/EPA
Environmental Protection
Agency
Systems Laooratory
P.O. Box 15027
Las Vega* NV 89114
Research and Development
Sampling and Analysis
of Wastes Generated by
Gray Iron Foundries
prepared for the
Office of Solid Waste
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EPA-600/4-81-028
April 1981
SAMPLING AND ANALYSIS OF WASTES
GENERATED BY GRAY IRON FOUNDRIES
by
W. F, Beckert, T. A. Hinners, L. R. Williams
and E. P. Meier
Quality Assurance Division
Environmental Monitoring Systems Laboratory
Las Vegas, Nevada 89114
and
T. E. Gran
Northrop Services, Inc.
Las Vegas, Nevada
prepared for the
Office of Solid Waste
U.S. ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF RESEARCH AND DEVELOPMENT
ENVIRONMENTAL MONITORING SYSTEMS LABORATORY
LAS VEGAS, NEVADA 89114
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DISCLAIMER
This report has been reviewed by the Environmental Monitoring Systems
Laboratory, U.S. Environmental Protection Agency, and approved for
publication. Mention of trade names or commercial products does not
constitute endorsement or recommendation for use.
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CONTENTS
TaD I 6S »o»»e»»ee««««e«o»o»oe»e». ««».«..»« V
Acknowledgment. ........ ................ vi
Introduction. . „ * ................ . . 1
Description of the Gray Iron and Ductile Iron
Manufacturing Processes. ..................... 1
Waste Generation and Management 3
.Sampling Sites Selection 4
Sampling 6
Pennsylvania Sampling Trip 6
Michigan Sampling Trip 7
Problem Samples 9
Sample Splitting and Handling ..... 10
Sample Preparation 11
Sample Extraction. ........ ....... 11
Sample Digestion ......... 11
Sample Analysis 12
Screening Analysis Using Inductively Coupled Plasma
(ICP) Emission Spectroscopy. ....... 12
Analysis Using Atomic Absorption Spectrophotonetry (AAS) ...... 12
Quality Assurance ..... 14
Results and Discussion 18
Appendices
1 Questionnaires Distributed to the Gray Iron Foundries
to be Sampled 28
2 Sequence of Events Associated with the Sampling of
Each Foundry 34
3 Summary of all Samples Collected 37
4 Sample Listing for the Gray Iron Foundry Project -
Pennsylvania 39
111
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CONTENTS (Continued)
5 Sample Listing for the Gray Iron Foundry Project -
Michigan 41
6 Recommendations for Future Sampling Trips . 44
7 Aliquots Prepared, Aliquot Recipients and Shipping Dates 46
8 List of Extracts and Digests Shipped to LFE and the
University of Wisconsin . . . . . . „ 52
9 Section 7.0 - Extraction Procedure Toxicity 53
10 Digestion Procedure for Gray Iron Foundry Waste Samples 75
11 Chain of Custody Record (Gray Iron Foundry Study Samples) .... 76
12 ICP Data for EP Extracts 77
13 ICP Data for Waste Digests 80
iv
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TABLES
Number - Page
1. Summary of Atomic Absorption Screening Analyses of
Waste EP Extracts and Waste Digests ............... 15
2o Percentage of Cadmium, Chromium and Lead Extracted
From the Raw Wastes by the EP .................. 19
3. Confirmatory Atonic Absorption Analyses of EP
Extracts 21
4. Comparison of LFE Extracts AA Data with EMSL-LV Data 23
5. Comparison of LFE Digests AA Data with EMSL-LV Data 24
6. Comparison of University of Wisconsin Extracts AA
Data with EMSL-LV Data , . . 25
7. Comparison of University of Wisconsin Digests AA
Data with EMSL-LV Data. 26
8. Furnace Charges Used (in % of Total), as Reported
by the Foundries in the Questionnaires. ............. 27
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ACKNOWLEDGMENTS
We wish to acknowledge the considerable efforts and the valuable
assistance of the many people involved in the various phases of this study.
Their contributions helped in the successful completion of the work described
in this report.
This study was sponsored by the Office of Solid Waste. Oave Friedman,
Jim Poppiti, Kathy Schweich and John Warren were instrumental in defining the
scope of the study, conducting the telephone surveys, designing the sampling
plan and coordinating the study with the American Foundrymen Society.
The American Foundrymen Society secured the cooperation of the foundries
involved. The cooperation of the personnel at each foundry was invaluable in
designing the sampling plan and during sample collection.
Dr. William Boyle, University of Wisconsin, under contract to the
American Foundrymen Society, and LFE Environmental Analysis Laboratories,
under contract to the Environmental Monitoring Systems Laboratory, Las Vegas,
conducted analyses of waste samples, split extracts and split digests. We
especially thank Dr. Boyle for valuable discussions and for his permission to
use his data for this report.
Northrop Service, Inc., employees collected the samples and conducted the
extractions and digestions. We especially acknowledge the help of Mark Shanis
and Amy Smiecinsky.
Finally, Arthur Jarvis, Earl Whittaker, David Hemphill, Paul Mills and
Jim Shawver from the Environmental Monitoring Systems Laboratory, Las Vegas,
were instrumental in designing the QA plan for this study and in sample
splitting, and Gordon Bratten and Glenn Gaden in analyzing the extracts and
digests.
The commitment of the above and their efforts helped to make the study a
success.
vi
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INTRODUCTION
Emission control dusts from gray and ductile iron-foundry furnaces are
generated when the heavy metal contaminants, coke dust, ash, etc., found in
the raw material or generated during the manufacturing process, are entrained
in the furnace fumes. The particles are entrapped in air pollution control
devices and the collected material disposed of. After evaluating the
information available, the Agency tentatively determined that the dusts were
hazardous wastes within the meaning of the Resource Conservation and Recovery
Act (RCRA). The Agency thus proposed, on July 16, 1980 (45 FR 47836), to list
such material as a hazardous waste. This conclusion is based on the following
considerations:
1. Waste extracts from gray and ductile iron emission control dusts
have been shown to contain high concentrations of the heavy metals
lead and cadmium. In many cases the concentrations exceeded 100
times the drinking water standards for lead and cadmium, and in some
cases exceeded 1,000 times the standard.
2. Large quantities of these wastes are generated annually, increasing
the quantity of lead and cadmium available for environmental
release.
3. These wastes may be disposed of in wetland or discharge-type areas,
increasing the hazardous constituents' migratory potential.
In response to the comments received and in acknowledgement of the
economic impact of such a listing, EPA decided to gather further information
on gray iron foundry emission control residuals, in order to determine if, in
fact, the waste should not be listed. Thus, on January 16, 1981 (46 FR 4616),
the Agency deferred final action on listing these wastes pending the outcome
of this study.
DESCRIPTION OF THE GRAY IRON AND DUCTILE IRON MANUFACTURING PROCESSES
Close to 1,200 gray iron foundries and 81 ductile iron foundries comprise
these industries. Foundries are located throughout the United States,
however, a large portion of the plants are found in the Great Lakes area.
In gray iron, most of its carbon content is present as flakes of free
graphite. Gray iron is classified into 10 classes based on the minimum tensile
strength of a cast bar. The tensile strength is affected by the amount of
free graphite present as well as the size, shape and distribution of the
graphite flakes. Flake size, shape and distribution are strongly
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influenced by metallurgical factors in the melting of the iron and its
subsequent treatment while molten, and by solidification rates and cooling in
the mold.
Ductile iron (also known as nodular iron, spherulitic iron, etc.) is
similar to gray iron with respect to its earbons silicon and iron contentc
The important difference between ductile and gray iron is that the graphite in
ductile iron separates as spheroids or nodules (instead of flakes as in gray
iron) under the influence of a few hundredths of a percent of magnesium in the
composition.
Similar types of melting equipment are used to produce both gray and
ductile iron, and since the temperature and general metallurgical requirements
are also similar for both processes, single foundries can produce both types
of iron. Furthermore, since the same types of raw materials are used to
produce each type of iron, waste composition also tends to be similar.
Three types of melting furnaces are used for the production of gray iron
and ductile iron: cupola, electric arc, and electric induction furnaces. EPA
estimates that 95 percent of the furnaces used for producing gray iron and
ductile iron are cupola furnaces. The differences among the types of melting
furnaces are discussed below.
1. Cupola Furnaces
The cupola furnace is a vertical shaft furnace consisting of a
cylindrical steel shell lined with refractories and equipped with a wind
box and tuyeres for the admission of air. A charging opening is provided
at an upper level for the introduction of melting stock and fuel. Near
the bottom are holes and spouts for removal of molten metal and slag.
Air for combustion is forced into the cupola through tuyeres located
above the slag well. The products of combustion, i.e., particles of
coke, ash, metals, sulfur dioxide, carbon monoxide, carbon dioxide, etc.,
comprise the cupola emissions. Air pollution emission standards require
that these emissions be controlled, and both dry and wet control systems
are utilized for this purpose.
2. Electric Arc Furnaces
An electric arc furnace is essentially a refractory hearth in which
material can be melted by heat from electric arcs. Arc furnaces are
operated in a batch fashion with tap-to-tap times of 1-1/2 to 2 hours.
Power, in the range of 500-600 kwh/ton, is introduced through three
carbon electrodes. These electrodes are consumed in the process of
melting the charge material. They oxidize at a rate of 5 to 8 kg per
metric ton of steel (10.5 to 17 Ibs/ton). The waste products from the
process are smoke, slag, carbon monoxide, carbon dioxide and oxides of
metals emitted as submicron fumes. Dry collection air pollution control
equipment (usually baghouse) is generally used to control electric arc
furnace emissions.
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3. Induction Furnaces
Induction melting furnaces have been used for many years to
produce nonferrous metals. Innovations in the power application area
during the last 20 years made them competitive with cupolas and arc
furnaces in gray iron and steel production. This type of furnace has
some very desirable features. There is little or no contamination of the
metal bath, no electrodes are necessary, the composition can be
accurately controlled, good stirring is inherent and, while no combustion
occurs, the temperature obtainable is theoretically unlimited. The
induction furnace provides good furnace atmosphere control, since no fuel
is introduced into the crucible. As long as clean materials such as
castings and clean metal scrap are used, no air pollution control
equipment is necessary. If contaminated scrap is charged or magnesium is
added to manufacture ductile iron, air pollution control devices are
required to collect the fumes that are generated.
WASTE GENERATION AND MANAGEMENT
The cupola furnaces in gray and ductile iron foundries require emission
control systems. Both wet and dry systems are utilized. Venturi scrubbers
are used exclusively for wet scrubbing of cupola furnace fumes and baghouses
are used exclusively for dry collection of emissions.
It is estimated that for gray and ductile iron foundries, 10-22 pounds of
emission control dust is generated for every ton of metal produced.
Approximately 95 percent or 1,185 foundries use cupola melting furnaces. In
1979, 16,741,000 tons of metal were produced by this industry. If 95 percent
of this amount is assumed to be produced by the 95 percent of the gray and
ductile iron plants, then from 84,000 to 184,000 tons of dust will be
generated by the industry per year. This estimate is probably low.
Foundry wastes are land disposed. Wastes from many foundries are
monofilled, but others are disposed at municipal or private sanitary landfills
which also accept other types of solid waste. Disposal procedures include
random dumping and grading, combination with other municipal and industrial
wastes, and grading upon deposition followed by application of earth and
topsoil cover. The physical settings of the disposal sites vary; locations
are generally selected on the basis of availability of land at an appropriate
cost within a reasonable haul distance from the foundry. It has been a fairly
common practice to dispose of foundry wastes in wetland or discharge-type
areas where waste materials can become saturated with surface waters or
shallow groundwaters.
The objective of this study was to determine how often the wastes
generated by a representative number of gray iron foundries were identified as
hazardous by the EPA Extraction Procedure. The parameters of interest were
cadmium, chromium and lead with criteria levels of 1, 5 and 5 mg/1,
respectively, for identification of a waste as hazardous. A secondary
objective was to determine the total concentration of these elements in the
wastes studied.
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SAMPLING SITES SELECTION
The selection of the foundries to be sampled and the notification of the
companies were carried out by the Office of Solid Waste (OSW). The goal of
the selection process was to provide a representative cross section of the
types of foundries of interest and to minimize the logistical problems and
expense associated with sample acquisition.
Factors considered in selecting the sampling sites included the nature of
the charge used, furnace type and scrubber type. A telephone survey of all
gray iron foundries located in Pennsylvania and Michigan was conducted to
obtain data on these factors. A majority of the foundries were reached and
provided the requested information. No information was obtained from
approximately 15 foundries, either because they would not release the
information requested, were closed down during the entire course of the
survey, or could not be contacted due to unlisted or constantly busy telephone
numbers.
Based on the information obtained through the telephone survey, the
furnace charge was divided into five classes:
a) clean
b) contaminated with lubricants only
c) contaminated with paints, coatings
d) combination of b and c
e) other.
Charges classified as (b) or (c) contained 40 percent or more of the
respective constituent, while charges classified as (a) were relatively free
of (b) or (c). Class (e) represents charges where the composition was unclear
or was such that class (b) or (c) scrap constituted less than 30 percent of
the total charge.
The information on the individual furnace charge compositions was
provided by foundry representatives during a telephone survey, and it was also
pointed out by those representatives that the reported charge compositions
were characteristic for the individual foundries. Their information was
accepted as quoted and formed the basis for the sampling and analytical
program. A questionnaire was subsequently distributed to all the foundries
that were to be sampled in which a detailed description of the charge was
requested. A sample of the questionnaire form is included as Appendix 1.
The scrubbers were of the Venturi and the baghouse type, and the furnaces
encountered of the cupola and electric arc or induction type.
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The foundries included in this study were selected on the basis of the
factors listed above, on the clarity of response to the charge questions and
on geographic location. The latter point was important because of the limited
resources available for sampling., Therefore, the foundries chosen generally
cluster around towns with airports in order to allow the sampling crew to fly
in, rent a truck and perform the sampling with a minimum of expenseo However,
in no case was quality sacrificed for budget.
The selected foundries were notified of the pending sampling and analysis
endeavor by OSW. Northrop Services, Inc. (NSI), under contract to EMSL-LV,
was to do the actual sampling; their representative established contacts with
the selected foundries to discuss sampling details and schedules.
Independently, the American Foundrymen Society (AFS) requested the cooperation
of the foundries. The AFS also requested from EPA that aliquots of the
collected wastes be sent to a laboratory under contract to the AFS, and that
samples of mixed wastes be collected, as available, and sent directly to the
AFS contract laboratory.
