*'*
A COMPARATIVE EVALUATION OF TWO EXTRACTION
PROCEDURES: THE TCLP AND THE EP
by
R. Mark Bricka, Teresa T. Holmes, and M. John Cullinane, Jr.
U.S. Army Engineer Waterways Experiment Station :
Vicksburg", Mississippi 39180-6199
Interagency Agreement No. DA930146-01-05
Project Officer
Carlton C. Wiles
Land Pollution Control Division
Risk Reduction Engineering Laboratory
Cincinnati, Ohio 45268
RISK REDUCTION ENGINEERING LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
CINCINNATI, OHIO 45268
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NOTICE
The information in this document has been funded wholly or in part by the
U.S. Environmental Protection Agency under Interagency Agreement
DA930146-01-05 with the U.S. Army Engineer Waterways Experiment Station. It
has been subjected to the Agency's peer and administrative review and approved
for publication as an EPA document. Mention of trade names or commercial
products does not constitute endorsement or recommendation for use.
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FOREWORD |
Today's rapidly developing and changing technologies and industrial prod-
ucts and practices frequently carry with them the increased generation of
materials that, if improperly dealt with, can threaten both public health and
the environment. The U.S. Environmental Protection Agency is charged by Con-
gress with protecting the Nation's land, air, and water resources. Under a
mandate of national environmental laws, the Agency strives to formulate and
implement actions leading to a compatible balance between improving the
quality of life and minimizing the risks to the environment. These laws
direct the EPA to perform research to define our environmental problems, mea-
sure the impacts, and search for solutions. ;
The Risk Reduction Engineering Laboratory is responsible for planning,
implementing, and managing,research, development, and demonstration programs
to provide an authoritative and defensible information that can; be used by
both regulators and the regulated in their common efforts to protect the envi-
ronment: from the hazards, of industrial and municipal waste. This;publication
is one of the products of that research and provides a vital communication
between the researcher and the user community. ;
This report compares, the results of the TCLP and the EP extraction pro-
cedures. This information should be of assistance to regulators and busi-
nesses subjected to the waste characterization requirements of the Resource
Conservation and Recovery Act. The goal is to provide an understanding of the
similarities, differences, limitations, and correlations between these extrac-
tion procedures. :
E. Timothy Oppelt, Director;
Risk Reduction Engineering Laboratory
111
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ABSTRACT
The 1984 amendments to the Resource Conservation and Recovery Act (RCRA)
require that the U.S. Environmental Protection Agency (EPA) restrict the land
disposal of hazardous wastes. The EPA has identified four characteristics
that could be used to classify a waste as hazardous: corrosivity, ignitabil-
ity, reactivity, and toxicity. A waste exhibiting any one of these properties
is classified as hazardous.
The Extraction Procedure Toxicity Characteristic (EP) test is used to
determine if a waste poses an unacceptable risk to ground water if improperly
managed and therefore should be managed as a hazardous waste. Regulatory
thresholds, based on the EP test, have been established for eight metals, four
pesticides, and two herbicides.
The Toxicity Characteristic Leaching Procedure (TCLP EPA Method 1311) was
developed to address a Congressional mandate to identify additional character-
istics of wastes, primarily organic constituents that may pose a threat to the
environment. The TCLP has been promulgated for use in determining specific
treatment standards associated with the land disposal restrictions of RCRA.
The TCLP has also been proposed as a replacement procedure for the EP test.
Using the TCLP procedure, che EPA has also proposed to expand with hazardous
waste regulatory levels the list of contaminants from the 14 Listed in the EP
protocol to a total of 52. The additional contaminants include 20 volatile
organics, 16 send/volatile organics, and 2 pesticides.
The purpose of this study was to compare the results of the TCLP with
those of the EP. The study was divided into three substudies. In the first
substudy, a synthetic heavy metal waste was chemically solidified/stabilized,
and a variety of interfering compounds were added to the solidified/stabilized
waste. The solidified/stabilized waste was cured for 28 days and subjected, to
the TCLP and EP extractions. The extracts were analyzed for Cd, Cr, Ni, and
Hg. In the second substudy, two heavy metal synthetic wastes and a per-
chloroethene still-bottom waste were used. The two synthetic heavy metal
wastes were chemically solidified/stabilized, and the perchloroethene waste
was untreated. Twelve volatile organic compounds were added to each waste
type at two ratios. The EP and the TCLP extractions were performed on three
samples from each waste type. The extract from each sample was analyzed for
As, Ag, Ba, Cd, Cu, Ni, Pb, and Zn and the 12 volatile organic compounds. In
the third substudy, volatile losses due to the mechanics of the TCLP and EP
extractions were investigated, by spiking ,the TCLP and EP extracts with known
concentrations of organic compounds. The results of this study indicate that,
for most of the metal contaminants, the TCLP and EP produce similar results
when TCLP extraction fluid 2 is used but differ when TCLP extraction fluid 1
is used. The results of testing for volatile organic contaminants indicate
that, for 8 of the 12 contaminants, the concentrations measured in the TCLP
leachates were significantly greater than ;those measured in the EP leachates.
This report was submitted in fulfillment of Interagency Agreement
No. DA930146-01-05 with the U.S. Army Engineer Waterways Experiment Station,
Vicksburg, MS, under sponsorship of the U.S. Environmental Protection Agency.
It covers a period from 10/l/84t through 9/30/89, and work was completed as of
the latter date.
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CONTENTS
« -# .*: ? . Page_
........... j . . . ill
Foreword .............................................. , .
Abstract [[[ '; ' ' " vi
Figures .... [[[ ' ' ' ' lx
Tables [[[ ; ' . ' ' xii
Abbreviations and Symbols ......................................... ...
Acknowledgments [[[ ' ' " ' .
Conversion Factors, Non-Si to SI (Metric) Units of Measurement. ...:... xiv
:... 1
Background ' '
1. Introduction
Background
Leaching procedure methods.
Associated proj ects
Purpose and scope - - ,' ' ' ' ,
Organization of the report ;' |
2, Conclusions .;
3 . Recommendations :
4. Materials and Methods
Proj ect overview ,
Study A - I"" II
Study B ' "
Statistical procedures r |
5. Results and Discussion.' ; ^
Study A : ' ^
Study B : y-
Spike and recovery study ;. . . . ->i
Quality assurance/quality control ; °^
Procedural difficulties encountered with the TCLP j.... 61
References
Appendices '<
A. Extraction procedure toxicity test and structural I
integrity test > ^
B. Toxicity characteristic leaching procedure >
C. Laboratory determination of moisture content of '
hazardous waste materials }^
D. Physical properties of the organic compounds |. J-J-3
E. Study A raw data | 115
F. Graphical representation of the results of TCLP and |
EP extractions for Study A metals . . . 135
G. Study B metals raw data ....;....
H. Graphical representation of the results of TCLP and
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FIGURES
Number Page
1 Extraction procedure flowchart , 3
2 TCLP flowchart ; 6
3 Project flowchart for overall study. . 15
4 Project flowchart for Study A ', 16
5 Project flowchart for Study B 17
6 Flowchart of the PCE waste production 27
7 Average normalized Study A cadmium extract concentrations
expressed as the TCLP concentration divided by the EP
concentration 36
8 Average normalized Study A chromium extract concentrations
expressed as the TCLP concentration divided by the EP
concentration 37
9 Average normalized Study A nickel extract concentrations
expressed as the TCLP concentration divided by the EP
concentration 38
LO Average normalized Study A mercury extract concentrations
expressed as the TCLP concentration divided by the EP
concentration 39
11 Average normalized Study B metal extract concentrations
expressed as the TCLP concentration divided by the EP
concentration 49
12 Average normalized Study B 0.1% organic extract concentrations
expressed as the TCLP concentration divided by the EP
concentration '. 55
13 Average normalized Study B 1.0% organic extract concentrations
expressed as the TCLP concentration divided by the EP
concentration 56
A-l EP extractor 81
A-2 EP rotary extractor 81
A-3 EP EPRI extractor 82
A-4 EP compaction tester 85
B-l TCLP flowchart 92
B-2 TCLP rotary agitator 94
B-3 TCLP zero-headspace extraction vessel 95
F-l Normalized EP extract concentrations versus the normalized TCLP
extract concentrations for the Study A cadmium contaminant 136
F-2 Normalized EP extract concentrations versus the normalized TCLP
extract concentrations for the Study A chromium contaminant 136
VI
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Number
F-3 Normalized EP extract concentrations versus the normalized TGLP
extract concentrations for the Study A nickel contaminant.
F-4 Normalized EP extract concentrations versus the normalized TCLP
extract concentrations for the Study A mercury contaminant
H-l Normalized EP extract concentrations versus the normalized
TCLP extract concentrations for the Study B antimony and silver
148
contaminants \
H-2 Normalized EP extract concentrations versus the normalized TCLP
extract concentrations for the Study B arsenic contaminant. 148
H-3 Normalized EP extract concentrations versus the normalized TCLP
extract concentrations for the Study B cadmium contaminant.. . t 149
H-4 Normalized EP extract concentrations versus the normalized TCLP
extract concentrations for the Study B chromium contaminant. 149
H-5 Normalized EP extract concentrations versus the normalized TCLP
extract concentrations for the Study B lead contaminant -. 150
H-6 Normalized EP extract concentrations versus the normalized TCLP
extract concentrations for che Study B mercury, zinc and
copper contaminants :
H-7 Normalized EP extract concentrations versus the normalized TCLP
extract concentrations for the Study B nickel and barium .
contaminants ........
J-l Normalized EP extract concentrations versus the normalized TCLP
extract concentrations for the Study B benzene contaminant...; 166
J-2 Normalized EP extract concentrations versus the normalized TCLP
extract concentrations for the Study B carbon tetrachloride ;
contaminant |
J-3 Normalized EP extract concentrations versus the normalized TCLP
extract concentrations for the Study B chloroform contaminant 167
J-4 Normalized EP extract concentrations versus the normalized TCLP
extract concentrations for the Study B 1,2-dichloroethane '
contaminant <
i
J-5 Normalized EP extract concentrations versus the normalized TGLP
extract concentrations for the Study B ethylbenzene contaminant 168
J-6 Normalized EP extract concentrations versus the normalized TCLP
extract concentrations for the Study B 1,1,2,2-tetrachloroetHane
1_ o o
contaminant *
J-7 Normalized EP extract concentrations versus the normalized TGLP
extract concentrations for the Study B tetrachloroethene ;
contaminant ;
J-8 Normalized EP extract concentrations versus the normalized TCLP
extract concentrations for the Study B 1,1,1-trichloroethane.
contaminant '
J-9 Normalized EP extract concentrations versus the normalized TCLP
extract concentrations for the Study B trichloroethene
contaminant '
vi i
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Number
J-10 Normalized EP extract concentrations versus the normalized TCLP
extract concentrations for the Study, B toluene contaminant
J-ll Normalized EP extract concentrations versus the normalized TCLP
extract concentrations for the Study B 4-methyl-2-pentanone
contaminant
J-12 Normalized EP extract concentrations versus the normalized TCLP
extract concentrations for the Study B 2-butanone
contaminant
Page,
170
171
171
Vlll
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TABLES
Number ',
1 Maximum Concentration of Contaminants for Characteristic,
of EP Toxicity ;
2 Volatile Contaminants as Listed by the TCLP : 8
3 Analysis of the WES Sludge ' ;- 18
4 Compositional Analyses of Binder Materials 20
5 Chemical Analyses of Binder Materials : 21
6 Interference Compounds Utilized in Study A ' 22
!
7 Test Specimen Matrix for Study A Metals Data: ;
Extraction Sample Age at the Time of Analysis !. . 23
' 25
8 Chemical Analysis Methods ' ' ' '
9fi
9 Bulk Analysis of WTC Solution ^
10 Bulk Analysis of Perchloroethlene Waste .|.... 27
11 Organic Compounds Added to Study B Sludges ;. 28
12 , Volatile Spike Additions for Study B '. 29
13 Study A Multifactor Factorial Experimental Design . . . . 31
14 Study B Multifactor Factorial Experimental Design 31
15 Study A: Average TCLP and EP Extract Concentrations. ...'.,.. 33
16 Summary Statistics for the Study A Metals Data .; 35
17 Results of AVMFT Performed on Normalized ;
Study A TCLP and EP Metals Results j 40
18 Results of Paired-Sample T Test Performed on Normalized!
Study A TCLP and EP Nickel and Mercury Data } . . . . 40
19 Study B Average TCLP and EP Extract Concentrations for ;
Metal Contaminants
20 Summary Statistics for Study B Metals Data 45
21 Results of Statistical Analysis for Normalized .
Study B TCLP and EP Metal Extracts 47
22 Results of Paired-Sample T Test for Normalized
Study B TCLP and EP Metal Extracts
23 Study B Average TCLP and EP Extract Concentration for the
Organic Contaminants
24 Results of Statistical Analysis for Normalized TCLP
and EP Organic Extract Concentrations 53
48
25 , Result of the Paired-Sample T Test for Normalized Study B
TCLP and EP Organic Extract Concentrations. \ 54
26 Study B Organic Sludge Bulk Analyses 58
27 Average Percent of Volatiles Lost from Prespike \
Samples
ix -
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Number
28 Average Percent of Volatiles Lost from Postspike
Samples 59
29 Analysis of Method Blanks for the Metals Study A TCLP/EP
Test 61
30 Analysis of Method Blanks for the Metals Study B TCLP/EP
Test j. 63
31 Analysis of Method Blanks for the Volatile Organics Study B
TCLP/EP Test 64
32 Study A Metals Percent Accuracy of the Analytical
Laboratory' s Internal Standards '........ 65
33 Study B Metals Percent Accuracy of the Analytical
Laboratory's Internal Standards 66
34 Study B Organic Internal Surrogate Spikes 67
35 Study B Organic Duplicate and Percent Recovery Analyses 68
36 Study A Metals Percent Accuracy of the External Standards... 74
37 Study B Metals Percent Accuracy of External Standards 75
38 Concentration of 1,1-Dichloroethene Measured in Che TCLP and
EP Extracts 75
A-l Maximum Concentration of Contaminants for Characteristic
of EP Toxicity 80
A-2 EPA-Approved Filter Holders 83
A-3 EPA-Approved Filtration Media. . . ;. 84
B-l Volatile Contaminants 93
B-2 Suitable Rotary Agitation Apparatus 94
B-3 Suitable Zero-Headspace Extractor Vessels 95
B-4 Suitable Filter Holders 97
B-5 Suitable Filter Media 97
D-l Physical Properties for the Organic Compounds Used in This
Study 113
E-l TCLP and EP Extract Analysis for Cadmium 115
E-2 TCLP and EP Extract Analysis for Chromium 120
E-3 TCLP and EP Extract Analysis for Mercury 124
E-4 TCLP and EP Extract Analysis for Nickel 129
G-l Study B TCLP and EP Extract Analysis for the WES Sludge
Metal Contaminants 139
G-2 Study B TCLP and EP Extract Analysis for the WTC Waste Metal
Contaminants 141
G-3 Study B TCLP and EP Extract Analysis for the PCE Waste Metal
Contaminants !. 143
x
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Number ' ,
1-1 Study B TCLP and EP Extract Analyses for Carbon ;
Tetrachloride 153
1-2 Study B TCLP and EP Extract Analyses for Chloroform ;. . . . 154
1-3 Study B TCLP and EP Extract Analyses for 1,2- ;
Dichloroethane '
1-4 Study B TCLP and EP Extract Analyses for
1,1,1-Trichloroethane. .
1-5 Study B TCLP and EP Extract Analyses for Trichloroethene|. ... 157
1-6 Study B TCLP and EP Extract Analyses for Benzene ' 158
1-7 Study B TCLP and EP Extract Analyses for
1,1,2,2-Tetrachloroethane , 159
1-8 Study B TCLP and EP Extract Analyses for :
Tetrachloroethene ,- 160
1-9 Study B TCLP and EP Extract Analyses for Toluene :. . . . 161
1-10 Study B TCLP and EP Extract. Analyses for Ethylbenzene. ....... 162
I-11 Study B TCL? and EP Extract Analyses for 2-Butanone |. . . . 163
1-12 Study B TCLP and EP Extract Analyses for
4-Methyl-2-Pentanone ; 164
XI
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LIST OF ABBREVIATIONS AND SYMBOLS
ABBREVIATIONS
ANOVA
AVMFT
BDAT
EP
EPTC
HOPE
LD50
PCE
PTFE
QA/QC
RCRA
SIP
s/s
TCLP
ZHE
SYMBOLS
B
EC
ECn
M
V
W
-- analysis of variance
-- analysis of the variance'multifactor factorial test
-- best demonstrated available technology
-- Extraction Procedure Toxicity Test
-- Extraction Procedure Toxicity Characteristic
-- high density polyethylene
-- lethal dose to 50 percent of the population
-- perchloroethene
-- polytetrafluoroethylene
-- quality assurance/quality control
-- Resource Conservation and Recovery Act
-- Structural Integrity Procedure
-- solidification/stabilization
-- Toxicity Characteristic Leaching Procedure (EPA Method 1311)
-- Zero-headspace extraction
-- weight fraction of raw waste in che solidified/stabilized
interfered waste mixture1
-- contaminant concentration measured in the TCLP or EP
extract, mg/1
-- normalized extract concentration, mg/kg
-- solids concentration of the solidified/stabilized waste
extracted, expressed as a decimal
-- volume of extraction fluid, liters
-- weight of the wet waste extracted, kg
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ACKNOWLEDGMENTS ;
This report presents the results of a laboratory investigation that com-
pared the TCLP and EP extraction procedures. This research will assist the
U.S. Environmental Protection Agency (EPA) in the development of testing
methods for evaluating hazardous waste.
The study was conducted during the period November 1986 through March
1988 This report was written by Mr. R. Mark Bricka, Ms. Teresa T. Holmes,
and Dr. M. John Cullinane, Jr., Water Supply and Waste Treatment Group
(WSWTG), Environmental Engineering Division (EED), Environmental Laboratory
(EL), US Army Engineer Waterways Experiment Station (WES). The research was
sponsored by the USEPA Office of Research and Development under interagency
agreement No. DA930146-01-05. The EPA Project Officers were Mr. Carlton Wiles
and Mr. Paul de Percin. Special assistance was given by Mr. David:Friedman of
the EPA Office of Solid Waste. >
Chemical analyses were performed by the Analytical Laboratory:Group, EL.
Technician support was provided by Messrs. Jim Ball, Dan Williams,and
Larry L. Pugh. Direct supervision was provided by Mr. Norman R. ;
Francirigues, Jr., Chief, WSWTG. General supervision was provided by
Dr. Raymond L. Montgomery, Chief, EED, and Dr. John Harrison, Chief, EL.
Commander and Director of WES was COL Larry B. Fulton, EN. Technical
Director was Dr. Robert W. Whalin. :
Xlll
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CONVERSION FACTORS, NON-SI TO SI (METRIC)
UNITS OF MEASUREMENT
Non-Si units of measurement used in this report can be converted to SI
(metric) units as follows:
To Obtain
Multiply
gallons (US liquid)
horsepower (550 foot-pounds
(force) per second)
pounds (force) per square inch
pounds (mass)
pounds (mass) per cubic foot
pounds (mass) per gallon
Bv
3.785412
745.6999
I
6;894757
0.4535924
16.01846
0:12
cubic decimeters
watts
kilopascals
kilograms
kilograms per cubic
meter
kilograms per cubic
decimeter
xiv
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SECTION 1 ;
INTRODUCTION I
!
BACKGROUND '
In 1976 the Congress of the United States enacted Public Law 94-580, the
"Resource Conservation and Recovery Act of 1976" (RCRA). Section 3001 of the
Act required that the U.S. Environmental Protection Agency (USEPA) promulgate
criteria to differentiate hazardous and nonhazardous wastes (Government
Institutes, Inc. 1983). |
The USEPA established three methods for defining hazardous waste. First,
a waste is defined as hazardous if it is listed in Table 1 of Volume 45 of the
Federal Register (USEPA 1980). Second, a waste is determined to[be an "Acute
Hazardous Waste" if the waste is (a) found to be fatal to humans;in low doses
or (b) it is shown in studies to have an oral LD50 (lethal dose tjo 50 percent
of the population tested) in rats of less than 2 mg/1 or a dermal LD50 in
rabbits of less than 200 mg (Hill 1986). Third, a waste is designated as
hazardous if it exhibits a characteristic (ignitability, reactivity, corro-
sivity, or toxicity) of a hazardous waste as outlined in 40 CFR Part 261, Sub-
part C (USEPA 1987). ;
Waste Characterization - . ;
Def iiiition--
The four characteristics that the USEPA established to define a nonlisted
waste as a hazardous waste include: ignitability, reactivity, cprrosivity,
and toxicity. A waste exhibiting one or more of these characteristics is
classified by the USEPA as hazardous. A waste classified as hazardous, either
listed or characteristic, must be handled in accordance with Subtitle C of
RCRA. This report will deal with the toxicity characteristics. :
Toxicity-- '
One of the most significant dangers posed by hazardous wastes stems from
the leaching of toxic constituents into ground water (Government Institutes,
Inc. 1983). The USEPA's Extraction Procedure Toxicity Test (EP) addresses the
properties of a waste which are directly related to the actual potential of
the waste to pose a hazard to ground water. During the development of the EP,
the USEPA's "primary concern was that hazardous waste might, unl|ess subject to
regulatory control, be sent to a sanitary (municipal) landfill" |(Friedman
1985). Based on this concern, the EP was designed to simulate the leaching of
a solid hazardous waste co-disposed with municipal waste in a sanitary land-
fill and to assess the potential impact of the leachate on ground-water
contamination.
The toxicity characteristic is assessed using the EP. The |waste is sub-
jected to the EP, and the extract is analyzed for eight metals, jfour pesti-
cides, and two herbicides. If the EP extract contains these contaminants
above'the limits set by the USEPA, it is determined to exhibit the toxicity
characteristic and is thus a hazardous waste (USEPA 1986d). The EP is
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summarized in the section below, entitled "Leaching Procedure Methods," and is
presented in its entirety in Appendix A.
Toxicity Characteristic Leaching Procedure
The Toxicity Characteristic Leaching Procedure (TCLP) is a "second-
generation" extraction procedure developed by the USEPA. The TCLP is proposed
as a replacement for the EP test as a waste characterization tool. The TCLP
method is summarized below in the section entitled "Leaching Procedure
Methods" and is presented in its entirety in Appendix B.
Regulations defining a waste as hazardous were first promulgated in 1980.
At that time, the USEPA recognized that the EP addressed only a small portion
of the recognized toxic constituents (Friedman 1985). The USEPA initiated
work to develop a leaching procedure that would address additional toxic con-
stituents of hazardous waste, primarily a number of organic compounds. The
TCLP has been proposed as a method of addressing the shortcomings of the EP
(Friedman 1985). Since the TCLP was first published in the Federal Register
(USEPA 1986a), it has undergone several modifications. This study was con-
ducted according to the June 13, 1986, publication of the TCLP (USEPA 1986b).
More recently, the November 7, 1986, version of the TCLP method has been
published in the Code of Federal Regulations, Part 267, Appendix I (USEPA
1987). :
LEACHING PROCEDURE METHODS
Extraction Procedure
Toxieitv Test Method
I
The Extraction Procedure Toxicity Test, as outlined in USEPA's Test
Methods for Evaluating Solid Waste, SW-846 (USEPA 1982), is presented in
Appendix A. Specific modifications to this procedure implemented during this
study are described in Section 2, "Materials and Methods." The EP extraction
consists of five steps that are summarized below. A flowchart illustrating
the steps in the EP is presented as Figure 1.
Separation Procedure--
A waste containing unbound liquid is filtered, and if the solid phase is
less than 0.5% of the waste, the solid phase is discarded and the filtrate
analyzed for trace elements, pesticides, and herbicides (step 5). If the
waste contains more than 0.5% solids, the solid phase is extracted and the
liquid phase is stored for later use.
Structural Integrity Procedure/ :
Particle Size Reduction--
Prior to extraction, the solid material must pass through a 9.5-mm
standard sieve, have a surface area per gram of waste of 3.1 cm2, or, if it:
consists of a single piece, be subjected :to the Structural Integrity Proce-
dure. This procedure is used to demonstrate the ability of the waste to
remain intact after disposal. If the waste does not meet one of these condi-
tions, it must be ground to pass the 9.5-mm sieve.
-------
Wet Wast
Contains
Nonf ilter
Solids
1
e Sample
<" 0 5% j
able ^
r
Liquid Solid __^co|
Separation .
Liqt
Disc
Jid
>9.5
\
id
r
ard
tiiiii
Sample Size
Reduction
v
1 PI
Solid 4
i
Discard
-k
Represe
Waste S
>100C
4
Dry Wast
^
Partic
<9.l
^
Extraction o
^
ntative Wet Waste Sample.'
ample . Contains > 0.5%
irams r Nonfilterable ,
, , Solid*
1 1
s Sample : -^
Liquid
1 bo"u Separal
e Size Li^
s
!
5mm Monolithic
1
Structural
Integrity
Procedure
Solid Waste ^^ dt Pn
i r
Liquid Solid Separation
Li
EPf
i
quid :
1.
I4'
Extract
i
Analysis Methods
v
Solid
ion
uid
r
at4°C
= 2
Figure 1. Extraction procedure flowchart.
-------
Extraction of Solid Material--
The solid material from step 2 is extracted for 24 hours in an aqueous
medium whose pH is maintained at or below 5.0 using 0.5 N acetic acid. The pH
is maintained either automatically or manually. (In acidifying to pH 5, no
more than 4.0 ml of acid solution per gram of material being extracted may be
used.)
Final Separation of the Extraction
from the Remaining Solid--
After extraction, the liquid:solid ratio is adjusted to 20:1 and the
mixed solid and extraction liquid are separated by filtration. The solid is
discarded and the liquid ,is combined with any filtrate obtained in step 1.
This is the EP extract that is analyzed and compared to the threshold values
listed in Table 1 (USEPA 1982).
Testing (Analysis) of EP Extract-- :
Inorganic and organic species are identified and quantified using the
appropriate 7000 and 8000 series of methods of analyses. These methods are
listed in USEPA's manual "Test Methods for Evaluation of Solid Waste," SW-846
(USEPA 1982, 1986b)
Toxxcity Characteristic Leaching
Procedure Method (EPA Method 1311)
The TCLP is conducted in two parts. The first is employed for the
extraction of nonvolatile compounds; the, second is employed for the extraction
of volatile compounds. A flowchart illustrating the details of the TCLP is
shown as Figure 2.
Procedure When Volatiles Are Not Involved--
The TCLP for nonvolatile contaminants is a five-step procedure as
described below.
Separation procedure--A waste containing unbound liquid is filtered; if
the solid phase is less than 0.5% of the waste, the solid phase is discarded
and the filtrate is analyzed for the desired nonvolatile contaminants. If the
waste contains more than 0.5% solids, th'e solid phase is extracted and the
liquid phase is stored for later use.
Particle size reduction--Prior to extraction, the solid material should
have a particle size capable of passing a 9.5-mm standard sieve or a surface
area per gram of material equal to or greater than 3.1 cm2. If the surface
area is smaller than the 3.1 cm2, the particle size of the material should, be
reduced.
Extraction fluid determination--Prior to extraction, a small sample of
the waste is tested for alkalinity. Materials with an alkalinity less than
pH 5.0 are extracted using extraction fluid 1. More alkaline materials are
extracted using extraction fluid 2. Extraction fluid 1 is a pH 4.93 acetic
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TABLE 1. MAXIMUM CONCENTRATION OF CONTAMINANTS
FOR CHARACTERISTIC OF EP TOXICITY
EPA
Hazardous
Waste Number
D004
D005
D006
D007
D008
D009
DO 10
D011
D012
DO 13
DO 14
DO 15
DO 16
DO 17
Contaminant
Arsenic
Barium
Cadmium
Chromium
Lead
Mercury
Selenium
Silver
Endrin (1 ,2,3 ,4, 10, 10-Hexachloro-l
7-epoxy-l , 4 , 4a , 5 , 6 , 7 , 8 , 8a-octahydro-l
4-endo, endo-5,8-dimethano-naphthalene)
Lindane (1,2,3,4,5, 6-Hexa-chloro-cyclohexane ,
gamma isomer)
Methoxychlor (1 , 1, l-Trichloro-2 , 2-bis
(p-methoxyphenyl) ethane)
Toxaphene (C10H10C18, Technical chlorinated
camphene, 67-69% chlorine)
2,4-D (2,4-Dichlorophenoxyacetic acid)
2,4,5-TP (Silvex) (2,4,5-
Trichlorophenoxypropionic acid)
5
Maximum
Concentration
(mg/1)
5.0
; 100.0
1.0
i
5.0
; 5.0 .
; 0.2
; i.o
i 5.0 : .
