20
<40
mg/L
mg/kg
6000 800 mg/kg
6440 680 mg/kg
105% 85%
4.62
20
18500
680000
756000
108%
<0.01
20
<40
mg/L
mg/kg
800 mg/kg
684 mg/kg
86%
* Digestion Dilution Factor - 0.5gm/100ml
-------
Preparation Procedure: Total Digestion
Date:
28-May-86
Page: 2 of 3
CONCENTRATION
Sampl
No.
Pb/Zn
Pb/Zn
e
As
Smelter Slag duplicate
*Digestion DF =200
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
Smelter Slag spike
*Digestion DF «200
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
Cu Smelter Slag
*Digestion OF =200
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
Cu Smelter Slag duplicate
*Digestion DF =200
Unadj, Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
0.762
1
152
6000
7200
117%
0.073
20
292
Ba
0.897
20
3590
128000
144000
110%
1.83
20
7320
12000 280000
14200 316000
116% 110%
<0.05
20
<200
0.094
20
376
400 16000
456 21900
114% 135%
<0.05
20
<200
0.096
20
384
400 16000
396 22300
99% 137%
Cd
0.006
20
24
800
860
105%
0.011
20
44
1600
1770
108%
0.016
1
3.2
400
396
98%
0.018
1
3.6
400
424
105%
Cr
0.03
20
120
4000
4760
116%
0.04
20
160
6000
6920
113%
0.069
20
276
12000
15400
126%
0.072
20
288
Pb
Ag
5.12 <0.01
20 20
20500 <40
680000
760000
109%
units
mg/L
mg/kg
800 mg/kg
672 mg/kg
84%
8.34 0.025
20 1
33400 5.0
1200000
1630000
133%
0.132
1
26.4
1200
1150
94%
<0.05
1
<10
12000 1200
15300 1130
125% 94%
800
712
88!
<0.01
20
<40
mg/L
mg/kg
mg/kg
mg/kg
/.
mg/L
mg/kg
800 mg/kg
712 mg/kg
89%
<0.01
20
<40
mg/L
mg/kg
800 mg/kg
676 mg/kg
85%
* Digestion Dilution Factor » 0.5gm/100ml
-------
Preparation Procedure: Total Digestion
Date:
28-May-86
Page: 3 of 3
CONCENTRATION
Sa
Pb
Pb
EPA
EPA
mple
No.
Smelter Slag
*Digestion DF =200
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
Smelter Slag duplicate
*Digestion DF =200
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
Preaward #1
*Digestion DF =200
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
Preaward #1 duplicate
*Digestion DF =200
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
As
<0.05
20
<200
800
1030
129%
<0.05
20
<200
800
952
119%
3.2
20
12800
28000
43200
109%
3.39
20
13600
28000
44400
110%
Ba
0.065
20
260
12000
16900
139%
0.07
20
280
12000
12300
100%
3.31
20
13200
28000
42400
104%
2
20
8000
16000
24600
104%
Cd
0.018
20
72
2400
2490
101%
0.02
20
80
2400
2430
98%
6.29
20
25200
52000
83200
112%
6.24
20
25000
52000
82400
110%
Cr
0.103
20
412
14000
17800
124%
0.102
20
408
14000
14700
102%
2.74
20
11000
24000
36000
104%
2.62
20
10500
24000
35400
104%
Pb
7.26
20
29000
1000000
1470000
144%
7.13
20
28500
1000000
1080000
105%
23
20
92000
200000
305000
107%
27.3
20
109000
220000
342000
106%
Ag
<0.01
20
<40
800
668
84?
<0.01
20
<40
800
692
87'
0.088
1
17.6
800
732
89
0.04
1
8.0
800
660
82'
units
mg/L
nig/ kg
mg/kg
mg/kg
',
mg/L
mg/kg
mg/kg
mg/kg
Y,
mg/L
mg/kg
mg/kg
mg/kg
y.
mg/L
mg/kg
mg/kg
mg/kg
4
Digestion Dilution Factor « 0.5gm/100ml
-------
Preparation Procedure: EP TOXICITY TEST
Date:
29-May-86
Page: 1 of 3
CONCENTRATION
(units - mg/L)'
Sample
No.