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SAMPLING
Two sampling trips were conducted. The sampling trip to Pennsylvania
lasted from July 28 to August 2, 1980; the trip to Michigan from August 17 to
August 29, 1980. On both trips, scrubber waste samples were collected and
sent by Federal Express P-l mail to the EMSL-LV, and mixed waste samples were
sent by Federal Express Standard Air Freight to the AFS contract analytical
laboratory at the University of Wisconsin (Dr. W. Boyle). When requested, the
foundries received split samples of the wastes collected from their facilities
for this program. The sequence of sampling events, a list of essential
sampling equipment and a checklist for packing samples for shipment are
included as Appendix 2.
It had been hoped that two foundries could be sampled per day; however,
in practice this was not.always the case. As anticipated, it was possible to
sample multiple wastes at some sites. Since the exact nature of the waste
storage and disposal facilities at each site were unknown, the sampling team
leader used his best judgement to obtain a representative sample (or samples)
of each waste of interest. Appendix 3 is a summary of all samples collected.
The gray iron foundries that were sampled are identified in Appendix 3 and in
the remainder of this report by a two-letter code where the first letter (P or
M) identifies the state where the foundry is located (Pennsylvania or
Michigan). The foundries are not identified by their address in this report.
One gallon samples were obtained for both solid and liquid wastes. The
sample size for baghouse dusts was increased to two gallons during the
Michigan trip.
PENNSYLVANIA SAMPLING TRIP
Nine foundries were sampled; 13 scrubber waste samples were collected and
sent to EMSL-LV and 10 mixed waste samples were collected and sent to the
University of Wisconsin.
All furnaces sampled were cupola furnaces, except at foundry PH, which
was an electric arc furnace. The scrubber types were either dry baghouse, wet
Venturi, wet or dry quencher (wet from temperature-controlled spray nozzles
which come on whenever the incoming furnance air temperature is greater than
about 350-400°C), or a combination of a quencher (or Venturi) type and a
baghouse.
The EPA questionnaires were left with foundry personnel, with
instructions to complete and mail them to Dr. Thomas Gran, NSI, Las Vegas.
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Appendix 4 lists the sources and distribution of those samples that were
shipped to the EMSL-LV and University of Wisconsin (AFS contractor) for
analysis. Almost all of these samples were dry or sludges of relatively low
water content. The baghouse dusts were all dry and talc-like in physical
appearance. The mixed samples were dry, or, at most, just damp. At most
foundries,, the mixed waste was primarily composed of casting sand. Smaller
proportions of slag wert also presents usually as chunks. .However, only
pieces of slag that were less than about 1/2 inch in diameter were Included 1n
the samples of mixed waste sent to the University of Wisconsin. The opening
of the cubitainers used for most of the mixed samples is only about 1/2 inch
in diameter, and therefore layer pieces could not be shipped.
At some foundries there was no true mixed waste available. In these
cases, the sampling team followed a foundry-specific procedure for sampling
what was available based on information provided by the plant. In some cases,
only casting sand was readily accessible for sampling.
Most wet scrubber equipment had bins for collection of the solids
produced. Some of these materials were dry when sampled. Excess water from
wet samples was decanted as much as possible before they were deposited into
sample containers. The dried samples appeared to be composed primarily of
coke particles.
At foundry PB, all wastewater was recycled before it was discarded into a
settling lagoon. A sample of this wastewater was collected from a sampling
port located just upstream from the point of discharge into the settling pond.
All solid samples were poured or pushed into the cubitainers through a
plastic funnel. The funnel was cleaned with paper towels and tap water before
each use. Most samples were scooped up with a sampling trowel.
MICHIGAN SAMPLING TRIP
Fourteen furnaces from 12 foundries were sampled; 17 scrubber waste
samples were sent to EMSL-LV, and 13 mixed waste samples were sent to the
University of Wisconsin.
Two of the furnaces sampled were of the electric arc type (MKK and MR
foundries). The sample collected from the MS foundry came from a baghouse
scrubber which collected waste from cupola exhaust air. Ten of the furnaces
visited had wet scrubbers with some type of Venturi system for collecting
waste from cupola exhaust air. Some of these scrubber systems also had wet
subsystems (often called quench towers, wet caps, or prequenchers).
Some of the wet scrubber wastes had been treated with base for
neutralization, while others were treated with flocculents to aid
agglomeration prior to settling. Wet scrubber waste pH was monitored with pH
paper during the last half of the Michigan trip.
All plant representatives had completed the EPA questionnaires upon
arrival of the sampling team.
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Two-gallon samples were taken of all baghouse dusts and one-gallon
samples of all the other wastes. Each gallon was composed of many small
portions obtained with a trowel or scoop from the most recent (preferably,
same day), defined scrubber or mixed waste (preferably, from one "melt"). The
trowel samples were taken in a representative pattern throughout the area to
be sampled. Guidelines presented in "Samplers and Sampling Procedures for
Hazardous Waste Streams" (EPA-600/2-80-018, January 1980) were followed when
it was appropriate and practical to do so.
All of the solid waste samples were poured or pushed into cubitainers
through a glass or plastic funnel. The funnels were cleaned with .paper towels
and tap water before each use.
Appendix 5 lists the sources and distribution of those samples that were
shipped to the EMSL-LV and University of Wisconsin (AFS contractor) for
analysis.
It should be noted that there are two samples numbered 58. An
investigation showed that no mix-up between the samples had occurred. The two
samples were collected at two different locations, on two different days.
Each sample was appropriately packaged and labeled, on the same day it was
collected. The first sample was labeled for shipment to the University of
Wisconsin, and the second to the EMSL-LV. EMSL-LV personnel who logged in the
sample and associated paperwork at Las Vegas confirmed that the correct sample
and paperwork had been shipped to Las Vegas.
The baghouse dusts were all dry, gray-white, and talc-like in physical
appearance, except for the baghouse scrubbing waste from cupola exhaust air
streams. Larger particulates, most probably coke particles, seemed to be
mixed in with the fine dust in the latter case.
Many of the Venturi-scrubbed cupolas also had "wet caps" in operation.
In almost all cases the larger coke-type particles and fine scrubber waste
particles were combined before reaching the point in the waste disposal
processes from which samples were collected. The resulting material was
usually a wet gray sludge containing coarse to fine particles.
In most cases, wet scrubber waste was sampled from holding tanks or
hoppers; therefore, the initial water content was usually high. As much water
as possible was decanted or squeezed from the cubitainers.
Unlike any other sample, the scrubber waste sample collected at the MO
foundry was noticeably warm for several hours after collection indicating that
some kind of reaction was occurring. The unusual behavior of this waste
prompted the sampling team to check from this time the scrubber waste pH,
since acidity or alkalinity of the scrubber waste at different points in the
waste management process could affect the mobility of metals in the waste upon
disposal as landfill, etc. It was found that the scrubber waste pH varied
from acidic to basic. It was learned that most plants add base to the
scrubber waste in the first collection tank to reduce corrosion of pipes,
tanks and fittings.
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When high lead content was detected in the first Pennsylvania sample
analyzed, the sampling team proceeded to look for possible sources of lead
among the remaining waste samples. Scrap was therefore carefully examined
during the last half of the Michigan trip. Wheel rims were noted at the MO
and MS foundries, and at least one lead wheel weight was observed at the MS
foundry, contrary to the plant representative's verbal description of his
scrap*
In general, scrap used by the foundries appeared to be very clean, and in
a number of locations the plant representatives stated that no machine scrap
was being used (i.e., only pig iron, casting returns, and/or pieces of
structural steel).
PROBLEM SAMPLES
At the ML foundry the wet scrubber waste flows immediately out of the
plant via a regulated passage into an open gully, and then into a series of
three connected holding ponds. Waste slag is also sluiced into the gully. It
was expected that the mixed sample (sample #49), taken from the head of the
gully, would be composed almost entirely of the heavier, large slag particles.
The physical appearance of the sample confirmed our expectations. The fine
scrubber waste particulates probably flow down the gully with the wastewater
and settle out in the first or second settling pond. Two liquid samples
(sample #50 and #51) were taken to represent the scrubber waste. The first
sample was taken from the scrubber sluice water (approximately 1 to 2 grams of
settleable solids per gallon sample). The second sample was a composite
liquid sample from the first pond. This composite liquid sample was taken
from the perimeter of the first pond--at a bend in the flow pattern opposite
from the entry point of the sluice water—using the pond sampler and a 1-liter
beaker. It was felt that this sample might indicate what metals were leaching
from the settled scrubber waste* No solid sample was collected from this
foundry since it was not known exactly where the scrubber waste settled out,
and it was felt that sampling at an arbitrary location would not produce a
representative sample.
The solid wet scrubber waste sample from the MU foundry was taken from a
hopper that had been accumulating wet scrubber waste for a month. The most
recent waste (about l/10th of the total) was used in making up the gallon
sample. It was felt that this was the best sample that could be taken, since,
if it took about 30 days to accumulate 10 gallons, a single day's run would
not provide adequate sample size. In addition, the plant representative
stated that the composition of the basic furnace charge was almost always the
same, and that the location of the hopper provided protection from the
elements. There was no way for metals in the scrubber waste to escape from
the hopper.
Some recommendations to be considered for future sampling trips are
listed in Appendix 6.
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SAMPLE SPLITTING AND HANDLING
The foundry waste samples received at EMSL-LV were inspected and
immediately assigned to an individual who became responsible for the custody
of the samples. All transfers of samples were recorded on the appropriate
chain-of-custody forms.
The samples were divided by EMSL-LV personnel into aliquots weighing at
least 450 g each. Each aliquot was assigned a number and was randomly either
given to the in-house contractor, mailed to LFE or the University of
Wisconsin, or added to the secured EMSL-LV sample bank. Appendix 7 lists the
aliquots prepared and their disposition.
Solid samples that were dry enough to be dusty were thoroughly shaken in
the original sample containers. Aliquots of 450 g or more were then portioned
into clean 16-ounce plastic bottles. For some of these samples, two 16-ounce
bottles were required per aliquot. Solid samples that were wet but did not
contain sufficient liquid to allow a liquid/solid separation by draining were
mixed by shaking and squeezing the bottle before removing aliquots.
From solid-liquid samples, the liquid was drained, collected and its
volume measured, and the total weight of the residual solids determined.
Aliquots (>450 g) of the drained solid were weighed into plastic bottles and a
proportional amount of the liquid was returned to restore the original liquid-
to-sol id ratio.
The liquid sample #8 contained a small amount of filtrable solids. The
sample was therefore thoroughly shaken before portioning it into approximately
500-ml aliquots. The samples f50 and #51 contained only a very small amount
of filtrable solids. Both samples were filtered and since the weight of the
solids were <0.5 percent of the sample weights, the solids were discarded and
the filtrates treated as extracts.
On November 21, 1980, aliquots of some of the extracts and digests-
prepared at EMSL-LV by NSI~were sent to LFE and the University of Wisconsin
for analysis. Appendix 8 identifies the extracts and digests shipped.
Extracts #109712 and #109713 were simulated extracts containing 16.0 ppm each
of Pb, Cd, and Cr in 0.7 percent nitric acid.
10
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SAMPLE PREPARATION
SAMPLE EXTRACTION
Under strict chain-of-custody procedures, aliquots of the raw foundry
waste samples were split into 100-g portions and extracted in triplicate by
NSI personnel at the EMSL-LV laboratory facility. The NBS tumbling-type
extractor was used throughout the study. The official Extraction Procedure
(EP) was followed as specified in the Federal Register (45 FR 33127, May 19,
1980) and explained in detail in Section 7 of "Test Methods for Evaluating
Solid Waste," Office of Water and Waste Management, SW-846. A copy of Section
7 of this manual is included as Appendix 9. The extracts were then digested
(as outlined in Section 8 of the above manual) for the metals of interest and
given to EMSL-LV personnel for analysis.
SAMPLE DIGESTION
Aliquots of the raw foundry waste samples were digested in triplicate by
NSI personnel following the procedures detailed in Appendix 10. The digests
were given to EMSL-LV personnel for analysis.
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SAMPLE ANALYSIS
All extracts and digests were screened for 16 elements using inductively
coupled plasma (ICP) emission spectroscopy and then analyzed using atomic
absorption spectrophotometry (AAS) for lead, cadmium and chromium. Where
indicated by ICP data, additional AAS analyses were performed for metals that
exceeded the toxicity characteristic.
SCREENING ANALYSIS USING INDUCTIVELY COUPLED PLASMA (ICP) EMISSION
SPECTROSCOPY
All extracts and digests were screened using ICP spectroscopy for the
following 16 elements: Al, As, B, Be, Ba, Ca, Cd, Co, Cr, Cu, Fe, Mg, Ni, Pb,
V, and In. The EMSL-LV instrument used for these screening analyses was an
Applied Research Laboratories Inductively Coupled Plasma-Optical Emission
Spectrometry instrument with a 27.12 MHz radio frequency generator operated at
1.6 kw. The sample aerosol in this instrument is generated by direct
aspiration into a concentric glass nebulizer. The spectrometer used with the
plasma excitation source has a 1-meter optical focal length and employs
photomultiplier tube detectors for each analytical spectral line. The
analyses were conducted in accordance with manufacturer's recommendations for
operation of the instrument. For ICP measurements single pass analyses were
conducted where one pass consisted of calibration plus measurements on each
solution. A Digital Equipment Corporation POP 11/10 mini-computer was used
for data handling and control of the ICP-OES during analysis. The software
allows for up to a third order polynomial definition of the calibration curve.
This software also permits corrections for interfering element spectral lines
(limited to the monitored elements) as well as for stray light created within
the spectometer.
ANALYSIS USING ATOMIC ABSORPTION SPECTROPHOTOMETRY (AAS)
All extracts and digests were analyzed for lead, cadmium and chromium
(and in some cases other elements) with an automated Perkin-Elmer Model 603 AA
spectrophotometer. The procedures used are detailed in Section 8 of "Test
Methods for Evaluating Solid Waste", EPA, Office of Water and Waste
Management, SW-864. The AAS was equipped with a microprocessor and an
automatic sample introduction system. It was interfaced with a PDP-11
computer for conventional flame analysis of fluids suitable for aspiration; it
was also equipped with a deuterium background corrector which can compensate
for non-analyte absorption. This was a screening-type analysis, and the
method of additions was not used.
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-------
Whenever the results of the AAS screening analysis of an extract
indicated that the amount of cadmium, chromium or lead in the extract exceeded
the criteria levels of 1, 5 and 5 mg/1s respectively, another aliquot of the
same raw sample was extracted and analyzed for confirmation using the method
of additions*
' 13
-------
QUALITY ASSURANCE
Each sample location was described and a schematic drawing of the
sampling site entered Into a hard-bound field log book with tear-out duplicate
pages for carbon copies. The sample descriptions included the time and date
of collection, exact location, name of sampler and type of sample. The carbon
copies were sent with the samples to EMSL-LV. All samples were shipped to
EMSL-LV via air carrier (Federal Express). The solid samples were sent in
1-gall on cubitainers with corrugated cardboard packaging; liquid samples were
sent in plastic 1-gallon bottles packaged in plastic bags and placed in a
wooden box (DOT 19-A-070) cushioned with vermiculite.