; 0.02
; o.4
; 10.0 I
: 0.5
; 10.0
i
1.0
1
\
1
i
-------
WET WASTE SAMPLE
CONTAINS < 0.5%
NON FILTERABLE SOLIDS
REPRESENTATIVE WASTE
SAMPLE
WET WASTE SAMPLE
CONTAINS>0.5%
NONFILTERABLE SOLIDS
DRY WASTE SAMPLE
LIQUID/SOLID
SEPARATION
0.6 - 0.8 urn
GLASS FIBER
FILTERS
DISCARD
SOLID
SOLID'
SOLID
LIQUID/SOLID
SEPARATION
0.6 - 0.8 urn
GLASS FIBER
FILTERS
REDUCE PARTICLE SIZE IF
> 9.5 mm1 OR
SURFACE AREA < 3.1 cm2
T
LIQUID
STORE AT
4°C
PRESCREENING
TO SELECT EXTRACTION
FLUID
ZERO HEAD EXTRACTION
OF SOLID FOR
VOLATILE CONTAMINANTS
TCLP EXTRACTION OF
SOLID FOR NON-
VOLATILE CONTAMINANTS
DISCARD
SOLID
LIQUID/SOLID
SEPARATION
0.6 - 0.8 urn
GLASS FIBER
FILTERS
I
LIQUID
I
LIQUID/SOLID
SEPARATION
0.6 - 0.8 urn
GLASS FIBER
FILTERS
SOLID
DISCARDED
LIQUID
TCLP EXTRACT
TCLP EXTRACT
TCLP EXTRACT
» ANALYTICAL METHODS *
TCLP EXTRACT
Figure 2. TCLP flowchart.
-------
acid/sodium acetate buffer solution. Extraction fluid 2 is an acetic acid
solution having a pH of 2.88. '
Extraction of the solid material--The solid waste is placed tn an extrac-
tion bottle, and 20 times the weight of the solid waste of the appropriate
extraction fluid is used to slurry the solid waste. The waste is|extracted
for 18 hours. ' i
Final separation of the extraction from the remaining solid-^Following
extraction, the liquid is separated from the solid by filtration.; The solid
is discarded, and the liquid is combined with any filtrate obtained in step 1,
This is the TCLP extract that is analyzed for nonvolatile contaminants.
Procedure When Volatiles Are Involved-- .
The TCLP used for the extraction of volatile contaminants is. a four-step
procedure as described below. Table 2 specifies the volatile contaminants
listed by the TCLP. , i
'Separation procedure--A separation procedure, similar to the one used for
the nonvolatile extraction, is performed. This procedure was described in the
subsection entitled "Procedure When Volatiles Are Not Involved." '
Particle size reduction--The method used to reduce the particle size of
the waste extracted for volatile compounds is similar to the particle size
reduction method used for the nonvolatile extraction. This methojd is also
described under the nonvolatile section. ;
Zero-headspace extraction of the solid material--The solid waste is
extracted utilizing extraction fluid 1 regardless of pH. The was,te is placed
in a zero-headspace extraction (ZHE) device and slurried (under zero head con-
ditions) with extraction fluid at 20 times the weight of the waste. The waste
is extracted for 18 hours. i
Final separation of the extraction from the remaining solid--Following
extraction, the liquid is simultaneously filtered and removed from the ZHE
device The solid is discarded, and the extraction liquid is combined with
any filtrate obtained in step 1. This is the TCLP extract that is analyzed
for volatile contaminants. ;
Comparison of EP and TCLP Methods ;
There are many contrasts between the EP and TCLP methods (Callaway, Parr,
and Bellinger 1987), some of which are quite prominent; others are buried^deep
within the procedures. The most obvious difference is that the TCLP requires
the use of the ZHE vessel for volatile compounds and an extraction fluid
selection step for nonvolatile extractions. Other differences include:
1 In the TCLP method for nonvolatiles, one of two extraction fluids is
selected to extract the solid waste sample. The type of extraction
fluid is determined in an initial test on the waste and|is based on
the waste's alkalinity. Extraction fluid 1 is an acetape buffer at a
pH of 4.93 ± 0.05. Extraction fluid 2 is an acetic acid solution
-------
TABLE 2. VOLATILE CONTAMINANTS AS LISTED BY THE TCLP*
1. Acetone
2. n-Butyl alcohol
3. Carbon disulfide
4. Carbon tetrachloride
5. Chlorobenzene
6. Methylene chloride
7. Methyl ethyl ketone
8. Methyl isobutyl ketone
9. Tetrachloroethylene
10. Toluene
11. 1,1,1-Trichloroethane
12. Trichloroethylene
13. Trichlorofluoromethane
14. Xylene
* If any or all of these compounds are of concern, the zero-headspace extrac-
tion vessel shall be used. If other (nonvolatile) compounds are of concern,
the conventional extraction bottle shall be used.
with a pH of 2.88 + 0.05. The EP uses distilled deionized water as
an extraction fluid, and 0.5 N acetic acid is added to the solid
waste/water slurry to maintain the pH at 5.0 + 0.2. The acetic
acid is added as required, up to a maximum of 4 g of 0.5 N acetic
acid per 1 g of solid waste extracted.
2. The TCLP method for volatiles requires the use of extraction fluid 1.
The EP has no volatiles extraction procedure.
3. The TCLP requires that the ZHE vessel be used for volatiles extrac-
tion. Extraction bottles made cif glass, polytetrafluoroethylene
(PTFE), or type 316 stainless steel are specified for organic or
inorganic contaminants. High density polyethylene (HDPE), poly-
propylene, or polyvinyl chloride may be utilized as extraction
vessels when nonvolatile compounds are extracted. The EP is vague
about extraction vessel design.
4. The TCLP procedure requires the use of 0.6- to 0.8-?m glass fiber
filters and excludes the use of prefilters. The EP requires the use
of 0.45-?m cellulose triacetate filters and allows the use of glass
fiber prefilters.
5. The TCLP requires that the particle size of the solid be small enough
to pass a 9.5-mm standard sieve. The EP allows the use of the Struc-
tural Integrity Procedure if the sample is monolithic in nature. If
the sample is not a monolith, the EP requires that the particle size
be small enough to pass a 9.5-mnj standard sieve.
6. The TCLP requires rotary agitation in an end-over-end fashion at 30
± 2 rpm. The EP allows the use of either a stirred open vessel or a
rotary end-over-end agitator.
-------
7. The extraction period for the TCLP is 18 hours. The extraction
period for the EP is 24 hours ± 2 hours. |
8. The EP requires monitoring and adjustment of the pH during the
extraction. The TCLP does not. '
ASSOCIATED PROJECTS j
i
The waste materials utilized in this study were also used in. three' other
studies funded by the USEPA and conducted at the U.S. Army Engineer Waterways
Experiment Station. These studies include: (1) Investigation of\ Test Methods
for Solidified Waste Characterization - A Cooperative Program," (2) "Evalua-
tion of Factors Affecting Stabilization/Solidification of Toxic and Hazardous
Waste," and (3) "Evaluation of Stabilization/Solidification as a Best Demon-
strated Available Technology." Brief descriptions of these projects and their
relationships to this study are presented below. !
Investigation of Test Methods
for Solidified Waste Character-
ization - A Cooperative Program :
This study was designed to develop and evaluate techniques tp assess the
effectiveness of a variety of solidification/stabilization1 (S/S): tech-
nologies . Three laboratories, the U.S. Army Engineer Waterways Experiment
Station (WES), the Wastewater Technology Centre (WTC), and the Alberta Envi-
ronmental Centre (AEC), participated in the study. Five raw wastes were
solidified/stabilized by 15 commercial S/S vendors. The resulting solidi-
fied/stabilized materials were shipped to the three labs (WES, WT|C, .and AEC),
and 12 testing protocols were performed on the solidified/stabilized mate-
rials . Details of the cooperative study are outlined in the report entitled
"Laboratory Assessment of Short-Term Test Methods for the Evaluation of
Solidified/Stabilized Waste Materials" (Holmes and Bricka 1988) apd in
"Investigation of Test Methods for Solidified Waste Characterization: A
Cooperative Program" (Stegemann and Cote, in press). ;
One of the five raw wastes developed for the cooperative study was a
synthetic metal solution formulated by the WTC laboratory. This waste is
referred to as the "WTC waste" through the remainder of this report.
Evaluation of Factors Affecting [
S/S of Toxic and Hazardous Wastes \
This study (referred to as "The Interference Project") was designed to
assess the effects of a variety of industrial chemicals on the physical and
chemical properties of typical S/S processes. '
1 Solidification/stabilization is a process that involves the mixing of a
hazardous waste with a binder material to enhance the physical and chemical
properties of the waste and to chemically bind any free liquid (U,SEPA
1986a). '
-------
Many hazardous wastes contain materials that are known to inhibit the setting
and strength development properties of S/S techniques. The effects of
five organic and five inorganic chemicals on a solidified/stabilized synthetic
heavy metal sludge were evaluated. The Synthetic metal sludge was solidified/
stabilized using three generic binders. The details of this study are out-
lined in a report entitled "An Assessment of Materials That Interfere with
Stabilization/Solidification Processes" (Cullinane, Bricka, and Francingues
1987).
The synthetic metal plating sludge evaluated in the Interference Project
was also used in this TCLP/EP comparison study. The synthetic metal plating
sludge is identified as the "WES waste" through the remainder of this report.
Evaluation of S/S as a Best Demon-
strated Available Technology (BOAT)
The BDAT S/S study determined whether S/S techniques could be applied to
a variety of "listed" wastes and evaluated the effects of the S/S techniques
on the mobility of the contaminants contained in the wastes. Data collected
as part of the BDAT S/S study are being utilized by the USEPA to support the
development of treatment standards for wastes subject to the land disposal
restrictions (USEPA 1987). The details of this study are outlined in a series
of reports (see Bricka, Holmes, and Cullinane 1988).
One of the listed wastes evaluated in the BDAT S/S study, a by-product
from the reclamation of spent perchloroethene solvent, was also used in this
TCLP/EP comparison study. Throughout the remainder of this report, the
perchloroethene solvent waste is identified as the "PCE waste."
PURPOSE AND SCOPE . .
The purpose of this study was to compare the results of the TCLP to those
of the EP. This comparison was accomplished by dividing this study into sub-
studies. The first substudy evaluated the metal-extraction effectiveness of
the two methods. The second substudy investigated the extraction of volatile
compounds. The third substudy examined the volatile losses due to the
mechanics of conducting the extractions and the storage of extracts prior to
analyses.
ORGANIZATION OF THE REPORT
Section 1: Introduction
The introduction briefly describes the origin of the EP and TCLP extrac-
tions , the difference between the TCLP and EP extractions, various proj ects
associated with this study, and the scope of the study.
Sections 2 and 3:
Conclusions and Recommendations
i
Conclusions based on the results of this study and recommendations for
future research are presented in these sections.
-------
Section 4: Materials and Methods
\
This section describes the three separate substudies conducted as part of
this research effort. Each substudy details the methods used for preparing
the wastes and the extraction procedures performed. ',
Section 5: Results . :
This section presents the results of the EP and TCLP extraction and com-
pares the extraction tests. :
11
-------
SECTION 2
CONCLUSIONS
This study was conducted to compare ;the results of the TCLP and the EP,
The EP and TCLP extractions were performed on a number of different wastes
subjected to a variety of conditions. Based on the results of this study, the
following conclusions can be drawn.
(1) Generally, the TCLP was a more aggressive leaching procedure than
the EP.
(a) When the TCLP extraction fluid 2 was used for the extraction of
metal contaminants, the EP and TCLP produced similar results.
(b) When the TCLP extraction fluid'1 was used for the extraction of
metal contaminants, the EP and TCLP produced statistically different results,
with the TCLP generally being the more aggressive extraction.
(c) The TCLP zero-headspace extraction was only a slightly more aggres-
sive extraction for volatile organics than the EP extraction in this study.
(2) Although the TCLP zero-headspace extraction was a more aggressive
extraction procedure than the EP for theivolatile organics, the difference in
the concentrations of volatile organics in the TCLP and EP extracts was less
than expected. ',
i
(3) When the ZHE vessel was used, cross contamination presented a poten-
tial problem.
(4) The TCLP and EP extraction of the solidified/stabilized specimens
appeared to produce conditions that permit dechlorination reactions to occur.
Significant amounts of 1,1-dichloroethene were detected in the TCLP and EP
extracts although no 1,1-dichloroethene was added, and none was detected in
the raw wastes.
12
-------
SECTION 3 ;
RECOMMENDATIONS !
The TCLP method, while more difficult to perform that the EP; method, is
an extraction test that can be performed in most laboratories. The TCLP
method, unlike the EP method, addresses semivolatile and volatile; contami-
nants.. Several areas should be clarified in the TCLP extraction method. The
following recommendations are based on the results of this study.;
(1) The ZHE vessel is difficult to clean. The TCLP method heeds to make
recommendations on the most effective method of cleaning the ZHE vessel. Mod-
ification of the valve design is highly recommended to improve cleaning
techniques. ' ;
(2) The TCLP method is vague about procedures for sample collection from
the ZHE vessel when Tedlar bags are not used. A section describing the col-
lection of a sample using volatile vials should be included in the TCLP
method.
(3) Additional research should be initiated to investigate why volatile
chlorinated compounds extracted from solidified/stabilized wastes are con-
verted to other chlorinated forms. ;
13
-------
SECTION 4
MATERIALS AND METHODS
PROJECT OVERVIEW
General Approach to the Investigation
This project includes two independent evaluations, Study A and Study B.
These studies compare the results from the EP and TCLP extraction procedures
using common waste types. Project flowcharts for both studies are presented
in Figures 3 through 5.
Study A--
Study A was conducted in four phases, as summarized below.
Phase I--A synthetic metal plating sludge containing cadmium (Cd), chro-
mium (Cr), nickel (Ni), and mercury (Hg) was prepared.
Phase II--The synthetic sludge was solidified/stabilized using a lime
kiln dust binding agent. Prior to the initial set, the solidified/stabilized
sludge was divided into portions, and a single "interfering" .compound was
mixed with each portion of solidified/stabilized sludge. A total of 10 inter-
fering compounds were added to the various portions of the sludge.
Phase III--The kiln dust/sludge/interference mixtures were cured for
28 days. After curing, each waste mixture was subjected to the EP extraction
and the TGLP extraction. The extracts of the TCLP and EP were analyzed for
Cd, Cr, Ni, and Hg.
Phase IV--The results of chemical analyses performed for the TCLP and EP
extracts were compared to evaluate differences between the two extraction
methods.
Study B--
Study B was conducted in four phases as summarized below.
Phase._!--Three wastes, the metal sludge used in Study A, a synthetic
metal waste solution, and a perchloroethene still-bottom waste (K030), were
used in Study B. The synthetic metal solution and the metal sludge were
solidified/stabilized using Type I Portland cement as a binding agent.^ The
perchloroethene sludge was not solidified/stabilized. Prior to the initial
set, each of these solidified/stabilized mixtures and the untreated perchloro-
ethene waste were divided into two portions. Twelve volatile organic com-
pounds were added to each portion at approximate concentrations of 0.1% and
1.0%, respectively. ,
Phase II--These six mixtures were placed in sealed bottles and allowed to
cure for 14 days. After curing, each waste material was subjected to the EP
and TCLP extractions. The TCLP and EP extracts were analyzed for metals and
volatile organic compounds.
14
-------
PROJECT: LABORATORY COMPARATIVE EVALUATION
OF THE
TCLP AND EP
I
STUDY A
I
1
STUDY B
1
CONTINUED IN FIGURE 4 CONTINUED IN FIGURE 5 ,
Figure 3. Project flowchart for overall study.
Phase IIIThe EP and TCLP extracts were spiked with known concentrations
of three volatile organic compounds. The extract solutions were spiked during
two steps of the EP and the TCLP methods: prior to the extraction, and after
the liquid/solid separation step. These spike compounds were used to detect
any volatile losses that might occur during implementation of the extraction
procedure or storage of the extracts prior to chemical analysis. |
Phase IVThe results of chemical analyses on the TCLP and EiP extracts
were compared to evaluate differences between the two extraction methods.
Wastes Selected for Study \
Three wastes were selected for use in this evaluation: a synthetic metal
plating sludge (WES waste), a synthetic metal plating solution (WTC waste),
and a, perchloroethene still-bottom waste (PCE waste). The rationale for
selecting these wastes is discussed below.
WES Waste !
The WES waste was a synthetic sludge made from reagent grade chemicals.
This waste contains high concentrations of toxic metals (Cd, Cr, Ni, and Hg)
and was a good candidate for study because it was likely to leach the contami-
nants at detectable levels. '[
WTC Waste ;
The WTC waste was prepared from reagent grade chemicals and|contained
high concentrations of arsenic, cadmium, chromium, and lead. Twp of these
metals were not found in the WES waste, therefore adding to the number of
parameters evaluated by this investigation. j
!
PCE Waste ;
t
The PCE waste was an actual industrial waste produced as a by-product
from the reclamation of spent dry cleaning solvent. It contained 14 toxic
metals, including antimony, arsenic, barium, beryllium, cadium, chromium,
copper, lead, mercury, nickel, selenium, silver, thallium, and zinc.
15
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-------
STUDY A
Waste Description !
The WES sludge is a synthetic waste.produced by hydroxide precipitation
of a concentrated metal nitrate solution: The metal nitrate solution was pre-
pared by dissolving four metal nitrate salts, cadmium nitrate (Cd(N03)2'4H20) ,
chromium nitrate (Cr(N03)3-9H20), nickelous nitrate (Ni(N03)2-6H20) , and mercury
nitrate (Hg(N03)2'H20) in 500 gal* of American Society for Testing and
Materials type III water (ASTM 1986). This mixture produces a solution with
metal ion concentrations approximately 600 times the EP limits. This metal
nitrate solution was treated with 97.5 Ib of calcium hydroxide to precipitate
the metal ions from solution. The resulting sludge was separated from the
supernatant, and the sludge was filtered using an Eimco Model 3613 vacuum
filter. Typically, the filtration process produced a sludge with 27% to 35%
solids by weight. The dewatered sludge was homogenized with a model 20-E Stow
paddle type mixer and passed through a 30-mesh screen to remove large
particles. A moisture analysis was performed on the homogenized sludge. The
method used in determining the moisture content is outlined in Appendix C.
Based on the sludge's moisture content, supernatant was added to the sludge to
adjust the solids content of the sludge to 25% +0.5. This 25% solids sludge.
was a semifluid with an approximate density of 11,7 Ib/gal, and a pH of 11.
Results of the average bulk chemical analyses for this sludge are presented in
Table 3. This material was stored at 4° C until needed for testing.
ANALYSES OFTHE WES SLUDGE
Parameter
Cadmium
Chromium
Nickel
Mercury
Calcium
Total solids
Ionic
Species
Cd+2 ',
Cr+3
Ni+2
Hg+2 :
Ca+2
. _
Concentration
(mg/kg wet weight)
4 , 000
18,000
19 , 000
200
60,000
25%
Preparation of Test Samples
Approximately 250 Ib of 25% sludge was divided into ten 25-Ib samples.
The sludge was solidified/stabilized using lime kiln dust. Compositional and
chemical analyses of the kiln dust used in this study are summarized in
* A table of factors for converting non-Si units of measurement to SI
(metric) units is presented on page xiii.
18
-------
Tables 4 and 5. Each 25-lb sample of sludge was solidified/stabilized with
27.5 Ib of the lime kiln dust. Prior to the initial set, each sample was sub-
divided into four equal portions. One of the ten interfering compounds
(Table 6) was added to each portion at approximate percentages* of 0%, 2%, 5%,
or 8% (wet weight interference compound to kiln dust/sludge mixture). Due to
the large number of samples required, all the specimens used in t^his study
could not be prepared at one time. The sludge/kiln dust/interference mixtures
were prepared in several batches according to the schedule preserited in
Table 7. . '
After each waste/kiln dust/interference mixture was thoroughly homog-
enized, two samples were prepared by pouring the slurry into two |850-ml
plastic disposable cylindrical molds. The samples were cured in :the molds at
23° C and 98 percent relative humidity for a minimum of 24 hours and removed
from the molds whenever they developed sufficient strength to'be'free stand-
ing. After removal from the molds, the samples continued curing for a period
of 28 days under the same conditions. ;
At the end of the 28-day cure period, the samples were ground with a mor-
tar and pestle to pass a 9.5-mm sieve. Ground materials from, duplicate sam-
ples were recombined and sealed in 1,000-ml polyethylene bottles.; Thus, a
single sample was prepared for each of the 10 interfering compounds at the
four interference compound percentages. ' . .
The bottles were agitated in an end-over-end fashion.to mix their con-
tents, and samples were collected to determine the moisture content of the
materials (as outlined' in Appendix C). Duplicate subsamples were collected
from each bottle containing the ground materials. These duplicate subsamples
were subjected to EP and TCLP methods outlined in Appendices A and B. A
method blank was carried through the extraction procedures for each inter-
ference compound. The matrix of test specimens subjected to the|EP and TCLP
extractions along with the age of the extraction sample at the time of analy-
sis is presented as Table 7. |
1
Analytical Procedures - . -.
The EP and TCLP extracts were analyzed for various metals. !The analyti-
cal and digestion methods used are presented in Table 8. j
Quality Assurance/Quality Control :
Both internal and external laboratory quality assurance/quality control
(QA/QC) measures were performed during the course of Study A. External QA/QC
is defined as that which is performed by the laboratory conducting the extrac-
tions; internal QA/QC is the which performed by the laboratory that analyzes
the extract for the contaminants of interest. External QA/QC consisted of
(1) carrying method blanks through the extractions every 9th sample and
(2) submitting standards to the analytical laboratory every 10th| sample.
Internal QA/QC consisted of performing the metal analysis by the method of
standard additions. !
Actual concentrations were 0%, 1.96%, 4.76%, and 7.41%.
19
-------
TABLE 4. COMPOSITIONAL ANALYSES OF BINDER MATERIALS
Compositional
Analysis
Silicon dioxide (Si02)
Aluminum oxide (Al^O.,)
Iron (III) oxide (Fe^)
Calcium oxide (CaO)
Magnesium oxide (MgO)
Sulfite (S03)
Insoluble residue
Moisture loss
Loss on ignition
Titanium (IV) oxide (TiO£)
Manganese oxide (Mn-O.,)
Phosphorus pentoxide (P2°5
Total Alkali
Sodium oxide (Na_0)
Potassium oxide (K20)
Sodium (Na)
Potassium (K)
Total as Na00
Acid-Soluble Alkali
Sodium oxide (Na20)
Potassium oxide (K?0)
Sodium (Na)
Potassium (K)
Water-Soluble Alkali
Sodium oxide (Na?0)
Potassium oxide (K_0)
Sodium (Na)
Potassium (K)
Type I
Cement
(as percent)
20.47
5.40
3.58
64.77
0.87
2.73
0.17
0.43
0.96
0.28
0,06
) 0.28
0.12§
0.28
0.05
0.11
0.30
0.12
0.28
0.05
0.11
0.018
0.139
0.0075
0.0577
Flyash
Class F
(as percent)
49.67
29.15
7.11
1.26
1.43
0.23*
70.70t
0.12f
4.07
0.20
0.00
1.00
0.23
2.33
0.10
0.97
1.76
0.06
0.50
0.03
0.21
0.050
0.105
0.0210
0.0440
Kiln Dust
(as percent)
6.94
4.23
1.47
62.93
0.44
7.01
3.09
0.05
14.08
:o.n
0.00
0.05
0.25S
0.40
0.10
0.17
0.51
0.25
0.40
0.10
0.17
0.021
0.050
0.0088
0.0208
* Acid-soluble sulfate.
f Includes SiO (silicon
dioxide) . ;
f Free water. ;
§ Cement, lime, and kiln dust alkalies totally dissolve in acid; therefore,
total acid and acid-soluble analysis will be the same.
-------
TABLE 5. CHEMICAL ANALYSES OF BINDER MATERIALS
Chemical
Analysis
Silicon (Si)
Total sulfur (S)
Titanium (Ti)
Phosphorus (P)
Antimony (Sb)
Arsenic (As)
Beryllium (Be)
Cadmium (Cd)
Chromium (Cr)
Copper (Cu)
Lead (Pb)
Mercury (Hg)
Nickel (Ni)
Selenium (Se)
Silver (Ag)
Thallium (Tl)
Zinc (Zn)
Aluminum (Al)
Barium (Ba)
Calcium (Ca)
Cadmium (Cd)
Iron (Fe)
Magne s ium (Mg )
Manganese (Mn)
Sodium (Na)
Tin (Sn)
Vanadium (V)
Cement
Type I
(mg/kg)
95,700
10,800
1,400
900
<1.77
13.1
2.13
0.284
61.3
14.9
2,13
<0.100
25.9
<17.7
<3.54
<10.6
41.8
23,100
178
454,000
<10.6
25,400
5,460
503
1,270
195
55.6
Kiln Dust
(mg/kg)
1,900
700
50
60
<1.63
14.7
4.24
2.28
30.0
12.7
15,6
<0.100
33.6
<16.3
<3.26
<9.78
107
13,500
119
440,000
<9.78
14,800
3,040
64.2
2,110
73.0
34.6
Fly ash
; Class F
(mg/kg)
: 32,400
' 31,200
: eoo
! 200
!
i 13.3
' 172
! 28.9
!
: 1.01
' 139
196
i
57.7
; <0.100
; 190
: <19.5
<3.90
i
i 13.6,
' 211
; 150,000
1,350
; 12,000
i 77.2
] 50,700
; 6,040
' 156
2,740
I 118
351
21
-------
TABLE 6. INTERFERENCE COMPOUNDS UTILIZED IN STUDY A
Organic Interference
Inorganic Interference
Oil
Grease
Hexachlorobenzene-HCB
Trichloroethene-TCE
Phenol
Lead nitrate-Pb(N03)2
Zinc nitrate-Zn(N03)2
Copper nitrate-Cu(N03)2
Sodium hydroxide-NaOH
Sodium sulfate-Na2SO/,
STUDY B
Waste Description
WES Sludge--
The WES sludge used in Study B was the same synthetic metal waste that:
was used in Study A. A detailed description of how this waste was prepared is
givan in the Study A "Waste Description" section.
WTG Waste-- ;
The WTC metal solution was prepared by dissolving 0.04 mole of chromium
chloride (CrCl3'9H20) , cadmium nitrate (Cd(N03)2-2H20) , lead nitrate (Pb(N03)2) ,
sodium arsenite (NaAs02) , and phenol in ASTM type I water (ASTM 1986). This
solution had a total dissolved solids content of 3.4%, a density of 62 lb/ft3,
and a pH of 2.5. Results of the bulk chemical analysis for this waste are
presented in Table 9. This material was 'stored at 4° C until needed, for
testing.
PCE Waste--
The PCE waste was generated as a by-product from the reclamation of spent
dry cleaning solvent. The PCE waste is a listed hazardous waste (K030) (USEPA
1987). The waste production and reclamation process is summarized below.
Perchloroethene is typically used as a cleaning solvent in dry cleaning
operations. When the PCE becomes contaminated with dirt and solids it is
passed through paper cartridge filters to remove the dirt and solids and
extend the useful life of the PCE. Eventually, these paper filters become
fouled, and the entire cartridge must be disposed. The PCE solvent retained
in the filter can be reclaimed for reuse :by utilizing a batch distillation
treatment method. A schematic diagram of the batch distillation unit is shown
in Figure 6. The PCE waste utilized in this study was the residual, or
bottoms product, resulting from this type of distillation operation. A chemi-
cal analysis of the PCE waste is presented in Table 10.
22
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24
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TABLE 8 CHEMICAL ANALYSIS METHODS i
Parameter
of Interest
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Copper
Lead
Mercury
Nickel
Selenium
Silver
Thallium
Zinc
Volatile organics
US EPA*
Digestion Method
NA
NA
3020
3020
3020
3020
3020
3020
NA
3020
3020
3020
3020
3020
NA
i US EPA
Analytical Method
7041* with Zeeman
1 7760*
i 6010f
; eoiot
7131*
i 7191*
6010f
7421*
1
i 7470*
i eoiot
7740* with Zeeman
: 7761*
; 7841f
' 6010*
[
; 8240
* USEPA.SW-846 2nd edition (USEPA 1982). ;
USEPA SW-846 3rd edition (USEPA 1986d). !
i
Preparation of Test Samples j
WES Sludge-- ; '
Approximately 4.2 Ib of Type I Portland cement was mixed with 14 Ib of
the 25% solids WES sludge in a Hobart C-100 mixer. A compositional analysis
of the cement is presented in Table 4. After thorough mixing and prior to the
initial set, this solidified/stabilized sludge was divided into two equal por-
tions, each weighing 8.59 Ib. To the first portion, 0.086 and 0:0086 Ib,
respectively, of each of the 12 organics listed in Table 11 was added to the
cement/sludge slurry and thoroughly mixed. This resulted in cement/sludge
mixtures that contained approximately 1.0% (by weight) and 0.1%,;respectively,
total of organics. Each of these mixtures was poured into three,1-liter
25
-------
TABLE 9. BULK ANALYSIS OF WTC SOLUTION
Ionic
Parameter Species
Arsenic As+3
Cadmium Cu*2
Chromium Cr*3
Lead Pb+2
Phenol
Total solids (percent)
pH
Bulk density (g/cm3)
Concentration*
2,400
4,600
1,600
8,100
3,700
3
2
1
.4
.5
.0
* Expressed as milligrams per kilogram wet weight unless specified otherwise.
polyethylene bottles and sealed. The cement/sludge/organic mixtures were
cured at 4° C in the sealed bottles until they were needed for testing.