Blank
Sn Smel
Sn Smel
As Ba Cd Cr
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
ter Slag
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
ter Slag duplicate
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
Pb/Zn Smelter Slag
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
<0.05 <0
1
<0.05 <0
0.1
0.097 0
97%
<0.05 0
1
<0.05 0
0.1
0.089
89%
<0.05 0
1
<0.05 0
0.2
0.183
92%
<0.05
1
<0.05
0.2
0.218
109%
.003 <0
1
.003 <0
0.1
.098 0
98%
.435 0
1
.435 0
1
1.45 0
102%
.431 <0
1
.431 <0
1
1.45 0
102%
2.84 0
1
2.84 0
6
8.59 0
96%
.004 <0
1
.004 <0
0.1
.094 0
94%
-
.006 0
1
.006 0
0.1
.101 0
95%
.004 <0
1
.004 <0
0.1
.094
94%
.035 <0
1
.035 <0
0.1
.128 0
93%
.004
1
.004
0.1
.096
96%
.005
1
.005
0.1
.098
93%
.004
1
.004
0.1
0.1
100%
.004
1
.004
0.1
.095
95%
Pb
<0.05
1
<0.05
0.2
0.164
82%
0.071
1
0.071
0.3
0.335
88%
<0.05
1
<0.05
0.2
0.197
99%
35.7
1
35.7
70
103
96%
Ag
<0.01
1
<0.01
0.2
0.168
84%
<0.01
1
<0.01
0.2
0.172
86%
<0.01
1
<0.01
0.2
0.169
85%
<0.01
1
<0.01
0.2
0.167
84%
-------
Preparation Procedure: EP TOXICITY TEST
Date:
Sample
No.
29-May-86
Page: 2 of 3
CONCENTRATION
(units - mg/L)
As
Ba
Cd
Cr
Pb
Ag
Pb/Zn Smelter Slag duplicate
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
<0.05 2.67 0.037 <0.004
1111
<0.05 2.67 0.037 <0.004
0.2 6 0.1 0.1
0.228 8.64 0.132 0.092
114% 100% 95% 92%
36.9 <0.01
1 1
36.9 <0.01
70 0.2
105 0.167
97% 84%
Cu Smelter Slag
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
<0.05 0.075 <0.004 <0.004 <0.05 <0.01
1111 11
<0.05 0.075 <0.004 <0.004 <0.05 <0.01
0.2 0.2 0.1 0.1 0.2 0.2
0.165 0.259 0.094 0.098 0.177 0.17
83% 92% 94% 98% 89% 85%
Cu Smelter Slag duplicate
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
<0.05 0.047 0.009 <0.004 <0.05 <0.01
1111 11
<0.05 0.047 0.009 <0.004 <0.05 <0.01
0.2 0.2 0.1 0.1 0.2 0.2
0.179 0.232 0.097 0.098 0.175 0.164
90% 93% 88% 98% 88% 82%
Pb Smelter Slag
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
<0.05 0.041 0.117 <0.004
1 1 20 1
<0.05 0.041 2.34 <0.004
17.6 <0.01
20 1
352 <0.01
4 2 80 2 12000 4
5.06 2.04 93.4 1.98 13760 3.42
127% 98% 114% 99% 112% 86%
-------
Preparation Procedure: EP TOXICITY TEST
Date:
29-May-86
Page: 3 of 3
CONCENTRATION
(units = mg/L)
Sample
No.
Pb Smel
As
ter Slag dupl icate
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
EPA Preaward #1
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
EPA Preaward #1 duplicate
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
<0.05
1
<0.05
4
5.26
132%
0.078
20
1.56
60
77.2
126%
0.081
20
1.62
60
63.8
104%
Ba
0.057
1
0.057
2
2.04
99%
0.031
20
0.62
22
28.8
128%
0.032
20
0.64
22
29
129%
Cd
0.087 <0
20
1.74 <0
60
70.2
114%
Cr
.004
1
.004
2
2.04
102%
27.8 0.024
20 20
556 0.48
22000
23500
104%
20
22.8
112%
27.2 0.026
20 20
544 0.52
22000
23800
106%
20
23.6
115%
Pb
21.2
20
424
16000
18800
115%
0.773
20
15.5
540
776
141%
0.807
20
16.1
580
620
104%
Ag
<0.01
1
<0.01
4
3.14
79%
0.061
1
0.061
4
3.48
85%
0.054
1
0.054
4
3.56
88%
-------
Preparation Procedure: EP TOXICITY TEST WITHOUT pH ADJUSTMENT
Date:
Sample
No.