All information pertaining to sample splitting, extraction and digestion
was recorded in bound laboratory notebooks. All samples, extracts and digests
were kept under chain of custody at all times. A copy of the chain-of-custody
form is shown as Appendix 11. Aliquots of all raw waste samples shipped to
EMSL-LV (except for the liquid samples #50 and #51) were, at the request of
the American Foundrymen Society, sent to the University of Wisconsin for
independent analysis. Twelve raw waste samples, including three blind splits,
were sent to LFE, an independent contractor, for extraction, digestion and
analysis. Eight out of the 36 solid waste samples extracted, digested and
analyzed at EMSL-LV were blind splits. The analytical results from these
blind splits are included in Table 1 and Appendices 12 and 13.
Aliquots of nine extracts and nine digests prepared at EMSL-LV, as well
as one simulated extract, were sent to LFE and the University of Wisconsin for
independent analysis (see Results and Discussion).
The splitting of samples, extracts and digests was performed by an
independent quality assurance team that was in no other way involved in the
study. All samples, including all duplicates, were therefore "blind" to the
sample preparation team, the analytical team and the contractor.
All extractions and digestions were performed in triplicate. As part of
the AAS analytical procedure, a standard was routinely analyzed every ten
samples. Filtration blanks were run to determine the effectiveness of
filtration equipment cleaning.
Extracts, digests and reagent blanks were analyzed with a single pass
procedure for TCP measurements and with a double pass procedure for AA
measurements. One analysis pass consisted of calibration plus measurement on
each solution.
14
-------
TABLE 1. SUMMARY OF ATOMIC ABSORPTION SCREENING ANALYSES OF WASTE
EP EXTRACTS AND WASTE DIGESTS*
Field Waste
Foundry Sample Aliquot
Code Number Number
EP Extraets (mg/1)
Hasttt (mg/kg.)
Cadmium
Chromium
Lead
GadnriuB
Chromium
Lead
PA
PA
PB
PS
PC
PC
PD
PD
PE
PE "
PE
PF
PF
PG
PH
PI
MJ
MK
MKK
MKK
MKK
ML
ML
MM
1
2
6
8
1085
1053
1002
1006
12 1035
12 SP 1042
16 1068
16 SP 1075
19 1027
19 SP 1033
20 1064
1045
1059
1077
1022
1016
1101
1211
1108
46 1115
46 SP 1122
50* 1123
51* 1124
52 1125
22
24
28
34
36
40
42
44
0.026 * 0.004 0.06 ± 0.006
0.014 * 0.003 0.06 £ 0.001
1.091 * 0.003 0.07 * 0.001
0.010 * 0.006 BO
0.015 * 0.003 0.06 ± 0.008
0.007 £ 0.001 0.07 ± 0.002
1.012 £ 0.001 0.07 t 0.006
0.926 £ 0.016 0.06 $ 0.004
0.013 t 0.002 0.07 t 0.001
0.012 ± 0.001 0.07 £ 0.004
0.015 ± 0.009 0.07 t 0.005
0.006 t 0.001 0.07 ± 0.003
0.027 ± 0.002 0.07 t 0.002
0.081 ± 0.007 0.07 £ 0.003
1.683 t 0.028 0.07 t 0.005
0.021 t 0.000 0.07 t 0.003
0.022 £ 0.002 0.10 t 0.006
0.557 £ O.OOS 0.05 t 0.003
1.319 £ 0.102 0.10 t 0.006
0.023 ± 0.012 0.07 £ 0.002
0.024 t 0.002 0.09 t 0.01
0.215
0.011
2.013 ± 0.248
31 £ 3 2140 ± 40
72 £ 4 180 t SO
38 ± 1 20770 £ 370
BO 30
193 £ 40 360 t 60
227 £ 9 340 £ 80
43 £ 0.9 18810 £ 2010
43 £ 0.9 17520 £ 100
33 £ 6 9680 £ 250
360 £ 430
980 £ 30
30 £ 0.7
3.1 £ 0.7 4.3 £ 0.6
0.6 £ 0.2 1.0 £ 0.0
23.8 £ 0.8 79.9 £ 0.9
BO 30
0.2 £ 0.04 3.0 £ 0.6
0.2 £ 0.03 2.3 £ 0.3
109 £ 7 35.0 £ 0.9
120 £ 1 31.3 £ 0.3
0.5 £ 0.1 3.3 £ 0.6
0.4 £ 0.04 4.3 £ 2.6 36 £ 7
0.5 £ 0.3 4.3 £ 0.3 40 £ 1
0.2 £ 0.2 1.0 £ 0.0 26 £ 2
0.2 £ 0.02 6.3 £ 0.3 75 £ 2 290 £ 4
10.2 £ 2.2 20.0 £ 2.9 78 £ 2 13030 £ 560
10.4 £ 1.5 79.4 £ 0.9 1186 £ 3 10260 £ 20
0.5 £ 0.05 3.2 £ 0.3 133 £ 3 950 £ 50
0.8 £ 0.1 4.3 t 0.2 159 £ 13 680 £ 30
0.8 £ 0.04 42.2 £ 0.6 165 £ 4 2650 £ 130
1.7 £ 0.4 134.1 £ 1.9 1548 £ 24 6210 £ 170
80 3.6 £ 0.5 426 £ 57 100 £ 40
0.2 £ 0.03 3.7 £ 0.1 392 £ 42 110 £ 20
0.05 0.2 —* —* —*
0.07 0.4 —* —* —*
0.11 £ 0.02 25.5 £ 5.7 1063.7 £ 6.4 148 £ 11 29630 £ 1170
(continued)
* Average and standard deviation values are shown for triplicate portions prepared and measured at
EPA-Las Vegas.
t Amounts of metals released from the wastes by the digestion procedure employed.
* No digestion was performed since waste contained <0.5% flltrable solids.
BO » mg/1 values for extracts below 0.004 for Cd, 0.03 for Cr and 0.05 for Pb; 100 x these values
for mg/kg 1n wastes.
SP - Blind splits.
15
-------
TABLE 1. (Continued)
Foundry
Code
MM
MN
MNN
MNN
HO
NP
MQ
MR
MR
MR
MR
MS
MT
MU
Field
Sample
Number
54
54 SP
56
56 SP
58
60
64
66
66 SP
68
68 SP
70
74
78
Waste
AH quo
Hunter
1132
1139
1140
1147
1148
1156
1164
1171
1178
1179
1186
1187
1195
1203
Cadmium
0.293 t 0.053
0.243 * 0.015
0.015 * 0.006
0.015 £ 0.001
0.019 £ 0.004
0.062 £ 0.020
0.007 £ 0.001
2.279 £ 0.111
2.220 t 0.085
0.046 t 0.002
0.062 ± 0.030
0.598 £ 0.057
0.010 t 0.001
0.034 £ 0.0006
EP Extracts (mg/1)
Chromium
0.06 ± 0.004
0.07 t 0.02
0.06 t 0.008
0.14 £ 0.13
0.06 ± 0.002
0.11 t 0.009
0.06 t 0.001
0.80 ±0.06
0.86 t 0.002
0.29 t 0.007
0.33 £ 0.005
0.09 ± 0.008
0.06 ± 0.004
0.05 £ 0.003
Lead
20.4 £3.8
9.4 £ 0.4
0.6 t 0.09
0.6 £ 0.1
0.2 t 0.03
2.3 t 0.3
BO
BO
BO
BO
BO
12.6 ± 1.4
0.4 t 0.02
BO
Cadmium
17.1 t 0.6
15.5 t 0.9
2.1 £ 0.0
8.5 t 0.1
2.3 t 0.2
7.5 t 0.0
2.9 ± 0.2
178.9 £ 8.3
173.7 ± 11.5
8.1 £ 0.2
8.2 t 0.2
116.4 ± 7.1
7.5 ± 1.1
3.0 £ 0.0
Waste* (rag/kg)
Chromium
71 * 1
74 t 7
108 ± 6
322 t 3
76 t 2
301 t 36
105 £ 2
2786 £ 231
2671 ± 72
2210 £ 327
2178 £ 47
131 £ 2
148 £ 9
122 £ 10
Lead
2630 £ 20
2370 t 90
370 £ 30
790 £ 30
250 £ 30
1950 £ 140
90 £ 4
390 £ 3
380 £ 20
440 £ 20.
450 £ 3
3540 £ 330
1920 £ 50
440 £ 50
* Average and standard deviation values are shown for triplicate portions prepared and measured at
EPA-Las Vegas.
t Amounts of metals released from the wastes by the digestion procedure employed.
BO » mg/1 values for extracts below 0.004 for Cd. 0.03 for Cr and 0.05 for Pb; 100 x these values
for mg/kg 1n wastes.
SP - Blind splits.
Three types of standards were used at EMSL-LV for this project:
1. Spex Industries Mixed Standards for TCP calibration
2. Fisher Atomic Absorption Standard Solutions for AA calibration.
These standards were also used to prepare spikes for extracts and
digests.
3. NBS Standard Reference Material (SRM 1633) Coal Fly Ash, certified
for several elements including Cd, Cr, and Pb, to evaluate the
efficiency and precision of the extraction and digestion procedures,
Instruments were calibrated daily when analyses were conducted.
Whenever the AAS screening analysis of an extract produced values for
cadmium and/or lead that were above the criteria levels, another aliquot of
the same raw waste sample was extracted and analyzed for confirmation by the
method of standard additions (see Results and Discussion).
16
-------
Extract data are reported as mg/1, the units used in the hazardous waste
criteria level for toxicity specified in the Federal Register (45 FR 33127,
May 19^ 1980} for the Extraction Procedure. Digest d^ta^are^r?ported^as mg/]cg
of dry~sampfe material to allow convenient estimates ToT~tM~massT of an
5.1.enieniL£_Qntained in a given load of the solid waste. The concentrations_in_
the extract and digest solutions are not directly comparable because the ratio
of final liquid volume to solid wgight is £0/1 or more for the extracts and
100/1 for the digests. Furthermore, an EP extract is, according to the
definition in the Federal Register quoted above, either the undiluted filtered
liquid portion of a waste containing less than 1/2 percent of filtrable solids
(examples in this study are samples #50 and #51), or the actual EP extract
combined with any liquid that was separated from the sample by filtration
before the extraction step. The digestion, however, was always performed on
the total solids of the dried samples.
17
-------
RESULTS AND DISCUSSION
All extracts and digests were screened for 18 elements using ICP
spectroscopy. The screening results for the extracts and digests are
tabulated in Appendices 12 and 13, respectively. Neither the barium nor the
arsenic concentrations in the extracts exceeded 50 percent of the criteria
levels (100 and 5 mg/1, respectively), even without background correction, so
no attempt was made to analyze for these two elements using AAS.
All extracts and digests were analyzed for cadmium, chromium and lead
using AAS without use of the method of additions. The results for the
extracts and digests are listed in Table 1. The extracts from the field
sample numbers 6, 16, 34, 44, 52 and 66 exceeded the critical concentrations
for cadmium of 1 mg/1, and the extracts from the field samples numbers 6, 16,
28, 34, 52, 54 and 70 exceeded the limit for lead (5 mg/1). None of the
extracts exceeded the limit for chromium. The analytical results from the
aliquots of the raw waste samples sent to the University of Wisconsin (36) and
to LFE (12) are tabulated in Appendix 14. The same wastes identified as
hazardous by the University of Wisconsin and LFE had also been identified as
hazardous at the EMSL-LV. Differences between the values in Table 1 and
Appendix 14 are at least in part the result of sample inhomogeneity.
The concentrations of cadmium, chromium and lead in the digests are often
three orders of magnitude higher than those in corresponding EP extracts.
However, these numbers cannot be directly compared as was explained earlier.
To allow for an easier comparison, the amounts of cadmium, chromium and lead
extracted from the samples using the EP are listed in Table 2 as percentages
of the amounts found in the digests.
In order to confirm these results, fresh aliquots of the wastes with the
above field sample numbers were extracted using the EPA Extraction Procedure,
the extracts were digested and the digests analyzed for cadmium, chromium and
lead. The results are listed in Table 3. The 95 percent confidence intervals
for the unspiked extract values in Table 3 can be obtained by multiplying the
standard deviation values by 4.30 according to the method of additions
procedure in Statistical Theory and Methodology of Trace Analysis. Liteanu, C.
and Rica, I., John Wiley and Sons, 1980, pp. 162-166. All lead and cadmium
values except one (cadmium in sample #16) were confirmed to exceed the
criteria levels.
The occasional large difference between the screening and the
confirmatory AAS values is due to the variation between aliquots of the same
field sample. This variation is not surprising since many of these wastes
were heterogeneous and difficult to mix, as had been explained earlier.
Mixing techniques that change the particle sizes (e.g., grinding and milling)
18
-------
TABLE 2. PERCENTAGE OF CADMIUM, CHROMIUM AND LEAD EXTRACTED FROM THE
RAW WASTES BY THE EP*
Foundry
Code
PA
PA
P&
PB
PC
PC
PD
PD
PE
PE
PE
PF
PF
PG
PH
PI
MJ
MK
MKK
MKK
MKK
ML
ML
MM
MN
MN
Field
Sample
Number
1
2
6
8
12
12
16
16
19
19
20
22
24
28
34
36
40
42
44
46
46
50
51
52
54
54
Waste
Aliquot
Number
1085
1053
1002
1006
1035
1042
1068
1075
1027
1033
1064
1045
1059
1077
1022
1016
1101
1211
1108
1115
1122
1123
1124
1125
1132
1139
Percentage Extracted
Cadmium
12 t 2
28 ± 6
27,3 i 0.08
I
10 ± 2
6 ± I
57.8 ± 0.06
59.2 ± 1
7.9 ± 1.2
5.0 ± 0.4
7.0 ± 4.2
10 ± 2
7.9 ± 0.6
8.1 ± 0.7
42.4 ± 0.7
13 ± 0
10 ± 0.9
26.4 ± 0.2
19.67 ± 1.52
13 ± 7
13 ± 1
I
I
3.78 ± 0.47
34.3 ± 6.2
31.4 ± 1.9
Chromium
2 ± 0.2
2 ± 0.03
2 ± 0.02
I
0.6 ± 0.08
0.6 ± 0.02
3 ± 0.3
3 ± 0.2
4 ± 0.06
4 ± 0.2
4 ± 0.2
5 ± 0.2
2 ± 0.05
2 ± 0.08
0.1 i 0.008
1 ± 0.04
1.2 ± 0.08
0.6 ± 0.04
0.13 ± 0.008
0.3 ± 0.009
0.4 ± 0.05
I
I
1.5 ± 0.3
2 ± 0.1
2 ± 0.5
Lead
2.9 ± 0.6
7 ± 2
2.3 ± 0.08
I
1 ± 0.2
1 ± 0.2
11.6 ± 0.7
13.7 ± 0.1
0.1 ± 0.02
0.9 ± 0.09
1 ± 0.6
10 ± 10
1 ± 0.1
1.56 ± 0.34
2.03 ± 0.29
1 ± 0.1
2 ± 0.3
0.6 ± 0.03
0.55 ± 0.13
I
4 ± 0.5
I
I
1.72 ± 0.38
15.5 ± 2.9
7.9 ± 0.3
(continued)
* Based on AA Data from Table 1 after conversion of the
EP values to mg/kg basis.