WTC Waste
Approximately 4.4 Ib of the WTC synthetic metal solution was solidified/
stabilized with 4.4 Ib of Type I Portland cement, 4.4 Ib of a type F flyash.
and 4.4 Ib of a soil. A composite analysis of the cement and flyash is given
in Table 4. The soil was a Sandy Clay CL Gray Type as classified by the
Unified Soil Classification system (USAEWES 1960). The waste/cement/flyash/
soil mixture was split into two 8.8-lb portions. Then, 0.088 Ib or 0.0088 Ib
of each of the organic compounds listed in Table 11 was added to each portion.
The mixtures were poured into polyethylene bottles and sealed. The sealed
bottles were stored at 4° C until needed for testing.
PCE Waste---
Unlike the WES and WTC wastes, the PCE waste was not solidified. Using
the Hobart mixer, 6.6 Ib of raw PCE waste was homogenized. The PCE waste was
split into two 3.3-lb portions. Then, Oi.033 Ib or 0.0033 Ib of each of the
organic compounds listed in Table 11 was mixed with each portion, respec-
tively. These mixtures were poured into polyethylene bottles and sealed. The
sealed bottles were stored at 4° C until needed for testing.
Sample Extraction--
The WES and WTC wastes cured for a period of 14 days, and the PCE waste
aged for 14 days. The waste materials were crushed in the sealed plastic bot-
tles to minimize volatile losses. Each waste material was then ground in a
26
-------
WASTE
FEED
BATCH
DISTILLATION
STORAGE
BOTTOMS PCE WASTE
USED IN THIS STUDY
CONTINUOUS
FRACTIONATION
COLUMN
STORAGE
THIN FILM
EVAPORATION
> Mlh
STORAGE
JFRAI SPIRI
TS
. PERCHLOROETHYLENE
PRODUCT
* TO FRACTIONATION COLUMN
BOTTOMS PRODUCT
Figure 6. Flowchart of PCE waste production.
TABLE 10." BULK ANALYSES OF PERCHLOROETHYLENE WASTE;
Parameter
Concentratxon
! (rag/kg) .
Antimony
Barium
Beryllium
Cadmium
Chromium
Copper
Nickel
Silver
Zinc
Arsenic
Lead
Mercury
Selenium
Thallium
Total organic halogens
Chemical oxygen demand
11.2
| 265
; 0.3
; 19.1
| 185
i 2.390
I 223
I 5.8
! 1,600
8.9
r
| 376
; 2.0
i
; 1.7
, <1.0
: 4,660
1887,000
; 6.07
27
-------
TABLE 11. ORGANIC COMPOUNDS ADDED TO STUDY B SLUDGES f_
1. Chloroform 7. 1,1,2,2-Tetrachloroethane
2. 1,2-Dichloroethane 8. Tetrachloroethene
3. 1,1,1-Trichloroethane 9. Toluene
4. Carbon Tetrachloride 10. Ethlybenzene
5. Trichloroethene ' 11. Methyl Ethyl Ketone
6. Benzene 12. Methyl Isobutyl Ketone
chilled mortar (also to minimize volatile losses) and screened through a
9.5-mm sieve. The resulting fines, for each waste, were placed in glass jars
and mixed. Samples were collected from each jar for moisture analyses
(Appendix C). After each waste (WES 0.1%, WES 1.0%, WTC 0.1%, WTC 1.0%, PCE
0.1%, and PCE 1.0%) was homogenized, the wastes were subjected to triplicate
EP and TCLP extractions as presented in Appendices A and B. The EP was per-
formed in tumbled, closed glass containers. The TCLP was conducted using the
ZHE vessel for the extraction of volatile organics and closed glass containers
for the extraction of nonvolatiles (metals).
Analytical Procedures :
The EP and TCLP extracts were analyzed for metals and volatile organic
compounds. The analytical and digestion methods used in this study are
presented in Table 8. Extract samples submitted for metal analysis were
digested; extract samples submitted for volatile organic analyses were not:
digested.
Spike and Recovery Study
Loss of volatile organics during conduct of the EP and the TCLP methods
and subsequent sample handling was evaluated. Three volatile organic spikes,
1,1,2-trichloroethane, carbon disulfide,; and chlorobenzene, were added to the
extraction fluid at two points in the extraction process. Spikes were added
prior to waste extraction (the prespike) and following the extraction pro-
cedure but prior to any analyses (the postspike). The volatile organic spikes
chosen had a wide range of vapor pressures and solubilities. Selected
properties of these volatile organic compounds are listed in Appendix D. The
volatile organic compounds used as spikes were alternated as prespikes and
postspikes, as listed in Table 12. I
i
Quality Assurance/Quality Control
Internal and external laboratory QA/QC measures were performed for
Study B. Method blanks were carried through the metal and volatile extraction
every fourth sample. Duplicate, spike recovery, and surrogate recovery analy-
ses were performed as part of internal QA/QC measures, for the volatile analy-
ses. The method of standard addition was utilized for all metal analyses.
28
-------
TABLE 12. VOLATILE SPIKE ADDITIONS FOR STUDY B
Prespike
Addition
Organic Extraction Spike Concentration
Level Test Compound (mg/1)
WES
0.1% TCLP 112 TCA*
EP
1.0% TCLP CLBEN
CS2
EP CLBEN
CS2
PCE
0.1% TCLP 112 TCA
EP
1.0% TCLP CLBEN
CS2
EP CLBEN
CS2.
WTC
0.1% TCLP 112 TCA
CS2
EP 112 TCA
CS2
1.0% TCLP CS2
EP CS2
Waste
252
45
130
50
127
Waste
82
_«.
20
48
20
30
Waste
15
25
15
25
30
30
Postspike
Addition
Spike Concentration
Compound ; (mg/1)
!
CLBEN t !
CS2f ;
112 TCA ;
CLBEN
CS2 i
112 TCA :
>
112 TCA :
CLBEN :
CS2 ;
CLBEN
CS2
I
:
:
CLBEN !
CLBEN ;
i
CLBEN I
f
CLBEN
120
50
143
55
127
250
250
20
48
21
20
7
7
10
10
* 1,1,2-Trichloroethane.
t Chlorobenzene.
f Carbon disulfide.
29
-------
STATISTICAL, PROCEDURES
Statistical analyses were performed, using the Statistical Analysis Sys-
tem (SAS) software package provided by SAS Institute, Inc. (1987). An analy-
sis of the variance multifactor factorial test, as described by Miller and
Freund (1985), was conducted on data sets produced by Study A and Study B. An
analysis of variance (ANOVA) procedure outlined in Chapter 11 of the SAS/STAT
user guide (SAS Institute, Inc. 1987) was used to perform this statistical.
procedure.
When it was determined that the levels of interaction were significant, a
"paired-sample T test" (Miller and Freund 1985) was used to determine if the
EP and TCLP results differed significantly. A MEANS procedure outlined in
Chapter 33 of the SAS/STAT user guide (SAS Institute, Inc. 1987) was used to
perform this statistical procedure. ;
Concentrations below detection levels were estimated by dividing the
detection level by 2 rather than using the actual detection level or zero, as
an estimate of the concentration. This is an accepted method of reporting
concentration values near the detection limit (Francis and Maskarinec 1986).
The multifactor factorial experimental designs for Study A and Study B
are illustrated in Tables 13 and 14, respectively. One multifactor factorial
method was performed for each contaminant. Decisions on whether to reject: or
accept the null hypothesis were made using an alpha level of significance of
0.05, or 20:1 odds.
30
-------
TABLE 13. STUDY A MULTIFACTOR FACTORIAL EXPERIMENTAL DESIGN
Level
1
2
3
4
5
6
7
8
9
10
A. B. C. i
Interference Interference Extraction i D.
Compound Concentration Test Replicate
Oil 0% TCLP : 1
Grease 2% EP : 2
HCB* 5%
Phenol 8% ;
TCEt !
i
Lead ;
nitrate ;
Zinc ;
nitrate !
Copper
nitrate . ;
i
Sodium j
hydroxide
Sodium
sulfate :
* Hexachlorobenzene.
t Trichloroethene.
TABLE 14. STUDY B MULTIFACTOR FACTORIAL EXPERIMENTAL DESIGN
Level
1
2
3
A. Sludge
Type .
WES
WTC
PCE
B . Organic
Concentration
1.0%
0.1%
C. Extrac-
tion Test ;
TCLP
EP i
D.
Replicate
1
2
31
-------
SECTION 5
RESULTS AND DISCUSSION
STUDY A
The results from the EP and TCLP extractions conducted during Study A are
presented in Tables 15 and 16 and Figures 7 through 10. Raw data for each
sample subjected to an EP or TCLP extraction are presented in Appendix E.
Table 15 presents the average (averaged over the duplicate samples)
extract concentrations for the TCLP and EP test for each contaminant. Summary
statistics for this data set are presented in Table 16. The values presented
in Table 16 are averaged across the different interference compounds and con-
centrations and thus cannot be utilized for a detailed interpretation of the
data. However, this information can be used to visualize general trends.in
the data set. Table 16 indicates that a larger concentration of mercury is
detected in the TCLP and EP leachates than the other metals. Table 16 also
indicates that the TCLP average extract values for chromium are 1.3 times
larger than the average EP extract values.
To establish a basis for comparing the many batches of sludge that were
extracted as part of Study A, it was necessary to normalize the data. The
extract concentrations that were compared in this study were normalized to
their dry-raw waste concentration. Normalization corrects for dilution by the
interference materials, small changes in the binder ratio, and variations in
the moisture contents of the extracted materials. Normalized extract concen-
trations were derived using the following equation:
ECn - (EC * V)/(W * M * B) (1)
where ECn - normalized extract concentration, mg/kg
EC - contaminant concentration measured in the TCLP or EP extract, mg/1
V - volume of extraction fluid, liters
W - weight of the wet treated waste extracted, kg
M - solids concentration of the solidified/stabilized waste extracted,
expressed as a decimal
B - weight fraction of raw waste in the solidified/stabilized/
interfered waste mixture, calculated as follows: .
weight of raw waste
(weight of raw waste + weight of binder + weight
of interference agent)
Results of the analysis of the variance multifactor factorial test
(AVMFT) performed on the Study A normalized extract concentrations are
presented in Table 17. When the results of the AVMFT indicated the levels of
interactions between the tests and the other variables were significant, a
paired-sample T test was also performed. If the test interactions are sig-
nificant, the paired T test result must be utilized to evaluate the data. The
32
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20
15
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INTERFERENCE
CONCENTRATION
INTERFERENCE COMPOUND
Figure 7. Average normalized Study A cadmium extract
concentrations expressed as the TCLP
concentration divided by the EP
concentration.
36
-------
so
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20
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INTERFERENCE
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INTERFERENCE COMPOUND
Figure 8.
Average normalized Study A chromium extract
concentrations expressed as the TCLP
concentration divided by the EP
concentration.
37
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TABLE
17. RESULTS OF AVMFT PERFORMED ON NORMALIZED STUDY A TCLP
AND EP METALS RESULTS
Metal
Contaminant
Cadmium
Chromium
Nickel
Mercury
Inter-
ference
Compound*
Y
Y
Y
Y,
Interference
Concentrationt
N
Y
N
Y,
(Results Presented
Extrac-
tion
Testf
N
Y
N
Y
as "Yes
Replicdte
N
N
N
N
or No")f
Test
Inter-
action
N
N
Y.
Y
R
Value §
0.5961
0.9413
0.7716
0.9826
* Compounds are listed in Table 6.
t Interference concentrations = 0%, 2%, 5%, and 8%.
f EP and TCLP.
§ R values give an indication of how well the statistical model fits the
data. As the fit of the model improves, the R value approaches 1.0.
ff Yes (Y) indicates there is statistical difference between the variables
compared at a = 0.05 .
TABLE 18. RESULTS OF PAIRED-SAMPLE T TEST PER-
FORMED ON NORMALIZED STUDY A TCLP AND EP
NICKEL AND MERCURY DATA
Metal Contaminant . 'Extraction Test1*
Nickel '. N
Mercury Y
Note: The paired T test was performed only when
the levels of interaction were found to be
significant in the AVMFT.
* Yes (Y) indicates there! is statistical dif-
ference between the EP and TCLP results at
a = 0.05 .
40
-------
results of the paired T test are presented in Table 18. As indicated by
Tables 17 and IS, using a level of significance of a = 0.05 , the results of
the TCLP and EP extractions for chromium and mercury are statistically dif-
ferent, while the results for nickel and cadmium contaminants were not
statistically different. j
Results of the TCLP and EP extractions for each metal contaminant in
Study A-are presented in Appendix F, Figures Fl through F4. In these figures,
the normalized EP extract concentrations are plotted versus the riormalized
TCLP extract concentrations. A discussion accompanies these figures.
Figures 7 through 10 present the normalized TCLP and EP extracts
expressed as multiples of the average EP values for the duplicate samples.
The values presented in these figures were calculated as shown bj| the
following equation: ;
(TCLP, + TCLP9)/2 :
1 2 (3)
(EP1 + EP2)/2 ;
where TCLP' and TCLP- = normalized TCLP replicate extract concentration for
the contaminant of interest, mg/g
EP and EP? = normalized EP replicate extract concentration for the
1 contaminant of interest, mg/g :
Thus., for these figures, a value of 1.0 indicates that the amount of a partic-
ular contaminant measured in the TCLP extract is equal to the amount of that
contaminant measured in the EP extracts. Values greater than 1.0 indicate
that the TCLP extract concentration is greater than the EP extract concentra-
tion, and values less than 1.0 indicate that the EP concentration is greater
.than the TCLP. ' ' ;
Figure 9, showing the nickel data, indicates that for the majority of the
conditions evaluated, the EP and-TCLP produce similar results. Figures 8 and
10 illustrate that the TCLP extraction is more aggressive for chromium and
mercury. Figure 10 (the mercury data) indicates that of the 40 conditions
investigated in Study A, 28 resulted in TCLP extracts containing! higher con-
centrations of mercury. Figure 8 (the chromium data) indicates that 25 of the
40 conditions resulted in TCLP extracts containing higher concentrations of
chromium. ;
It is interesting to note that inspection of Figure 7 provides informa-
tion which is in direct conflict with the results of the statistical analysis.
Figure 7 (the cadmium data) indicates that, for 33 of the 40 conditions eval-
uated, the EP extracts contained higher concentrations of cadmium. Figure 7
indicates that the results of the EP and TCLP differ, while the statistical
results presented in Table 17 indicate no difference between the extract con-
centrations. Based on this information, there is a possibility ;that a Type II
error was made. (A Type II error occurs when the results of the EP and TCLP
extraction are actually different but this is not revealed by the analysis of
the variance statistic.)
41
-------
Although it is interesting that for, some contaminants the EP and TCLP
extraction results differ, it is beyond the scope of this study to pinpoint
the variables that are responsible for the dissimilarities. However, there is
one observation that should be noted. Due to the fact that every TCLP extrac-
tion for Study A utilized extraction fluid 2, and every EP extraction required
the full 400 ml of 0.5 acetic acid (Appendix A), the buffering capacity of the
EP and TCLP extraction fluids was equal.; This leads to the conjecture that
the EP and TCLP extractions should be similar in their aggressiveness. Con-
trary to the similarity between extraction fluids, the TCLP results varied
from the EP results for mercury and chromium. Consequently, the variations
between the EP and TCLP extracts cannot be attributed just to pH influences
but must be a function of other differences between the extraction procedures,
such as time of extraction, method of agitation, etc. .
STUDY B
Results for the Metal Contaminants
The results for the Study B metal EP and TCLP extraction tests are pre-
sented in Tables 19 through 22 and Figure 11. Raw data for each sample sub-
jected to the EP or TCLP extraction for ;metal compounds are presented in
Appendix Gs Tables Gl through G3. Table 19 presents the average (averaged
over the three replicates) metal extract concentrations for the TCLP and EP
tests. Results presented in this table generally indicate that the TCLP-
generated extracts contained higher concentrations of the metal contaminants
than the EP extracts.
Summary statistics for this data set are presented in Table 20. As indi-
cated in this table, 10 of the 15 average metal values were higher in the TCLP
than the EP extracts. This table also illustrates that the EP data generally
varied over a larger range than the TCLP data.
Results of the AVMFT performed on the Study B metal data are presented in
Table 21. As in Study A, when the results of the AVMFT indicate that the
levels of test interaction are significant, a paired T test was performed.
Results of the paired T test are presented in Table 22. Statistical analysis
for the WES waste indicates that there is not a significant difference between
the EP and TCLP extraction for any of the metals except mercury. The statis-
tical analysis for the WTC waste indicates that the EP and TCLP differ signi-
ficantly for arsenic and lead and were not statistically different for
chromium. The results of the PCE waste extractions indicated that there were
statistical differences between concentrations of copper, zinc, and barium
contaminants measured in the TCLP and EP extracts. Several values are
reported in Table 21 as "DL." This indicates that the concentration of these
contaminants were, in the TCLP and EP extracts, at or below the detection
limits. These extracts have no basis for comparison; consequently, the
results for the PCE-arsenic, PCE-silver,; and WTC-cadmium are omitted for the
remainder of the discussion.
A graphical representation of the results of the TCLP and EP extractions
for each metal contaminant in Study B is presented in Appendix H, Figures Hi
through H7. In these figures, the normalized EP extract concentrations are
plotted versus the normalized TCLP extract concentrations. A discussion of
the results accompanies these figures.
42
-------
TABLE 19. STUDY B AVERAGE TCLP AND EP EXTRACT CONCENTRATIONS FOR
METAL CONTAMINANTS (AVERAGED OVER THREE REPLICATE SAMPLES)
Metal
Contaminant
Antimony
Arsenic
Barium
Cadmium
Chromium
Copper
Sludge
WES
WTC
PCE
WES
WTC
PCE
WES
WTC
PCE
WES
WTC
PCE
WES
WTC
PCE
WES
WTC
PCE
*t -.
Organic Level
Percentage
0.1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
(Continued)
Extract Concentration
(mg/1)
EP ;
NA*
NA '
NA
NA
0.0273 :
0.023
NA ;
NA '
0.021 ;
0.028
0.0041
0.005 ;
NA ;
NA :
NA '
NA ;
0.382 i
0.334
0.001 i
0.030
0.0004 \
<0.0001 ;
NA ;
NA ,
0.024 :
0.130 i
0.041
0.032
NA
NA
NA
NA i
NA
t
NA
10.747 i
10.833
TCLP
NA
NA
NA
NA
0.0367
0.038
NA
NA
0.055
0.121
<0.005
0.007
NA
NA
NA
NA
0.459
0.561
0.010
0.007
0.0002
0,0018
NA
NA
0.070
0.056
0.040
0.036
NA
NA
NA
NA
NA
NA
13.067
16. ,333
* Not analyzed.
43
-------
TABLE 19. (Concluded)
Metal
Contaminant
Lead
Mercury
Nickel
Silver
Zinc
Sludge
WES
WTC
PCE
WES
WTC
PCE
WES
WTC
PCE
WES
WTC
PCE
WES
WTC
PCE
Organic Level
Percentage
6.1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
0,1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
0.1
1.0
p.l
1.0
0.1
1.0
0.1
1.0
Extract Concentration
(mg/1)
EP
NA
NA
0.007
0.013
0.036
0.028
7.957
0.019
NA
NA
NA
NA
0.021
0.184
NA
NA
NA
NA
NA
NA
NA
NA
0.002
0.004
NA
NA
NA
NA
29.267
16.733
TCLP
NA
NA
0 . 228
0.044
0.065
0.074
7.843
8.310
NA
NA
NA
NA
0.120
0.205
NA
NA
NA
NA
NA
NA
NA
NA
<0.001
<0.001
NA
NA
NA
NA
32.200
32.933
44
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TABLE 21. RESULTS OF STATISTICAL ANALYSIS FOR NORMALIZED
STUDY B TCLP AND EP METAL EXTRACTS
Sludge
WES
WTC .
PCE
Metal
Contaminant
Cadmium
Chromium
Nickel
Mercury
Arsenic
Cadmium
Chromium
Lead
Antimony
Arsenic
Copper
Lead
Silver
Zinc
Barium
Organic
Levels*
N
N
N
Y
Y
DL
N
Y
N
DL
Y
N
DL
N
N
Extraction
Testt
N
N
N
Y
Y
DL
N
Y
Y
DL
Y
Y
DL
Y
Y
Replicate
N
N
N
N
N
DL
N
N
N
DL
N
N
DL
N
N
Test :
Inter-
action
i
N !
N '
N i
Y .
Y
__ ,
N
Y
N |
Y
N i
;
Y ;
Y ;
R Valuef
0.598
0.424
0.653
0.973
0.973
0.530
0.906
0.947
0.929
0.878
0.902
0.913
Note: Results presented as "Yes (Y)" or "No (N)." Yes indicates there is
statistical difference between the variable compared at a = 0.05 .
DL = detection limit.
* 0.1% and 1.0%.
t SP and TCLP. .
t R :values give an indication of how well the statistical model fits the
data. As the fit of the model improves, the R value approaches 1.0.
Figure 11 presents, for all three sludges, the normalized TCLP and EP
extracts expressed as multiples of EP values averaged for the replicate sam-
ples,, The figure illustrates that the TCLP is a more aggressive!extraction
for the metal contaminants. On the average, the extract from the TCLP con-
tained concentrations of metals approximately twice as large as the metal con-
centrations measured in EP extracts. 1
The results of the Study B metal extractions are summarized.as follows.
(1) The results of the statistical analysis indicate that, for the PCE
waste, the TCLP and EP extractions produce extracts that are significantly
different. This may be explained by the fact that the PCE sludge had a pH of
6 and was not solidified/stabilized. Because of the low alkalinity of this
material, extraction fluid 1 was used for the TCLP extraction, and little acid
was added in the EP extraction. Thus, the TCLP and EP extraction fluids were
substantially different. It is suspected that the results of the TCLP and EP
extractions varied as the result of the difference in extraction; fluids.
47
-------
TABLE 22. RESULTS OF PAIRED-SAMPLE T TEST FOR NORMALIZED
STUDY B TCLP AND EP METAL EXTRACTS
Sludge
Metal Extraction
Contaminant Test*
Cadmium
Chromium
Nickel
Mercury ;
Arse'nic
Cadmium '
Chromium
Lead
Antimony
Arsenic
Copper
Lead
Silver ,
Zinc ,
Barium
Note: The paired T test was performed only when the levels of interaction
were found to be significant in the AVMFT.
* Yes (Y) indicates there is statistical difference between the EP and TCLP
results at a = 0.05 .
(2) For a majority of the cases studied, the WES and WTC wastes produced
TCLP and EP extracts that were not statistically different. Arsenic and lead
were the only contaminants for which the TCLP and EP statistically differed.
One possible explanation for the EP and TCLP generating extracts with similar
contaminant concentrations is that the WTC and WES wastes were solidified/
stabilized, resulting in high alkalinity. Consequently, the TCLP extraction
for the WES and WTC wastes required the use of extraction fluid 2. The EP
extraction, performed on the WES and WTC wastes, also required the addition of
the full 400 ml of acetic acid because of the low alkalinity. When 400 ml of
0.5 N acetic acid is added to 1,600 ml of water, the alkaline neutralization
capacity of the EP extraction fluid and the TCLP's extraction fluid 2 are
equal. Equal alkaline neutralization capacity offers one explanation for the
WTC and WES sludges producing similar TCLP and EP extracts.
Results for the Organic Contaminants
The results of the organic analyses for the Study B extraction procedures
are presented in Tables 23 through 25 and Figures 12 through 13. The raw data
for each sample subjected to an EP or TCLP extraction for the organic com-
pounds are also presented in Appendix I, Tables II through 112. Table 23
presents the average (averaged over the! three replicates) extract concentra-
tions for the TCLP and EP tests. The results presented in this table indicate
48
-------
500
400 -
300
200
100i"
ORGANIC
CONCENTRATION
D 0.1%
H 1.0%
In
n
co
UJ
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0.
- WEE-
-PCE
-WTC-
INTERFERENCE COMPOUND
Figure 11. Average normalized Study B metal extract concentrations
expressed as the TCLP concentration divided by! the EP
concentration.
49
-------
TABLE 23. STUDY B AVERAGE TCLP AND EP EXTRACT CONCENTRATIONS
FOR THE ORGANIC' CONTAMINANTS
(AVERAGED OVER THREE REPLICATE EXTRACT SAMPLES)
Organic
Contaminant
Chloroform
1 , 2-Dichloroe thane
1,1, 1-T'richloroethane
Carbon Tetrachloride
Trichloroethene
Sludge
WES
PCE
WTC
WES
PCE
WTC
WES
PCE
WTC
WES
PCE
WTC
WES
PCE
WTC
Organic
Level
0.1%
1.0%
0'. 1%
1.0%
0.1%
1.0%
0.1%
1.0%
o'.i%
1.0%
0.1%
1.0%
0,.1%
1.0%
0.1% '
1.0%
0.1%
1.0%
C.I"
1.0%
0.1%
1.0%
0.1%
1 . 0%
0.1%
1.0%
0.1%
1.0%
0.1%
1.0%
Extract
EP
0.88
13.97
1.01
23.77
0.22
8.98
1.57
38.70
3.61
57.30
0.76
45.03
0.96
18.33
0.55
15.07
0.29
15.07
0.42
3.93
0.23
10.00
0.10
5.00
3.47
64.63
1.48
33.73
2.32
98.07
Concentration
(mg/1)
TCLP
1.40
27.27
1.56
32.70
.20
9.13
1.27
61.37
4.23
71.40
0.49
44 . 23
1.93
46.80
4.80
2.5.07
0.45
2.4.83
0.89
7.60
0.50
1.0.00
0.20
5.00
6.90
134.33
3.54
39.97
2.55
135.67
(Continued)
(Sheet 1 of 3)
50
-------
TABLE 23. (Continued)
Organic
Contaminant
Benzeme
1,1,2,2-
Tetrachloroethane
Tetrachloroethene
Toluene
Ethylbenzene
Sludge
WES
PCE
WTC
WES
PCE
WTC
WES
PCE
WTC
WES
PCE
WTC
WES
PCE
WTC
Organic
Level
0.1%
1.0%
0.1%
1.0%
0.1%
1.0%
0.1%
1.0%
0.1%
1.0%
0.1%
1.0%
0.1%
1.0%
0.1%
1.0%
0.1%
1.0%
0.1%
1.0%
0.1%
1.0%
0.1%
1.0%
0.1%
1.0%
0.1%
1.0%
0.1%
1.0%
Extract
EP
1.60
42.97
2.62
54.17
0.91
55.23
0.25
1.00
7.31
92.70
0.10
5.00
3.10
25.97
3.03
28.30
1.00
18.87
3.03
55.43
1.37
36.67
1.24
65.67
5.27
33.83
2.03
34.53
2.93
36.10
i Concentration
(mg/1)
TCLP
' 2.30
85.33
5 . 29
! 76.57
0.79
62.40
0.22
; 5.00
9.04
79.63
0.20
5.00
7.00
38.67
3.19
13.37
1.60
; 39.87
; 4.43
93.6/
2.50
35.77
1.39
89.57
17.33
47.33
; 2.33
; 20.93
3.94
; 95.60
(Continued)
(Sheet 2 of 3)
51
-------
TABLE 23. (Concluded)
Organic
Contaminant
Sludge
Organic
Level
Extract Concentration
(mg/1) .
EP
TCLP
Butanone
WES
PCE
WTC
0.1%
1.0%
0.1%
1.0%
0.1%
1.0%
35.80
188.00
5.19
133,33
9.59
163.00
17.00
256.67
5.39
134.33
6.29
165.67
4-Methyl-2-Pentanone WES
PCE
WTC
0.1%
1.0%
0.1%
1.0%
0.1%
1.0%
41.33
192.67
11.63
233.00
7.67
298.00
13.33
313.33
10.63
247.00
4.88
306.00
(Sheet 3 of 3)
52
-------
TABLE 24. RESULTS OF STATISTICAL ANALYSIS FOR NORMALIZED
TCLP AND EP ORGANIC EXTRACT CONCENTRATIONS ;
Organic Extraction
Constituent Sludge* Testt
Chloroform
1 , 2-Dichloroethane
1,1, l--Trichloroethane
Carbon Tetrachloride
Trichloroethene
Benzene
1,1,2, 2-Tetrachloroethane
Tetrachloroethene
Toluene
Ethylbenzene
2-Butanone
4-Methyl-2-Pentanone
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
N
Y
N
Y
Y
N
' Y
Y
Y
N
Y
Organic
Level^
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Replicate
N
N
N
N
N
N
N
N
N
N
N
N
Ext ra-
tion
Test
Inter- R
action Value?