29-May-86
Page: 1 of 2
CONCENTRATION
(units = mg/L)
As
Ba
Cd
Cr
Pb
Blank
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
<0.05 <0.003 <0.004 <0.004 <0.05 <0.01
1111 1 1
<0.05 <0.003 <0.004 <0.004 <0.05 <0.01
0.1 0.1 0.1 0.1 0.2 0.2
0.104 0.1 0.097 0.102 0.223 0.181
104%' 100% 97% 102% 112% 91%
Sn Smelter Slag
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
<0.05 0.095 <0.004 0.007 <0.05 <0.01
1111 1 1
<0.05 0.095 <0.004 0.007 <0.05 <0.01
0.1 0.2 0.1 0.1 0.2 0.2
0.098 0.295 0.093 0.103 0.179 0.174
98% 100% 93% 96% 90% 87%
Sn Smelter Slag duplicate
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
<0.05 0.112 <0.004 0.007 <0.05 <0.01
1111 1 1
<0.05 0.112 <0.004 0.007 <0.05 <0.01
0.1
0.117
117%
0.2 0.1 0.1 0.2 0.2
0.3 0,095 0.106 0.185 0.176
94% 95% 99% 93%
Pb/Zn Smelter Slag
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
<0.05 0.363 <0.004 <0.004 <0.05
-------
Preparation Procedure: EP TOXICITY TEST WITHOUT pH ADJUSTMENT
Date:
29-May-86
Page: 2 of 2
CONCENTRATION
(units = mg/L)
Sa
Cu
Pb
EPA
mple
No.
Smelter Slag
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
Smelter Slag
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
Preaward #1
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
As
<0.05
1
<0.05
0.1
0.105
105%
<0.05
1
<0.05
0.1
0.1
100%
0.073
1
0.073
0.2
0.253
90%
Ba
0.047 <0
1
0.047 <0
0.1
0.147
100%
0.054
1
0.054
0.1
0.152
98%
0.281
1
0.281
0.6
0.826
91%
Cd
.0
.0
0
0
1
1.
1.
3.
1
3
8
27
1
04 <0
1
04 <0
.1
.1 0
00%
08 <0
1
08 <0
2
43 0
18%
.4 0
1
.4 0
17
.8 0
14%
Cr
.004
1
.004
0.1
.104
104%
.004
1
.004
0.1
.111
111%
.011
1
.011
0.1
.102
91%
Pb
<0.05
1
<0.05
0.2
0.182
91%
4.65
1
4.65
10
14.1
95%
0.236
1
0.236
0.5
0.663
85%
Ag
<0.01
1
<0.01
0.2
0.18
90
<0.01
1
<0.01
0.2
0.181
91'
0.028
1
0.028
0.2
0.206
89'
'/o
i
y.
-------
Preparation Procedure: ASTM EXTRACTION
Date:
Sample
No.
29-May-86
Page: 1 of 2
CONCENTRATION
(units = mg/L)
As
Ba
Cd
Cr
Pb
Ag
Blank
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
<0.05 <0.003 0.005 <0.004 <0.05 <0.01
1111 11
<0.05 <0.003 0<005 <0.004 <0.05 <0.01
0.1 0.1 0.1 0.1 0.2 0.2
0.097 0.1 0.099 0.104 0.199 0.178
97% 100% 94% 104% 100% 89%
Sn Smelter Slag
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
0.05 0.063 <0.004 0.008 <0.05 <0.01
1111 11
0.05 0.063 <0.004 0.008 <0.05 <0.01
0.1 0.15 0.1 0.1 0.2 0.2
0.146 0.211 0.098 0.105 0.181 0.176
96% 99% 98% 97% 91% 88%
Pb/Zn Smelter Slag
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
<0.05 0.217
1 1
<0.05 0.217
0.065 <0.004
1 1
0.065 <0.004
0.1 0.4 0.1 0.1
0.133 0.607 0.165 0.101
133% 98% 100% 101%
8.94 <0.01
1 1
8.94 <0.01
18 0.2
30.4 0.187
119% 94%
Cr Smelter Slag
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
<0.05 0.042 <0.004 <0.004 <0.05 <0.01
1111 11
<0.05 0.042 <0.004 <0.004 <0.05 <0.01
0.1 0.1 0.1 0.1 0.2 0.2
0.081 0.14 0.095 0.101 0.183 0.178
81% 98% 95% 101% 92% 89%
-------
Preparation Procedure: ASTM EXTRACTION
Date:
29-May-86
Page: 2 of 2
CONCENTRATION
(units - mg/L)
Sa
Cu
Pb
EPA
mple
No.