I indicates insufficient data (concentrations below detection limits).
19
-------
TABLE 2. (Continued)*
Foundry
Code
MNN
MNN
MO
MP
MQ
MR
MR
MR
MR
MS
MT
MU
Field
Sample
Number
56
56
58
60
64
66
66
68
68
70
74
78
Waste
Aliquot
Number
1140
1147
1148
1156
1164
1171
1178
1179
1186
1187
1195
1203
Percentage Extracted
Cadmium
14 ± 6
3.5 i 0.2
16 ± 4
16 i 5
5 ± 0.7
25.48 ± 1.24
25.56 ± 0.99
11 ± 0.5
15 ± 7
10.3 ± 1.0
2.7 ± 0.3
23 ± 0.4
Chrorni urn
1 i 0.1
0.87 ± 0.81
2 ± 0.05
0.73 ± 0.06
1 ± 0.02
0.57 ± 0.04
0.64 ± 0.002
0.26 ± 0.01
0.30 ± 0.005
1 ± 0.1
0.8 ± 0.05
0.8 ± 0.05
Lead
3 ± 0.5
2 ± 0.2
2 ± 0.2
2.4 ± 0.3
I
I
I •
I
I
7.12 ± 0.79
0.4 ± 0.02
I
* Based on AA Data from Table 1 after conversion of the EP values to mg/kg
basis.
I indicates ^sufficient data (concentrations below detection limits).
could not be used since breaking up the particles would most likely change the
Teachability characteristics of the material.
To verify our analytical results, aliquots of digested extracts that
exceeded the critical concentrations for cadmium, lead or both, were sent to
LFE and to the University of Wisconsin for analysis. Three portions of each
sample aliquot had been extracted; an aliquot of one of these extracts (per
sample) was sent to each laboratory. A list of these extracts is included in
Appendix 9. It should be noted that for identification of the waste aliquots
only the first five digits should be compared. Tables 4 to 7 list the LFE
data, the University of Wisconsin data, and the corresponding EMSL-LV values.
Samples #QC-109712 and #QC-109713 were simulated extracts (containing 16 ppm
each of cadmium, chromium and lead in 0.7 percent HN03) that were transferred
to the LFE, University of Wisconsin and EMSL-LV analysts as blind samples.
The reason that the EMSL-LV values in Tables 4 to 7 are not identical to those
in Table 1 is that Table 1 lists averages of the values from extracts of three
different extractions of the same waste, whereas the values reported in Tables
4 to 7 are in each case only one of the values that were used to get the
average value.
20
-------
TABLE 3. CONFIRMATORY ATOMIC ABSORPTION ANALYSES OF EP EXTRACTS1'2
Field Waste
Foundry Sample Aliquot
Code Number Number
PS 6 1004
P? £ 100*
PS € 1004
PB 16 1076
PD 16 1076
PD 16 1076
PG 28 1081
PG 28 1081
PG 28 1081
PH 34 1023
PH 34 1023
PH 34 1023
MKK 44 1112
MKK 44 1112
MKK 44 1112
Element
Cadmium
Chromium
Lead
Cadmium
Chromium
Lead
Cadmium
Chromium
Lead
Cadmium
Chromium
Lead
Cadmium
Chromium
Lead
(Jnsplked
Readl ng
0.220
0.03
9.7
0.178
BO
17.7
0.026
BO
2.3
0.362
0.04
3.3
0.290
0.04
BO
Spike
Level
(mg/1 )
0.500
0.750
1.000
2.50
4.00
5.00
5.0
7.5
10.0
0.500
0.750
1.000
2.50 .
4.00
5.00
5.0
7.5
10.0
0.500
0.750
1.000
2.50
4.00
5.00
5.0
7.5
10.0
0.500
Oo750
1.000
2.50
4.00
5.00
5.0
7.5
10.0
0.500
0.750
1.000
2.50
4.00
5.00
5.0
7.5
10.0
Spiked
Reading —
0.719
0.970
1.225
2«73
4.39
5.54
15.0
17.5
20.0
0.676
0.921
1.177
2.66
4.20
5.30
22.7
25.2
27.6
0.521
0.771
1.024
2.67
4.25
5.37
7.5
10.2
12.7
0.861
1.106
Ic365
2.68
4.28
5.40
3.9
11.5
14.2
0.781
1.036
1.291
2.65
4.21
5.36
5.4
8.1
10.6
Spike
Recovery
ft)
100
100
100
10?
109
110
105
104
103
100
99
100
106
105
106
101
101
99
99
99
100
107
106
107
103
104
103
100
99
100
106
106
107
103
103
104
98
100
100
104
104
106
108
108
106
Undiluted
Extract
(mg/T)-
1.089
47.3
0.888
BO
89.3
0.123
BO
11.0
1.802"
0.12
18.1
1.432
0.10
Std.
0«v.
0.015
0.9
0.017
•«•
0.7
0.012
— -
0.3
0.031
0.13
0.4
0.035
0.21
BO —
(continued)
ifhe deuterim background corrector was not used for the chromium analyses because of inherent
corrector limitations and because the EP extract chromium concentrations are below the
hazardous waste criteria even without background correction. Readings were made on extracts
diluted 5-fold per SW-846.
2BD Indicates values below the detection limits of 0.005 mg/1 for Cd, 0.025 mg/1 for Cr and 0.47
mg/1 for Pb. Lower detection limits for Pb are obtained when background corrector 1s not used.
21
-------
TABLE 3. (Continued)
Field Haste
Foundry Sample Aliquot
MM 52 1130
MM 52 1130
MM 52 1130
MN 54 1139
MN 54 1139
MN 54 1139
MR 66 1171
MR 66 1171
MR 66 1171
MS 70 1193
MS 70 1193
MS 70 1193
Unsplked
Element Reading
CadariuH 0.848
Chromium BO
Lead 7.8
Cadmium 0.073
Chromium 80
Lead 2.31
Cadmium 0.548
Chromium 0.22
Lead BD
Cadmium 0.079
Chroml urn . BO
Lead 1.5
Spike
Level
(mg/1)
0.500
0.750
1.000
2.50
4.00
5.00
5.0
7.5
10.0
0.500
0.750
1.000
2.50
4.00
5.00
5.0
7.5
10.0
0.500
0.750
1.000
2.50
4.00
5.00
5.0
7.5
10.0
0.500
0.750
1.000
2.50
4.00
5.00
5.0
7.5
10.0
Spiked
Reading
1.344
1.601
1.858
2.64
4.22
5.38
12.7
15.4
17.9
0.572
0.817
1.076
2.60
4.20
5.26
8.2
10.6
13.2
1.045
1.297
1.556
2.77
4.32
5.40
5.0
7.7
10.4
0.568
0.820
1.076
2.69
4.33
5.45
6.8
9.3
11.8
Spike
Recovery
99
100
101
106
106
108
100
101
102
100
99
100
104
105
105
107
103
103
99
100
101
102
103
104
100
103
104
98
99
100
108
108
109
106
104
103
Undiluted
Extract Std.
(mg/1) Dev.
4.184 0.051
BO
38.3 0.9
0.358 0.023
BD
13.8 0.69
2.709 0.038
0.99 0.13
80
0.379 0.029
BO
7.5 0.5
line deuterium background corrector MBS not used for the chromium analyses because of Inherent
corrector limitations and because the EP extract chromium concentrations are below the
hazardous waste criteria even without background correction. Readings were made on extracts
diluted 5-fold per SW-846.
2BD indicates values below the detection limits of 0.005 mg/1 for Cd, 0.025 mg/1 for Cr and 0.47
mg/1 for Pb. Lower detection limits for Pb are obtained when background corrector 1s not used.
22
-------
__ —-—.-- | rtDfefcrr^T » UUnrnf\A j«Jll ur ur L. i_/\ i r\nv» i o rvi un i n n>jLJ rt — **rt*t+t- *n---ftrrt_rr-_-- _-.. -_-
Foundry Waste
+ Sample Aliquot
Code Number
PB6 100222
PD16 106822
PG28 107732
PH34 102212
MKK44 110831
MM52 112511
MN54 113231
MR66 117111
MS70 118711
Linear Regression
Slope *
Intercept »
Corr. Coeff. 3
QC STD 109711
True Value =
Agreement =
LFE Data (rag/1)
Cadmi urn
1.00
0.85
0.06
1.57
1.26
1.75
0.30
2.04
0.61
0.946
±0.018
-0.029
±0.023
0.9988
14.6
16.0
91%
Chromi urn
0.06
0.06
0.10
0.12
0.08
0.11
0.06
0.87
0.09
1.007
±0.029
0.003
±0.009
0.9971
16.4
16.0
102%
Lead
24.4
115
8cO
11.4
2.2
21.5
22.4
<0.2
13.6
0.990
±0.003
0.109
±0.134
0.9999
16.0
16.0
100%
EMSL-LV Data (mg/1)
Cadmi urn
Ie088
1.011
0.074
1.692
1.386
1.852
0.327
2.166
0.661
16.2
16.0
101%
Chromi urn
0.07
0.07
0.07
0.08
0.10
0.10
0.06
0.86
0.10
16.2
16.0
101%
Lead
24.4
116
7.7
11.3
2.0
21.4
22.9
<0.05
14.1
16.6
16.0
104%
An attempt was made to correlate high extract values for cadmium and/or
lead with the type of furnace, scrubber and charge (as reported by the
foundries in the questionnaires). Those variables are displayed in Table 8.
All extracts from the three wastes produced by the electric arc process
exceeded the limit for cadmium and one of them also for lead, although the
composition of the charges used by the three foundries varied widely. Only 3
23
-------
TABLE 5. COMPARISON OF LFE DIGESTS AA DATA WITH EMSL-LV DATA
Foundry
+ Sample
Code
PB6
PD16
PG28
PH34
MKK44
MM52
MN54
MR66
MS70
Waste
Aliquot
Number
100241
106861
107753
102251
110841
112561
113251
117151
118761
LFE
Cadmium
73
31
21
72
118
958
15
168
100
Data (mg/kg)
Chromi urn
154
69
151
1,770
1,480
164
71
2,680
135
EMSL-LV Data
Lead
21,800
19,000
13,800
10,500
6,720
31,500
2,650
390
3,480
Cadmium
80.1
34.0
23.0
78.6
132
1,070
17.7
180
110
(mg/kg)
Chromium Lead
89
44
80
1,183
1,525
159
70
2,863
130
20,500
19,200
12,700
10,300
6,120
30,100
2,630
. 390
3,350
Linear Regression
Slope »
Intercept »
Corr.
Coeff . =
0.895
±0.002
1.359
±0.937
0.9999
0.968
±0.080
80.6
±92.6
0.9840
1.040
±0.018
31
±265
0.9990
of 15 wastes from the Venturi-type scrubbers exceeded the limit for lead (and
in one case for cadmium) whereas six out of eight wastes collected with the
baghouse system exceeded the limit for one or both of these elements. The
extract from the waste of the MS foundry where lead-weighted wheels were noted
among the scrap exceeded the limit for lead by 50 percent. However, no
correlation could be found between the charges used (as reported by the
foundries) and the levels of cadmium and lead in the extracts.
24
-------
TABLE 6. COMPARISON OF
Foundry Waste
+ Sample Aliquot
Code Number
PB6 100223
PD16 106823
PG28 107733
PH34 102213
MKK44 110833
MM52 112513
MN54 113233
MR66 117113
MS70 118713
Linear Regression
Slope »
Intercept 3
Corr. Coeff. =
QC STD 109711
True Value =
Agreement =
• UNIVERSITY OF WISCONSIN EXTRACTS AA D
WITH EMSL-LV DATA
W1 cons in Data (mg/1)
Cadmium
1.04
1.01
0.07
1.63
1.34
1.78
0.33
2.23
0.66
1.009
±0.021
-0.015
±0.027
0.9985
16.2
16.0
101%
•••••••••••••^••^••••••••l
Chromi urn
<0.07
<0.07
<0.07
<0.07
<0.07
<0.07
<0.07
0.58
<0.07
a
ea 20
16.0
ca 125%
••••••••••^•••^••^MMHWM
Lead
22.6
102
8.4
11.6
2.3
20.7
22.5
<0.6
14.0
b
0.949
±0.036
0.767
±0 .589
0.9964
16.7
16.0
104%
••••••••••••••^•i^^^BB^H
EMSL
Cadmium
1.082
0.997
0.074
1.678
1.354
1.810
0.327
2.148
0.661
16 c2
16.0
101%
•^••••••^••^•HHMim
-LV Data
Chromi
0.07
0.07
0.07
0.08
0.10
0.10
0.06
0.83
0.12
16.2
16.0
101%
ATA
(mg/1)
urn Lead
24.0
116.1
7.3
11.7
2.0
20.6
22.0
<0.05
14.3
16.6
16.0
104%
alnsufficient data for regression analysis
"Highest concentration pair (Waste PD16) not included.
25
-------
TABLE 7. COMPARISON OF UNIVERSITY OF WISCONSIN DIGESTS AA DATA
WITH EMSL-LV DATA
Foundry
+ Sampl
Code
PB6
PD16
PG28
PH34
MKK44
MM52
MN54
MS70
Linear
Waste
e Aliquot
Number
100243
106863
107753
102253
110843
112563
113253
118763
Regression
Slope =
Intercept =
Corr. Coeff. =
Wisconsin Data
Cadnri urn Chromi
79
32
20
77
129
E
16
112
1.013
±0.016
-2.343
±1.278
0.9994
(mg/kg)
urn Lead
20,300
18,700
13,300
9,900
6,400
29,400
2,600
3,300
0.970
±0.017
302
±291
0.9992
EMSL-LV
Cadmi urn
80.1
34.0
23.0
78.6
132
1,070
17.7
110
Data
Chromi
89
44
80
1,183
1,525
159
70
130
(mg/kg)
urn Lead
20,500
19,200
12,700
10,300
6,120
30,100
2,630
3,350
E Indicates concentration that exceeded calibrated range.