; N 0.93
\
; N 0.93
i Y 0.96
i
; N 0.93
| Y 0.98
Y 0.98
\ N 0.98
i
Y 0.99
Y 0 . 99
! Y 0.95
! N 0.96
Y 0.98
i
Note: Results presented as "Yes" (Y) or "No" (N). Yes indicates that there is
statistical difference between the variable compared at a = 0.05 .
* WES, PCE, and WTC sludges. j
t EP and TCLP. - . . !
t 0.1% and 1.0%.
§ R values give an indication of how well the statistical model fits the data.
as the fit of the model improves, the R value approaches 1.0.
53
-------
TABLE 25. RESULTS OF PAIRED-SAMPLE T TEST FOR
NORMALIZED STUDY B TGLP AND EP ORGANIC
EXTRACT CONCENTRATIONS
OrganicExtraction
Constituent Test*
Chloroform '
1,2-Dichloroethane
1,1,1-Trichloroethane Y
Carbon Tetrachloride
Trichloroethene Y
Benz ene ^
1,1,2,2-Tetrachloroethane
Tetrachloroethene N
Toluene , Y
Ethylbenzene Y
2-Butanone
4-Methyl-2-Pentanone N
Note: The paired T test was performed only when
the levels of interaction were found to be
significant in the AVMFT.
* Yes (Y) indicates there is statistical dif-
ference between the EP and TCLP results at
a = 0.05 .
that, generally, the TCLP test generated extracts that contained higher con-
centrations of organic contaminants than, the EP extracts. Higher concentra-
tions of organics in the TCLP extracts were expected because the TCLP
extraction was performed under zero~head;space conditions. However, the dif-
ference was not as great as expected.
Results of the AVMFT performed on the Study B organic data are presented
in Table 24. As in Study A, when the results of the AVMFT indicated that the
levels of test interaction are significant, a paired T test was performed.
The results of the paired T test are presented in Table 25. The TCLP and EP
extracts are statistically different for over half of the organic constituents
evaluated. Statistical analysis for only six of the organic constituents
(1,2-dichloroethane, carbon tetrachloride, 1,1,2,2-tetrachloroethane, tetra-
chloroethene, 2-butanone, and 4-methyl-2-pentanone) indicated no statistical
difference between leach test extracts. : Contaminant levels of two (1,1,2,2-
tetrachloroethene and carbon tetrachloride) of the six organic constituents
were near the detection limit. Consequently, 1,2-dichloroethane, tetrachloro-
ethene, 2-butanone, and 4-methyl-2-pentanone were the only organics extracted
from the waste equally by the EP and TCLP.
A graphical representation of the results of the TCLP and EP extractions
for the organic compounds in Study B is .presented in Appendix J, Figures Jl
through J12. In these figures, the normalized EP extract concentrations are
plotted versus the normalized TCLP extract concentrations. A discussion of
the results accompanies these figures.
54
-------
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Figures 12 and 13 present the results for the 0.1% and 1.0% organic
extracts (WES, PEC, and WTC). These figures show the normalized,TCLP and EP
extract expressed as multiples of the EP values, averaged for the three
replicate specimens. These figures illustrate that, typically, TCLP organic
extract concentrations are 1.5 times larger than those measured in the EP
extracts. However, these figures also indicate some exceptions to this
general finding. Compounds detected in the EP extracts at concentrations
greater than 1.1 times the TCLP extracts included: 152-dichloroethane,
benzene, 1,1,2,2-tetrachloroethane, 2-butanone, and 4-methy1-2-pentanone (for
the 0.1% organic extracts) and tetrachloroethene and ethylbenzene for the 1.0%
organic extracts. \
Before this study was initiated, it was expected that the TCLP would
generate extracts with much higher concentrations of organics than the EP
extracts. As shown in Figures 12 and 13, the extracts from the TCLP have only
slightly higher concentrations of organics than the organics measured in the
EP extracts. i
Another interesting observation is seen in the data presented in
Table 26. This table presents the bulk analysis of the sludges immediately
before the TCLP or EP extractions. The initial concentrations (the sludge
concentration prior to extraction) of organics in the 1.0% sludges were 3.8 to
510 times greater than the initial organic concentrations of the;0.1% sludges.
While up to 510 times more organics were originally present in the 1.0%
sludge, the EP and TCLP produce extracts with organic concentrations only
1.5 times higher than the extract produced by the 0.1% sludge. It should be
noted that if all the organic compounds were extracted from the sludges, the
resulting organic/water mixture would be well below any solubility limits.
One would expect the larger driving force in the 1.0% sludge to produce a more
concentrated extract than the 0.1% sludge. However, this was not the case.
Attempts were made to correlate the data presented in Figures 11 and 12
with various physical properties' such as vapor pressure, solubility, pH, anc
boiling point; however, no evidence of correlation with any of these variables
was found. This refutes postulations such as (1) the more volatile compounds
should be detected in the TCLP extracts at greater concentration1 than the EP
extracts or (2) the difference in pH of the EP and TCLP extraction fluids
could result in more extraction of the organic compounds from the waste. Due
to the complex nature of the wastes and the many variables involved with the
EP and TCLP extractions, no explanations are made to clarify why (in some
cases) the EP generated leachates with higher concentrations of organics than
the TCLP. It appears that vapor pressure, solubility, pH, and boiling point
are not linked to this phenomenon. j
SPIKE AND RECOVERY STUDY ;
;
The results of the spike and recovery study for samples tha;t were
prespiked are presented in Table 27, and the results for the postspike samples
are presented in Table 28. The results in Tables 27 and 28 are presented as
Physical data for the organic compounds are presented in Table D-l,
Appendix D.
i
!
57
-------
TABLE 26. STUDY B ORGANIC SLUDGE BULK ANALYSES
(PRESENTED ON WETLAND DRY BASIS)
Chloroform
1 , 2-Dichloroethane
1,1, 1-Trichloroethane
Carbon Tetrachloride
Trichloroethene
Benzene
1,1,2, 2-Tetrachloroe thane
Tetrachloroethene
Toluene
Ethylbenzene
2-Butanone
4-Methy 1-2 -P ent anone
Chloroform
1 , 2-Dichloroethane
1,1, 1-Trichloroethane
Carbon Tetrachloride
Trichloroethene
Benzene
1,1,2, 2-Tetrachloroethane
Tetrachloroethene
Toluene
Ethylbenzene
2-Butanone
4-Methyl-2-Pentanone
Chloroform
1 , 2-Dichloroethane
1,1, 1-Trichloroethane
Carbon Tetrachloride
Trichloroethene
Benzene
1,1,2, 2-Tetrachloroethane
Tetrachloroethene
Toluene
Ethylbenzene
2-Butanone
4-Methyl-2-Pentanone
0.
Wet
(mg/kg)
WES
70.3
264.4
62.0
62.6
221.7
131.2
24.4
255.5
232.6
427.5
3,707.9
2,892.8
PCE
217.7
445.4
328.6
194.8
870.9
830.9
4,104.8
3,625.4
729.1
5,832.6
485.4
1,018.7
WTC
2.9
13.1
4.2
1.2
44.6
11.2
1.2
51.2
28.9
114.9
192.5
150.2
1%;
Dry
(mg/kg)
Sludge^
35.9
134.9
31.6
1 31.9
113.1
66.9
12.4
130.3
118.7
218.0
1,891.4
1,475.6
Sludge
169.6
347.0
256.0
151.7
678.5
647.4
3,198.1
2,824.6
i 568.0
! 4,544.2
378.2
793.7
Sludge
2.4
10.8
3.4
1 i.o
36.7
9.2
1.0
42.0
23.7
94.3
158.0
123.3
1.0%
Wet
(mg/kg)
6,443.6
11,248.8
18,581.4
7,572.4
42,257.7
22,077.9
249.8
41,158.8
33,066.9
47,952.0
47,052.9
70,030.0
6,337.3
9,769.6
8,516.0
4,536.6
17,808.1
18,106.5
22,185.5
16,216.3
18,902.4
24,175.2
25,667.5
25,866.4
576.4
1,931.4
2,180.3
333.5
9,537.4
3,793.0
125.4
7,566.2
6,590.5
10,552.8
3,195.7
10,652.4
Dry
(mg/kg)
3,212.8
5,608.6
9,264.7
3,775.6
21,069.7
11,008.1
124.5
20,521.8
16,487.2
23,908.9
23,460.6
34,916.9
4,512.8
6,956.9
6,064.3
3,230.5
12,681.1
12,893.6
15,798.3
11,547.6
13,460.4
17,2.15.1
18,277.8
18,419.5
458.4
1,535.8
1,733.7
265 . 2
7,584.1
3,016.2
99.7
6,016.6
5,240.8
8,391.6
2,541.2
8,470.8
58
-------
TABLE 27. AVERAGE PERCENT OF VOLATILES LOST FROM PRESPIKE SAMPLES
Sludge
WTC
WTC
WTC
WTC
PCE
PCE
Leach
Test
TCLP
EP
TCLP
EP
TCLP
EP
Organic
Level
(percent)
0.1
0.1
1
1
1
1
Spike
Chlorobenzene
(percent)
*
*
*
*
ND
ND
Compound
Carbon Bisulfide
' (percent)
i NDt
: 99.24
ND
; ND
; ND
, ND
Sample not spiked with analyte.
Compound was below the detection limit; thus, not detected in.the extract.
TABLE 28. AVERAGE PERCENT OF VOLATILES LOST FROM POSTSPIKE SAMPLES
Sludge
WTC
WTC
WTC
WTC
PCE
PCE
Leach
Test
TCLP
EP
TCLP
EP
TCLP
EP
Organic
Level
(percent)
0.1
0.1
1
1
0.1
0.1
Spike
Chlorobenzene
(percent)
23.53
5.50
4.58
25.77
8.62
16.59
Compound
Carbon Disulfide
; (percent)
' *
1 *
1 *
; *
! 23.60
i 9.11
* Sample not spiked with analyte.
59
-------
the percent of spike compound lost from the extract. A problem encountered
with the organic spikes was that the compounds used to spike the WES sludge
extracts did not adequately disperse. While the problem was corrected for the
chlorobenzene and carbon disulfide spikes, it was not corrected for the 1,1,2-
trichloroethane spike. Consequently, the spike data for the WES sludge
extracts and the 1,1,2-trichloroethane spike are omitted from this discussion.
Prespike Extracts
Results of the prespike extracts (Table 27) indicate that greater than
99 percent of the compounds used as spikes were lost both from the TCLP and EP
extracts. These losses of the prespike chlorobenzene and carbon disulfide can
be explained either by (1) absorption of 'these compounds by the solid waste
used in the extraction or (2) loss of these compounds from the EP and TCLP
extracts during the extraction process.
Postspike Extracts '
Chlorobenzene
Results of the triplicate extracts p'ostspiked with chlorobenzene were
statistically evaluated using an A by B two-way classification analysis of the
variance technique (Miller and Freund 1985). Results of this analysis indi-
cate that, at an alpha level of significance of 0.05, there is no statistical
evidence that either the replication, tests (EP or TCLP), or sludges
(WTC-0.1%, WTC-1.0%, or PCE-0.1%) differ. These results were expected based
on the fact that there was no variation in any of the extraction methods after
the postspike was injected into the extract sample.
Carbon Disulfide
Results of the triplicate extracts postspiked with carbon disulfide were
also statistically evaluated. In this case only two conditions were compared,
the EP and TCLP for the PCE sludge at 0.1% organic level. These samples were
compared using a student "T" test (Miller and Freund 1985) . Results from this
analysis indicated that, at an alpha level of significance of 0.05, there was
no statistical evidence that the amount of spike lost from the EP extracts
differed from the spike lost from the TCLP extracts.
Summary
Although there was little difference between loss of postspike compounds
from the extracts, the postspike data yield some useful information. First,
in the worst case, a maximum of 25% of the volatile spike was lost during
sample placement into the sample vial, storage, and analysis. Second, the
high recoveries observed for the postspiked sample for chlorobenzene and car-
bon disulfide indicate that these materials probably were well dispersed.
Thus, the large prespike losses cannot be attributed to poor sample disper-
sion.
60
-------
QUALITY ASSURANCE/QUALITY CONTROL :
The results of the method blanks for the Study A metal analyses are
presented in Table 29; for the Study B metal analyses in Table 30; and for the
Study B volatile organic analyses in Table 31. The method blanks for both
Study A and B metal analyses indicate that some of the contaminants are
detected in the method blanks; however, for the majority of the samples that
were analyzed, the method blanks are relatively uncontaminated (excluding
nickel). Although nickel concentrations 10 times the detection limit are
detected in the method blanks, no method blank corrections for nickel, or any
metal compounds, are made. This decision is based on the fact that the con-
centrations of most of the metal compounds are well above the detection
limits.
The results of the method blanks for the Study B volatile organics data
indicate that, for many contaminants, the concentration of organics detected
in the blank extracts is well above the detection limit. This indicates that
some residual contamination of the extraction media is occurring1. It is sus-
pected that this contamination may be the result of residual left in the ZHE
apparatus, although many precautions were taken to prevent such contamination.
Results of the internal QA/QC are presented in Tables 32 through 35. As
indicated in these tables, the internal QA/QC was excellent. :
Results of the external QA/QC are presented in Tables 36 and 37. The
results of the external sample do not reflect the level of quality indicated
by the internal QA/QC. However, except for some of the mercury data, the
external QA/QC data represent a relatively high degree of quality throughout
this study. i
PROCEDURAL DIFFICULTIES ENCOUNTERED WITH THE TCLP ;
The TCLP extraction is more difficult to perform than the EP extraction.
Factors that contribute to the difficulty include: ,
(1) The TCLP requires two extractions, one for volatiles and another for
nonvolatiles. The EP only requires one extraction. :
(2) The TCLP uses two extraction fluids and requires a prescreening test
to determine which extraction fluid to use. The EP requires one; extraction
fluid. ;
(3) The TCLP ZHE vessel is difficult to clean, as illustrated by the
high degree of contamination in the ZHE blanks (Table 31). It is suspected
that the valve on the ZHE may trap small amounts of liquid which may contami-
nate subsequent extractions. '.
(4) The TCLP method does not provide clear directions on the use of
volatile organic vials for extract collection. Since the sample must be
exposed to the atmosphere during sample collection, incorrect sample handling
may result in large volatile organic losses. r
61
-------
TABLE 29. ANALYSIS OF METHOD BLANKS FOR THE METALS STUDY A TCLP/EP TEST
Interference
Compound
Study A Metal Contaminants (mg/1)
Test
Cd
Cr
Ni
Copper
Grease
Hexachlorobenzene
Sodium sulfate
Sodium hydroxide
Oil
Lead
Phenol
Trichloroethene
Zinc
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
SP
TCLP
0.0007 :
<0.0001
0.0048
<0.0001
0.0005 l
O.0001 :
0.0008
0.0002 :
0.0004
<0.0001
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64
-------
TABLE 32. STUDY A METALS PERCENT ACCURACY OF THE ANALYTICAL LABORATORY'S
INTERNAL STANDARDS
Interference
Compound
Oil
Grease
Lead
Copper
Zinc
Sodium hydroxide
Sodium sulfate
Phenol
Hexachlorobenzene
Trichloroethene
NBS* Traceable Internal Standard
Cadium
98.5
89.6
98.5
94.0
95.5
97.0
73.1
83.6
85.1
91.0
Chromium
(Percent
94.3
97.1
94.3
91.4
95,7
98.6
89.3
95 f 7
94.3
98.6
Nickel
Accuracy) ;
98.3 !
96.6
99.2 '
\
90.4 :
93.3
97.1 !
94.6
92.5 :
95.4
93.3
Mercury
94.6
98.0
94.6
98.7
97.4
97.4
98.7
98.0
100.0
94.6
* National Bureau of Standards.
65
-------
TABLE 33. STUDY B METALS PERCENT ACCURACY OF ANALYTICAL LABORATORY'S
INTERNAL STANDARDS
Type of
Waste
WTC
WES
PCE
Contaminant
Arsenic
Cadmium
Lead
Chromium
Cadmium
Chromium
Nickel
Mercury
Arsenic
Antimony
Copper
Lead
Silver
Barium
Zinc
; Standards
: A
' B
A
B
; A
B
C
; D
A
B
1
A
A
B
i C
A
; A
B
A
A
B
C
A
B
A
B
A
i B
i c
A
B
Standard
Accuracy
98.0
96.6
93.4
97.1
80.0
95.6
97.0
97.0
92.2
92.2
89.4
98.6
97.5
97.5
96.8
94.3
100.0
81.1
95.0
99.0
99.0
86.2
86.2
85.7
85.7
90.7
92.2
90.7
97.7
97.7
66
-------
TABLE 34. STUDY
i
t
B ORGANIC INTERNAL SURROGATE SPIKES
Sludge
Organic
Test Level
Replicate
Surrogate Spike
Toluene D8 1-2-DCA D4*
BFBT
(Percent Recovery)
WES
WTC
PCE
PCE
TCLP 0.1%
1.0%
EP 0.1%
1.0%
TCLP 0.1%
1.0%
EP 0.1%
1.0%
EP 0.1%
EP 1.0%
TCLP 0.1%
TCLP 1.0%
Rl
R2
R3
BL*
Rl
R2
R3
Rl
R2
R3
BL
Rl
R2
R3
Rl
R2
R3
BL '
Rl
R2
R3
Rl
R2
R3
BL
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
94.9
108.0
98.5
97.3
97.6
100.0
100.0
99.2
100.0
107.0
105.0
108.0
109 . 0
100.0
97.0
100.0
97.0
96.4
101.0
105.0
97.1
102.0
102.0
99.2
109.0
96.2
99.7
98.6
101.0
95.8
98.4
101.0
99.7
99.2
99.4
101.0
99.3
99.7
97.2
96.7
90.8 :
103.0 '
82.4
80.7 ;
118.0
83.0 :
108.0 1
102.0 '
98.5
96.0 i
98.1
99.9 (
94.4 '
102.0 :
90.0
119.0 :
99.0 .
93.1
100.0 ,
93.4
100.0
90.1
90.8
94.4
93.0
93.0
92.7
98.4
89.3
97.6
102.0
95.0 i
92.8
93.8 ;
100.0 '
102.0
91.7 '
98.8
99.2
96.2.
96.0
114.0
112.0
105.0
104.0
90.0
101.0
99.8
112.0
96.6
113.0
89.0
93.6
108.0
92.7
100.0
' 102.0
90.9
98.7
102.0
103.0
98.0
99.3
100.0
100.0
98.8
95.8
100.0
103.0
94.4
96.3
100.0
98.5
99.9
97.3
87.1
101.0
96.5
92.6
<93.3
* 1-2-Dichloroethane D4.
t' Bromof luorobenzene.
f Blank.
67
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TABLE 36. STUDY A METALS PERCENT ACCURACY OF THE EXTERNAL STANDARDS
Extraction
Test
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
Interference
Compound
Oil
Grease
Lead
Copper
Zinc
Sodium hydroxide
Sodium sulfate
Phenol
Hexachl or ob enz ene
Trichloroethene
Cadium
90.3
103.6
100.0
112.0
103.4
99.6
106.4
108.8
102.0
95.5
104.0
118.0
!
10.1
104.6
87 .4
105.4
102 .;8
90.5
90.0
110,;0
External
Chromium
74.6
94.4
94.6
96.4
96.8
92.0
101.2.
102,4
97.6
81.0
88.4
112.0
75.4
94.0
87.2
86.0
96.8
83.0
88.8
106.4
Standard
Nickel
95.0
98.1
100.7
101.7
99.5
95.9
104.9
98.4
101.1
96.9
100.4
102.7
101.6
102.1
101.7
100.8
97.5
99.7
97.2
103.9
Mercury
<0.16
<0.32
90.0
53.0
<0.16
<0.32
70.0
64.5
67.0
96.0
60.0
57.0
49.0
188.0
67.6
58.0
42.0
56.0
67.0
140.0
factor that must be considered. If the contaminants of interest in the
solidified/stabilized waste are converted to 1,1-DCE during the extraction,
the concentration of 1,1-DCE in the extracts must be measured. If 1,1-DCE is
an omitted parameter, large concentrations of volatile contaminants leaching
from the solidified/stabilized waste will remain undetected. This could even-
tually result in long-term environmental degradation. Additional research is
needed to clarify this issue.
74
-------
TABLE 37. STUDY B METALS PERCENT ACCURACY OF
EXTERNAL STANDARDS
Type of
Waste
WES
WTC
PCE
Contaminant
Cadmium
Chromium
Nickel
Mercury
Arsenic
Cadmium
Chromium
Lead
Antimony
Arsenic
Barium
Copper
Lead
Silver
Zinc
Percent
Accuracy
98.0
90.4 '
99.8 '
82.6
1
NA* ;
NA :
NA !
NA ;
NA ;
NA
88.8
NA :
68.4
NA ,
NA
Not analyzed.
TABLE 38. CONCENTRATION OF 1,1-DICHLOROETHENE MEASURED
IN THE TCLP AND EP EXTRACTS
Sludge
WES
PCE
WTC
Extraction
Test
EP
TCLP
EP
TCLP
EP
TCLP
Concentration
0.1%
1.0%
0.1%
1.0%
0.1%
1.0%
0.1%
1.0%
0.1%
1.0%
0.1%
1.0%
; Extract
; Concentration
! (mg/1)
; 67.77
92.10
! 175.00
183.00
; <0.33
<10.00
<0.50
<10.00
i 4.05
; <5.00
9.94
<5.00
75
-------
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USEPA. 1987 (Jul). Code of Federal Regulations, Vol 40, U.S. Government
Printing Office, Washington, DC.
Verschueren, Karel. 1977. Handbook of Environmental Data on Organic Chemi-
cals, 2nd ed., Van Nostrand Reinhold Company, New York. I
77
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-------
APPENDIX A
EXTRACTION PROCEDURE (EP) TOXICITY TEST AND 1
STRUCTURAL INTEGRITY TEST*
1.0 Scope and Application (
1.1 The extraction procedure (EP) described in this method is designed
to simulate the leaching a waste will undergo if disposed of in an improperly
designed sanitary landfill. Method 1310 is applicable to liquid; solid, and
multiphasic samples. !
2.0 Summary of Method
2.1 If a representative sample of the waste contains more than 0.5%
solids, the solid phase of the sample is extracted with deionized water which
is maintained at a pH of 5 ± 0.2 using acetic acid. The extract is analyzed
to determine if any of the threshold limits listed in Table A-l are exceeded.
Table A-l also specifies the approved method of analysis. Wastes that contain
less than 0.5% solids are not subjected to extraction, but are directly ana-
lyzed and evaluated in a manner identical to that of extracts.
3.0 Interferences <
3.1 Potential interferences that may be encountered during analysis are
discussed in the individual analytical methods referenced in Table A-l.
4.0 Apparatus and Materials . ;
4.1 Extractor: For purposes of this test, an acceptable extractor is'
one that will impart sufficient agitation to the mixture to (1) prevent strat-
ifica.tion of the sample and extraction fluid and (2) ensure that'all sample
surfaces are continuously brought into contact with well-mixed extraction
fluid. Examples of suitable extractors are shown in Figures A-l through A-3
of this method and are available from Associated Design and Manufacturing Co.,
Alexandria, VA; Glas-Col Apparatus Co., Terre Haute, IN; Millipofe, Bedford,
MA; and Rexnard, Milwaukee, WI.
4.2 pH meter or pH controller: Chemtrix, Inc., Hillsboro, ;OR, is a pos-
sible source of a pH controller. ;
4.3 Filter holder: A filter holder capable of supporting a 0.45-/i fil-
ter membrane and able to withstand the pressure needed to accomplish separa-
tion. Suitable filter holders range from simple vacuum units to[relatively
complex systems that can exert up to 75 psi of pressure. The type of filter
holder used depends upon the properties of the mixture to be filtered. Filter
holders known to EPA and deemed suitable for use are listed in Table A-2.
4.4 Filter membrane: Filter membrane suitable for conducting the
required filtration shall be fabricated from a material that (1) is not
* Source: U.S. Environmental Protection Agency, 1982, "Test Methods for
Evaluating Solid Waste," SW-846, 2nd ed., Office of Solid Waste and
Emergency Response, Washington, DC.
79
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TABLE A-l. MAXIMUM CONCENTRATION OF CONTAMINANTS
Contaminant
Arsenic
Barium ,
Cadmium
Total chromium
i
Hexavalent chromium
Lead
Mercury
Selenium
Silver
Endrin (1,2,3,4,10,10-Hexachloro-l
7-epoxy-l,4,4a,5,6,7,8,8a-octahydro-l
4 - endo , endo -5,8- dime thanonaphthalene ) ,
Lindane (1,2,3,4,5,6-
Hexachlorocyclohexane , gamma isomer)
Methoxychlor (l,l,l-Trichloro-2,2-bis ;
(p-methoxyphenyl) ethane) '
Toxaphene (C1OH10C18, Technical
chlorinated camphene, 67-69% ',
chlorine)
2,4-D (2,4-Dichlorophenoxyacetic acid)
2. 4.5-TP (Silvex) (2.4.5-
Maximum
Concentration
(mg/1)
5.0
100 . 0
1.0
5.0
5.0
5.0
0.2
i.o
5.0
0.02
0.4
10.0
0.5
10.0
1.0
Analytical
Method
7060, 7061
7080, 7081
7130, 7131
7190, 7191
7195, 7196,
7197
7420, 7421
7470
7740, 7741
7760, 7761
8080
8080
8080
8080
8150
8150
Trichlorophenoxypropionic acid)
80
-------
9%
X
' £^^"
/ i
/ ^^
/
/ \
5.0
.
.
IN.
. n *~>i
^ U . L -
1 3
.
[ J
1
O
NONCLOGGING SUPPORT BUSHING
1-IN. BLADE AT 30° TO HORIZONTAL
Figure A-l. EP extractor. '
1/15-HP ELSCTRIC MOTOR
29 RPM ^D1-~
2-LITER PLASTIC OR
GLASS BOTTLES
SCREWS FOR HOLDING BOTTLES
Figure A-2. EP rotary extractor.
81
-------
M
O
M
JJ
X
OS
pu
w
PJ
w
en
.
S)
H
82
-------
TABLE A-2. EPA-APPROVED FILTER HOLDERS
Manufacturer
Size
Model No.
Comments
Vacuum filters
Nalgene
Nuclepore
Millipore
Pressure filters
Nuclepore
Micro Filtration
' Systems
Millipore
500 ml
47 mm
47 mm
44-0045
410400
XX10 047 00
142 mm 425900
142 mm 302300
142 mm
YT30 142 HW
Disposable plastic unit,
includes prefilter and
filter pads, aind reservoir;
should be used when
solution is tp be analyzed
for inorganic ;constituents
physically changed by the waste material to be filtered and (2) does not
absorb or leach the chemical species for which a waste's EP Extract will be
analyzed. Table A-3 lists filter media known to the agency and generally
found to be suitable for solid waste testing. ;
4.4.1 In cases of doubt, contact the filter manufacturer to determine if
the membrane or the prefilter is adversely affected by the particular waste.
If no information is available, submerge the filter in the waste's liquid
phase. After 48 hr, a filter that undergoes visible physical change (i.e.,
curls, dissolves, shrinks, or swells) is unsuitable for use.
4.4.2.1 Prepare a standard solution of the chemical species of interest.
4.4.2.2 Analyze the standard for its concentration of the chemical
species.
4.4.2.3 Filter the standard and reanalyze. If the concentration of the
filtrate differs from the original standard, the filter membraneileaches or
absorbs one or more of the chemical species. '.
4.5 Structural integrity tester: One having a 3.18-cm-diameter hammer
weighing 0.33 kg and having a free fall of 15.24 cm shall be used. This
device is available from Associated Design and Manufacturing Company,
Alexandria, VA, as Part No. 125, or it may be fabricated to meet1the specifi-
cations shown in Figure A-4.
83
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TABLE A-3. EPA-APPROVED FILTRATION MEDIA
Supplier
Filter to be used
for aqueous systems
Filter to be used
for organic systems
Coarse prefilter
Gelman
Nuclepore
Millipore
Medium prefilters
Nuclepore
Millipore
61631, 61635
210907, 211707
AP25 035 00,
AP25 127 50
210905, 211705
AP20 035 00,
AP20 124 50
61631, 61635
210907, 211707
AP25 035 00,
AP25 127 50
210905, 211705
AP20 035 00,
AP20 124 50
Fine prefilters
Gelman
Nuclepore
Millipore
64798, 64803
210903, 211703
APIS 035 00,
AP15 124 50
64798, 64803
210903, 211703
APIS 035 00,
APIS 124 50
Fine filters (0.45-?)