Smelter Slag duplicate
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
Smelter Slag
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
Preaward #1
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
As
<0.05
1
<0.05
0.2
0.17
85%
<0.05
1
<0.05
0.2
0.182
91%
0.55
1
0.55
22
26.3
117%
Ba
0.0
0.0
0
0.1
1
0.0
0.0
0
0.1
0.0
0.
1
32 <0
1
32 <0
.1
32
00%
39
1
39
.1
38
98%
23
20
46
20
29
43%
Cd
.0
.0
0
0
1
1.
1.
8.
1
1
8
12
1
04
1
04
.1
.1
00%
98
1
98
4
36
14%
.0
20
20
00
00
48%
Cr
0.0
0.0
0
0.1
1
0.0
0.0
0
0.1
0.0
0.
10
06
1
06
.1
17
11%
05
1
05
.1
04
99%
12
20
24
10
.1
99%
Pb
<0.0
<0.0
0
0.
3.
3.
13
1
0.1
3
1
1
1
5
1
5
.2
19
95%
64
1
64
8
.7
12%
65
20
.3
20
37
11%
Ag
<0.01
1
<0.01
0.2
0.181
91%
<0.01
1
<0.01
0.2
0,184
92%
0.146
1
0.146
6
5.36
87%
-------
Preparation Procedure: SYNTHETIC RAINWATER LEACH (SRL)
Date:
29-May-86
Page: 1 of 2
CONCENTRATION
(units = mg/L)
Sampl
No.
Blank
Sn Sme
Pb/Zn
Pb/Zn
e
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
Her Slag
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
Smelter Slag
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
Smelter Slag duplicate
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
As
<0.05 <0
1
<0.05 <0
0.2
0.192 0
96%
<0.05
1
<0.05
0.2
0.21
105%
<0.05 0
20
<0.5
20
22.7
114%
0.31 C
1
0.31
12
12.6
102%
Ba
.003 <0
1
.003 <0
0.1
.099 0
99%
1.18 <0
1
1.18 <0
3
4.03 0
95%-
.378
20
7.56
300
317
103%
1.152 C
20
3.04 C
120
129
105%
Cd (
.004 <0
1
.004 <0
0.1
.095 0
95%
.004 0
1
.004 0
0.1
.098 0
98%
0.02 0
1
0.02 0
2
2.12
105%
.025 0
1
1.025 0
2
2.12
105%
:r
.004
1
.004
0.1
.096
96%
.025
1
.025
0.1
.123
98%
.006
1
.006
2
2.1
105%
.005
1
.005
2
2.13
106%
Pb
<0.05
1
<0.05
0.2
0.169
85%
0.632
1
0.632
1.3
1.84
93%
2.76
20
55.2
2000
2180
106?
1.62
20
32.4
1200
1340
109?
Ag
<0.001
1
<0.001
0.2
0.177
89%
<0.001
1
<0.001
0.2
0.17
85%
<0.001
20
<0.2
4
3.57
89%
<0.01
20
<0.2
4
3.76
>, 94%
-------
Preparation Procedure: SYNTHETIC RAINWATER LEACH (SRL)
Date:
29-May-86
Page: 2 of 2
CONCENTRATION
(units = mg/L)
Sample
No.
Ca Smelter Slag
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
Pb Smelter Slag
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
EPA Preaward #1
Unadj. Cone.
Dilution Factor
Reported Value
Spike Added
Obs. Spk. Value
% Recovery
As
<0.05
1
<0.05
0.2
0.172
86%
<0.05
20
<1.