26
-------
TABLE 8. FURNACE CHARGES USED (
Foundry Code PA PB PC PD PE .
Cast borings
Cast Iron briquet 10
Gates 35 20 10 10
Own returns 35 5 10 10 55
Pig Iron 25 35 30
Scrap castings 20 5 10 4
Steel bushllng
Steel forglngs
Steel rail 7 15
Crankshafts
Motorblock 1
£J Crushed auto
Plate steel 1 7
Structural steel 27 6
Punching* 1
Stampings
Cast Iron 20 23 5
"Country" cast
Cupola cast 23
Machine scrap 25 23
Other 4
Furnace type C C C C C
Scrubber type V B/Q V B B/Q
Positives Pb.Cd Pb
* No Information available
C » Cupola, EA - Electric Arc, V - Venturl,
In % of Total), AS REPORTED BY THE FOUNDRIES IN IHE QJEST1
PF PG PH P! MJ MK
5 15 10 10
60 5 15 11 10 10
20 20 15 26 50
10 11 10
5
5
20 5
10
10 30 15 10
5
5
25 5
5
5
10 11 26 10
11
11 5
11 26
15
C C EA C C C
B/Q V/Q B V V V/Q
Pb Pb.Cd
B » Baghouse, Q » Quencher
MKK ML MM* MN HNN MQ HP MJ) 'MR
50
1 15 25
)NNAIRES
MS MT MU
3.5 15 20 14.5 20 10
3.5 15 15 22 14.5 40 60 45 25 25 5
17.5 15 37 19 10 40 25 14 25
3.5 7 14.5 12
3.5 5
3.5 15
3.5 10
3.5 8 14.5 10
3.5
3.5 5 2 4.S 13
3.5 5 2 4.S 16
3.5 5 4.5 " 17
3.5 5 12
3.5 58 15 2 4.5
2
3.5
2 14.5
1.5 5 12
EAC C C C C C C EA
B V/Q V/Q V/Q V/Q V/Q V V/Q B
Cd Pb,Cd Pb £<$
>
45
48
10
C C C
B V V/Q
Pb
'
-------
APPENDIX 1
QUESTIONNAIRES DISTRIBUTED TO THE GRAY IRON FOUNDRIES TO BE SAMPLED
GRAY IRON FOUNDRY STUDY: BACKGROUND INFORMATION
Name of company
Name of foundry visited
Street address
Person and mailing address
for sending back reports
Name of person providing
information
Title
Telephone number
28
-------
QUESTIONS
Questions _ Contractor's Comments
a. What type of furnace(s) is(are) used |
to melt tht furnace charge for grey iron i
castings? |
b. What other alloys or products are melted
in the furnace?
2. What type of air pollution control device
is used on the furnace(s)? (Check appro-
priate answer(s) below.,)
a. Dry (Baghouse): (If checked,
please answer the following
questions.)
i. How is dust from the baghouse
disposed of?
Landfilled as dust
Wetted down before land-
filled
Mixed with plant wastewater
(If checked, at what point
in your flow chart?)
Mixed with wastewater sludge
Other. (Please specify)
ii. How many pounds of emission control
dust are generated per ton of
metal produced?
b. Wet (Scrubber): (If checked,
please answer the following
questions.)
29
-------
-Questions Contractor's Comments
i. How is wastewater from the furnace
scrubber treated:
Treated separately from
other process waste streams
Treated then mixed with other
process waste streams
Mixed with other process
waste streams, then treated
Other. Please specify:
ii. Type of wet scrubber (e.g., Venturi,
Wet Cap)
111. How is the sludge from the wastewater
treatment process disposed of?
Landfilled separately
Mixed with other foundry
wastes, then landfilled
Other. (Please specify.)
3. a. What type of scrap is normally used for
the gray iron? (Please check any of
the following which are used.)
a. Cast borings
b. Cast iron briquettes
30
-------
Questions Contractor's Comments
c« __ Free
do _„___„, Gates
e. _ Own returns
' -
f. ___ P1g iron
9« _— . Scrap casting
h. , _ __ Steel bus hi ing
i • _______ Steel forgi ngs
j. _ Steel rail
k. _ Crankshafts
-
1 . _ Motorbl ock
m. _ Crushed autobodies
n. _ Plate steel
-
o. _ Structural steel
-
p. _ Punchings
q. _ Stampings
r. _ _ Cast iron scrap
s. _ "Country Cast" (from farm
machinery)
t. _ "Cupola Cast" (from iron
scrap)
u. _ Machine Scrap
_ Other. (Please specify.)
b. Please list the percentage used of
each of the above scrap types for the
last four days:
31
-------
Questions Contractor's Comments
Day 1
Day 2
Day 3
32
-------
-Questions — Contractor's Comments
I I
Day 4
4. Do you expect any of your scrap to
contribute significant amounts of either
cadmium, chromium, lead, zinc, tin or
other nonferrous metals to your waste
{i.e., emission control dusts or waste-
water treatment sludges)? If so, which
components and which metals?
5. What data do you have on the chemical composi-
tion of your waste?
With the exception of any "Contractor's Comments" above, I certify
that the information I have provided above on the above-named gray
iron foundry is accurate and correct to the best of my knowledge.
Signed Date
(signature of person providing
information)
33
-------
APPENDIX 2
SEQUENCE OF EVENTS ASSOCIATED WITH THE SAMPLING OF EACH FOUNDRY
1» Prepare chain of custody forms, EPA questionnaries, labels, envelopes.
2. Select and prepare sampling clothing and equipment.
3. Drive to sampling site.
4. Make presentation and hand questionnaire to foundry personnel. Discuss
with foundry representatives what samples are to be taken. Have plant
representative sign the chain-of-custody forms.
5. Don sampling clothing, select and prepare sampling equipment for
transport.
6. Sampling:
a. Decide on sampling pattern.
b. Fill sample container (one person takes the sample, while the second
person holds (and shakes) the container).
c. Record sampling procedure, pattern (including dimensions) and
miscellaneous observations in the logbook. Fill out the sample
label.
d. Wipe off the outside of the sampler container. Put the label on the
container. Clean sampling equipment (at least dry wipe).
7. Repeat sampling procedure 6 at each sampling location. This usually
includes taking one sample, in a one-gallon container, of dry or wet
scrubber waste, and one sample, in a one-gallon container, of mixed
waste.
8. Transport the closed containers back to the transport vehicle (van).
9. Remove sampling clothing. Put sampling clothing and equipment in plastic
bags. Complete logbook entries.
10. Drive to freight shipping location for samples to be shipped.
34
-------
11. Place chain-of-custody form and daily field logbook sheets in a sealed
envelope. Place envelope in the inside on the top of the shipping box,
12. Seal caps on sample container(s) with EPA chain-of-custody tape.
13. Fill out Federal Express shipping and Tally Record Service forms,
14. Cubitainers are shipped 1n cardboard boxes. Liquid to semlliquid samples
are shipped in wide-mouthed bottles in wooden crates containing vermic-
ulite, and lined with a plastic bag.
List of Essential Sampling Equipment
1. 2 Hardhats
2. 2 Pairs of Boots
3. 2-3 Pairs of Coveralls
4. 2 Pairs of Goggles
5. Brush
6. Labels
7. Envelopes
8. Pens (indelible) :
9. Box Wrap Tape and Chain-of-Custody Tape
10. Cubitainers (1-gallon size)
11. Glass Bottles with Lids (1-gallon size)
12. Cardboard Shipping Boxes for Cubitainers
13. Special Wooden Crates for Shipping Glass Bottles
14. Paper Towels
15. Trowel and Funnel
16. Gloves - green (powdered inside, tight) latex, and larger, opaque white
17. Plastic Bags
18. Duffle Bag
35
-------
Checklist for Packing Samples for Shipment
4-.—tabe4-sample container.
2. Seal Hd with cha 1n-of-custody tape.
3. Fill out chain-of-custody form and lab analysis form (or lab/field
logbook).
4-. Enclose forms 1n envelope.
5. Enclose envelope and sample in shipping container.
6. Tape container shut and label.
36
-------
APPENDIX 3
SUMMARY OF ALL SAMPLES COLLECTED
Foundry
Code
PA
PA
PB
PB
PC
PO
PE
PE
PF
PF
PG
PH
PI
ru
MK
MKK
MKK
Field
Sample
Number
1*. 3**
2*. 4**
5***. 6*
7***, 8*
9***, 10**
11***, 12*
13***, 14**
15***, 16*
17***, 18**
19*
20*. 21**
22* , 23***
24* , 25***
26**, 27***
28* , 29***
30**, 31***
32**, 34*
(#33 not
collected)
35***, 36*
37***, 38**
39** , 40*
41***, 42*
43***, 44*
45***, 46*
47***, 48**
Scrubber
System
Type
Funnel
Venturl
Funnel
Venturl
Baghouse
Preceded
by Quencher
Baghouse
Preceded
by Quencher
Funnel
Venturl
Baghouse
Baghouse
Preceded
by Quencher
Baghouse
Preceded
by Quencher
Baghouse
Preceded
by Quencher
Baghouse
Preceded
by Quencher
Venturl
with
Quencher
Baghouse
Ventur-f
Venturl
Venturl
with
Quencher
Baghouse
Venturl
with
Quencher
Type of
Waste
Solid
Wet
Solid
Wet
Solid
Dry
Liquid
Solid
Wet
Solid
Dry
Quencher
Solid
Dry
Baghouse
Solid
Dry
Quencher
Solid
Dry
Baghouse
Solid
Dry
Venturl
Solid
Wet
Solid
Dry
Solid
Wet
Solid
Dry
Solid
Dry
Solid
Dry
Quencher
Solid
Dry
Description
8
B
C
F
B
H
A
C
A
C
3
C
B
B
B
C
A
Date Taken
7/28/80
7/28/80
7/29/80
7/29/80
7/29/80
7/30/80
7/31/80
7/31/80
7/31/80
7/31/80
8/01/80
8/01/80
8/02/80
8/18/80
8/18/80
8/19/80
8/18/80
Comments
Cupola
0
Cupola
I
Cupola
Cupola
G
Cupola
Cupola
Cupol a
J
Cupol a
J
Cupola
Cupola
Cupola
K
Electric Arc
Cupola
Cupola
Cupola
Electric Arc
Electric Arc
N
(continued)
37
-------
APPENDIX 3. (Continued)
Foundry
Code
ML
ML
MM
MM- - -
MNN
MO
MP
MQ
MR
MR
MS
MT
MU
Field
Sampl e
Number
49**, 50*
51*
52* , 53**
-54* , 55***
56* , 57***
58**
58* , 59**
60* , 61**
62***, 63***
64* , 65**
66* , 57**
68* , 69**
70* , 71**
72***, 73***
74* , 75**
76***, 77***
78* , 79**
Scrubber
System
Type
VentuH
with
Quencher
Venturl
with
Quencher
Venturl
with
Quencher
Venturl
with
Quencher
Venturl
with
Quencher
Venturl
with
Quencher
Venturl
Venturl
with
Quencher
Baghouse
Baghouse
Baghouse
Venturl
VentuH
with
Quencher
Type of
Waste
Liquid
Liquid
Solid
Wet
Solid
Wet
Solid
Dry
Solid
Wet
Solid
Wet
Solid
Wet
Sol id
Dry
Solid
Dry
Solid
Dry
Solid
Wet
Solid
Dry
Description
F
M
B
B
3
B
A
B
C
C
C
B
3
Date Taken
8/19/80
8/19/80
8/19/80
8/20/80
8/20/80
8/21/80
8/25/80
8/25/80
8/26/80
8/26/80
8/27/80
8/28/80
8/28/80
Comments
Cupol a
Cupola
Cupola
0
Cupola
(Permanent
Mold Process)
Cupola
(Shell Mold
Process)
Cupola
Cupola
<
Cupola
Electric Arc
Electric Arc
Cupola
P
Cupola
Cupola
* Samples shippped to EMSL-LV.
** Mixed waste samples shipped to:
Or. William Boyle
Oept. of Civil and Environmental Engineering
3230 Engineering Building
University of Wisconsin
Madison, WI 53706
** Samples requested by foundry.
A Coarse pebble-sized and sand-like material, black.
B A fine black sand-like material with occasional larger particles, grit-like in texture.
C A very fine brown powder much like talc.
0 From previous charge runs.
E From current charge run.
F Liquid containing black sand-like material which varies from extremely fine to SB-size particles.
G Contains more than furnace scrubber waste.
H A very fine gray powder mixed with larger pieces of slag.
I Material accumulated over 2-months time.
J Used a coagulant in the system.
K Vacuum belt system to separate water from waste.
L Waste Pond.
M Mostly slag.
N Half of sample was from quencher and half from the Venturi scrubber.
0 Lead wheel weight seen on scrap.
38
-------
APPENDIX
SAMPLE LISTING FOR THE GRAY IRON
Date
7/28
7/28
7/28
7/28
7/29
7/29
7/29
7/29
7/29
7/29
7/29
7/29
7/29
7/29
7/30
7/30
7/30
7/30
* S =
Q -
t Cool
Foundry Code
PA
PA
PA
PA
PB
PB
PB
PB
PB
PC
PC
PC
PC
PD
PD
PD
PD
Scrubber; M = Mixed
Quencher; B = Baghouse
ing Liquid
Sampl e
Number
1
2
3
4
5 split
0
8 SP1U
\l split
13 split
Jf split
ID
« split
; V = Venturi
39
FOUNDRY PROJECT -
Consignee
EMSL-LV
EMSL-LV
U« of Wise.