Gelman
Pall
Nuclepore
Millipore
Selas
60173, 60177
NX04750, NX14225
142218
HAWP 047 00,
HAWP 142 50
83485-02,
83486-02
60540 or 66149,
60544 or 66151
142218*
FHUP 047 00,
FHLP 142 50
83485-02,
83486-02
* Susceptible to decomposition by certain polar organic solvents.
84
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o
COMBINED
WEIGHT
0.33 KG (0.73 LB)
SAMPLE,
ELASTOMERIC
SAMPLE HOLDER
.3.3 CM
(1.3 IN.)
9.4 CM
O
oo
(3.7 IN.)
Figure A-4. EP compaction tester.
85
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5.0 Reagents I
5.1 Deionized water: Water should be monitored for impurities.
5.2 0.5 N acetic acid: This can be made by diluting concentrated
glacial acetic acid (17.5 N). The glacial acetic acid should be of high
purity and monitored for impurities.
5.3 Analytical standards should be;prepared according to the analytical
methods referenced in Table A-l.
6.0 Sample Collection. Preservation and Handling
6.1 All samples must be collected using a sampling plan that addresses
the considerations discussed in Section One of USEPA's SW-846.
6.2 Preservatives must not be added to samples.
6.3 Samples can be refrigerated if; it is determined that refrigeration
will not affect the integrity of the sample.
7.0 Procedure
7.1 If the waste does not contain any free liquid, go to Section 7.9.
If the sample is liquid or multiphase, continue as follows. Weigh filter mem-
brane and prefilter to +0.01 g. Handle membrane and prefilters with blunt
curved-tip forceps or vacuum tweezers, or by applying suction with a pipette.
7.2 Assemble filter holder, membranes, and prefilters following the
manufacturer's instructions. Place the 0.45-? membrane on the support screen
and add prefilters in ascending order of pore size. Do not prewet filter
membrane.
7.3 Weigh out a representative subsample of the waste (100 g minimum).
7.4 Allow slurries to stand to permit the solid phase to settle. Wastes
that settle slowly may be centrifuged prior to filtration.
7.5 Wet the filter with a small portion of the waste's or extraction
mixture's liquid phase. Transfer the remaining material to the filter holder
and apply vacuum or gentle pressure (10 to 15 psi) until all liquid passes
through the filter. Stop filtration when air or pressurizing gas moves
through the membrane. If this point is .not reached under vacuum or gentle
pressure, slowly increase the pressure in 10-psi increments to 75 psi. Halt
filtration when liquid flow stops. This liquid will constitute part or all of
the extract (refer to Section 7.16). The liquid should be refrigerated until
time of analysis.
NOTE: Oil samples or samples that contain oil are treated in exactlj'- the
same way as any other sample. The liquid portion of the sample is fil-
tered and treated as part of the EP extract. If the liquid portion of
the sample will not filter (this is usually the case with heavy oils or
greases), it is carried through the EP extraction as a solid.
86
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7.6 Remove the solid phase and filter media and, while not allowing it
to dry, weigh to ±0.01 g. The wet weight of the residue is determined by cal-
culating the weight difference between the weight of the filters ;(Section 7.1)
and the weight of the solid phase and the filter media. ;
7.7 The waste will be handled differently from this point oh depending
on whether it contains more or less than 0.5% solids. If the sample appears
to have less than 0.5% solids, the percent solids will be determined by the
following procedure. . j
7.7.1 Dry the filter and residue at 80° C until two successive weighings
yield the same value. i
7.7.2 Calculate the percent solids using the following equation:
Weight of filtered Tared weight
solid and filters - of filters .nn - n . ,
: 7 ~~r~: x 100 - % solids
Initial weight of waste material
NOTE: This procedure is only used to determine whether the ,solid must be
extracted or whether it can be discarded unextracted. It is; not used in
calculating the amount of water or acid to use in the extraction step.
Do not extract solid material that has been dried at 80° C. | A new sample
will have to be used for extraction if a percent solids determination is
performed. '
,7.8 If the solid comprises less than 0.5% of the waste, discard the
solid and proceed immediately to Section 7.17, treating the liquid phase as
the extract. - ' '
7.9 The solid material obtained from Section 7.5 and all materials that
do not contain free liquids should be evaluated for particle size. If the
solid material has a surface area per gram of material equal to or greater
than 3.1 cm2 or passes through a 9.5-mm standard sieve, the operator should
proceed to Section 7.11. If the surface area is smaller or the particle size
larger than specified above, the solid material would be prepared for extrac-
tion by crushing, cutting, or grinding the material so that it passes through
a 9.5-mm sieve or, if the material is in a single piece, by subjecting the
material to the "Structural Integrity Procedure" described in Section 7.10.
7.10 Structural Integrity Procedure (SIP):
7.10.1 Cut a 3.3-cm-diameter by 7.1-cm-long cylinder from the waste
material. For wastes that have been treated using a fixation process, the
waste may be cast in the form of a cylinder and allowed to cure for 30 days
prior to testing. i
7.10.2 Place waste into sample holder and assemble the tester. Raises
the hammer to its maximum height and drop. Repeat 14 additional 'times.
7.10.3 Remove solid material from tester and scrape off any particles
adhering to sample holder. Weigh the waste to the nearest 0.01 g and transfer
it to the extractor. :
87
-------
7.11 If the sample contains more than 0.5% solids, use the.wet weight of
the solid phase obtained in Section 7.6 for purposes of calculating the amount
of liquid and acid to employ for extraction by using the following equation:
W - W£ - Wt
where
W - wet weight in grams of solid to be charged to extractor
W£ - wet weight in grams of filtered solids and filter media
Wt - weight in grams of tared filters
If the waste does not contain any free liquids, 100 g of the material will be
subjected to the extraction procedure. ;
7.12 Place the appropriate amount of material (refer to Section 7.11)
into the extractor and add 16 times its weight of deionized water.
7.13 After the solid material and deionized water are placed in the
extractor, the operator should begin agitation and measure the pH of the solu-
tion in the extractor. If the pH is greater than 5.0, the pH of the solution
should be decreased to 5.0 ± 0.2 by adding 0.5 N acetic acid. If the pH is
equal to or less than 5.0, no acetic acicl should be added. The pH of the
solution should be monitored, as described below, during the course of the
extraction and, if the pH rises above 5.2, 0.5 N acetic acid should be added
to lower the pH to 5.0 ± 0.2. However, in no event shall the aggregate amount
of acid added to the solution exceed 4 ml of acid per gram of solid. The mix-
ture should be agitated for 24 hr and maintained at 20° to 40° C during this
time. It is recommended that the operator monitor and adjust the pH during
the course of the extraction with a device such as the Type 45-A pH Controller
manufactured by Chemtrix, Inc., Hillsboro, OR, or its equivalent, in conjunc-
tion with a metering pump and reservoir of 0.5 N acetic acid. If such a sys-
tem is not available, the following manual procedure shall be employed.
7.13.1 A pH meter should be calibrated in accordance with the manu-
facturer 's specifications.
7.13.2 The pH of the solution should be checked and, if necessary, 0.5 N
acetic acid should be manually added to the extractor until the pH reaches
5.0 ± 0.2. The pH of the solution should be adjusted at 15-, 30-, and 60-min
intervals, moving to the next longer interval if the pH does not have to be
adjusted more than 0.5 pH unit.
7.13.3 The adjustment procedure should be continued for at least 6 hr.
7.13.4 If, at the end of the 24-hr; extraction period, the pH of the
solution is not below 5.2 and the maximum amount of acid (4 ml per gram of
solids) has not been added, the pH should be adjusted to 5.0 + 0.2 and the
extraction continued for an additional 4 hr, during which the pH should be
adjusted at 1-hr intervals.
7.14 At the end of the extraction period, deionized water should be
added to the extractor in an amount determined by the following equation:
88
-------
V'- (20)(W) - 16(W) - A j
I
where i
V = milliters of deipnized water to be added
W = weight of solid, in grams, charged to extractor
A = milliters of 0.5 N acetic acid added during extraction :
7.15 The material in the extractor should be separated into; its compo-
nent liquid and solid phases in the following manner.
7.15.1 Allow slurries to stand to permit the solid phase to settle
(wastes that are slow to settle may be centrifuged prior to filtration) and
set up the filter apparatus (refer to Sections 4.3 and 4.4). ;
7.15.2 Wet the filter with a small portion of the waste's or extraction
mixture's liquid phase. Transfer the remaining material to the filter holder
and apply vacuum or gentle pressure (10 to 15 psi) until all liquid passes
through the filter. Stop filtration when air or pressurizing gas! moves
through the membrane. If this point is not reached under vacuum or gentle
pressure, slowly increase the pressure in 10-psi increments to 75 psi. Halt
filtration when, liquid flow stops. j
7.16 The liquids resulting from Sections 7.5 and 7.15 should be com-
bined. This combined liquid (or the waste itself if it has less .than 0.5%
solids, as noted in Section 7.8) is the extract and should be analyzed for the
presence of any of the contaminants specified in Table A-l using :the analyt-
ical procedures designated in Section 7.17.
7.17 The extract will be prepared and analyzed according to the anal}rt-
ical methods specified in Table A-l. All of these analytical methods are
included in this manual. The method of standard addition will be/employed for
all metal analyses. j
NOTE: If the EP extract includes two phases, concentrationjof contami-
nants is determined by using a simple weighted average. For example: An EP
extract contains 50 ml of oil and 1,000 ml of an aqueous phase. jContaminant
concentrations are determined for each phase. The final contamination concen-
tration is taken to be
fSOY(Contaminant cone, in oil) (1.OOP)(Contaminant cone, of aqueous phase)
1,050 ' -r ' ' 1,050 |
89
-------
7.18 The extract concentrations are, compared to the maximum contamina-
tion limits listed in Table A-l. If the extract concentrations are equal to
or greater than the respective values, the waste is considered to be EP
toxic.*
8.0 Quality Control
8.1 All quality control data should be maintained and available for easy
reference or inspection.
8.2 Employ a minimum of one blank per sample batch to determine if con-
tamination or any memory effects are occurring.
8.3 All quality control measures suggested in the referenced analytical
methods should be followed. !
* Chromium concentrations have to be interpreted differently. A waste con-
taining chromium will be determined to ;be EP toxic if (1) the waste extract
has an initial pH of less than 7 and contains more than 5 mg/1 of hexavalent
chromium in the resulting extract, (2)[the waste extract has an initial pH
greater than 7 and a final pH greater than 7 and contains more than 5 mg/1
of hexavalent chromium in the extract,;or (3) the waste extract has an
initial pH greater than 7 and a final pH less than 7 and contains more than
5 mg/1 of total chromium, unless the chromium is trivalent. To determine
whether the chromium is trivalent, the:sample must be processed according to
an alkaline digestion method (Method 3060) and analyzed for hexavalent
chromium (Method 7195, 7196, or 7197).
90
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APPENDIX B
TOXICITY CHARACTERISTIC LEACHING PROCEDURE* !
1.0 Scope and Application
1.1 The TCLP is designed to determine the mobility of both ;organic arid
inorganic contaminants present in liquid, solid, and multiphasic wastes.
1.2 If a total analysis of the waste demonstrates that individual con-
taminants are not present in the waste, or that they are present,! but at such
low concentrations that the appropriate regulatory thresholds could not pos-
sibly be exceeded, the TCLP need not be run.
2.0 Summary of Method (see Figure B-l) ;
2.1 For wastes containing less than 0.5% solids, the waste,, after fil-
tration through a 0.6- to 0.8-? glass fiber filter, is defined as the TCLP
extract.
2.2 For wastes containing greater than 0.5% solids, the liquid phase, if
any, is separated from the solid phase and stored for later analysis. The
particle size of the solid phase is reduced (if necessary), weighed, and
extracted with an amount of extraction fluid equal to 20 times the weight of
the solid phase. The extraction fluid employed is a function of |the alka-
linity of the solid phase of the waste. A special extractor vessel is used
when testing for volatiles (see Table B-l). Following extraction, the liquid
extract is separated from the solid phase by 0.6- to 0.8-? glass ifiber filter
filtration.
2.3 If compatible (e.g. precipitate or multiple phases will not form on
combination), the initial liquid phase of the waste is added to the liquid
extract, and these liquids are analyzed together. If incompatible, the
liquids are analyzed separately and the results are mathematically combined to
yield the volume-weighted average concentration. j
3.0 Interferences ,
i
3.1 Potential interferences that may be encountered during :analysis are
discussed in the individual analytical methods. !
4.0 Apparatus and Materials '
4.1 Agitation apparatus: An acceptable agitation apparatus is one that
is capable of rotating the extraction vessel in an end-over-end fashion (see
Figure B-2) at 30 + 2 rpm. Suitable devices known to EPA are identified in
Table B-2. , ,
* Source: U.S. Environmental Protection Agency, 1986, Federal Register.
Vol 51 (13 Jun), No. 114, Washington, DC.
91
-------
WET WASTE SAMPLE
CONTAINS < 0.5%
NONFILTERABLE SOLIDS
REPRESENTATIVE WASTE
SAMPLE
WET WASTE SAMPLE
CONTAINS>0.5%
NONFILTERABLE SOLIDS
DRYWASTE;SAMPLE
LIQUID/SOLID
SEPARATION
0.6 - 0.8 um
GLASS FIBER
FILTERS
DISCARD
SOLID
SOLID
SOLID
LIQUID/SOLID
SEPARATION
0.6 - 0.8 um
GLASS FIBER
FILTERS
REDUCE PARTICLE SIZE IF
> 9.5 mm OR
SURFACE AREA < 3.1 cm2
LIQUID
STORE AT
4°C
PRESCREENING
TO SELECT EXTRACTION
FLUID
ZERO HEAD EXTRACTION
OF SOLID FOR
VOLATILE CONTAMINANTS
TCLP EXTRACTION OF
SOLID FOR NON-
VOLATILE CONTAMINANTS
DISCARD
SOLID
LIQUID/SOLID
SEPARATION
0.6 - 0.8 um
GLASS FIBER
FILTERS
I
LIQUID
I
I
LIQUID/SOLID
SEPARATION
0.6 - 0.8 um
GLASS FIBER
FILTERS
. SOLID
DISCARDED
LIQUID
TCLP EXTRACT
TCLP EXTRACT
i' V
ANALYTICAL METHODS
TCLP EXTRACT
TCLP EXTRACT
Figure B-l. TCLP flowchart.
92
-------
TABLE B-l
Compound I
Acetone
Acrylonitrile
Benzene
n-Butyl alcohol
Carbon disulfide
Carbon tetrachloride
Chlorobenzene
Chloroform
1, 2-Dichloroethylene
1 , 1-Dichloroethylene
Ethyl acetate
Ethyl benzene
Ethyl ether
Isobutanol
Methanol
Methylene chloride
Methyl ethyl ketone
Methyl isobutyl ketone
1,1,1, 2 -Tetrachloroethane
1 , 1 , 2 , 2 -Tetrachloroethane
Tetrachloroethene
Toluene
1 , 1 , 1-Trichloroethane
1,1, 2 -Trichloroe thane
Trichloroethylene
TrichlorofTuorome thane
1 , 1 , 2-Trichloro-l , 2,2- trif luoroethane
Vinyl chloride
Xylane
67-64-1
107-13-1
! 71-43-2
71-36-6
75-15-0
56-23-5
108-90-7
' 67-66-3
107-06-2
; 75-35-4
141-78-6
; 100-41-4
j 60-29-7
: 78-83-1
67-56-1
75-09-2
78-93-3
: 108-10-1
630-20-6
79-34-5
127-18-4
; 108-88-3
' 71-55-6
79-00-5
79-01-6
i 75-69-4
! 76-13-1
75-01-4
1330-20-7
* Includes compounds identified in both the Land Disposal Restrictions Rule
and the Toxicity Characteristics.
93
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MOTOR
(30 ±2 RPM)
EXTRACTION VESSEL HOLDER
Figure B-2. TCLP rotary agitator.
TABLE B-2. SUITABLE ROTARY AGITATION APPARATUS*
Company
Location
Model
Associated Design
and Manufacturing
Co.
Alexandria, Virginia
(703)549-5999
4-vessel
device
6-vessel
device
Lars Lande
Manufacturing
IRA Machine Shop
and Laboratory
EPRI Extractor
Whitmore Lake,
Michigan
(313)'449-4116
Santurce, Puerto Rico
(809)! 752-4004
10-vessel
device
16-vessel
device
6-vessel
device
* Any device which rotates the extraction vessel in an end-over-end fashion
at 30 ± 2 rpm is acceptable.
f Although this device is suitable, it is not commercially made. It may
also require retrofitting to accommodate ZHE devices.
4.2 Extraction vessel:
4.2.1 Zero-headspace extraction vessel (ZHE): When the waste is being
tested for mobility of any volatile contaminants (see Table B-l), an extrac-
tion vessel which allows for liquid/solid separation within the device and
which effectively precludes headspace (as depicted in Figure B-3) is used.
This type of vessel allows for initial liquid/solid separation extraction and
final extract filtration without having to open the vessel (see Sec-
tion 4.3.1). These vessels shall have an internal volume of 500 to 600 nil and
94!
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LIQUID INLET / OUTLET VALVE
WASTE/
EXTRACTION FLUID
PISTON
TOP
FLANGE
BODY
/\
vrroN
O-RINQS
(2 OR 3)
BOTTOM
FLANGE
PRESSURIZING GAS INLET / OUTLET VALVE
Figure B-3. TCLP zero-headspace extraction vessel.
be equipped to accommodate a 90-mm filter. Suitable ZHE devices known to EPA
are identified in Table B-3. These devices contain viton 0-rings which should
be replaced frequently. ;
4.2.2 Other extraction vessels: When the waste is being evaluated for
other than volatile contaminants; an extraction vessel that does ;not preclude
headspace (e.g., 2-liter bottle) is used. Suitable extraction vessels include
bottles made from various materials depending on the contaminants to be ana-
lyzed and the nature of the waste (see Section 4.3.3). These bottles are
available from a number of laboratory suppliers. When this type of extraction
vessel is used, the filtration device discussed in Section 4.3.2, is used for
initial liquid-solid separation and final extract filtration. '.
TABLE B-3. SUITABLE ZERO-HEADSPACE EXTRACTOR VESSELS
Company
Location
Model No.
Associated Design
and Manufacturing
Co.
Millipore Corporation
Alexandria, Virginia
(703)549-5999
Bedford,
Massachusetts
(800)225-3384
3740-ZHB
SD1P581C5
. 95
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4.3 Filtration devices:
4.3.1 Zero-headspace extractor vessel (see Figure B3): When the waste
is being evaluated for volatiles, the zero-headspace extraction vessel is used
for filtration. The device shall be capable of supporting and keeping in
place the glass fiber filter and be able to withstand the pressure needed to
accomplish separation (50 psi).
NOTE: When it is suspected that the glass fiber filter has been
ruptured, an in-line glass fiber filter may be used to filter the
extract.
4.3.2 Filter holder: When the waste is being evaluated for other than
volatile compounds, a filter holder capable of supporting a glass fiber filter
and able to withstand the pressure needed to accomplish separation is used.
Suitable filter holders range from simple vacuum units to relatively complex
systems capable of exerting pressure up to 50 psi and more. The type of fil-
ter holder used depends on the properties of the material to be filtered (see
Section 4.3.3). These devices shall have a minimum internal volume of 300 ml
and be equipped to accommodate a minimum filter size of 47 mm. Filter holders
known to EPA to be suitable for use are shown in Table B-4.
4.3.3 Materials of construction: Extraction vessels and filtration
devices shall be made of inert materials which will not leach or absorb waste
components. Glass polytetrafluoroethylehe (PTFE) or type 316 stainless steel
equipment may be used when evaluating the mobility of both organic and inor-
ganic components. Devices made of high density polyethylene (HDPE), polypro-
pylene, or polyvinyl chloride may be used when evaluating the mobility of
metals.
4.4 Filters: Filters shall be made of borosilicate glass fiber, contain
no binder materials, and have an effective pore size of 0.6 to 0.8 ? or equiv-
alent. Filters known to EPA to meet these specifications are identified in
Table B-5. Prefilters must not be used. When evaluating the mobility of
metals, filters shall be acid-washed prior to use by rinsing with 1.0 N nitric
acid followed by three consecutive rinses with deionized distilled water
(minimum of 500 ml per rinse). Glass fiber filters are fragile and should be
handled with care.
4.5 pH meters: Any of the commonly available pH meters are acceptable.
4.6 ZHE extract collection devices: Tedlar* bags or glass, stainless
steel, or PTFE gas-tight syringes are used to collect the initial liquid phase
and the final extract of the waste when !using the ZHE device.
4.7 ZHE extraction fluid collection devices: Any device capable of
transferring the extraction fluid into the ZHE without changing the nature of
the extraction fluid is acceptable (e.g.. a constant displacement pump, a gas-
tight syringe, pressure filtration unit ;(see Section 4.3.2), or another ZHE
device).
* Registered trademark of DuPont.
96
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TABLE B-4. SUITABLE FILTER HOLDERS*
;
Company
Nuclepore Corporation
Micro Filtration
Systems
Millipore Corporation
Location
Pleasanton,
California
(800)882-7711
Dublin, California
(415)828-6010
Bedford,
Massachusetts
(800)225-3384
Model ;
425910 :
410400
302400 '
YT30142HW ,
XX1004700 ;
Size
(mm)
142
47
142
142
47
* Any device capable of separating the liquid from the solid phase of the
waste is suitable, providing that it is chemically compatible with the waste
and the constituents to be analyzed. Plastic devices (not listed above) may
be used when only inorganic contaminants are of concern. ,
; TABLE B-5. SUITABLE FILTER MEDIA
; Nominal
: Pore
Company Location Model Size
Whatman Clifton, New Jersey GFF \ 0.7
Laboratory (201)773-5800 !
Products, Inc. :
4.8 Laboratory balance: Any laboratory balance accurate tor within
+0.01 gram (g) may be used (all weight measurements are to be within ±0.1 g) .
5.0 Reagents ';
5.1 Water: ASTM Type 1 deionized, carbon treated, decarbonized, fil-
tered water (or equivalent water that is treated to remove volatile compo-
nents) shall be used when evaluating wastes for volatile contamiriants. Other-
wise, ASTM Type 2 deionized distilled water (or equivalent) is us'ed. These
waters should be monitored periodically for impurities. i
5.2 1.0 N Hydrochloric acid (HC1) made from ACS Reagent grade.
5.3 1.0 N Nitric acid (HN02) made from ACS Reagent grade, i
5.4 1.0 N Sodium hydroxide (NaOH) made from ACS Reagent grade.
97 !
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5.5 Glacial acetic acid (HOAc) made from ACS Reagent grade.
5.6 Extraction fluid:
5.6.1 Extraction fluid 1: This fluid is made by adding 5.7 ml glacial
HOAc to 500 ml of the appropriate water (see Section 5.1), adding 64.3 ml of
1.0 N NaOH, and diluting to a volume of 1 liter. When correctly prepared, the
pH of this fluid will be 4.93 ± 0.05. |
5.6.2 Extraction fluid 2: This fluid is made by diluting 5.7 ml glacial
HOAc with ASTM Type 2 water (see Section 5.1) to a volume of 1 liter. When
correctly prepared, the pH of this fluid will be 2.88 ± 0.05.
NOTE: These extraction fluids shall be made up fresh daily. The pH
should be checked prior to use to ensure that the fluids are made up
accurately, and they should be monitored frequently for impurities.
5.7 Analytical standards shall be prepared according to the appropriate
analytical method.
6.0 Sample Collection. Preservation, and Handling
6.1 All samples shall be collected using a sampling plan that addresses
the considerations discussed in "Test Methods for Evaluating Solid Wastes"
(SW-846). ;
6.2 Preservatives shall not be added to samples.
6.3 Samples can be refrigerated unless it results in irreversible phys-
ical changes to the waste.
6.4 When the waste is to be evaluated for volatile contaminants, care
must be taken to ensure that these are not lost. Samples shall be taken and
stored in a manner which prevents the loss of volatile contaminants. If pos-
sible, any necessary particle size reduction should be conducted as the sample
is being taken (see Step 8.5). Refer to SW-846 for additional sampling arid
storage requirements when volatiles are contaminants of concern.
6.5 TCLP extracts should be prepared for analysis and analyzed as soon
as possible following extraction. If they need to be stored, even for a short
period of time, storage shall be at 4° C, and samples for volatiles analysis
shall not be allowed to come into contact with the atmosphere (i.e., no
headspace).
7.0 Procedure When Volatiles Are Not Involved
NOTES: Although a minimum sample size of 100 g is required, a larger
sample size may be necessary, depending on the percent solids of the
waste sample. Enough waste sample |should be collected such that at least
75 g of the solid phase of the waste (as determined using glass fiber
filter filtration) is extracted. This will ensure that there is adequate
extract for the required analyses (e.g. semivolatiles, metals, pesti-
cides, and herbicides).
98
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The determination of which extraction fluid to use -(see Step 7.12) may
also be conducted at the start of this procedure. This determination
shall be based on the solid phase of the waste (as obtained using glass
fiber filter filtration).
7.1 If the waste will obviously yield no free liquid when subjected to
pressure filtration, weigh out a representative subsample of the^aste (100-g
minimum) and proceed to Step 7.11. ;
7.2 If the sample is liquid or multiphasic, liquid/solid separation is .
required. This involves the filtration device discussed in Section 4.3.2 and
outlined in Steps 7.3 to 7.9.
7.3 Preweigh the filter and the container that will receive the
filtrate. ;
7.4 Assemble filter holder and filter following the manufacturer's
instructions. Place the filter on the support screen and secure> Acid-wash
the filter if evaluating the mobility of metals (see Section 4.4).
7.5 Weigh out a representative subsample of the waste (100-g minimum)
and record weight.
I
7.6 Allow slurries to stand to permit the solid phase to settle. Wastes
that settle slowly may be centrifuged prior to filtration. ,
7.7 Transfer the waste sample to the filter holder.
NOTES: If waste material has obviously adhered to the container used to
transfer the sample to the filtration apparatus, determine the weight of
this residue and subtract it from the sample weight determined in
Step 7.5, to determine the weight of the waste sample that will be fil-
tered. Gradually apply vacuum or gentle pressure of 1 to 10 psi, until
air or pressurizing gas moves through the filter. If this point is not
reached under 10 psi, and if no additional liquid has passed through the
filter in any 2-min interval, slowly increase the pressure in 10-psi
increments to a maximum of 50 psi. After each incremental increase of
10 psi, if the pressurizing gas has not moved through the filter and no
additional liquid has passed through the filter in any 2-mih interval,
proceed to the next 10-psi increment. When the pressurizing gas begins
to move through the filter, or when liquid flow has ceased kt 50 psi
(i.e., does not result in any additional filtrate within any 2-min
period), filtration is stopped. ,
Instantaneous application of high pressure can degrade the glass fiber
filter and may cause premature plugging.
7.8 The material in the filter holder is defined as the solid phase of
the waste, and the filtrate is defined as the liquid phase.
NOTE: Some wastes, such as oily wastes and some paint wastes, will obvi-
ously contain some material that appears to be a liquid; however, even
after applying vacuum or pressure filtration as outlined in Step 7.7,
this material may not filter. If this is the case, the material within
99
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the filtration device is defined as a solid and is carried through the
extraction as a solid. :
7.9 Determine the weight of the liquid phase by subtracting the weight
of the filtrate container (see Step 7.3) from the total weight of the
filtrate-filled container. The liquid phase may now be either analyzed (see
Step 7.15) or stored at 4° C until time of analysis. The weight of the solid
phase of the waste sample is determined by subtracting the weight of the
liquid phase from the weight of the total waste sample, as determined in
Step 7.5 or 7.7. Record the weight of the liquid and solid phases.
NOTE: If the weight of the solid phase of the waste is less than 75 g,
review Step 7.0.
7.10 The sample will be handled differently from this point, depending
on whether it contains more or less than;0.5% solids. If the sample obviously
has greater than 0.5% solids, go to Step ;7.11. If it appears that the solid
may comprise less than 0.5% of the total waste, the percent solids will be
determined as follows:
7.10.1 Remove the solid phase and filter from the filtration apparatus.
7.10.2 Dry the filter and solid phase at 100 ± 20° C until two succes-
sive weighings yield the same value. Record final weight.
7.10.3 Calculate the percent solids as follows: Weight of dry waste and
filters minus tared weight of filters divided by initial weight of waste
(Step 7.5 or 7.7) multiplied by 100 equals percent solids.
7.10.4 If the solid comprises less'than 0.5% of the waste, the solid is
discarded, and the liquid phase is defined as the TCLP extract. Proceed to
Step 7.14.
7.10.5 If the solid is greater than or equal to 0.5% of the waste,
return to Step 7.1, and begin the procedure with a new sample of waste. Do
not extract the solid that has been dried.
NOTE: This step is only used to determine whether the solid must be
extracted or whether it may be discarded unextracted. It is not used in
calculating the amount of extraction fluid to use in extracting the
waste, nor is the dried solid that is derived from this step subjected to
extraction. A new sample will have1to be prepared for extraction.