4
5.08
127%
6.98
20
140
280
462
115%
Ba
0.769 <0
1
0.769 <0
1.5
2.37 0
107%
0.052
20
1.04
40
45
110%
0.029
20
0.58
20
30.4
149%
Cd
.004
1
.004
0.1
.096
96%
0.07
20
1.4
60
64.2
105%
29.7
20
594
1200
1970
115%
Cr
0.005
1
0.005
0.1
0.105
100%
0.025
1
0.025
2
2.2
109%
3.07
20
61.4
120
183
101%
Pb
0.112
1
0.112
0.2
0.258
73%
11.1
20
222
9000
9900
108%
43.4
20
868
2000
3120
113%
Ag
<0.01
1
<0.01
0.2
0.172
86%
<0.01
20
<0.2
4
3.68
92%
0.063
1
0.063
4
3.6
88%
-------
APPENDIX 2
QUALITY CONTROL DATA
-------
METALS QUALITY ASSURANCE
3050 DIGESTION PROCEDURE
VERSAR INC.
Date: 29-May-86
Reference
Standard
CALB. BLK.
REG. BLK.l
REG. BLK. 2
Check
Standard
SPIKE 1
Field #:
Pb/Zn Slag
(mg/ kg)
Found
True
% Recovery
Results
Results
Results
Found
True
% Recovery
Samp, value
Spike value
Spike added
% Recovery
(units=mg/L)
ARSENIC
0.284
0.281
101%
<0.05
<0.05
0.309
0.281
110%
288
414
100
126%
Batch:
BARIUM
6.444
0.460
97%
<0.003
<0.003
0.4
0.460
95%
3060
5040
2000
99%
' 939.042
CADMIUM |
0.235 |
0.244 |
96% |
<0.004 |
<0.004 |
1
0.258 |
0.244 |
106%|
26 |
42 |
10 |
160% |
Reference
Standard
CALB. BLK.
REG. BLK.l
REG. BLK. 2
Check
Standard
SPIKE 1
Field #:
Pb/Zn Slag
(mg/kg)
(
Found
True
% Recovery
Results
Results
Results
Found
True
% Recovery
Samp, value
Spike value
Spike added
% Recovery
units*mg/L)
CHROMIUM
0.298
0.313
95%
<0.004
<0.004
0.31
0.313
99%
<8
10
10
100%
LEAD
0.492
0.488
101%
<0.05
<0.05
0.50
0.488
102%
17600
24600
7000
100%
SILVER
0.048
0.052
92%
<0.01
<0.01
0.048
0.052
92%
<20
<20
10
NC
Comments: * See page 2 for duplicate results
NC » not calcuable
-------
V E R S A R INC.
METALS QUALITY ASSURAMCE
3C50 DIGESTION PROCEDURE (page 2)
DUPLICATE PRECISION FORM
(units=mg/kg)
Date:
Batch:
29-May-86
939.042
DUPLICATE 1
Field *:
Sn Slag
DUPLICATE 2
Field it:
Pb/Zn Slag
DUPLICATE 3
Field #:
Cu Slag
DUPLICATE 4
Field #:
Pb Slag
DUPLICATE 5
Field #:
EPA PREAUARD
#1
I
I.
I
1
Samp, value)
Dup. value |
RPO |
1
Samp, value)
Dup. value |
RPD |
1
Samp, value)
Dup. value |
RPD |
1
Samp, value)
Dup. value |
RPO |
1
Samp, value)
Dup. value |
RPD |
ARSENIC
<50
<50
NC
288
316
9X
<5.
<50.
NC
<50
<50
NC
13700
14400
5X
BARIUM |
I
I
810 |
718 |
12X|
I
3060 I
2980 I
3X|
I
5.1 |
6.5 |
24X|
I
190 |
196 |
3*l
I
13200 |
14000 |
6%)
CADMIUM
<4
<4
NC
26
28
7X
<0.4
<8
NC
70
82
16X
26400
27600
4X
CHROMIUM |
1
1
109 |
119 |
9X|
I
<8 |
<0.4 |
NC |
I
4.2 |
7.3 |
54X|
I
36 |
40 |
11X|
I
11000 |
11900 |
8X|
LEAD |
'
I
144 |
375 |
89X|
I
17600 |
15300 |
-14X|
1
<5 I
<100 |
NC |
I
31400 |
33800 |
7X|
I
113200 |
117200 |
3X|
SILVER
<10
<10
NC
<20
<1.