U. of Wise.
PB
EMSL-LV
PB
EMSL-LV
PB
Uc of WisCc
PC
EMSL-LV
PC
U. of Wise.
PD
EMSL-LV
PD
U. of Wise.
PENNSYLVANIA
Waste
Type*
S(Y)
S(V)
M
M
S(B)
S(B)
st
s+
M
M
S(V)
S(V)
M
M
S(B)
SCB)
M
M
Wet (W)/
Dry (D)
W
W
D
D
D
D
W
W
D
D
W
W
D
D
D
D
D
D
(continued)
-------
APPENDIX 4. (Continued)
Date Foundry Code
7/31
7/31
7/31
7/31
7/31
7/31
7/31
7/31
7/31
8/01
8/01
8/01
8/01
8/01
8/01
8/01
8/02
8/02
8/02
8/02
PE
PE
PE
PF
PF
PF
PF
PF
PF
PG
PG
PG
PG
PH
PH
PH
PI
PI
PI
PI
Sampl e
Number
19
20
21
y spin
g split
26 split
28
29
33? S»l1t
32
33
34
35 split
OD
37
38
Consignee
EMSL-LV
EMSL-LV
U. of Wise.
EMSL-LV
PF
EMSL-LV
PF
U. of Wise.
PF
EMSL-LV
PG
U. of Wise.
PG
U. of Wise.
Not collected
EMSL-LV
PI
EMSL-LV
PI
U. of Wise.
Waste
Type*
S(Q)
S(B)
M
S(Q)
S(Q)
S(B)
S(B)
M
M
S(Q)
S(Q)
M
M
M
S(B)
S(Q)
S(Q)
M
M
Wet (W)/
Dry (D)
D
D
D
D
D
D
D
D
D
W
W
D
D
D
D
W
W
D
D
* S = Scrubber; M = Mixed
Q = Quencher; B = Baghouse; V = Venturi
40
-------
APPENDIX 5
SAMPLE LISTING FOR THE GRAY IRON FOUNDRY PROJECT - MICHIGAN
Date
8/I&
8/18
8/18
8/18
8/18
8/18
'8/18
---- 8/ig
8/19
8/19
8/19
8/19
Foundry Code
MJ
MJ
MK
MK
MKK
MKK
MKK
MKK
MKK
MKK
MKK
ML
ML
ML
MM
MM
Sampl e
Number
39
40
l\ SP1U
43
44-1 split
44-11
11 s»m
48 SP1U
49
50
51
52
53
Consignee
U. of Wise.
EMSL-LV
MK
EMSL-LV
MK
EMSL-LV
EMSL-LV
MK
EMSL-LV
MK
Uc of Wise.
U. of Wise.
EMSL-LV
EMSL-LV
EMSL-LV
U. of Wise.
Waste
Type*
M
S(V)
S(V)
S(V)
S(B)
S(B)
S(B)
S(Q)
S(Q)
M
M
M
S(V)
S/M
S(V)
M
Wet (W)/
Dry (D)
D
W
W
W
D
D
D
D
D
D
D
D(slag)
^(sluice
water)
t(pond
water)
W
D
(continued)
* S = Scrubber; M = Mixed
Q = Quencher; B = Baghouse; V = Venturi
I = Part I of baghouse sample; II = Part II of baghouse sample.
f Liquid
41
-------
APPENDIX 5. (Continued)
Date
8/20
8/20
8/20
8/21
8/21
8/25
8/25
8/25
8/25
8/25
8/25
8/26
8/26
8/26
8/26
8/26
8/26
* S
Q
I
58-2-S
Foundry
MN
MN
MNN
MNN
MNN
MO
MO
MP
MP
MP
MP
MQ
MQ
MR
MR
MR
' MR
MR
MR
= Scrubber;
- Quencher;
Sampl e
Code Number
54 split
55 H
56 split
57 H
58
58-2-S
59
. 60
61
62 (split
of 60)
63 (split
of 61)
64
65
66-1
66-11
67
68-1
68-11
69
M = Mixed
Consignee
EMSL-LV
MN
EMSL-LV
MNN
U. of Wise
EMSL-LV
U. of Wise
EMSL-LV
U. of Wise
MP
MP
EMSL-LV
U. of Wise
EMSL-LV
EMSL-LV
U. of Wise
EMSL-LV
EMSL-LV
U. of Wise
Waste
Type*
S(V)
S(V)
S(Y)
S(V)
M
son
M
son
M
S(V)
M
S(V)
M
S(B#2)
S(B#2)
M(B#2)
S(B#3)
S(B#3)
M(B#3)
Wet (W)/
Dry (D)
W
W
W
W
W
W
D
W
W
W
W
W
D
D
D
D
D
D
D
(continued)
B = Baghouse; V = Venturi
= Part I of baghouse sample; II =
= Second sa
tmple 158 (scrubber wasl
Part II of
:e)
baghouse sample.
42
-------
APPENDIX 5. (Continued)
Date Foundry Code
8/27
8/27
8/27
8/27
8/28
8/28
8/28
8/28
8/28
8/28
MS
MS
MS
MS
MT
MT
MT
MT
MU
MU
Sampl e
Number
70°I
70-11
71
72 (splits
73 of 70
and 71)
74
75
76 (split
of 74)
77 (split
of 75)
78
79
Consignee
EMSL-IV
EMSL-LV
Uc of Wise.
MS
MS
EMSL-LV
U. of Wise.
MT
MT
EMSL-LV
Us of Wise.
Waste
Type*
S(B)
S(B)
M
S(B)
M
S(V)
M
S(V)
M
S(V)
M
Wet (W)/
Dry (D)
D
D
D
D
D
W
D
W
D
W
D
* S - Scrubber; M = Mixed
Q s Quencher; B3 Baghouse; V s Venturi
I of baghouse sample; II = Part II of baghouse sample,
43
-------
APPENDIX 6
RECOMMENDATIONS FOR FUTURE SAMPLING TRIPS
-T»—TFfar- to the sampling 1t should be determined who will be authorized to
receive the samples. The samples should be relinquished from the field
samples to a Federal Express representative, and Federal Express would
then relinquish the samples to the consignee specified on the SSS Tally
Record. All shipping boxes should be labeled with date and sample
number.
2. Wide-mouth, pre-tested plastic containers should be used for scrubber or
composite samples, and new gall on-tin-cans lined with four layers of
plastic bags for composite samples (not when organics are to be
determined!).
3.
Sufficient changes of suitable company-provided clothing should be
brought along and time allowed for cleaning to enable samplers to wear
clean clothing to each new sample location, especially for hazardous
sample collection.
4.
The rented vehicle should be easy to clean, and efforts should be made in
planning to prevent the vehicle from becoming unreasonably dirty as a
result of sampling activities.
5.
Disposable high-quality face masks and Teflon-coated sample scoops should
be used when sampling hazardous waste.
6.
Provisions should be made before leaving on a sampling trip to insure
availability of adequate replacement sites in case some sites can not be
sampled. Communications about cancellations of site visits should be
swiftly relayed to sampling and support personnel.
7.
The way observation on pH and scrap descriptions are recorded by the
samplers should be formalized and generally agreed to by the EPA and
industry before sampling. Permission to take pictures of the scrap pile
should be secured.
8.
Enough address labels should be typed before the trip to label all sample
boxes except those that will be labeled with the Federal Express shipping
packet. In addition, Federal Express shipping and SSS Tally forms should
be prepared in advance as much as possible.
44
-------
9. Duffle-type bags should be used to conveniently transport sample equip-
ment and containers into and around foundries. —_^_.
10. A visual distance indicator could be used to estimate pile and waste site
dimensions.
Foorrdry-representatives should be askid the following technical questions
before the sampling trip starts:
a. Do you have a wet cap or quencher system? Do you operate these
parts of your system wet or dry? How often do you melt? How often
do you dump your scrubber waste?
b. What is the source(s) of the waste we sample? When was the waste
last dumped or removed, and how muchs if any, is left?
c. What materials are composited (combined) with the scrubber waste
before, or when, the scrubber waste is disposed? What is the
typical ratio of materials in the combination? Exactly how is the
compositing performed?
d. Does your plant have true (unleached) composite waste (i.e.,
scrubber plus other waste) available for sampling? How is it
disposed (especially, from where, how much at a time, and how
frequently)?
e. Is any of your waste stored in a pond as the first total composite
location before disposal (i.e., will we have to use the pond
sampler)?
f. Is the waste stored in a barrel or large tank wjth_ojily^a_slngLle,.
^=^bufighole opening?
45
-------
APPENDIX 7
ALIQUOTS PREPARED, ALIQUOT RECIPIENTS AND SHIPPING DATES
Field
Sampl e
Number
PA 1
PA 2
PB 6
PB 8
PC 12
Aliquot
Number
1085
1086
1087
1088
1089
1090
1053
1054
1055
1056
1057
1058
1001
1002
1003
1004
1005
1006
1007
1008
1009
1010
1011
1035
1036
1037
1038
Al i quot
Weight (g)
713
738
757
794
677
549
693
605
639
622
737
563
450
452
450
518
500
500
500
500
500
500
457
552
581
632
676
Disposition
and Shipping Date
NSI, 8/7/80
Univ. of Wisconsin,
Univ. of Wisconsin,
Sample Bank
Sample Bank
Sample Bank
NSI, 8/7/80
Univ. of Wisconsin,
Sample Bank
Sample Bank
Sample Bank
Sample Bank
Univ. of Wisconsin,
NSI, 8/6/80
Univ. of Wisconsin,
EMSL-LV, 11/17/80
Sample Bank
NSI, 8/6/80
Sample Bank
Sample Bank
Sample Bank
Univ. of Wisconsin,
Sample Bank
NSI, 8/7/80
Univ. of Wisconsin,
LFE, 8/12/80
Sample Bank
8/12/80
10/23/80
8/12/80
10/15/80
8/12/80
8/12/80
8/12/80
(continued)
46
-------
APPENDIX 7. (Continued)
Field
Sampl e
Number
PC 12
(continued)
PD 16
PE 19
P£ 20
PF 22
PF 24
Aliquot
Numbtr
1039
1040
1041
1042
1043
1044
1068
1069
1070
1071
1072
1073
1074
1075
1076
1027
1028
1029
1030
1031
1032
1033
1034
1064
1065
1066
1067
1045
1046
1047
1048
1049
1050
1051
1052
1059
1060
1061
1062
1063
Aliquot
Weight (g)
667
641
848
714
624
361
545
519
505
506
560
513
557
535
190
450
450
450
450
450
450
450
417
531
513
525
387
472
499
551
510
' 566
517
513
426
600
507
508
451
424
Disposition
and Shipping Date
Sample Bank
Sample Bank
Univ. of Wisconsin, 8/12/80
NSI, 8/12/80
LFE, 8/12/80
Sample Bank
NSI, 8/7/80
Univ. of Wisconsin, 8/12/80
LFE, 8/12/80
Univ. of Wisconsin, 10/15/80
Univ. of Wisconsin, 10/15/80
Univ. of Wisconsin, 8/12/80
LFE, 8/12/80
NSI, 8/12/80
EMSL-LV, 11/17/80
NSI, 8/7/80
Univ. of Wisconsin, 8/12/80
LFE, 8/12/80
Univ. of Wisconsin, 10/15/80
Univ. of Wisconsin, 10/15/80
Univ. of Wisconsin, 8/12/80
NSIS 8/12/80
LFES 8/12/80
NSI, 8/7/80
Univ. of Wisconsin, 8/12/80
Univ. of Wisconsin, 10/15/80
Sample Bank
NSI, 8/7/80
Univ. of Wisconsin, 8/12/80
Univ. of Wisconsin, 10/15/80
Sample Bank
Sample Bank
Sample Bank
Sample Bank
Sample Bank
NSI, 8/7/80
Univ. of Wisconsin, 8/12/80
Univ. of Wisconsin, 10/15/80
Sample Bank
Sample Bank
47
(continued)
-------
APPENDIX 7. (Continued)
Field
Sample Aliquot
Number Number
PG 28 1077
1078
1079
1080
1081
1082
1083
1084
PH 34 1022
1023
1024
1025
1026
PI 36 1012
1013
1014
1015
1016
1017
1018
1019
1020
1021
MJ 40 1101
1102
1103
1104
1105
1106
1107
MK 42 1211
1212
1213
1214
1215
1216
1217
Aliquot
Weight (g)
720
729
735
730
680
802
687
714
453
458
466
482
352
561
608
574
597
573
577
611
590
580
480
490
485
545
550
470
505
690
650
540
690
660
580
710
730
Disposition
and Shipping Date
NSI, 8/7/80
Univ. of Wisconsin,
Sample Bank
Sample Bank
EMSL-IV, 11/17/80
Sample Bank
Sample Bank
Sample Bank
NSI, 8/7/80
EMSL-LV, 11/17/80
Univ. of Wisconsin,
Univ. of Wisconsin,
Sample Bank
Sample Bank
Sample Bank
Univ. of Wisconsin,
Sample Bank
NSI, 8/6/80
Sample Bank
Univ. of Wisconsin,
Sample Bank
Sample Bank
Sample Bank
NSI, 9/23/80
Univ. of Wisconsin,
LFE, 9/25/80
Univ. of Wisconsin,
Sample Bank
Sample Bank
Sample Bank
NSI, 9/25/80
Univ. of Wisconsin,
LFE, 9/25/80"
Sample Bank
Sample Bank
Sample Bank
Sample Bank
8/12/80
8/12/80
10/15/80
8/12/80
10/23/80
9/25/80
10/15/80
9/25/80
(continued)
48
-------
APPENDIX 7. (Continued)
- --- FieTrf ---------- -••-
Sample Aliquot
Number Number
Ul/'l/ A A 1 IftQ
fmR 44 IlUo
1109
1110
1111
1112
1113
1114
MKK 46 1115
1116
1117
1118
1119
1120
1121
1122
ML 50 1123
11231
ML 51 1124
11241
MM 52 1125
1126
1127
1128
1129
1130
1131
MN 54 1132
1133
1134
1135
1136
1137
1138
1139
MNN 56 1140
1141
1142
1143
Al 1 quot
Weight (g)
A en
s>SU
465
460
465
450
465
510
460
460
505
475
470
465
455
595
3770
200
3300
200
694
761
739
706
806
711
806
675
720
800
810
648
730
763
861
780
780
820
750
Disposition
and Shipping Date
UCT OV^/Qft
Nais 7/&J/OU
Univ. of Wisconsin, 9/25/80
*LFE, 9/25/80
Univ. of Wisconsin, 10/15/80
EMSL-LV, 11/17/80
Sample Bank
Sample Bank
NSI, 9/23/80
Univ. of Wisconsin, 9/25/80
*LFE, 9/25/80
Univ. of Wisconsin, 9/25/80
LFE, 9/25/80
Univ. of Wisconsin, 10/15/80
Sample Bank
NSI, 9/23/80
Sample Bank (as extract)
NSI, 10/23/80
Sample Bank
NSI, 10/23/80
NSI, 9/23/80
Univ. of Wisconsin, 9/25/80
*LFE , 9/25/80
Sample Bank
Sample Bank
EMSL-LV, 11/17/80
Sample Bank
NSI, 9/23/80
Univ. of Wisconsin, 9/25/80
*LFE, 9/25/80
EMSL-LV, 11/17/80
Sample Bank
Univ. of Wisconsin, 9/25/80
*LFE, 9/25/80
NSI, 9/23/80
NSI, 9/23/80
Univ. of Wisconsin, 9/25/80
*LFE, 9/25/80
Sample Bank
(continued)
Sample not analyzed
49
-------
APPENDIX 7. (Continued)
Field
Sampl e
Number
MN 56
(continued)
MO 58
MP 60
MQ 64
MR 66
Aliquot
Number
1144
1145
1146
1147
1148
1149
1150
1151
1152
1153
1154
1155
1156
1157
1158
1159
1160
1161
1162
1163
1164
1165
1166
1167
1168
1169
1170
1171
1172
1173
1174
1175
1176
1177
1178
Aliquot
Weight (g)
820
834
890
840
840
709
751
819
777
788
819
788
720
780
750
850
730
818
730
872
861
965
810
790
875
885
815
580
570
495
460
470
480
470
520
Disposition
and Shipping Date
Sample Bank
Univ. of Wisconsin, 9/25/80
LFE, 9/25/80
NSI, 9/23/80
NS1, 9/23/80
Univ. of Wisconsin, 9/25/80
*LFE, 9/25/80
Sample Bank
Sample Bank
Sample Bank
Sample Bank
Sample Bank
NSI, 9/25/80
Univ. of Wisconsin, 9/25/80
*LFE, 9/25/80
Sample Bank
Sample Bank
Sample Bank
Sample Bank
Sample Bank
NSI, 9/25/80
Univ. of Wisconsin, 9/25/80
*LFE, 9/25/80
Sample Bank
Sample Bank
Sample Bank
Sample Bank
NSI, 9/25/80
Univ. of Wisconsin, 9/25/80
*LFE, 9/25/80
Univ. of Wisconsin, 10/15/80
Univ. of Wisconsin, 10/15/80
Univ. of Wisconsin, 9/25/80
LFE, 9/25/80
NSI, 9/25/80
(continued)
Sample not analyzed
50
-------
Field
Sample Aliquot
Number Number
MR 68 1179
1180
1181
1182
1183
1184
1185
1186
MS 70 1187
1188
1189
1190
1191
1192
1193
1194
MT 74 1195
1196
1197
1198
1199
1200
1201
1202
MU 78 1203
1204
1205
1206
1207
1208
1209
1210
Aliquot
Weight (g)
620
610
' 660
575
600
535
710
560
600
600
570
550
560
580
620
735
790
760
805
820
850
810
770
820
490
600
495
575
805
755
655
645
--
Disposition
and Shipping Dai
NSI, 9/25/80
Univ. of Wisconsin,
*LFE, 9/25/80
Univ. of Wisconsin,
Univ. of Wisconsin,
Univ. of Wisconsin,
*LFE, 9/25/80
NSI, 9/25/80
MSI, 9/25/80
Univ. of Wisconsin,
*LFE, 9/25/80
Univ. of Wisconsin,
Sample Bank
Sample Bank
EMSL-LV, 11/17/80
Sample Bank
NSI, 9/25/80
Univ. of Wisconsin,
*LFE, 9/25/80
Sample Bank
Sample Bank
Sample Bank
Sample Bank
Sample Bank
NSI, 9/25/80
Univ. of Wisconsin,
LFE, 9/25/80
Sample Bank
Sample Bank
Sample Bank
Sample Bank
Sample Bank
be
9/25/80
10/15/80
10/15/80
9/25/80
9/25/80
10/15/80
9/25/80
-
9/25/80
* Sample not analyzed
51
-------
APPENDIX 8
LIST OF EXTRACTS AND DIGESTS SHIPPED TO
LFE AND THE UNIVERSITY OF WISCONSIN
Extracts shipped to LFE:
I 10682A
10022A
1097121
10221A
10773A
11711A
11323A
11871A
11083A
11251A
Digest shipped to LFE;
# 100241
102251
107753
106861
118761
112561
113251
117151
110841
Extracts shipped to the University of Wisconsin:
# 100223
102213
106823
107733
1097131
110833
112513
113233
117113
118713
Digests shipped to the University of Wisconsin:
I 100243
102253
106863
1 Simulated Extracts
107753
110843
112563
113253
117153
118763
52
-------
APPENDIX 9
Section 7.0
EXTRACTION PROCEDURE TOXICITY
Introduction
The Extraction Procedure (EP) is designed to simulate the leaching a
waste will undergo if disposed of in an improperly designed sanitary landfill.