7.11 If the sample has more than 0.5% solids, it is now evaluated for
particle size. If the solid material has a surface area per gram of material
equal to or greater than 3.1 cm2 or is capable of passing through a 9.5-mm
standard sieve, proceed to Step 7.12. If the surface area is smaller or the
particle size is larger than that described above, the solid material is pre-
pared for extraction by crushing, cutting, or grinding the solid material to a
surface area or particle size as described above. When surface area or
particle size has been appropriately altered, proceed to Step 7.12.
100
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7.12 This step describes the determination of the appropriate extracting
fluid to use (see Sections 5.0 and 7.0).
7.12.1 Weigh out a small subsample of the solid phase of the waste,
reduce the solid (if necessary) to a particle size of approximately 1 mm in
diameter or less, and transfer a 5.0-g portion to a 500-ml beaker or
Erlenmeyer flask.
7.12.2 Add 96.5 ml distilled deionized water (ASTM Type 2)' cover with
watchglass, and stir vigorously for 5 min using a magnetic stirrer. Measure
and record the pH. If the pH is <5.0, extraction fluid 1 is used. Proceed to
Step 7.13.
7.12.3 If the pH from Step 7.12.2 is >5.0, add 3.5 ml 1..0 IjT HC1, slurry
for 30 sec, cover with a watchglass, heat to 50° C, and hold for ' 10 min.
7.12.4 Let the solution cool to room temperature and record pH. If pH
is <5.0, use extraction fluid 1. If the pH is >5.0, extraction fluid 2 is
used. I
!
7.13 Calculate the weight of the remaining solid material by subtracting
the weight of the subsample taken for Step 7.12 from the original amount of
solid material, as obtained from Step 7.1 or 7.9. Transfer remaining solid
material into the extractor vessel, including the filter used to separate the
initial liquid from the solid phase. ;
NOTES: If any of the solid phase remains adhered to the walls of the
filter holder, or the container used to transfer the waste, its weight
shall be determined and subtracted from the weight of the solid phase of
the waste, as determined above; this weight is used in calculating the
amount of extraction fluid to add into the extractor bottle.
Slowly add an amount of the. appropriate extraction fluid (see Step 7.12)
into the extractor bottle equal to 20 times the weight of tljie solid phase
that has been placed into the extractor bottle. Close extractor bottle
tightly, secure in rotary extractor device, and rotate at 30 + 2 rpm for
18 hr. The temperature shall be maintained at 22° + 3° C during the
extraction period. ,
As agitation continues, pressure may build up within the extractor bottle
(due to the evolution of gases such as carbon dioxide). To;relieve these
pressures, the extractor bottle may be periodically opened and vented
into a hood. i
i
7.14 Following the 18-hr extraction, the material in the extractor
vessel is separated into its component liquid and solid phases b^ filtering
through a new glass fiber filter as outlined in Step 7.7. This new filter
shall be acid-washed (see Section 4.4) if evaluating the mobility of metals.
7.15 The TCLP extract is now prepared as follows:
101
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7.15.1 If the waste contained no initial liquid phase, the filtered
liquid material obtained from Step 7.14 is defined as the TCLP extract. Pro-
ceed to Step 7.16.
i
7.15.2 If compatible (e.g. will not form precipitate or multiple
phases), the filtered liquid resulting from Step 7.14 is combined with the
initial liquid phase of the waste as obtained in Step 7.9. This combined
liquid is defined as the TCLP extract. Proceed to Step 7.16.
7.15.3 If the initial liquid phase of the waste, as obtained from
Step 7.9, is not or may not be compatibly with the filtered liquid resulting
from Step 7.14, these liquids are not combined. These liquids are collec-
tively defined as the TCLP extract, analyzed separately, and the results com-
bined mathematically. Proceed to Step 7.16.
7.16 The TCLP extract will be prepared and analyzed according to the
appropriate SW-846 analytical methods identified in Appendix III of
40 CFR 261. TCLP extracts to be analyzed for metals shall be acid-digested.
If the individual phases are to be analyzed separately, determine the volume
of the individual phases (to 0.1 ml), conduct the appropriate analyses, and
combine the results mathematically by using a simple weighted average:
(V1)(c1) + (V2)(c2)
~
Final contaminant concentraion :: ~
12
where
Vx - volume of the first phase, liters
Cx - concentration of the contaminant of concern in the first phase,
milligrams per liter
V2 - volume of the second phase, liters
C2 - concentration of the contaminant of concern in the second phase,
milligrams per liter . ;
7.17 The contaminant concentrations in the TCLP extract are compared to
the thresholds identified in the appropriate regulations. Refer to Section 9
for quality assurance requirements . i
8.0 Procedure When Volatiles Are Involved
NOTES: The ZHE device has approximately a 500-ml internal capacity.
Although a minimum sample size of 100 g was required in the Section 7
procedure, the ZHE can only accommodate a maximum 100 -percent solids
sample of 25 g, due to the need to 'add an amount of extraction fluid
equal to 20 times the weight of the solid phase. Step 8.4 provides the
means by which to determine the approximate sample size for the ZHE
device .
Although the following procedure allows for particle size reduction
during the conduct of the procedure, this could result in the loss of
volatile compounds. If possible, any necessary particle size reduction
(see Step 8.5) should be conducted on the sample as it is being taken.
102
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Particle size reduction should only be conducted during the procedure if
there is no other choice.
In carrying out the following steps, do not allow the waste'to be exposed
to the atmosphere for any more time than is absolutely necessary.
I
8.1 Preweigh the (evacuated) container that will receive the filtrate
(see Section 4.6), and set aside. ;
8.2 Place the ZHE piston, within the body of the ZHE (it may be helpful
to first moisten the piston 0-rings slightly with extraction fluid). Secure
the gas inlet/outlet flange (bottom flange) onto the ZHE body in accordance
with the manufacturer's instructions. Secure the glass fiber filter between
the support screens and set aside. Set liquid inlet/outlet flange (top.
flange) aside. '
8.3 If the waste will obviously yield no free liquid when subjected to
pressure filtration, weigh out a representative subsample of the;waste (25-g
maximum - see Step 8.0), record weight, and proceed to Step 8.5.'
i
8.4 This step provides the means by which to determine the approximate
sample size for the ZHE device. If the waste is liquid or multiphasic, follow
the procedure outlined in Steps 7.2 to 7.9 (using the Section 7 filtration
apparatus) and obtain the percent solids by dividing the weight of the solid
phase of the waste by the original sample size used. If the waste obviously
contains greater than 0.5% solids, go to Step 8.4.2. If it appears that the
solid, may comprise less than 0.5% of the waste, go to Step 8.4.1.
\
8.4.1 Determine the percent solids by using the procedure outlined in
Step 7.10. If the waste contains less than 0.5% solids, weigh out a new 100-g
minimum representative sample, proceed to Step 8.7, and follow until the
liquid phase of the waste is filtered using the ZHE device (Step 8.8). This
liquid filtrate is defined as the TCLP extract and is analyzed directly. If
the waste contains greater than or equal to 0.5% solids, repeat Step 8.4 using
a new 100-g minimum sample, determine the percent solids, and proceed to
Step 8.4.2. ;
8.4.2 If the sample is <25% solids, weigh out a new 100-g minimum repre-
sentative sample and proceed to Step 8.5. If the sample is >25%isolids, the
maximum amount of sample the ZHE can accommodate is determined by dividing
25 g by the percent solids obtained from Step 8.4. Weigh out a new represen-
tative sample of the determined size. '
8.5 After a representative sample of the waste (sample size determined
from Step 8.4) has been weighed out and recorded, the sample is now evaluated
for particle size (see Step 8.0). If the solid material within the waste
obviously has a surface area per gram of material equal to or greater than
3.1 cm2, or is capable of passing through a 9.5-mm standard sieve, proceed
immediately to Step 8.6. If the surface area is smaller or the particle size
is larger than that described above, the solid material that does not meet the
above criteria is separated from the liquid phase by sieving (or'equivalent
means), and the solid is prepared for extraction by crushing, cutting, or
grinding to a surface area or particle size as described above. ;
103
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NOTE: Wastes and appropriate equipment should be refrigerated, if pos-
sible, to 4° C prior to particle size reduction. Grinding and milling
machinery which generates heat shall not be used for particle size reduc-
tion. If reduction of the solid phase of the waste is necessary, expo-
sure of the waste to the atmosphere should be avoided to the extent pos-
sible. When surface area or particle size has been appropriately
altered, the solid is recombined with the rest of the waste.
8.6 Waste slurries need not be allowed to stand to permit the solid
phase to settle. Wastes that settle slowly shall not be centrifuged prior to
filtration.
8,7 Transfer the entire sample (liquid and solid phases) quickly to the
ZHE. Secure the filter and support screens into the top flange of the device
and secure the top flange to the ZHE body in accordance with the manufac-
turer's instructions. Tighten all ZHE fittings and place the device in the
vertical position (gas inlet/outlet flange on the bottom). Do not attach the
extract collection device to the top plate.
NOTE: If waste material has obviously adhered to the container used to
transfer the sample to the ZHE, determine the weight of this residue and
subtract it from the sample -weight determined in Step 8.4, to determine
the weight of the waste sample that: will be filtered.
Attach a gas line to the gas inlet/outlet valve (bottom flange), and with
the liquid inlet/outlet valve (top flange) open, begin applying gentle
pressure of 1 to 10 psi (or more if; necessary) to slowly force all head-
space out of the ZHE device. At the first appearance of liquid from the
liquid inlet/outlet valve, quickly close the valve and discontinue
pressure.
8.8 Attach evacuated preweighed filtrate collection container to the
liquid inlet/outlet value and open valve. Begin applying gentle pressure of
1 to 10 psi to force the liquid phase into the filtrate collection container.
If no additional liquid has passed through the filter in any 2-min interval,
slowly increase the pressure in 10-psi increments to a maximum of 50 psi,
After each incremental increase of 10 psi, if no additional liquid has passed
through the filter in any 2-min interval!, proceed to the next 10-psi incre-
ment. When liquid flow has ceased such that continued pressure filtration at
50 psi does not result in any additional filtrate within any 2-min period,
filtration is stopped. Close the liquid inlet/outlet valve, discontinue pres-
sure to the piston, and disconnect the filtrate collection container.
NOTE: Instantaneous application of high pressure can degrade the glass
fiber filter and may cause premature plugging.
8.9 The material in the ZHE is defined as the solid phase of the waste,
and the filtrate is defined as the liquid phase.
NOTE: Some wastes, such as oily wastes and some paint wastes, will
obviously contain some material that appears to be a liquid; however,
even after applying pressure filtration, this material will not filter.
If this is the case, the material within the filtration device is defined
as a solid and is carried through the TCLP extraction as a solid.
104
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If the original waste contained less than 0.5% solids (see Step 8.4),
this filtrate is defined as the TCLP extraction and is analyzed directly.
Proceed to Step 8.13.
8.10 Determine the weight of the liquid phase by subtracting the weight
of the filtrate container (see Step 8.1) from the total weight of the
filtrate-filled container. The liquid phase may now be either analyzed (see
Steps 8.13 and 8.14) or stored at 4° C until time of analysis. The weight of
the solid phase of the waste sample is determined by subtracting :the.weight of
the liquid phase from the weight of the total waste sample (see Step 8.4).
Record the final weight of the liquid and solid phases. !
8,. 11 The following paragraphs detail the addition of the appropriate
amount of extraction fluid to the solid material within the ZHE and agitation
of the ZHE vessel. Extraction fluid 1 is used in all cases (see [Section 5.6).
8.11.1 With the ZHE in the vertical position, attach a line; from the
extraction fluid reservoir to the liquid inlet/outlet valve. The, line used
shall contain fresh extraction fluid and should be preflushed with fluid to
eliminate any air pockets in the line. Release gas pressure on the ZHE piston
(from the gas inlet/outlet valve), open the liquid inlet/outlet valve, and
begin transferring extraction fluid (by pumping or similar means) into the
ZHE. Continue pumping extraction fluid into the ZHE until the amount of fluid
introduced into the device equals 20 times the weight of the solid phase of
the waste that is in the ZHE.
i
I
8.11.2. After the extraction fluid has been added, immediately close the
liquid inlet/outlet valve and disconnect the extraction fluid line. Check the
ZHE to make sure that all valves are in their closed positions. Pick up the
ZHE and physically rotate the device in an end-over-end fashion 2 or 3 times.
Reposition the ZHE in the vertical position with the liquid inlet/outlet valve
on top. Put 5 to 10 psi behind the piston (if necessary), and slowly open the
liquid inlet/outlet valve to bleed out any headspace (into a hood) that may
have been introduced due to the addition of extraction fluid. This bleeding
shall be done quickly and shall be stopped at the first appearance of liquid
from the valve. Repressurize the ZHE with 5 to 10 psi and check all ZHE fit-
tings to ensure that they are closed. i
8.11.3 Place the ZHE in the rotary extractor apparatus (if |it is not
already there) and rotate the ZHE at 30 + 2 rpm for 18 hr. The temperature
shall be maintained at 22° ± 3° C during agitation.
8.12 Following the 18-hr extraction, check the pressure behind the ZHE
piston by quickly opening and closing the gas inlet/outlet valve -and noting
the escape of gas. If the pressure has not been maintained (i.e.:, no gas
release observed), the device is leaking. Replace ZHE 0-rings or other
fittings, as necessary, and redo the extraction with a new sample of waste.
If the pressure within the device has been maintained, the material in the
extractor vessel is once again separated into its component liquid and solid
phases. If the waste contained an initial liquid phase, the liquid may be
filtered directly into the same filtrate collection container (i.>e. Tedlar
bag, gas-tight syringe) holding the initial liquid phase of the waste, unless
doing so would create multiple phases or there is not enough volume left
within the filtrate collection container. A separate filtrate collection con-
tainer must be used in these cases. Filter through the glass filler filter,
105
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using the ZHE device as discussed in Step 8.8. All extract shall be filtered
and collected if the extract is multiphasic or if the waste contained an ini-
tial liquid phase.
NOTE: If the glass fiber filter is - not intact following agitation, the
filtration device discussed in the Note to Section 4.3.1 may be used to
filter the material within the ZHE. ;
8.13 If the waste contained no initial liquid phase, the filtered liquid
material obtained from Step 8.12 is defined as the TCLP extract. If the waste
contained an initial liquid phase, the filtered liquid material obtained from
Step 8.12 and the initial liquid phase (Step 8.8) are collectively defined as
the TCLP extract.
8.14 The TCLP extract will be prepkred and analyzed according to the
appropriate SW-846 analytical methods, as identified in Appendix III of 40 CFR
261. If the individual phases are to be analyzed separately, determine the
volume of the individual phases (to 0.1 ml), conduct the appropriate analyses,
and combine the results mathematically by using a simple volume weighted
average:
(V1)(C1) + (V2)(C2)
Final contaminant concentration v
1 2
where
Vx - volume of the first phase, liters
Cx - concentration of the contaminant of concern in the first phase,
milligrams per liter
V2 - volume of the second phase, lipers
Co - concentration of the contaminant of concern in the second phase,
£t
milligrams per liter
i
8.15 The contaminant concentrations in the TCLP extract are compared to
the thresholds identified in the appropriate regulations. Refer to Section 9
for quality assurance requirements.
9.0 Quality Assurance Requirements
9.1 All data, including quality assurance data, should be maintained and
available for reference or inspection. ;
9.2 A minimum of one blank for every 10 extractions that have been con-
ducted in an extraction vessel shall be;employed as a check to determine if
any memory effects from the extraction equipment are occurring. One blank
shall also be employed for every new batch of leaching fluid that is made up.
9.3 All quality control measures described in the appropriate analytical
methods shall be followed.
9.4 The method of standard addition shall be employed for each waste
type if recovery of the compound from spiked splits of the TCLP extract is not
between 50% and 150% or if the concentration of the constituent measured in
the extract is within 20% of the appropriate regulatory threshold. If more
than one extraction is being run on samples of the same waste, the method of
106
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standard addition need only be applied once and the percent recoveries applied
to the remainder of the extractions. ]
9.5 TCLP extracts shall be analyzed within the following periods after
generation: volatiles - 14 days; semivolatiles - 40 days; mercury - 28 days;
other metals - 180 days. , .
107
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108
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APPENDIX C
LABORATORY DETERMINATION OF MOISTURE CONTENT OF
HAZARDOUS WASTE MATERIALS
BACKGROUND
This method was developed to determine the moisture content x>f raw and
solidified/stabilized hazardous waste materials. Due to the wide diversity of
properties which hazardous wastes may exhibit, this method cannot; address, nor
is it applicable to, all waste types. Caution must be utilized when applying
this method. It may be necessary to modify this method to address conditions
mandated by the waste. ASTM method D 2216-80 was utilized as a guide in pre-
paring this method. ;
SIGNIFICANCE AND USE i
The waste content of a material is defined as the ratio, expressed as a
percentage, of the mass of "pore" or "free" water in a given mass of material
to the mass of the solid materials particles. A hazardous waste [material may
contain various constituents which may artificially add or subtract from the
results of moisture content. Such variables include: (1) chemically bound
water (water of hydration) which may be released at relative low;temperature,
thus appearing as free water loss, (2) organic materials which oxidize at low
temperature, and (3) any condition, except for "free" water loss, which may
increase or decrease the weight of sample upon drying. Discretion must be
utilized when applying this method to ensure such situations are;considered
and steps are taken to provide results consistent with the purpose of the
test. !
APPARATUS !
Drying oven - thermostatically controlled, preferably of the forced-draft
type, and capable of maintaining a uniform temperature of 60° C in the drying
chamber. This oven should also be capable of maintaining approximately
110° C. If a forced-draft oven is used, the draft should not be 'strong enough
to "blow" any sample from the specimen container. ,
Balances - having a precision of +0.0001 g. ;
Specimen containers - suitable containers made of materials resistant to cor-
rosion and a change in mass upon repeated heating and cooling. :
Mortar and pestle - capable of reducing the particle size of the|waste to
2.0 mm or less.
Sieve - a 2.0-mm (No. 10) sieve. '
i
Desiccator - a desiccator of suitable size containing a hydrous compound.
109
-------
SAMPLES
In all cases, representative portions of the material being sampled
should be collected. To ensure representative sampling, a great deal of
thought and planning will be necessary prior to any sampling activities. The
USEPA has suggested sampling procedures as outlined in "Test Methods for Eval-
uating Solid Waste," SW-846, 2nd ed. Following sample collection, large sam-
ples should be ground and homogenized prior to collecting the subsample. The
moisture determination should be performed as soon as possible after the sub-
sample has been collected.
PROCEDURE ;
1. Select a representative subsample in accordance with the previous
section.
2. Place the undried sample in a clean dry mortar and grind the sample
to pass a No. 10 sieve. Approximately 30 g of sample should be sieved and
rehomogenized in an appropriate dry container. Note: The moisture determina-
tion should be performed on the ground sample as soon as possible; if the sam-
ple must be stored for any period of time, it should be placed in a dry,
labeled, sealed container having minimal! headspace.
i
3. Dry each sample container in the oven at 110° C and cool to room tem-
perature prior to performing Step 4.
4. Using tongs to transfer the sample containers, weigh 3 dry labeled
sample containers and record their weights (Wc) . Tongs should be used in all
subsequent sample transfers. Do not touch the sample containers. except with
the tongs, once they have been dried.
5. Divide the sieved sample into three equal portions and place approxi-
mately 10 g of the moist sieved sample in each of the containers from Step 4.
Reweigh each container and record its weight (Ww) . Care should be taken to
avoid spilling any of the sample material; if any spillage occurs, this sample
should be discarded.
6. Place each sample in the drying oven maintained at a temperature of
60° ± 3° C. Dry each sample for a minimum period of 6 hr.
7. At the end of the 6-hr period, remove the sample container containing
the largest mass of sample and place it .in the desiccator. Allow the sample
to reach room temperature in the desiccator; then weigh this sample and record
its weight (Wdl, W,^, etc.).
8. Replace the sample used in Step 7 back in the oven and dry for a
minimum of an additional hour. Repeat Step 7 until this sample reaches a con-
stant weight (Wd) . Note: Constant weight for this procedure is defined as a
mass change of less than 0.1% of the total sample weight between two succes-
sive drying periods of a minimum of 1 hr. After this sample has reached a
constant weight, repeat Step 7 for the remaining samples.
110
-------
CALCULATIONS !
Calculate the constant weight as follows:
"West = {[Wdu^ - wd(i)] / wdtl)} * 100 : (c-1)
where '.
Wost - constant weight of the largest sample expressed as a percentage
(Wcst must be less than 0.1%) :
wd(i-i) °" weignt °f ^e largest sample, one weighing before the final
constant weight was taken, g
Wd(i) - weight of the largest sample at the final constant weight, g
/ [Ww - Wc] (C-2)
where*
Mf = moisture content expressed as a percentage ;
Ww = weight of the undried sample, g \
W0 - weight of the dried sample container, g
Ma = (Mfl + Mf2 + M£3)/3 (C-3)
where
Ma = average moisture content expressed as -a percentage
Mfl,f2,£3 moisture content of each sample ',
QUALITY CONTROL/QUALITY ASSURANCE
The following calculation is utilized to calculate the percent deviation
Pd = (Mfl - Ma)/Ma) * 100
The percent deviation is calculated for each sample. If the percent deviation
is greater than 2%, these data are discarded, and a complete moisture analysis
is repeated.
REPORT
The report (data sheet) shall include the following:
1. Identification of the sample being tested, by sample number.
Ill i
-------
2. Water content of the specimen, which is an average of three
specimens,
3. Any unusual characteristic of the sample that should be noted.
4. Any deviation from this protocol.
112
-------
APPENDIX D
PHYSICAL PROPERTIES OF THE ORGANIC COMPOUNDS
TABLE D-l. PHYSICAL PROPERTIES OF ORGANIC COMPOUNDS USED IN THIS STUDY
Compound
Benzene
2-Butanone
Carbon disulfide
Carbon tetrachloride
Chlorobenzene
Chloroform
1,2 Dichloroethane
1 , 1 Dichloroethene
Ethylbenzene
4 -Methyl - 2 - Pentanone
1,1,2,2 Tetrachloroethane
Tetrachloroethene
1,1,1 'Trichloroethane
1,1,2 Trichloroethane
Triohloroethene
Toluene
Molecular
Weight
78.11
72.10
76.14
153.82
112.56
119.38
98.98
96.94
106.16
100.20
167.86
165.83
133.41
133.41
131.39
92.10
Vapor
Pressure*
(mm Hg)
95.2
77.5
260*
90.0
8.8
150.5
61.0
591.0**
5.0
6.0
5.0
14.0
96.0
19.0
57.9
28.7**
Solubility*
(mg/1)
820-1,800 '
353,000+
2,300++ i
785
500
8,200 :
8,690
400
152 ]
17,000 ;
2,900
150-200
480-4,400 :
4,500 ;
1,100
234.8**
Boiling
Point
(C)
80.1
79.6
46.3
76 . 54
132
61.7
83.47
37.0
136.2
116-159
146.4
121.0
74.1
113.7
87.0
110.8
Source- All values except those named below were taken from "Water-Related
Environmental Fate of 129 Priority Pollutants; Volume II" (USEPA
1979).
Values for 2-Butanone, 4-Methyl-2-Pentanone, 1,1,2 Trichloroethane,
chlorobenzene, and carbon disulfide were taken from Handbook of
Environmental Data on Organic Chemicals (Verschueren 1977)
* Values reported at 20° C.
** Values reported at 25° C. i
+ Value reported at 10° C. . ;
++ Value reported at 22° C. i
113
-------
-------
APPENDIX E
STUDY A RAW DATA
TABLE E-l
Extrac -
Interference Interference tion
Compound Concentration Test
Oil 0% EP
TCLP
2% EP
TCLP
5% EP
TCLP
8% EP
TCLP
Grease 0% EP
TCLP
2% EP
TCLP
5% EP
TCLP
8% EP
TCLP
Replicate
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Extrac -
tion
Fluid*/
Acid
Added
(ml)
400
400
II
II
400 '
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400 "
400
II
II
400
400
II
II
400
400
II
II
Extracted
Concen-
tration
(mg/1)
i
0.0208
0.0206
0.0073
0.0015
0.0033
0.0034
0.0015
0.0015
0.002
0.0015
0.0188
0.0092
0.0031
0 . 0041
0.0138
0.0021
<0.0001
0.0171
0.0002
0.0007
0.004,
0.0168
<0.0001
<0.0001
0.0022
0.0094
<0.0001
0.0003
0.0072
0.0135
-------
TABLE E-l
Interference
Compound
Lead
Copper
Zinc
Interference
Concentration
0%
2%
2%
5%
8%
0%
2%
5%
8%
0%
2%
Extrac -
tion
Test
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
1
Replicate
>R1
R2
Rl
R2
;RI
R2
Rl
R2
Rl
!R2
'Rl
R2
:R1
R2
:R1
R2
'RI
R2
Rl
R2
Rl
R2
Rl
iR2
;R1
R2
Rl
R2
Rl
R2
, Rl
' R2
Rl
R2
Rl
; R2
Rl
R2
, Rl
R2
Extrac -
tion
Fluid/
Acid
Added
(ml)
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
Extracted
Concen-
tration
(mg/1)
0.0027
0.0013
0.0023
0.001
0.0051
0 . 0042
0.0057
0.0133
0.0093
0.0013
0.096
0.089
0.074
0.0139
0.015
0.0298
0.0039
0.0016
0.0001
<0.0001
0.0002
0 . 0053
0.0006
0.0005
0.0029
0.0037
<0 . 0001
<0 . 0001
0.0021
0.0011
0.0008
<0.0001
0.0956
<0 . 0001
<0.0001
0.011
0.0077
0.0081
0.0014
0.0015
Normalized
Extraction
Concentra-
tion,
(mg/kg)
0.000027
0.000013
0.000023
0.00001
0.000051
0 . 000042
0.000057
0.000133
0.000093
0.000013
0.00096
0.00089
0.00074
0.000139
0.00015
0.000298
0.000039
0.000016
0.000001
0.000001
0.000002
0.000052
0.000006
0.000005
0.000029
0.000037
0.000001
0.000001
0.000021
0.000011
0.000008
0.000001
0.000956
0.000001
0.000001
0.000110
0.000077
0.000081
0.000016
0.000015
(Continued)
(Sheet 2 of 5)
116
-------
Interference
Compound
Zinc (Cont.)
Hexachloro-
benzene
'
Trichloro-
e thene
Interference
Concentration
5%
8%
0%
2%
5%
8%
0%
2%
5%
8%
TABLE E-
Extrac-
tion
Test
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
1 C Continued) '
Replicate
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Extrac-
tion
Fluid/
Acid
Added
(ml)
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
i
Extracted
Concen-,
trationi
(mg/1)
0.0036
0.0087
0.0048i
0.0039;
0.0046-
0.0023:
0.0017)
0.003
0.0416,
0.0037'
0.0027^
0.0028'
0.006 :
0.0072J
0.0025'
0.0018;
0.0378
0.0056'
0.01671
0.0088!
0.0042;
0.0066|
0.0003;
0.0001;
0.0015;
0.0013'
<0.0001
<0 . 0001
0.0014,
0.0015!
0.0006;
<0.0001
0.0005
0.0022
<0 . 0001
<0.0001
0.001
0 . 0004
<0.0001
<0 . 0001
Normalized
Extraction
Concentra-
tion,
(mg/kg)
0.000036
0.000087
0.000054
0.000039
0.000046
0.000023
0.000017
0.000034
0.000498
0.000044
0.000032
0.000034
0.000073
0.000088
0.000031
0.000022
0.000463
0.000067
0.000205
0.00011
0.000052
0.000081
0.000004
0.000001
0.000018
0.000015
0.000001
0.000001
0.000017
0.000018
0.000007
0.000001
0.000006
0.000026
0.000001
0.000001
0.00001
0.000005
0.000001
0.000001
(Continued)
['(Sheet 3 of 5)
117
-------
TABLE E-l (Continued)
Interference
Compound
Phenol
Sodium
sulfate
Sodium
hydroxide
Interference
Concentration
0%
2%
5%
8%
0%
2%
5%
8%
0%
2%
Extrac-
tion
Test
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP,
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
I
Replicate
i
\ Rl
R2
Rl
i R2
Rl
1 R2
' Rl
R2
, Rl
R2
: Rl
R2
' Rl
; R2
Rl
R2
Rl
R2
Rl
R2
Rl
! R2
: Rl
. R2
Rl
R2
'' Rl
R2
! Rl
R2
Rl
; R2
: RI
R2
Rl
R2
Rl
R2
; Rl
R2
Extrac-
tion
Fluid/
Acid
Added
(ml)
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
Extracted
Concen-
tration
(mg/1)
0.0006
0.0024
0.0012
0.0028
0.0014
0.0028
0.0022
0.0061
0.0067
0.0026
O.0001
<0.0001
0,0048
0.0026
<0,0001
<0.0001
0.0071
0.0058
0.0008
0.0018
0.0057
0.0091
0.0009
0.0009
0 . 002
0.0115
0.0009
0.0010
0.0106
0.0063
0.0015
0.0025
<0.0001
0.0011
0.0004
<0.0001
0.0045
0.0061
0.0002
0.0004
Normalized
Extraction
Concentra-
tion,
(mg/kg)
0.000007
0.000029
0.000015
0.000034
0.000017
0.000035
0.000027
0.000076
0.000083
0.000032
0.000001
0.000001
0.000059
0.000032
0.000001
0.000001
0.000084
0.000069
0.000009
0,000021
0.000068
0.00011
O.C0001
0.00001
0.00002
0.000139
0.00001
0.00001
0.000129
0.000077
0.000018
0.000030
0.000001
0.000012
0.000004
0.000001
0.000053
0,000071
0.000002
0.000005
(Continued)
(Sheet 4 of 5)
-------
TABLE E-l (Concluded')
Interference
Compound
Interference
Concentration
Extrac-
tion
Test
Extrac-
tion
Fluid/
Acid
Added
Replicate (ml)
Normalized
Extracted Extraction
Concen- Concentra-
tration tion,
(mg/1)
Sodium
hydroxide
(Cont.)