NC
<1.
<20.
NC
<20
<20
NC
33
84
W|
Comments: NC-Not calculated due to values below detection limit
-------
V E
METALS QUALITY ASSURANCE
TOTAL DIGESTION PROCEDURE
. S A R INC.
Date: 29-May-86
Reference
Standard
CALB. BLK.
REG. BLK.l
REG. BLK. 2
Check
Standard
SPIKE 1
Field #:
Pb/Zn Slag
(mg/kg)
(
| Found
JTrue
|% Recovery
(Results
(Results
[Results
I
j Found
JTrue
j% Recovery
. ._
I
|Samp. value
j Spike value
j Spike added
|% Recovery
.1
units=mg/L)
ARSENIC
0.287
0.281
102%
<0.05
<0.05
<0.05
0.298
0.281
106%
144
292
400
37%
Batch:
BARIUM
i
0.438
0.460
95%
<0.003
0.122
<0.003
0.438
0.460
| 95%
3440
7320
4000
97%
939.042
.CADMIUM
0.250
0.244
102%
<0.004
<0.004
<0.004
0.235
0.244
96%
20
44
20
120%
(units=mg/L)
Reference
Standard
CALB. BLK.
REG. BLK.l
REG. BLK. 2
Check
Standard
SPIKE 1
Field #:
Pb/Zn Slag
(mg/kg)
(Found
(True
|% Recovery
(Results
(Results
(Results
1
| Found
(True
|% Recovery
i .,_
1
(Samp, value
(Spike value
(Spike added
|% Recovery
CHROMIUM
0.300
0.313
96%
<0.004
0.005
<0.004
0.31
0.313
99%
112
160
[ 20
| 240%
LEAD
0.473
0.488
97%
<0.05
0.057
<0.05
0.486
0.488
| 100%
j 18500
33400
14000
| 106%
SILVER
0.049
0.052
94%
<0.01
<0.01
<0.01
0.051
0.052
98%
<40.
5
20
25%
Comments: * See page 2 for duplicate results
-------
METALS QUALITY ASSURANCE
VERSAR IMC.
TOTAL DIGESTION PROCEDURE (page 2)
DUPLICATE PRECISION FORM
Date:
Batch:
29-May-86
939.042
DUPLICATE 1
Field #:
Sn Slag
DUPLICATE 2
Field #:
Pb/Zn Slag
DUPLICATE 3
Field #:
Cu Slag
DUPLICATE 4
Field #:
Pb Slag
DUPLICATE 5
Field #:
EPA PREAUARD
#1
I
(.
[
I !
{Samp, value)
|Dup. value |
IRPO [
I I
| Samp, value)
|Dup. value |
|RPO |
I
I I
| Samp, value)
|Dup. value |
IRPD |
I I
| Samp, value)
|Dup. value |
IRPD |
I I
| Samp, value)
|Dup. value |
IRPD |
. i
(units=mg/kg)
ARSENIC
<200
<200
NC
<200
152
NA
<200
<200
NC
<200
<200
NC
12800
13600
BARIUM | CADMIUM CHROM
I
I
I
IUM LEAD SILVER
912 | 1 1170 | 144 <40
920 | 1.8 1140 | 150 | <40
155) 57X|
I
3440 | 20
3590 | 24
4X| 18X|
I
376 | 3.2
384 | 3.6 |
2X| 12X|
1 1
260 | 72 |
280 | 80
7%) m|
1 1
13200 | 25200 | 1
8000 | 25000 | 1
6%) -49X) -1%)
3X| 4X| NC
I
112 | 18500 <40
120 20500 <40
7%) 10X| NC
I
276 26 <40
288 <10 | <40
4%) NC | NC
I
412 | 29000 <40
408 | 28500 <40
-1X| -2X| NC
I I
1000 92000 | 17.6
3500 109200 | 8
5X| 17X| -75X
Comments: NC-Not calculated due to values below detection limit
-------
METALS QUALITY ASSURANCE
EP TOXICITY EXTRACTION
V E R S A R INC.
Reference
Standard
CALB. BLK.