It is a laboratory test in which a representative sample of a waste is
extracted with distilled water maintained at pH = 5 using acetic acid. The
extract obtained from the EP (the "EP Extract") is then analyzed to determine
if any of the thresholds established for the 8 elements (i.e., arsenic,
barium, cadmium, chromium, lead, mercury, selenium, silver), four pesticides
(i.e., Endrin, Lindane, Methoxychlor, Toxaphene), and two herbicides (i.e.,
2,4,5-Tri chl orophenoxypropi oni c acid, 2,4-Di chl orophenoxy'acetic acid) have
been exceeded. If the EP Extract contains any one of the above substances in
an amount equal to or exceeding the levels specified in 40 CFR 261.24, the
waste possesses the characteristic of Extraction Procedure Toxicity and is a
hazardous waste.
The Extraction Procedure consists of 5 steps:
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 stored for later use.
2. Structural Integrity Procedure/Particle Size Reduction
Prior to extraction, the solid material must either pass through a
9.5 mm (0.375 in) standard sieve, have a surface area per gram of waste
of 3.1 cms or if it consists of a single piece, be subjected to the
Structural Integrity Procedure. The Structural Integrity Procedure is
used to demonstrate the ability of the waste to remain intact after
disposal. If the waste does not meet one of these conditions it must be
ground to pass the 9.5 mm sieve.
53
-------
3. Extraction of Solid Material
The solid material for step 2 is extracted for 24 hours in an
aqueous medium whose pH is maintained at or below 5, using 0.5 N acetic
acid. The pH is maintained either automatically or manually. Acidifica-
tion to pH 5 is subject to a specification as to total amount of acid to
be added to the system.,
4. Final Separation of the Extraction Liquid from the Remaining Solid
After extraction, the liquidrsolid ratio is adjusted to 20:1 and the
mixture of solid and extraction liquid is separated by filtration, the
solid discarded and the liquid combined with the filtrate obtained in
step 1. This is the EP Extract that is subjected to the evaluation
requirements in 40 CFR 261.24.
5. Testing (Analysis) of EP Extract
Inorganic and organic species are identified and quantified using
the appropriate methods in Section 8 of this manual.
54
-------
Wet Waste Sample
contains 6.S%
non-filterable
solids
I
Representative
Waste Sample
16© gratis
Wet Waste Sample
eontaine 0<>S%
non-filterable
solids
Dry Waste Sample
^ — .Solid
>r
Particle size)
i
Liquid Solid
Separation
Liquid
> 9.5 mm < 9.5 mm monolithic
Sample Size
Reduction
Solid
Discard
Extraction of Solid Waste
Structural
Integrity
Procedure
Liquid
Store at
4° C and/or
at pH#2
f
I Separation
I
uid
\,
EP Extract
i
Analysis Methods
Figure 7.0, Extraction Procedure Flowchart
55
-------
SUB-SECTION 7.1
CHARACTERISTIC OF EP TOXICITY REGULATION
A solid waste exhibits the characteristic of EP toxicity if, using the
test methods described in Appendix II of 40 CFR Part 261 or equivalent methods
approved by the Administrator under the procedures set forth in 40 CFR 260.20
and 260.21, the extract from a representative sample of the waste contains any
of the contaminants listed in Table 7.1-1 at a concentration equal to or
greater than the respective value given in that table. Where the waste
contains less than 0.5 percent filterable solids, the waste itself, after
filtering, is considered to be the extract for the purposes of this section.
A solid waste that exhibits the characteristic of EP toxicity, but is not
listed as a hazardous waste in Subpart D, has the EPA Hazardous Waste Number
specified in Table 7.1-1 which corresponds to the toxic contaminant causing it
to be hazardous.
56
-------
TABLE 7ol-l0 MAXIMUM CONCENTRATION OF CONTAMINANTS^ -
FOR CHARACTERISTIC OF EP TOXICITY ^; ,
EPA Maximum
Hazardous Waste Concentration
Number Contaminant (nrH-H
-------
APPENDIX II
EP TOXICITY TEST
Procedure
1. A representative sample of the waste to be tested (minimum size 100
grams) should be obtained using the methods specified in Appendix I of 40
CFR 261 or any other method capable of yielding a representative sample
within the meaning of 40 CFR 260.
2. The sample should be separated into its component liquid and solid phases
using the method described in "Separation Procedure" below. If the dry
weight of the solid residue* obtained using this method totals less than
0.5% of the original wet weight of the waste, the residue can be
discarded and the operator should treat the liquid phase as the extract
and proceed immediately to Step 8.
3. The solid material obtained from the Separation Procedure should be
evaluated for its 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 (0.375 inch) standard sieve, the operator should proceed
to Step 4. If the surface area is smaller or the particle size larger
than specified above, the solid material would be prepared for extraction
by crushing, cutting or grinding the material so that is passes through a
9.5 mm (0.375 inch) sieve or, if the material is in a single piece, by
subjecting the material to the "Structural Integrity Procedure" described
below.
4. The solid material obtained in Step 3 should be weighed immediately and
placed in an extractor with 16 times its weight of deionized water. Do
not allow the material to dry prior to weighing. For purposes of this
test, an acceptable extractor is one which will impart sufficient
agitation to the mixture to not only prevent stratification of the sample
and extraction fluid but also insure that all sample surfaces are
continuously brought Into contact with well-mixed extraction fluid.
The percent solids is determined by drying the filter pad at 80°C until it
reaches constant weight and then calculating the percent solids using the
following equation:
(weight of pad + solid) - (tare weight of pad) x 100 = % solids
initial wet weight of sample
58
-------
5. After the solid material and deionized water are placed in the extractor,
the operator should begin agitation and measure the pH of the solution
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 acicL If the pH
is equal to or less than 5.0, no acetic acid 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, 0.5N acetic acid should
be added to bring the pH down to 5.0 ± 0.2. However, in no event shall
the aggregate amount of acid added to the solution exceed 4-irri—of'^tcich
per gram of solid. The mixture should be agitated for 24 hours and
maintained at 20e»40°C (68°~104°F) 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 Cfiemtrix, Inc., Hillsboro, Oregon 97123 or 1ts~eqirfva'Tentr~tn
conjunction with a metering pump and reservoir of 0.5N acetic acid. If
such a system 1s not available, the following manual procedure shall be
employed:
a. A pH meter should be calibrated in accordance with the
manufacturer's specifications.
b. The pH of the solution should be checked and, if
necessary, 0.5N 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 minute
intervals, moving to the next longer interval if the pH
does not have to be adjusted more than 0.5 pH units.
c. The adjustment procedure should be continued for at least
6 hours.
d. If at the end of the 24-hour 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 four hours, during which the
pH should be adjusted at one hour intervals.
6. At the end of the 24-hour extraction period, deionized water should be
added to the extractor in an amount determined by the following equation
V = (20)(W) - 16(W) - A
V * ml deionized water to be added
W = weight in grams of solid charged to extractor
A = ml of 0.5N acetic acid added during extraction.
59
-------
7. The material in the extractor should be separated into its component
liquid and solid phases as described under "Separation Procedure."
8. The liquids resulting from Steps 2 and 7 should be combined. This
combined liquid (or the waste itself if it has less than 0.5% solids, as
noted in step 2) is the extract and should be analyzed for the presence
of any of the contaminants specified in Table I of 40 CFR 261.24 using
the Analytical Procedures designated below.
Separation Procedure
Apparatus
A filter holder, designed for filtration media having a nominal pore
size of 0.45 micrometer and capable of applying a 5.3 kg/cm2 (75 psig)
hydrostatic pressure to the solution being filtered shall be used. For
mixtures containing non-absorptive solids, where separation can be
effected without imposing a 5.3 kg/cm2 pressure differential, vacuum
filters employing a 0.45 micrometer filter media can be used.
Procedure*
1. Following manufacturer's directions, the filter unit should be assembled
with a filter bed consisting of a 0.45 micrometer filter membrane. For
difficult or slow-to-filter mixtures a prefilter bed consisting of the
following prefilters in increasing pore size (0.65 micrometer membrane,
fine glass fiber prefilter, and coarse glass fiber prefilter) can be
used.
2. The waste should be poured into the filtration unit.
3. The reservoir should be slowly pressurized until liquid begins to flow
from the filtrate outlet at which point the pressure in the filter should
be immediately lowered to 10-15 psig. Filtration should be continued
until liquid flow ceases.
This procedure is intended to result in separation of the "free" liquid
portion of the waste from any solid matter having a particle size >0.45um.
If the sample will not filter, various other separation techniques can be
used to aid in the filtration. As described above, pressure filtration is
employed to speed up the filtration process. This does not alter the nature
of the separation. If liquid does not separate during filtration, the waste
can be centrifuged. If separation occurs during centrffugation, the liquid
portion (centrifugate) is filtered through the 0.45um filter prior to
becoming mixed with the liquid portion of the waste obtained from the
initial filtration. Any material that will not pass through the filter
after centrifugation is considered a solid and is extracted.
60
-------
4c The pressure should be Increased stepwise 1n 10 pslg Increments to 75
pslg and filtration continued until flow ceases or the pressurizing gas
begins to exit from the filtrate outlet.
So The filter unit should be depressurized, the solid material removed and
weighed and then transferred to the extraction apparatus, or, in the case
of final filtration prior to analysis, discarded. If the solid is to be
extracted do not allow the material retained on the filter pad to dry
prior to weighing.
6. The liquid phase should be stored at 4°C for subsequent use in Step 8.
Structural Integrity Procedure
Apparatus
A Structural Integrity Tester having a 3.18 cm (1.25 in.) diameter hammer
weighing 0.33 kg (0.73 Ibs.) and having a free fall of 15.24 cm (6 in.) shall
be used. This device is available from Associated Design and Manufacturing
Company, Alexandria, VA, 22314, as Part No. 125, or it may be fabricated to
meet the specifications shown in Figure 7-2.
Procedure
1. The sample holder should be filled with the material to be tested. If
the sample of waste is a large.monolithic block, a portion should be cut
from the block having the dimensions of a 3.3 cm (1.3 1n.) diameter x 7.1
cm (2.8 in.) long cylinder. For a fixated waste, samples may be cast in
the form of a 3.3 cm (1.3 in.) diameter x 7.1 cm (2.8 in.) cylinder for
purposes of conducting this test. In such cases, the waste may be
allowed to cure for 30 days prior to further testing.
2. The sample should be placed into the Structural Integrity Tester, then
the hammer should be raised to its maximum height and dropped. This
should be repeated fifteen times.
3. The material should be removed from the sample holder, weighed, and
transferred to the extraction apparatus for extraction.
Procedures for Analyzing Extract
The test methods for analyzing the extract are as follows:
1. For arsenic, barium, cadmium, chromium, lead, mercury, selenium or
silver: "Methods for Analysis of Water and Wastes," Environmental
Monitoring and Support Laboratory, Office of Research and Development,
U.S. Environmental Protection Agency, Cincinnati, Ohio 45268 (EPA-600/4-
79-020, March 1979).