5%
8%
EP
TCLP
EP
TCLP
Rl
R2
Rl
R2
Rl
R2
Rl
R2
400
400
II
II
400
400
II
II
0.0034
0.0027
<0.0001
<0. OOOl!
0.0024:
0.0016
<0.0001
<0.000l
(mg/kg)
0.000042
0.000034
0.000001
0.000001
0.000028
0.000019
0.000001
0.000001
(Sheet 5 of 5)
119
-------
TABLE E-2. TCLP AND EP EXTRACT ANALYSIS FOR CHROMIUM
Interference Interference
Compound Concentration
Oil 0%
2%
5%
8%
Grease 0%
2%
5%
8%
Lead 0%
2%
Extrac-
tion
Test
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
i
Replicate
Rl
R2
iRl
R2
Rl
^R2
Rl
R2
!RI
-------
TABLE E-2 (Continued)
Interference
Compound
Lead (Cont.)
Copper
Zinc
Interference
Concentration
2%
5%
8%
0%
2%
5%
8%
0%
2%
5%
8%
Extrac-
tion
Test
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
Replicate
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Extrac-
tion
Fluid/
Acid
Added
(ml)
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
Extracted
Concen-
tration
(mg/1);
0.058
0.055 ;
0.031
0.029
0.047 ;
0.04 :
0.03 :
0.03
0.038 '
0.085
0.01
0.009 ;
0.038
0.039
0.114
0.061 .
0.071
0.065 !
0.038
0.034
0.048 ;
0.049 ;
0.011 ;
0.01 '
0.043 !
0.049 :
0.051 :
0.019 ;
0.071 !
0.065 j
0.047 ;
0.044 ;
0.062 .
0.062 :
0.098
0.07 !
0.1
0.096 !
0.09
0.101 ;
0.095 :
0.093
Normalized
Extraction
Concentra-
tion,
(mg/kg)
0.00058
0.00055
0.00031
0.00029
0.00047
0.00040
0.0003
0.0003
0.00038
0.00085
0.0001
0.00009
0.00038
0.00039
0.00114
0.00061
0.00071
0.00065
0.00038
0.00034
0.00048
0.00049
C. 00011
0.0001
0.00043
0.00049
0.00051
0.00019
0.00080
0.00065
0.00047
0.00044
0.00070
0.00062
0.00098
0.0007
0.001
0.00096
0.0009
0.00101
0.00095
0.0010
(Continued)
:(Sheet 2 of 4)
121
-------
TABLE E-2 (Continued)
Interference
Compound
Hexachloro-
benzene
Trichloro-
ethene
Phenol
Interference
Concentration
0%
2%
5%
8%
0%
2%
5%
8%
0%
2%
Extrac-
tion
Test
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
Replicate
R2
Rl
R2
Rl
:R2
' Rl
; R2
Rl
! R2
! Rl
R2
: Rl
'. R2
Rl
: R2
i
Rl
R2
Rl
R2
Rl
! R2
Rl
R2
Rl
R2
: RI
' R2
Rl
' R2
: Rl
: R2
Rl
R2
: Rl
R2
Rl
! R2
' Rl
' R2
Extrac-
tion
Fluid/
Acid
Added
(ml)
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
Extracted
Concen-
tration
(mg/1)
0.015
0.041
0.251
0.349
0.07
0.031
0.3
0.18
0.008
0.013
0.689
0.332
0.032
0,089
0.041
0.029
0.041
0.04
0.076
0.077
0.046
0.048
0.089
0.076
0.038
0.035
0.072
0.073
0.037
0.064
0.064
0.066
0.016
0.013
0.072
0.124
0.007
0.01
0.108
0.216
Normalized
Extraction
Concentra-
tion,
(mg/kg)
0.00018
0.00049
0.00300
0.00418
0.0009
0.00038
0.004
0.0022
0.0001
0.00016
0.00844
0.00407
0.00039
0.0011
0.00051
0.00036
0.00049
0.0005
0.00091
0.00092
0.00055
0.00057
O.OOli
0.00090
0.00046
0.00042
0.00087
0.00088
0.00044
0.00077
0.00077
0.00079
0.00020
0.00016
0.00088
0.00152
0.00009
0.0001
0.00134
0.00268
(Continued)
(Sheet 3 of 4)
122
-------
TABLE_ E-2 (Concluded)
Interference
Compound
Phenol
(Cent.)
Sodium
sulfate
Sodium
hydroxide
Interference
Concentration
5%
8%
0%
2%
5%
"8%
0%
2%
5%
8%
.
Extrac-
tion
Test
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
Replicate
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Extrac-
tion
Fluid/
Acid
Added
(ml)
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
Extracted
Concen4
tration
(mg/D.
0.006 '
0.005 i
o.oso ;
0.045
0.02 i
0.019
0.015 ;
0.016 ;
0.077 :
0.065 .
0.049 '
0.049
0.122;
0.13 .
0.153
0.156;
0.151
0.155,
.0.143
0.144;
0.14 ,
0.166;
0.146;
0.144|
0.07 '
0.1 -
0.08
0.08
0.126'
0.138,
0.113
0.118:
0.485r
0.483
0.411
0.415!
0.377:
0.381
0.307!
0.327
Normalized
Extraction
Concentra-
tion,
(mg/kg)
0.00007
0.00006
0.0006
0.00056
0.0002
0.00023
0.00019
0.00020
0.00091
0.00077
0.00058
0.00058
0.00146
0.00156
0.00183
0.00186
0.00183
0.00188
0.00173
0.00174
0.0017
0.00202
0.00178
0.00175
0.0008
0.001
0.0009
0.0009
0.00147
0.00161
0.00132
0.00138
0.00603
0.00600
0.00511
0.00516
0.00444
0.00449
0.00362
0.00385
(Sheet 4 of 4)
123
-------
TABLE E-3. TCLP AND EP EXTRACT ANALYSIS FOR MERCURY
Interference Interference
Compound Concentration
Oil 0%
2%
5%
8%
Grease 0%
2%
5%
8%
Lead 0%
2%
Extrac-
tion 1
Test Replicate
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
Rl
:R2
Rl
:R2
Rl
R2
i Rl
R2
; Rl
R2
, Rl
, R2
Rl
R2
Rl
R2
' Rl
R2
. Rl
R2
', RI
: R2
1 Rl
R2
Rl
R2
Rl
R2
: Rl
R2
Rl
; R2
! Rl
R2
: Rl
R2
, Rl
R2
(Continued)
Extrac-
tion
Fluid*/
Acid
Added
(ml) .
400
400
II
.11
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
,11
II
400
400
II
II
400
400
II
II
400
400
Extracted
Concen-
tration
(mg/1)
0.4
0.388
0.453
0.425
0.0157
0.0319
0.0287
0.0276
0.003
0.0032
0.0046
0.0068
0.0011
0.0011
0.0021.
0.0023
0.266
0.243
0.249
0.203
0.092
0.169
0.134
0.157
0.066
0.132
0.103
0.088
0.069
0.137
0.092
0.106
0.437
0.264
0.498
0.494
0.21
0.276
Normalized
Extraction
Concentra-
tion,
(mg/kg)
0.005
0.00475
0.00554
0.00520
0.000194
0.000393
0.000354
0.000340
0.00003
0.000039
0.000056
0.000083
0.000013
0.000013
0.000025
0.000027
0.00319
0.00291
0.00298
0.00243
0.0012
0.00199
0.00158
0.00185
0.00077
0.00154
0.00120
0.0010
0.00080
0.00159
0.0011
0.00123
0.00437
0.00264
0.00498
0.00494
0.0021
0.00276
II « TCLP extraction fluid 2.
(Sheet 1 of 5)
124
-------
Interference Interference
Compound Concentration
Lead (Cont.) 2%
5%
8%
Copper 0%
2%
5%
8%
Zinc 0%
2%
5%
8%
TABLE E-3
Extrac-
tion
Test
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
(Continued)
Replicate
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Extrac-
tion
Fluid/
Acid
Added
(ml) '
II
II
400
400
II
II
400
400
II
II
400
400
II
IT
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
- 400
400
Extracted
Concen-
tration
(mg/1)
0.501 !
0.498;
0.107 i
0.284:
0.37
0.443
0.291!
0.222!
0.4471
0.49 ;
0.17 '<
0.148;
0.287
0.225;
0.164!
0.357!
0.287;
0.332
0.346;
0.3531
0.205;
0.285;
0.195:
0.234,
0.24
0.264;
0.191
0.193;
0.32 :
0.285:
0.274'
0.285
0.279
0.282;
0.158;
0.231|
0.26 :
0.263
0.142:
0.097
Normalized
Extraction
Concentra-
tion,
(mg/kg)
0.00501
0.00498
0.00107
0.00284
0.0037
0.00443
0.00291
0.00222
0.00447
0.0049
0.0017
0.00148
0.00287
. 0.00225
0.00164
0.00357
0.00287
0.00332
0.00346
0.00353
0.00205
0.00285
G. 001 95
0.00234
0.0024
0.00264
0.00191
0.00193
0.0036
0.00285
0.00274
0.00285
0.00313
0.00282
0.00158
0.00231
0.0029
0.00263
0.00142
0.00097
(Continued)
(Sheet 2 of 5)
125
-------
TABLE E-3. (Continued)
Interference
Compound
Zinc (Cont.)
Hexachloro-
benzene
Trichloro-
ethene
Phenol
Interference
Concentration
8%
0%
2%
5%
8%
0%
2%
5%
8%
0%
Extrac-
tion
Test
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
Replicate
iRl
;R2
;R1
R2
|RI
R2
:R1
R2
:>R1
R2
Rl
R2
Rl
R2
:RI
:R2
.Rl
IR2
; Rl
R2
: RI
R2
.Rl
! R2
Rl
< R2
: Rl
R2
, Rl
R2
Rl
R2
Rl
R2
Rl
R2
, Rl
R2
Extrac-
tion
Fluid/
Acid
Added
(ml)
II
II
II
II
400
400
II
II
400
400
II
II
400 '
400
II
. II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
Extracted
Concen-
tration
(mg/1)
0.249
0.22
0.2830
0.2340
0.241
0.322
0.238
0.287
0.276
0.269
0.234
0.227
0.318
0.245
0.269
0.217
0.206
0.245
0.419
0.425
0.271
0.184
0.375
0.384
0.248
0.305
0.641
0.602
0.392
0.456
0.69
0.1
0.697
0.643
0.381
0.282
0.356
0.381
Normalized
Extraction
Concentra-
tion,
(mg/kg)
0.00249
0.0025
0.00338792
0.00280132
0.00289
0.00385
0.00290
0.00350
0.00337
0.00328
0.00287
0.00278
0.00390
0.00300
0.00332
0.00268
0.00254
0.00302
0.00500
0.00507
0.00323
0.00220
0.00445
0.00456
0.00295
0.00362
0.00771
0.00724
0.00471
0.00548
0.0083
0.001
0.00837
0.00772
0.00468
0.00346
0.00437
0.00468
(Continued)
(Sheet 3 of 5)
126
-------
TABLE E-3. (Continued)
'
Interference
Compound
Phenol
(Cont.)
Sodium
sulfate
Sodium
hydroxide
Interference
Concentration
2%
5%
8%
0%
2%
5%
8%
0%
2%
5%
Extrac-
tion
Test
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLF
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
Replicate
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Extrac-
tion
Fluid/
Acid
Added
(ml)
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
Extracted
Concen-
tration
(mg/1)
1.3 ;
1.32
1.3 :
1.3 !
1.3 :
1.3
1.35 :
1.3
1.32
1.32
1.48
1 . 35 :
0.199 '
0.141 '
0.257
0.246 :
0.166
0.124 ;
0.304
0.257 ,
0.094 i
0.135 ;
0.226 :
0.185
0.152
0.16
0.199 :
0.21 '
0.18 i
0.111 ;
0.151
0.155 !
0.29 i
0.264 ;
0.198 :
0.195 '
0.272 i
0 . 347
0.193'
0.186 ,
Normalized
Extraction
Concentra-^
tion,
(mg/kg)
0.016
0.0164
0.016
0.016
0.016
0.016
0.0178
0.016
0.0163
0.0163
0.0183
0.0167
0.00236
0.00167
0.00305
0.002.92
0.00198
0.00148
0.00363
0.00307
0.0011
0.00163
0.00273
0.00224
0.00185
0.0019
0.00242
0.0026
0.0020
0.00125
0.00170
0.00174
0.0034
0.00308
0.00231
0.00228
0.00338
0.00431
0.00240
0.00231
(Continued)
;(Sheet 4 of 5)
127
-------
TABLE E-3. (Concluded)
~~ ~~ ' Extrac-
tion Normalized
Fluid/ Extracted Extraction
Extrac- Acid Concen- Concentra-
Interference Interference tion Added tration tion,
Compound Concentration Test Replicate (ml)(mg/1)(mg/kg)
8% EP ;R1 400 0.326 0.00384
^roxide ' !*2 400 0.249 0.00293
(Coat.) TCLP ;R1 II 0.199 0.00234
1 ; . R2 II 0.376 0.00443
! (Sheet 5 of 5)
128
-------
TABLE E-4. TCLP AND EP EXTRACTS FOR NICKEL
Extrac-
Interference Interference tion
Compound Concentration Test Replicate
Oil 0% EP
TCLP
2% EP
TCLP
5% EP
TCLP
8% EP
TCLP
Grease 0% EP
TCLP
2% EP
TCLP
5% EP
TCLP
8% EP
TCLP
Lead 0% EP
TCLP
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
(Continued)
Extrac-
tion
Fluid*/
Acid
Added
(ml)
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
Extracted
Concen-
tration
(mg/1)
0.07 ;
0.068 i
0.068
0.03 ;
0.067
0.068
0.001
0.074 :
0.066 ,
0.065 !
0.014 ;
0.011 :
0.063
0.066
0.053. ,
0.092
0.201 :
0.154
0.012 ;
o.o4i ;
0.014 ;
0.02 !
0.015 ,
0.014 :
0.006 ;
0.006
0.009 ;
0.014
0.002|
0.015:
0.01 ,
0.007
0.013;
0.012
0.031'
0.031'
Normalized
Extraction
Concentra-
tion,
(mg/kg)
0.0009
0.00083
0.00083
0.0004
0.00083
0.00084
0.00001
0.00091
0.00081
0.00080
0.00017
0.00013
0.00074
0.00078
0.00062
0.0011
0.00241
0.00184
0.00014
0.00049
0.00016
0.0002
0.00018
0.00016
0.00007
0.00007
0.0001
0.00016
0.00002
0,00017
0.0001
0.00008
0.00013
0.00012
0.00031
0.00031
* II = TCLP extraction fluid 2.
;(Sheet 1 of 5)
129
-------
TABLE E-4. (Continued)
Interference Interference
Compound Concentration
Lead (Cont.) 2%
5%
8%
Copper 0%
2%
5%
8%
Zinc 0%
2%
5%
Extrac-
tion
Test
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
Replicate
Rl
:R2
Rl
R2
'. Rl
1 R2
. Rl
: R2
; RI
R2
' Rl
R2
. Rl
" R2
: Rl
R2
Rl
R2
Rl
, R2
Rl
R2
> Rl
, R2
Rl
R2
; Rl
1 R2
Rl
R2
i Rl
R2
Rl
R2
Rl
: R2
! Rl
: R2
Rl
R2
Extrac-
tion
Fluid/
Acid
Added
(ml)
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
Extracted
Concen-
tration
(mg/1)
0.005
0.012
0.015
0.015
0.009
0.006
0.052
0.043
0.026
0.024
0.073
0.117
0.012
0.022
0.03
0.013
0.014
0.033
0.035
0.022
0.011
0.018
O.OA4
0.012
0.018
0.017
0.079
0.024
0.066
0.064
0.036
0.03
0.084
0.098
0.0006
0.006
0.089
0.095
0.011
. 0.011
Normalized
Extraction
Concentra-
tion,
(mg/kg)
0.00005
0.00012
0.00015
0.00015
0.00009
0.00006
0.00052
0.00043
0.00026
0.00024
0.00073
0.00117
0.00012
0.00022
0.00030
0.00013
0.00014
0.00033
0.00035
0.00022
0.00011
0.00018
0.00044
0.00012
0.00018
0.00017
0.00079
0.00024
0.00066
0.00064
0.00040
0.00030
0.00084
0.00098
0.000007
0.00006
0.00089
0.00095
0.00012
0.00011
(Continued)
(Sheet 2 of 5)
130
-------
TABLE E-4. (Continued)
Interference
Compound
Zinc (Cont.)
Hexachloro-
benzene
Trichloro-
ethene
Phenol
Interference
Concentration
8%
0%
2%
5%
8%
0%
2%
5%
8%
0%
Extrac-
tion
Test
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
Replicate
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Extrac-
tion
Fluid/
Acid
Added
(ml)
400
400
II
II
400
400
II
II
400
400
II
II
400
400
TI
11
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
Extracted
Cone en-'
tration
(mg/1)
0.107 ;
0.1
0.13
0.007 :
0.01
0.029 i
0.074
0.102
0.011
0.018 l
0.075
0.043
0.015
0.013 ''
0.203 ;
0.1
0.017 i
0.278 ;
0.027
0.021 .
0.012
0.017 '
0.003 '
0.006
0.009
0.01 !
0.012
0.003 ;
0.009 i
0.013 ;
0.02 ;
0.003
0.008
0.012
0.005 !
0.003 ,
0.012
0.006 :
Normalized
Extraction
Concentra-
tion,
(mg/kg)
0.00107
0.001
0.0013
0.00008
0.0001
0.00035
0.00089
0.00122
0.00010
0.00022
0.00095
0.00052
0.00018
0.00016
0.00249
0.001
0.00021
0.00343
0.00033
0.00025
0.00014
0.00020
0.00004
0.00007
0.0001
0.0001
0.00014
0.00004
0.0001
0.00016
0.0002
0.00004
0.0001
0.00014
0.00006
0.00004
0.00015
0.00007
(Continued)
i(Sheet 3 of 5)
131
-------
TABLE E-4. (Continued)
Interference
Compound
Phenol
(Cont.)
Sodium
sulfate
Sodium
hydroxide
Interference
Concentration
0%
2%
5%
8%
0%
2%
5%
8%
0%
2%
Extrac-
tion
Test
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
EP
TCLP
Replicate
1
Rl
R2
Rl
R2
Rl
R2
Rl
: R2
Rl
. R2
: Rl
R2
Rl
R2
Rl
: R2
Rl
R2
Rl
R2
Rl
! R2
i Rl
1 R2
: Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
R2
Rl
: R2
Extrac-
tion
Fluid/
Acid
Added
(ml)
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
400
400
II
II
Extracted
Concen-
tration
(mg/1)
0.061
0.091
0.005
0.005
0.058
o.i
0.004
0.011
0.035
0.037
0.002
0.007
0.033
0.046
0.063
0.06
0.102
0.087
0.057
0.059
0.069
0.071
0.057
0.073
0.063
0.063
0.066
0.059
0.056
0.055
0.086
0.073
0.065
0.065
0.017
0.102
0.054
0.056
Normalized
Extraction
Concentra-
tion,
(mg/kg)
0.00075
0.0011
0.00006
0.00006
0.00072
0.001
0.00005
0.00014
0.00044
0.00046
0.00002
0.00009
0.00041
0.00057
' 0.00075
0.0007
0.00121
0.0010
0.00068
0.00070
0.00082
0.00085
0.00069
0.00088
0.00076
0.00076
0.00080
0.00072
0.00068
0.00067
0.00097
0.00082
0.00073
0.00073
0.00020
0.00119
0.00063
0.00065
(Continued)
(Sheet 4 of 5)
132
-------
TABLE E-4. (Concluded)
Interference Interference
Compound Concentration
Extrac-
tion
Fluid/
Extrac- Acid
tion Added
Test Replicate (ml)
: Normalized
Extracted Extraction
Concen- Conceutra-
tration tion,
(mg/1) (mg/kg)
Sodium
hydroxide
(Corit.)
5%
8%
EP
TCLP
EP
TCLP
Rl
R2
Rl
R2
Rl
R2
Rl
R2
400
400
II
II
400
400
II
II
o.oos:
0.006:
0.07 i
0.064
0.003
0.001
0.04 :
0.033
0.0001
0.00007
0.0009
0.00080
0.00004
0.00001
0.0004
0.00039
: (Sheet 5 of 5)
133
-------
-------
APPENDIX F
GRAPHICAL REPRESENTATION OF THE RESULTS
OF TCLP AND EP EXTRACTIONS FOR ';
STUDY A METALS
Figures F1-F4 are graphical representations of the TCLP and |EP extrac-
tions for each metal contaminant of Study A. In these figures the normalized
EP extract concentrations are plotted versus the normalized TCLP ^extract con-
centrations . A line with a slope of 1.0 is plotted on each graph. Points
which lie on this line indicate that the extract concentrations for the EP and
TCLP are equal. Points above this line indicate that the TCLP produced
extracts with higher concentrations of the contaminant, and points below this
line indicate that the EP resulted in extracts containing higher 'concentra-
tions of the contaminants. Based on this information, the mercuriy data (Fig-
ure F-4) indicate that the TCLP was the more aggressive extraction method
because more than 70 percent of the mercury data points lie above the line.
In order to compare Figures F-l through F-4, the difference in scales
must be considered. The scales for the chromium and mercury data, presented
in Figures F-2 and F-4, are equivalent. However, scales for the icadmium and
nickel data, presented in Figures'F-l and F-3, cannot be adjusted to match the
scales of Figures F-2 and F-4 and still maintain any reasonable resolution.
Therefore, the scale for nickel is 2.8 times smaller and the scale for the
, cadmium data is 17 times smaller than those used in the other figures.
The data presented in Figures F-l and F-3 are closely grouped near the
line, indicating equal EP and TCLP extract concentrations. Comparison of Fig-
ures F-l and F-3 to Figure F-4 illustrates that the results for the EP and
TCLP extracts for mercury differ and that the EP and TCLP extracts for cadmium
and nickel do not. Similar observations for the chromium are more difficult
to decipher.
135
-------
0,0004
0.0003 -
I
S 0.0002 -
0,0001 -
0.0001 0.0002
NORMALIZED EP DATA
0.0003
Figure F-l. Normalized EP extract concentrations versus the
normalized TCLP extract concentrations for the
Study A cadmium contaminant.
0.007
0,006 -
O.OOS -
a. 000* -
0,003
0.002
0,001 -
0.001
0.002
0.003 0.004
NORMALIZED EP DATA
O.OOS
O.OO6
0.007
Figure F-2.
Normalized EP extract concentrations versus the
normalized TCLP extract concentrations for the
Study A chromium contaminant.
136
-------
0.0025
0.0020 -
o
o
UJ
N
0.0015 -
1 0.0010
0.0005
0.005
0.0010 0.0015
NORMALIZED EP DATA
0.0020
0.002S
Figure F-3. Normalized EP extract concentrations versus the
normalized TCLP extract concentrations for'the
Study A nickel contaminant. :
O.O07
0.001
O.O02
0.003 O.OO4
NORMALIZED EP DATA
0.005
O.OO6
0.007
Figure F-4.
Normalized EP extract concentrations versus the
normalized TCLP extract concentrations for the
Study A mercury contaminant.
137
-------
-------
TABLE G-l.
APPENDIX G
STUDY B METALS RAW DATA |
STUDY B TCLP AND EP EXTRACT ANALYSIS FOR THE WES SLUDGE METAL
CONTAMINANTS
Metal Organic Replicate
Contaminant Test Level Number
Cadmium EP 0.1% Rl
R2
R3
1% Rl
R2
R3
TCLP 0.1% Rl
R2
R3
1% Rl
R2
'. R3
Chromium EP 0.1% Rl
R2
R3
1% Rl
R2
R3
TCLP .0.1% Rl
R2
R3
1% Rl
R2
R3
Nickel EP 0.1% Rl
R2
R3
1% Rl
R2
R3
Extrac-
tion
Fluid*/
Acid
Added
(ml)
400
400
400
400
400
400
II
II
II
II
II
II
400
400
400
400
400
400
II
II
II
II
II
II
400
400
400
400
400
400
!
Extract ;
Concentration
(mg/D ;
0.0012 (
0.0013 ,
0.0016
0.0006 i
0 . 06 .
0.0303
0.0051 :
0.0094 !
0.0164 '
0.0074 I
0.0073
0.0057 ;
0.027 !
0.023
0.021 ;
0.019
0.313 :
0.058
0.049
0 . 062
0.099
0.065
0.056 :
0.048 ;
0.034
0.011 ;
0.019
0.032 ;
0.352 !
o.i69 ;
Normalized
Extracted
Concentra-
tion (mg/1)
0 . 000024
0 . 000025
0.000031
0.00001
0.001
0.000608
0.00010
0 . 00018
0.000322
0.00015
0 . 00015
0 . 00011
0.00053
0 . 00045
0 . 00041
0.00038
0.00628
0.0012
0.00096
0 . 0012
0.0019
0 . 0013
0 . 0011
0.00096
0.00067
0.00022
0.00037
0.00064
0.00706
0.00339
(Continued')
i
* II = TCLP extraction fluid 2.
139
-------
Metal
Contaminant Test
Nickel TCLP
(Cont.)
Mercury EP
TCLP
Organic
Level
0.1%
1%
0.1%
1%
0.1%
1%
, _ '
f
Replicate
Number
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl i
R2
R3
Rl
R2
RS :
Rl
R2
R3
Extrac-
tion
Fluid/
Acid
Added
(ml)
II
II
II
II
II
II
400
400
400
400
400
400
. II
II
II
II
II
II
Extract
Concentration
(mg/1)
0.11
0.154
0.096
0.235
0.214
0.169
8.48
7.57
7.82
0.01
0.02
0.01
7.9
7.9
7.6
8.5
8.3
7.9
Normalized
Extracted
Concentra-
tion (mg/1)
0.0022
0.00302
0.0019
0.00471
0.00429
0.00335
0.166
0.148
0.153
0.0004
0.0004
0.0003
0.16
0.15
0.15
0.17
0.17
0.16
140
-------
TABLE G-2. STUDY B TCLP AND EP EXTRACT ANALYSIS FOR THE WTC WASTE
METAL CONTAMINANTS
Metal Organic Replicate
Contaminant Test Level Number
Arsenic EP 0.1% Rl
R2
R3
1% Rl
R2
: R3
TCLP 0.1% Rl
R2
R3
1% Rl
R2
R3
Cadiaium EP 0.1% Rl
R2
R3
1% . Rl
R2
R3
TCLP 0.1% Rl
R2
R3
1% Rl
R2
R3
Chromium EP 0.1% Rl
R2
R3
1% Rl
R2
R3
TCLP 0.1% Rl
R2
R3
Extrac-
tion
Fluid*/ Normalized
Acid Extract Extracted
Added Concentration Concentra-
(ml) (mg/1) tion (mg/1)
400
400
400
400
400
400
II
II
II
II
II
II
400
400
400
400
400
400
II
II
II
II
II
II
400
400
400
400
400
400
II
II
II
(Continued)
0.022 ;
0.019 :
0.022
0.032
0.027
0.024 ;
0.058
0.053 i
0.053 i
0.104 ;
0.136 ;
0.122 ;
0.005 '
<0.001
0.006 '
<0.001 :
-------
TABLE G-2 (Concluded)
Metal Organic Replicate
Contaminant Test Level Number
Extrac-
tion
Fluid/
Acid
Added
(ml)
Extract
Concentration
(mg/1)
Normalized
Extracted
Concentra-
tion (mg/1)
Chromium
(Cont.)