REG. BLK.l
REG. BLK. 2
__
Check
Standard
Found
True
% Recovery
Results
Results
Results
Found
True
% Recovery
(units-mg/L)
| ARSENIC
j
| 0.288
| 0.281
| 102%
| <0.05
| <0.05
1
Date: 29-May-86
Batch: 939.042
BARIUM | CADMIUM \
j
0.44 | 0.236 |
0.460 | 0.244 |
96% | 97% |
<0.003
<0.003
1
I 0.305 | 0.45
| 0.281 | 0.460
| 109%| 98%
<0.004 1
<0.004
0.252
0.244
103%
(units=mg/L)
Reference
Standard
CALB. BLK.
REG. BLK.l
REG. BLK. 2
Check
Standard
| Found
(True
|% Recovery
1
| Results
(Results
(Results
1
(Found
(True
|% Recovery
CHROMIUM |
._
0.302 |
0.313 |
96% |
<0.004 |
<0.004 j
1
0.31 |
0.313 |
99% |
LEAD
0.488
0.488
100%
<0.05
<0.05
0.514
0.488
105%
SILVER
0.049
0.052
94%
<0.01
<0.01
0.05
0.052
96%
Comments: * See page 2 for duplicate results
-------
METALS QUALITY ASSURANCE
V E R S A R INC.
EP TOXIC I TY EXTRACTION (page 2)
DUPLICATE PRECISION FORM
Date:
Batch:
29-May-86
939.042
DUPLICATE 1
Field #:
Sn Slag
DUPLICATE 2
Field #:
Pb/Zn Slag
DUPLICATE 3
Field #:
Cu Slag
DUPLICATE 4
Field #:
Pb Slag
DUPLICATE 5
Field tf:
EPA PREAUARD
#1 t
Samp, value
Dup. value
RPO
Samp, value
Dup. value
RPD
Samp, value
Dup. value
RPD
Samp, value
Dup. value
RPD
'
Samp, value
Dup. value
RPD
ARSENIC
<0.05
<0.05
NC
<0,05
<0.05
NC
<0.05
<0.05
NC
<0.05
<0.05
NC
1.56
1.62
4X
(units*
BARIUM |
1
1
1
0.435 |
0.431 |
1X|
1
2.84 1
2.67 j
-6X|
1
0.075 |
0.047 |
46X|
1
0.041 |
0.057 |
33XJ
I
0.62 |
0.64 |
3X|
mg/L)
CADMIUM
0.006
<0.004
NC
0.035
0.037
6X
<0.004
0.009
NC
2.34
1.74
29%
556
544
-a
CHROMIUM |
1
1
0.005 |
<0.004 |
NC |
1
<0.004 |
<0.004 |
NC |
1
<0.004 |
<0.004 |
NC |
1
<0.004 |
<0.004 |
NC |
1
0.48 |
0.52 |
8X|
LEAD
0.071
<0.05
NC
35.7
36.9
3%
<0.05
<0.05
NC
352
424
19%
15.5
16.1
4X
SILVER
<0.01
<0.01
NC
<0.01
<0.01
NC
-
<0.01
<0.01
NC
<0.01
<0.01
NC
0.061
0.054
12X|
Comments: NC-Not calculated due to values below detection limit
-------
METALS QUALITY ASSURANC
EP TOX TEST WITHOUT ACID
V E R S A R
Reference
Standard
CALB. BLK.
REG. BLK.l
REG. BLK. 2
Check
Standard
DUPLICATE 1
Field #:
Sn Slag
I N C.
Found
True
% Recovery
Results
Results
Results
Found
True
% Recovery
Samp, value
Dup. value
RPD
(units=mg/L)
ARSENIC
0.298
0.281
106%
<0.05
<0.05
0.293
0.281
104%
<0.05
<0.05
NC
Date:
Batch:
BARIUM
0.438
0.460
95%
<0.003
<0.003
0.443
0.460
96%
0.095
0.112
16%
29-May-86
939.042
CADMIUM
0.235
0.244
96%
<0.004
<0.004
0.242
0.244
99%
<0.004
<0.004
1 NC
Reference
Standard
....... ....
CALB. BLK.
REG. BLK.l
REG. BLK. 2
Check
Standard
DUPLICATE 1
Field #:
Sn Slag
Found
True
% Recovery
Results
Results
Results
Found
True
% Recovery
Samp, value
Dup. value
RPD
(units«mg/L)
CHROMIUM |
.... .
0.31 |
0.313 |
99%|
<0.004 |
<0.004 |
0.316 |
0.313 I
ioi%|
1
0.007 |
0.007 |
0% |
LEAD
0.486
0.488
100%
<0.05
<0.05
0.497
0.488
102%
<0.05
<0.05
NC
SILVER |
... ....
0.051 !
0.052 |
98% |
<0.01
<0.01
0.052
0.052
100%
<0.01
<0.01
NC
Comments: NC-RPD is not calculated when the sample or duplicate
value is less than the detection limit.
-------
METALS QUALITY ASSURANCE
ASTM EXTRACTION PROCEDURE
V E R S A R INC.
(units=mg/L)
Date:
Batch:
29-May-86
939.042
Reference
Standard
CALB. BLK.
REG. BLK.l
REG. BLK. 2
Check
Standard
DUPLICATE 1
Field #:
Cu Slag
Found
True
% Recovery
Results
Results
Results
Found
True
% Recovery
Samp, value
Dup. value
RPD
ARSENIC
0.305
0.281
109%
<0.05
<0.05
0.305
0.281
109%
<0.05
<0.05
NC
BARIUM
0.45
0.460
98%
<0.003
<0.003
0.446
0.460
| 97%
1
| 0.042
| 0.032
| -27%
CADMIUM
0.252
0.244
103%
<0.004
0.005
0.262
0.244
107%|
<0.004
<0.004
1 NC |
(units=mg/L)
CHROMIUM
LEAD
SILVER
Reference
Standard
Found
True
|% Recovery
CALB. BLK.
REG. BLK.l
REG. BLK. 2
Check
Results
Results
Results
Found
Standard (True
|% Recovery
DUPLICATE 1
Field #: |Samp. value
Cu Slag |Dup. value
|RPD
0.31
0.313
99%
<0.004
<0.004
0.322
0.313
-- I---
0.514 |
0.488 |
105%|
<0.05 |
<0.05 |
1
0.533 |
0.488 1
103%| 109%|
<0.004
0.006
NC
1
<0.05 |
<0.05 |
NC |
1
0.05 |
0.052 |
96% |
<0.01 |
<0.01 |
1
0.05 |
0.052 |
96% |
1
<0.01 |
<0.01 |
NC |
Comments: NC-RPD is not calculated when the sample or duplicate
value is less than the detection limit.
-------
METALS QUALITY ASSURANC
SRL EXTRACTION PROCEDURE
V E R S A R
Reference
Standard
CALB. BLK.
REG. BLK.l
REG. BLK. 2
Check
Standard
DUPLICATE 1
Field #:
Pb/Zn Slag
Reference
Standard
CALB. BLK.
REG. BLK.l
REG. BLK. 2
Check
Standard
DUPLICATE 1
Field #:
Pb/Zn Slag
I N C.
<
Found
True
% Recovery
Results
Results
Results
Found
True
% Recovery
Samp, value
Dup. value
RPD
(
Found
True
% Recovery
Results
Results
Results
Found
True
% Recovery
Samp, value
Oup. value
RPD
units=mg/L)
ARSENIC
0.296
0.281
105%
<0.02 |
<0.02
1
0.291
0.281
104%
<0.5
0.31
NC
units*mg/L)
CHROMIUM
0.305
0.313
97%
<0.004
<0.004
0.312
0.313
100%
0.006
0.005
-18%
Date:
Batch:
BARIUM |
0.437 I
0.460 |
95% |
<0.003 |
<0.003 !
1
0.464 |
0.460 |
101%|
1
7.56 |
3.04 |
-85%|
LEAD |
.......
0.483 |
0.488 |
99% |
<0.05 |
| <0.05 |
I
| 0.466 |
| 0.488 |
| 95% |
1 1
1 55.2 |
1 32.4 |
| -52%|
29-May-86
939.042
CADMIUM 1
0.24 |
0.244
98% |
<0.004
<0.004
0.242
0.244
99%
0.02
0.025
22%
SILVER
0.052
0.052 |
100%|
<0.003
<0.003
0.047
0.052
90%
1
<0.06
<0.06
NC
Comments: NC-RPD Is not calculated when the sample or duplicate
value is less than the detection limit.
------- |