Lead
TCLP
EP
TCLP
1%
0.1%
1%
0.1%
1%
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
II
II
II
400
400
400
400
400
400
II
II
II
II
II
II
0.035
0.036
0.036
0.005
0.009
0.008
0.011
0.013
0.015
0.175
0.322
0.186
0,053
0.039
0.041
0.00044
0.00045
0.00045
0.00006
0.0001
0.0001
0.00014
0.00016
0.00019
0.00213
0.00392
0.00227
0.00067
0.00049
0.00052
142
-------
TABLE G-3. STUDY B TCLP AND EP EXTRACT ANALYSIS FOR THE
PCE WASTE METAL CONTAMINANTS
Metal Organic Replicate
Contaminant Test Level Number
Antimony EP , 0.1% Rl
R2
R3
1.0% Rl
R2
R3
TCLP 0.1% Rl
R2
R3
1.0% Rl
R2
R3
Arsenic EP 0.1% Rl 10
R2
R3
1.0% Rl
R2
R3
TCLP 0.1% Rl
' R2
R3
1.0% Rl
R2
R3
Copper EP 0.1% Rl
R2
R3
1.0% Rl
R2
R3
TCLP 0.1% Rl
R2
R3
Extrac-
tion
Fluid*/
Acid Extract
Added Concentration
(ml) (mg/1) |
10
10
10
25
25
25
I
I
I
I
I
I
<0.005
10
10
25
25
25
I
T
I
I
I
I
10
10
10
25
25
25
I
I
I
0.027
0.028 '
0.027
0.02
0.027 I
0.022 I
0.034 :
0.038 ;
0.038 :
0.039
0.038 !
0.036 :
0.00006 <
0.005 :
0.007
<0.005
<0.005
<0.005
0.006 ;
G.006
0.007 ;
0.007 :
0.006 I
9.3 ;
9.84
13.1 :
10.7
11. :
10.8
12.9 '
13.2 i
13.1 ;.
Normalized
Extracted
Concentra-
tion (mg/1)
0.00035
0.00036
0.00035
0.00028
0.00038
0.00031
0.00044
0.00049
0.00049
0.00055
0.00053
0.00051
0.00006
0.00009
0.00007
0.00007
0.00007
0.00008
0.00008
0.0001
0.0001
0.00008
0.12
0.126
0.168
0.150
0.15
0.152.
0.166
0.169
0.168
(Continued)
* I = TCLP extraction fluid 1,
(Sheet 1 of 3)
143
-------
TABLE G-3. (Continued)
Metal
Contaminant
Copper
(Cont . )
Lead
Silver
Zinc
Organic
Test Level
TCLP 1 . 0%
EP 0.1%
1.0%
TCLP 0.1%
1.0%
EP 0.1%
1.0%
TCLP 0.1%
1.0%
EP 0.1%
1.0%
TCLP 0.1%
Replicate
Number
Rl
R2'
R3 :
Rl
R2
R3
Rl :
R2 !
R3 :
Rl ',
R2
R3
Rl !
R2 :
R3 ;
Rl '
R2
R3
Rl
R2 i
R3 :
Rl
R2
R3
Rl
R2 '
R3
Rl :
R2 :
R3
Rl
R2
R3
Rl :
R2
R3
Extrac-
tion
Fluid/
Acid
Added
(ml)
I
I
I
10
10
10
25
25
25
I
I
I
I
I
I
10
10
10
25
25
25
I
I
I
I
I
I
10
10
10
25
25
25
I
I
I
Extract
Concentration
(mg/1)
16.5
16.4
16.1
0.026
0.03
0.051
0.037
0.027
0.021
0.063
0.064
0.067
0.065
0.085
0.072
<0.001
<0.001
0.003
0.004
0.004
0.003
0.009
<0.001
<0.001
<0.001
O.001
<0.001
23.4
28.1
36.3
16.4
17.0
16.8
31.6
32.5
32.5
Normalized
Extracted
Concentra-
tion (mg/1)
0.232
0.230
0.226
0.00033
0.0004
0.00065
0.00052
0.00038
0.00029
0.00081
0.00082
0.00086
0.00091
0.0012
0.0010
0.00001
0.00001
0.00004
0.00006
0.00006
0.00004
0.0001
0.00001
0.00001
0.00001
0.00001
0.00001
0.300
0.361
0.466
0.230
0.24
0.236
0.406
0.417
0.417
(Continued)
(Sheet 2 of 3)
144
-------
TABLE G-3. (Concluded)
Metal
Contaminant Test
Zinc TCLF
(Cont.)
Barium EP
TCLP
Organic
Level
1.0%
0.1%
1.0%
0.1%
1.0%
Replicate
Number
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Extrac-
tion
Fluid/
Acid
Added
(ml)
I
I
I
10
10
10
25
25
25
I
I
1
I
I
I
'
Extract
Concentration
(mg/1) '
33.1 ;
32.3 ;
33.4 ;
0.315 ;
0.388
0.442
0.321 . i
0.362
0.321 ;
0.428 !
0.433
0.517
0.578
0.564
0.541
Normalized
Extracted
Concentra-
tion (mg/1)
0.465
0.454
0.469
0.00404
0.00498
0.00567
0.00451
0.00508
0.00451
0.00549
0.00556
0.00664
0.00812
0.00792
0.00760
145
-------
-------
APPENDIX H
GRAPHICAL REPRESENTATION OF THE RESULTS
OF TCLP AND EP EXTRACTIONS
FOR STUDY B METALS
Figures H-l through H-7 are graphical representations of the TCLP and EP
extractions for each metal contaminant of Study B. In these figures the nor-
malized EP concentrations are plotted versus the normalized TCLP jextract con-
centrations. A line with a slope of 1.0 is plotted on each graph. Points
which lie on this line indicate that the extract concentrations for the EP and
TCLP are equal. Points above this line indicate that the TCLP produced
extracts with higher concentrations of the contaminant, and points below this
line indicate that the EP resulted in extracts containing higher:concentra-
tions of the contaminants. ;
Figure H-5 illustrates that the lead contaminant was more aggressively
extracted by the TCLP for each extraction that was performed. Figure H-6
illustrates that the WES-1.0%-mercury data plot on the y-axis. These mercury
data points deviate from the majority of the average population and are sus-
pect. Figures H-2, H-4, and H-7, which present the cadmium, chromium, and
nickel data for the WES sludge, illustrate that analyses of the extracts from
the WES sludge produced data with more scatter than was observed.in the
extreicts of the other sludges. '
147
-------
0.0007
O PCE 0.1% (Sb)
A PCE1.0%(Sb)
0 PCE 0.1% (Ag)
V PCE 1.0* IAg)
O.O001
0.0002
NORMALIZED EP CONCENTRATION
0.0003
O.OOO4
i
Figure H-l. Normalized EP extract concentrations versus the
normalized TCLP extract concentrations for the
Study B antimony and silver contaminants.
0.0024
0.0020
0.0016
a. 0.0012
o
N
< 0.0008
c
o
z
0.0004
LEGEND
0.0001
O.OOO2 0.0003 0.0004
NORMALIZED EP CONCENTRATION !
o.ooos
o.ooos
Figure H-2.
Normalized EP extract concentrations versus the
normalized TCLP extract concentrations for the
Study B arsenic contaminant.
148
-------
00006
0.0003
O.OOO6 O.OOO9
NORMALIZED EP CONCENTRATION
0.001 S
Figure H-3.
Normalized EP extract concentrations versus the
normalized TCLP extract concentrations for ;the
Study B cadmium contaminant. ,
O.OO3
0.001
0.002 O.O03 0.004
NORMALIZED EP CONCENTRATION
0.006
0006
Figure H-4.
Normalized EP extract concentrations versus
the normalized TCLP extract concentrations
for the Study B chromium contaminant. ,
149
-------
0.006
0.005
c
111
o
0.004
0.003
0.003
0.001
LEGEND
O PCEO.1%
A PCE 1.0%
D WTCO.1%
V WTC1.0%
7 7
0.0002
0.0004 ' O.OOO6
NORMALIZED EP CONCENTRATION
0.0008
0.0010
Figure H-5.
Normalized EP extract concentrations versus
the normalized TCLP extract concentrations
for the Study B lead contaminant.
0.7
O WES 0.1% IHg)
WES 1.0% IHg)
D PCE 0.1% (Cu)
7 PCE 1.0% (Cu)
+. PCE 0.1% (Zn)
O PCE 1.0% (Zn)
0.2 0-3
NORMALIZED EP CONCENTRATION
Figure H-6.
Normalized EP extract concentrations versus the
normalized TCLP extract concentrations for the
Study B mercury, zinc and copper contaminants.
150
-------
0.011
0.010 -
O WES 0.1% INil
A WES 1.0% (Nil
PCEO.1% (Ba)
PCE 1.0% (Ba!
0.003 6.004 0.005
NORMALIZED EP CONCENTRATION
Figure H-7.
Normalized EP extract concentrations versus the
normalized TCLP extract concentrations for the
Study B nickel and barium contaminants.
151
-------
-------
APPENDIX I
STUDY B ORGANICS RAW DATA ;
TABLE 1-1. STUDY B TCLP AND EP EXTRACT ANALYSES FOR CARBON TETRACHLORIDE
Sludge
WES
WES
PCE
PCE
WTC
WTC
Extraction Organic
Test Level
EP 0.1%
1%
TCLP 0 . 1%
i
1%
EP 0.1%
1%
TCLP 0.1%
1%
EP 0.1%
1%
TCLP 0 . 1%
1%
Replicate
Number
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Extract
Concentration
(mg/D
0.51
0.5
<0.25
2.4
5.
4.4
1.4
0.66
0.61
<5 .
11.
6.8
<0.5
0.11
0.087
10.
<10.
<10.
<0.5
<0. 5
<0.5
<10.
<10.
<10.
<0 .1
<0. 1
<0.1
<5.
5.
<5.
<0.2
<0.2
<0.2
<5.
<5.
<5.
; Normalized
Extraction
; Concentration
i (mg/kg)
0 . 04
: 0.04
0.02
: o . 19
0.4
0.35
0.11
1 0.052
0 . 048
0.4
0.88
0.55
> 0.03
1 0.0056
! 0 . 0045
' 0.6
0.6
i 0.6
0.03
: 0.03
; 0.03
; 0.6
0.6
i 0.6
0.005
0.005
; 0.005
0.3
0.3
0.3
; 0 . 01
: o.oi
0 . 01
i 0.3
: 0.3
0.3
153
-------
TABLE 1-2. STUDY B TCLP AND EP EXTRACT ANALYSES FOR CHLOROFORM
Sludge
WES
WES
PCE
PCE
WTC
WTC
Extraction Organic
Test Level
EP 0.1%
1%
TCLP 0 . 1%
1%
EP 0.1%
1%
TCLP 0.1%
1%
EP 0.1%
1%
TCLP 0.1%
1%
Replicate
Number
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
£3
Rl
R2
R3
Extract
Concentration
(mg/1)
0.67
1.
0.96
13.5
13.3
15.1
1.8
0.9
1.5
38.8
18.
25.
0.97
1.06
1.01
20.5
23.6
27.2
1.5
1.55
1.62
32.5
35.4
30.2
0.237
0.22
0.221
8.16
9.48
9.29
<0.2
<0.2
<0.2
10.
8.32
9.08
Normalized
Extraction
Concentration
(mg/kg)
0.053
0.08
0.075
1.08
1.07
1.21
0.14
0.07
0.12
3.11
1.4
2.0
0.05
0.0544
0.0519
1.15
1.33
1.53
0.077
0.0796
0.0832
1.83
1.99
1.70
0.0116
0.011
0.0108
0.410
0.477
0.467
0.01
0.01
0.01
0.5
0.419
0.457
154
-------
TABLE 1-3. STUDY B TCLP AND EP EXTRACT ANALYSES FOR 1,2-DICHLOROETHANE
Sludge
WES
WES
PCE
PCE
WTC
WTC
Extraction Organic Replicate
Test Level Number
EP 0.1% Rl
R2
R3
1% Rl
R2
R3
TCLP 0.1% Rl
R2
R3
1% Rl
R2
R3
EP 0.1% Rl
R2
R3
1% Rl
R2
R3
TCLP 0.1% Rl
R2
R3
1% - Rl
R2
R3
EP 0.1% Rl
R2
R3
1% Rl
R2
R3
TCLP 0.1% Rl
R2
R3
1% Rl
R2
R3
Normalized
Extract ' Extraction
Concentration ; Concentration
(mg/1) - (mg/kg)
1.5
1.7
1.5
36.8
35.7
43.6 !
1.7 '
1. :
1.1
89.1 i
50.
45. :
3.57 I
3.66
3.59
53.4
57.6
60.9
4.
4.26 i
4.43
70.4 '
73.8 :
70.
0.81 :
0.735
0.735 ;
45.5
43.6 l
46.
0.633 !
0.442 :
0.392 !
47.2 !
43.2
42.3
0.12
0.13
0.12
2.95
2.86
3.50
0.13
0.08
0.086
7.15
4.
3.6
0.183
0.188
0.184
3.00
3.24
3.42
0.2
0.219
0.227
3.95
4.15
4.
0.039
0.0358
0.0358
2.29
2.19
2.3
0.0308
0.0215
0.0191
2.37
2.17
2.13
155
-------
TABLE 1-4. STUDY B TCLP AND EP EXTRACT ANALYSES FOR
1,1,1-TRICHLOROETHANE
Sludge
WES
WES
PCE
PCE
WTC
WTC
Extraction Organic
Test Level
EP 0.1%
1%
TCLP 0.1%
1%
EP 0.1%
1%
TCLP 0.1%
1%
EP 0.1%
1%
TCLP 0.1%
1%
Replicate
Number
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
R!
R2
R3
Rl
R2
P,3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Extract
Concentration
(mg/1)
0.92
1.1
0.87
16.9
18.4
19.7
2.7
1.4
1.7
58.4
39.
43.
0.45
0.62
0.59
12.
14.2
19.
1.2
1.22
1.18
24.6
25.8
24.8
0.306
0.287
0.286
13.4
16.5
15.3
0.563
0.457
0.34
29.5
22.9
22.1
Normalized
Extraction
Concentration
(mg/kg)
0.072
0.086
0.068
1.36
1.48
1.58
0.21
0.11
0.13
4.68
3.1
3.4
0.023
0,032
0.030
0.67
0.798
1.1
0.062
0.0626
0.0606
1.38
1.45
1 .39
0.0149
0.0140
0.0139
0.674
0.830
0.770
0.0274
0.0223
0.017
1.484
1.15
1.11
156
-------
TABLE 1-5. STUDY B TCLP AND EP EXTRACT ANALYSES FOR TRICHLOROETHENE
Extraction
Sludge Test
WES EP
WES TCLP
PCE EP
PCE TCLP
WTC ' ' EP
WTC TCLP
Organic
Level
0.1%
1%
0.1%
1%
0.1%
1%
0.1%
1%
0.1%
1%
0.1%
1%
Replicate
Number
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Extract
Concentration
(mg/1)
3.4
3.8
3.2
56.9
67.3
69.7
8.6
5.2
6.9
153.
120.
130.
1.41
1.75
1.27
28.7
34.1
38.4
4.8
2.88
2.94
37.4
39.2
43.3
2.46
2.17
2.33
94.2
98.
102.
2.73
2.58
2.33
147.
130.
130.
Normalized
; Extraction
Concentration
(mg/kg)
: 0.27
0.30
0.25
4.56
5.40
5.59
0.67
0.41
0.54
12.3
: 9.6
10.
1 0.0724
0.0898
; 0.0652
1.61
1.92
: 2.16
0.25
0.148
! 0.151
i 2.10
2.20
, 2.43
: 0.120
; 0.106
' 0.114
4.74
4.9
: 5.13
; 0.133
0.12.6
0.114
' 7.39
; 6.5
6.5
157
-------
STUDY B TCLP AND EP EXTRACT ANALYSES FOR BENZENE
1 ftUljlj J. " V » .71 J_ U U J- JJ J- W.LJi. JTXL1 J-/ JLJO, j_|j.k. .t j-vtiw j. j..u.i^.k.u .1. u .u w *.--,.» _._ ._ _ _
Sludge
WES
WES
PCE
PCE
WTC
WTC
Extraction Organic
Test Level
EP 0.1%
1%
TCLP 0.1%
1%
EP 0.1%
1%
TCLP 0 . 1%
1%
EP 0.1%
1%
TCLP 0.1%
1%
Replicate
Number
!
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
S3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Extract
Concentration
(mg/D
1.5
1.7
1.6
37.
44.
47.9
2.9
1.7
2.3
98.
81.
77.
2.63
2.92
2.3
43.2
56.1
63.2
5.6
. 5.07
5.21
72.8
77.5
79.4
0.946
0.874
0.902
53.5
55.6
56.6
0.88
0.812
0.686
71.8
58.7
56.7
Normalized
Extraction
Concentration
(mg/kg)
0.12
0.13
0.13
3.0
3.5
3.84
0.23
0.13
0.18
7.9
6.5
6.2
0.135
0,150
0.12
2.43
3.15
3.55
0.29
0.260
0.267
4.09
4.35
4.46
0.0461
0.0426
0.0440
2.69
2.80
2.85
0.043
0.0396
0.0334
3.61
2.95
2.85
158
-------
TABLE 1-7. STUDY B TCLP AND EP EXTRACT ANALYSES FOR 1,1,2,2-TETRACHLOROETHANE
Sludge
WES
WES
PCE
PCE
WTC
WTC
Extraction Organic
Test Level
EP 0.1%
1%
TCLP 0.1%
1%
EP O..l%
1%
TCLP 0.1%
1%
EP 0 . 1%
1%
TCLP 0.1%
1%
Replicate
Number
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Extract
Concentration
(mg/1)
<0.25
<0.25
<0.25 !
<1.
<1.
<1.
<0.25
<0.2
<0.2
-------
TABLE 1-8. STUDY B TCLP AND EP EXTRACT ANALYSES FOR TETRACHLOROETHENE
Sludge
WES
WES
PCE
PCE
KTC
WTC
Extraction Organic
Test Level
EP 0.1%
1%
TCLP 0.1%
1%
EP 0.1%
1%
TCLP 0.1%
1%
EP 0.1%.
1%
TCLP 0.1%
1%
Replicate
Number
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
R;
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Extract
Concentration
(mg/1)
2.7
3.6
3.
27.9
27.8
22.2
8.5
4.6
7.9
37.
40.
39.
3.25
3.1
2.74
28.5
26.7
29.7
3.3
3.09
3.17
12.2
13.6
14.3
1.08
0.922
1.01
17.
20.
19.6
1.66
1.6
1.55
39.9
39.7
40.
Normalized
Extraction
Concentration
(mg/kg)
0.21
0.28
0.2
2.24
2.23
1.78
0.67
0.36
0.62
3.0
3.
3.1
0.167
0.16
0.141
1.60
1.50
1.67
0.17
0.159
0.163
0.685
0.764
0.803
0.0526
0.0449
0.0492
0.86
1.
0.9860
0.0809
0.078
0.0755
2.01
2.00
2.
160
-------
TABLE 1-9. STUDY B TCLP AND EP EXTRACT ANALYSES FOR TOLUENE
Sludge
WES
WES
PCE
PCE
WTC
WTC
Extraction Organic
Test Level
EP 0.1%
1%
TCLP 0.1%
1%
EP 0.1%
1%
TCLP' 0.1%
1%
EP 0.1%
1%
TCLPt 0.1%
1%
Replicate
Number
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Extract
Concentration '
(mg/1)
2.8
3.3
3. -
55.3
58.2 ;
52.8
5.4
2.9
5.
100. ;
92. ;
89.
1.78 :
1.28
1.06
35. ;
35.9 :
39.1
2.5
2.47 ;
2.52
31.3
36.5
39.5
1.36
1.12
1.23
62.8
68.3 i
65.9
1.5
1.34
1.34
94.2 1
91.2 ;
83.3 i
Normalized
Extraction
Concentration
(mg/kg)
0.22
0.26
0.2
4.44
4.67
4.28 .
0.42
0.23
0.4
8.
7.4
7.1
0..0914
0.0657
0.0544
1.97
2.02
2.20
0.13
0.127
0.129
1.76
2.05
2.22
0.0663
0.0546
0.0599
3.16
3.44
3.31
0.073
0.0653
0.0653
4.74
4.59
4.19
161
-------
Sludge
WES
WES
PCE
PCE
WTC
WTC
Extraction Organic
Test Level
EP 0.1%
1%
TCLP 0 . 1%
1%
EP 0.1%
1%
TCLP 0 . 1%
1%
EP 0.1%
1%
TCLP 0.1%
1%
Replicate
Number
Rl
R2
R3
Rl
R2
R3
Rl
Rl
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R'2
R3
Rl
R;2
R3
Rl
R2
R3
Extract
Concentration
(mg/1)
4.6
5.5
5.7
35.
33.6
32.9
11.
16.
25.
46.
52.
44.
2.09
2.24
1.77
35.4
33.5
34.7
2.3
2.37
2.32
20.9
20.6
21.3
3.17
2.7
2.92
35.
36.1
37.2
3.74
3.85
4.24
80.7
127.
79.1
Normalized
Extraction
Concentration
(mg/kg)
0.36
0.43
0.45
2.8
2.70
2.64
0.86
1.3
2.0
3.7
4.2
3.5
0.107
0.115
0.0909
1.99
1.88
1.95
0.12
0.122
0.119
1.17
1.16
1.20
0.154
0.13
0.142
1.8
1.82
1.87
0.182
0.188
0.207
4.06
6.39
3.98
162
-------
TABLE 1-11. STUDY B TCLP AND EP EXTRACT ANALYSES FOR 2-BUTANONE
Sludge
WES
WES
PCE
PCE
WTC
WTC
Extraction Organic
Test Level
EP 0.1%
1%
TCLP 0.1%
1%
EP 0.1%
1%
TCLP 0.1%
1%
EP 0.1%
1%
TCLP 0.1%
1%
Replicate
Number
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl .
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Extract
Concentration ,
(mg/1) I
47.6
42.8 :
17.
. 171. :.
181. ' ;
212.
23.
14.
14.
280.
300.
190.
5.46
5.33
4.77
132.
137.
131.
4.7 i
5.18
6.28 :
132.
135.
136.
9.65 !
10.9
8.21
156.
180.
153. :
5.98
6.37
6.52
167.
166.
164.
Normalized
Extraction
Concentration
(mg/kg)
3.73
3.36
1.3
13.7
14.5
17.0
1.8
1.1
1.1
22.
24.
15.
0.280
0.274
0 . 245
7.41
7.70
7.36 ,
0.24
0.266
0.322
7.41
7.58
7.64
0.470
0.531
0.400
7.85
9.05
7.70
0.291
0.310
0.318
8.40
8.35
8.25
163
-------
TABLE 1-12.
STUDY B TCLP AND EP EXTRACT ANALYSES FOR
4-METHYL-2-PENTANONE
Sludge
WES
WES
PCE
PCE
WTC
WTC
Extraction Organic
Test Level
EP 0.1%
1%
TCLP 0.1%
1%
EP 0.1%
1%
TCLP 0.1%
1%
EP 0.1%
1%
TCLP 0.1%
1%
Replicate
Numter
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Rl
R2
R3
Extract
Concentration
(mg/1)
60.
50.
14.
175.
193.
210.
17.
11.
12.
350.
290.
300.
12.5
12.4
10.
236.
227.
236.
11.
10.3
10.6
220.
263.
258.
7.66
8.3
7.06
315.
278.
301.
4.64
5.17
4.84
297.
333.
288.
Normalized
Extraction
Concentration
(mg/kg)
5.
4. -
1.1
14.0
15.5
17.
1.3
0.86
0.94
28.
23.
24.
0.642
0.637
0.51
13.3
12.8
13.3
0.56
0.529
0.544
12.
14.8
14.5
0.373
0.40
0.344
15.8
14.0
15.1
0.226
0.252
0.236
14.9
16.8
14.5
164
-------
APPENDIX J :
GRAPHICAL REPRESENTATION OF THE RESULTS OF \
TCLP AND EP EXTRACTIONS FOR :
STUDY B ORGANICS
Figures J-l through J-12 are graphical representations of the TCLP and EP
extractions for each organic contaminant of Study B. In these figures the
normalized'EP extract concentrations are plotted versus the normalized TCLP
extract concentrations. A line with a slope of 1.0 is plotted on each graph.
Points which lie on this line indicate that the extract concentrations for the
EP and TCLP are equal. Points-above this line indicate that the TCLP produced
extracts with higher concentrations of the contaminant, and points below this
line indicate that the EP resulted in extracts containing higher concentra-
tions of the contaminants. ;
To compare Figures J-l through J-12, the difference in scales must be
considered. To maintain reasonable resolution, the scales were not equivalent
for any of the organic contaminants evaluated.
Inspection of Figures J-l through J-12 illustrates that for most contami-
nants with organic concentration level of 0.1%, the EP and TCLP data were
grouped closely around the line near the axis. This indicates that the TCLP
and the EP produce extracts of almost equal concentrations. All the contami-
nants with organic concentration levels of 1.0%, except 1,1,2,2,-
tetrachlorethane (Figure J-6) and tetrachloroethene (Figure J-7),,were more
aggressively extracted by the TCLP than the EP.
165
-------
12
11 -
10
I 9
| *
I ?
u
a. 6
U
H
2 s
I "
c
o
* 3
LEGEND
Figure J-l.
2 3
NORMALIZED EP CONCENTRATION
Normalized EP extract concentrations versus the
normalized TCLP extract concentrations for the
Study B benzene contaminant.
1,6
T
LEGEND
c
>-
z
u
»-
o
cr
o
1.0
i 03
0.6
0,4
0,2
0?
0
WES 0.1%
WES 1.0%
PCE 0.1%
PCE 1.0%
WTCO.1%
O WTC 1.0%
0.1
0.2 , 0.3 0.4
NORMALIZED EP CONCENTRATION
0.5
Figure J-2.
Normalized EP extract concentrations versus the
normalized TCLP extract concentrations for the
Study B carbon tetrachloride contaminant.
166
-------
cc
o
z
LEGEND
O WTC 1.0*
1.5
NORMALIZED EP CONCENTRATION
Figure J-3.
Normalized EP extract concentrations versus the
normalized TCLP extract concentrations for'the
Study B chloroform contaminant. >
10
z
o
z
o
o
_
1 3
O
Z
LEGEND
O WTC 1.0*
0.5
1.0
2.5
1.5 2-0
NORMALIZED EP CONCENTRATION ' ',
Figure J-4. Normalized EP extract concentrations versus the
normalized TCLP extract concentrations for! the
Study B 1,2-dichloroethane contaminant. ;
167
-------
10
1.0
2.0 3.0
NORMALIZED EP CONCENTRATION
Figure J-5,
Normalized EP extract concentrations versus the
normalized TCLP extract concentrations for the
Study B ethylbenzene contaminant.
o WES 0.1%
A WES 1.0%
0 PCEO.1%
7 PC£1.0%
WTCO.1%
O WTC 1.0*
234
NORMALIZED EP CONCENTRATION
Figure J-6.
Normalized EP extract concentrations versus the
normalized TCLP extract concentrations for the
Study B 1,1,2,2-tetrachloroethane contaminant.
168
-------
u
z
o
u
IE
O
z
LEGEND
0.5
1.0 1.5
NORMALIZED EP CONCENTRATION
2.0
2.S
Figure J7. Normalized EP extract concentrations versus;the
normalized TCLP extract concentrations for the
Study B tetrachloroethene contaminant.
T
7.0
6.3
5.6
z
o
P 4.9
a.
H
w 4,2
U
1
o. 3.S
2-8
2.1
1.4
0.7
LEGEND
O WES 0.1%
A WES 1.0%
D PCEO.1%
V PCE 1.0%
+ WTCO.1%
O WTC 1.0%
0.3
0.6
0.9 1.2 1-S
NORMALIZED EP CONCENTRATION
1.8
2.1
2.4
Figure J8. Normalized EP extract concentrations versusithe
normalized TCLP extract concentrations for the
Study B 1,1,1-trichloroethane contaminant. :
169
-------
18
14
10
LEGEND
WES O.IK
WES 1.0%
PCE 0.1%
PCE1.0%
WTC 0.1%
O WTC 1.0%
u
H
o
o o
234
NORMALIZED EP CONCENTRATION
Figure J-9.
Normalized EP extract concentrations versus the
normalized TCLP extract concentrations for the
Study B trichloroethene contaminant.
12
11
10
T
LEGEND
u
I
-------
WES 0.1%
WES 1.0%
PCE 0.1%
PCE 1.0%
WTCO.1%
(J
Z
o
u
5 is H
IT
O
2
NORMALIZED £P CONCENTRATION
Figure J-ll,
Normalized EP extract concentrations versus the
normalized TCLP extract concentrations for: the
Study B 4-methyl-2-pentanone contaminant.
WES 0.1%
WES 1.0%
PCE 0.1%
PCE 1.0%
WTCO.1%
WTC 1.0%
NORMALIZED EP CONCENTRATION
Figure J-12.
Normalized EP extract concentrations versu!s the
normalized TCLP extract concentrations for; the
Study B 2butanone contaminant.
171
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