2. For Endrin; Lindane; Methoxychlor; Toxaphene; 2,4-D; 2,4,5-TP (Silvex):
in "Methods for Benzidine, Chlorinated Organic Compounds, Pentachloro-
61
-------
phenol and Pesticides in Water and Wastewater," September 1978, U.S.
Environmental Protection Agency, Environmental Monitoring and Support
Laboratory, Cincinnati, Ohio 45268. As standardized in "Test Methods for
the Evaluation of Solid Waste, Physical/Chemical Methods."
For all analyses, the method of standard addition shall be used for the
quantification of species concentration. This method is described in "Test
Methods for the Evaluation of Solid Waste." (It is also described in "Methods
for Analysis of Water and Wastes.")
62
-------
Vj
mm.
•*:.'
15.2!
(6
I
J*
mm
I ,l
i
5cm
")
(3.1!
(1.2!
Combined
Weight
(.731b)
Sample
Eiastomeric*
Sample Holder
*EIastomeric Sample Holder Fabricated of
Material Firm Enough to Support the Sample
Figure 7.2. Compaction Tester
63
-------
Method 7«2
SEPARATION PROCEDURE
Scope and Application
This procedure is used to separate a waste into its liquid and solid
phases both prior to and after extraction.
Summary of Method
The Separation Procedure involves vacuum or pressure filtration of a
waste or extraction mixture. To minimize filtration time, pressure, settling,
centrifugation and prefilters may be employed as an adjunct to filtration.
Pressure filtration is required when vacuum filtration is inadequate for
complete separation.
Apparatus
1. Filter holder: A filter holder capable of supporting a 0.45 urn filter
membrane and able to withstand the pressure needed to accomplish
separation. Suitable filter holders range from simple vacuum units to
relatively complex systems that can exert up to 5.3 kg/cm2 (75 psi) of
pressure. The type of filter holder used depends upon the properties of
the mixture to be filtered. Filter holders known to the Agency and
deemed suitable for use are listed in Table 7.2-1.
2. Filter membrane: Filter membrane suitable for conducting the required
filtration shall be fabricated from a material which:
a. is not physically changed by the waste material to be filtered.
b. does not absorb or leach the chemical species for which a waste's EP
Extract will be analyzed. Table 7.2-2 lists filter media known to
the Agency and generally found to be suitable for solid waste
testing.
3. In cases of doubt contact the filter manufacturer to determine if either
membrane or prefilter are adversely affected by the particular waste. If
no information is available, submerge the filter in the waste's liquid
phase. After 48 hours a filter that undergoes visible physical change
(i.e., curls, dissolves, shrinks, or swells) is unsuitable for use.
64
-------
Use the following procedure to establish if a filter membrane will leach
or adsorb chemical species.
a* Prepare a standard solution of the chemical species of interest0
bo Analyze the standard for its concentration of the chemical species.
c. Filter the standard and re-analyze. If the concentration of the
filtrate differs from the original standard, the filter membrane
leaches or absorbs one or more of the chemical species.
General Procedure
1. Weigh filter membrane and prefilter to ± 0.01 gram. Handle membrane and
prefilters with blunt curved tip forceps or vacuum tweezers, or by
applying suction with a pipette.
2. Assemble filter holder, membranes, and prefilters following the
manufacturer's instructions. Place the 0.45 urn membrane on the support
screen and add prefilters in ascending order of pore size. Do no pre-wet
filter membrane.
3. Allow slurries to stand to permit the solid phase to settle. Slow to
settle wastes may be centrifuged prior to filtration.
4. 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 (10-15 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-
5. Remove solid phase and filter media and weigh to ± 0.01 gram. Discard
solid if it comprises less than 0.556 of the mixture (see below). If the
sample contains >0.5% solids use the wet weight of the solid phase
obtained in this separation for purposes of calculating amount of liquid
and acid to employ for extraction using the following equation:
W = Wf - Wt
W = wet weight in grams of solid to be charged to extractor
Wf * wet weight in grams of filtered solids and filter media
W-t = weight in grams of tared filters.
Procedure for Determining Percent Solids of a Waste
1. Determine percent solids of a waste sample by:
a. separately weighing the waste sample and filters.
65
-------
b. filtering the waste material.
c. drying the solid and filters at 80°C until two successive weighings
yield the same value. Calculate the percent solids using the
following equation:
weight of filtered solid and filters - tared weight of filters x 100 = % solids
initial weight of waste material
NOTE; This procedure is only used to determine if the solid must be
extracted or if 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 % solids
~~ determination is performed.
66
-------
TABLE 7.2-1
APPROVED FILTER HOLDERS
Manufacturer
Size
Model Number
Comments
Vacuum Filters
Nalgene
500 ml
Systems
M1111 pore
142 mm
45-0045 Disposable plastic unit,
includes prefliter and
filter pads, and reservoir.
Should only be used when
solution is to be analyzed
for inorganic constituents,
Nucl epore
Mi 1 1 i pore
Pressure Filters
Nucl epore
Micro Filtration
47 mm
47 mm
142 mm
142 mm
410400
XX10 047 00
420800
302300
YT30 142 HW
67
-------
TABLE 7.2-2
APPROVED FILTRATION MEDIA
Filter
Type
Coarse
Pref liter
Medi urn
Pref liters
Fine
Pref liters
Fine
Filters
(0.45um)
Supplier
Gel man
Nuclepore
MUlipore
Nuclepore
MUlipore
Nuclepore
Milli pore
Gel man
Pall
Nuclepore
Milli pore
Selas
Filter To Be Used
For Aqueous Systems
61653
61669
210907
211707
AP25 042 00
AP25 127 50
21095
211705
AP20 042 00
AP20 124 50
210903
211703
AP25 042 00
AP25 127 50
60173
60177
047NX50
142NX25
111107
112007
HAWP 047 00
HAWP 142 50
83485-02
83486-02
Filter To Be Used
For Organic Systems
61652
61669
210907
211707
AP25 042 00
AP25 127 00
21095
211705
AP20 042 00
AP20 124 50
210903
211703
AP25 042 00
AP25 127 50
60540
60544
181107
182007
FHLP 047 00
FHLP 142 00
83485-02
83486-02
68
-------
METHOD 7c4
STRUCTURAL INTEGRITY PROCEDURE
Application
The Structural Integrity Procedure (SIP) is employed to approximate the
physical degradation a monolithic waste undergoes in a landfill or when
compacted by earthmoving equipment.
Equipment
1. Structural Integrity Tester meeting the specifications detailed in Figure
7.4-1.
2. Sample holders of elastomeric material firm enough to support a
cylindrical waste sample 3.3 cm (1.32 in.) in diameter and 7.1 cm (2.84
in.) Tong.
Procedure
1. Cut a 3o3 cm in diameter by 7.1 cm long cylinder from the waste material.
For wastes which have been treated using a fixation process the waste may
be cast in the form of a cylinder and allowed to^curejforJSCLdays prior
to testing.
2. Place waste into sample holder and assemble the tester. Raise the hammer
to its maximum height and drop. Repeat 14 times.
3. Remove solid material from tester and scrap off any particles adhering to
sample holder. Weigh the waste to the nearest 0.01 gram and transfer it
to the Extractor.
69
-------
Sub-Section 7.5
EXTRACTORS
Introduction
An acceptable extractor is one which will prevent stratification of a
waste sample and extraction fluid and will insure that all sample surfaces
continuously contact well-mixed extraction fluid. There are two types of
acceptable extractors: 1) stirrers and 2) tumblers. Stirrers consist of a
container in which the waste/extraction fluid mixture is agitated by spinning
blades. Rotators agitate by turning a sample container end over end through a
360° revolution.
Stirrer
Scope and Application
One such stirrer approved for use in evaluating solid waste is
illustrated in Figure 7.5-1. It is a container in which a waste/extraction
fluid mixture is agitated by 2 blades spinning at >. 40 rpm. This extractor
can be used with either automatic or manual pH adjustment.
Precautions
1. Large particles (2. 0.25 in. in diameter) may be ground by the spinning
blades or abrade the container. If metal containers are employed this
may result in contamination of the EP Extract.
2. Monolithic wastes should not be extracted in the stirrer as they may bend
or break the stirring blades.
Summary of Operation
Place waste in extractor, add extraction fluid and stir for the required
period of time. Adjust pH while stirrer is in operation by addition of acid
through port in cover. pH may be continuously monitored using port in cover
designed to accept a pH electrode.
Manufacturers
Extractors of this design may be fabricated by the user or are known to
70
-------
be available commercially from Associated Design and Manufacturing Co. and
Mi Hi pore Corporation.
Rotary Extractor
Scope and Application
The rotary extractor consists of a rack or box type device holding a
number of plastic or glass bottles which rotate at approximately 29 rpm.
Rotary extractors are used with manual pH adjustment.
Precautions
le Use glass or fluorocarbon bottles for wastes whose EP Extract will be
analyzed for organic compounds. For extracts to be analyzed only for
metals, polyethylene bottles may be substituted.
2. Be careful not to tighten the screws too far and shatter the bottle when
using the design in Figure 7.2-2.
3. Do not use glass bottles for extracting large blocks of waste as these
may cause the bottles to shatter.
4. It is recommended that the bottles be alternated in an opposing manner in
the apparatus to minimize torque (e.g., when one bottle faces up, the
next bottle faces down.) When extracting an odd number of samples,
balance the extractor by adding a bottle containing an amount of water
approximately equal to the volume in the other bottles.
Equipment
1. Rotary extractors approved for use in evaluating the EP toxicity of solid
wastes are illustrated in Figure 7.5-2 and 7.5-3.
2. Plastic or glass bottles sized to fit the particular extractor.
3. The equipment illustrated in Figure 7.5-2 may be fabricated by the user
or is available comrnercially from Associated Design and Manufacturing Co.
4. The equipment illustrated in Figure 7.5-3 is available from the Acurex
Corporation.
Summary of Operation
Fill plastic or glass bottles with the solid material. Add distilled
deionized water to each bottle and start extractor. Stop extractor after 1
minute and adjust pH. Restart extractor and continue pH adjustment for the
first six hours of agitation as described in the "Manual pH Adjustment
Procedure" (Section 7.1). After 24 hours of agitation stop extractor, check
pH as described and, if within range specified, adjust volume of fluid and
remove for liquid/solid separation.
71
-------
•«—
5
ft3\\\\\\\^r
f*
i
f
4.0
1
r
.<
*
m
00 •*
&\\\\\\\\\\v\s
J,^
_J
i
i
9.0
!
— Non clogging support bushing
1 inch blade at 30° to horizontal
Figure 7.5-1. Extractor
72
-------
2-liter plastic or fllai» bottles
1/16 horaapowar electric motor
•craws for holding bonlas
Figure 7.5-2. Rotary Extractor
-------
1-gallon plastic
or gla*s bottle
Totally Enclosed
Fan Cooled Motor
40rpm. 1/8HP
Box Assembly
Plywood Construction
Foam Inner Liner
Figure 7.5-3. EPRI/Acurex Extractor
-------
APPENDIX 10
DIGESTION PROCEDURE FOR GRAY IRON FOUNDRY WASTE SAMPLES
le Acid-clean labware by soaking it at least four hours in 3 percent nitric
acid before triple rinsing with deionized water.
2. Transfer enough representative sample materials to a 250-ml beaker to
provide at least 30 grams when dry, using a plastic spatula for dry or
moist samples and a glass beaker for samples containing a liquid phase.
Dry the material at 103 - 105°C to constant weight.
3. Transfer representative 10.00-gram portions of the dry sample to three
250-ml beakers using a plastic spatula.
4. In a hood add 50 ml of nitric acid (1 + 1) to each beaker with sample and
to an empty beaker.
5. Cover beakers with watch glasses and evaporate liquids to near dryness on
a hotplate making certain that the solutions do not boil. Let digests
cool; add 40 ml concentrated nitric acid to each beaker and again
evaporate liquids to near drynes without boiling.
6. Let digests cool then add 10 ml nitric acid (1 + 1) to each beaker.
7. Add 30 percent hydrogen peroxide dropwise with caution until 10 ml per
beaker have been added.
8. Warm solutions slowly until effervescence subsides.
9. Let digests cool; add 10 ml nitric acid (1 + 1) to each beaker, reflux
covered for ten minutes.
10. Let digests cool; filter through Whatman No. 42 filter paper (or
equivalent), dilute to 1000 ml with deionized water, and mix.
75
-------
APPENDIX 11
CHAIN OF CUSTODY RECORD
GRAY IRON FOUNDRY STUDY SAMPLES
Sampling Site Address
Name:
Number/Street:
City/State: ZIP Code
Type of Waste:
Waste Process:
Other Information:
Method of Shipping:
Location Sample Sent To:
1. Relinquished By: Date / / Time:
Received By:
2. Relinquished By: Date / / Time:
Received By:
3. Relinquished By: Date / / Time:
Received By:
4. Relinquished By: Date / / Time:
Received By:
5. Relinquished By: Date / / Time:
Received By:
76
-------
APPENDIX 12. ICP DATA FOR EP EXTRACTS (mg/1)
Elment
Al
As
B
Ba
Be
Ca
Cd
Co
Cr
Cu
Fe
Mg
Hi
Pb
V
In
AVG
STO DEV
AVG
STO DEV
AVG
STO DEV
AVG
STD DEV
AVG
STD DEV
AVG
STO DEV
AVG
STD DEV
AVG
STD DEV
AVG
STD DEV
AVG
STO DEV
AVG
STO DEV
AVG
STO DEV
AVG
STD DEV
AVG
STO DEV
AVG
STD DEV
AVG
STD DEV
Detection
Limit
0.16
0.42
0.14
0.0084
0.0065
0.14
0.030
0.22
0.019
0.025
0.14
0.011
0.028
0.18
0.020
0.0068
1
15.6
0.3
BD
0.3
0.04
0.688
0.032
BO
-
187.4
1.4
BO
-
BD
-
0.04
0.03
BO
-
7.3
1.4
9.56
0.22
0.31
0.08
2.9
0.6
BD
-
3.138
0.146
2
10.4
1.5
1.0
0.03
0.2
0.02
0.443
0.018
BD
-
>300
-
BD
-
BD
-
0.13
0.03
0.14
0.04
0.9
0.4
17.24
0.53
0.60
0.01
0.8
0.6
BD
-
0.943
0.131
6
20.4
0.2
1.3
0.3
3.2
0.2
0.053
0.006
BD
-
155.6
1.1
0.93
0.04
BO
-
0.68
0.04
BD
-
S.2
2.9
>30
-
0.15
0.04
19.0
0.6
BD
-
BO
12 12 SPLIT
0.8
0.2
0.9
0.2
0.2
0.1
0.531
0.012
BD
-
>300
-
BO
-
M>
-
0.09
0.03
BO
-
7.4
3.6
12.14
0.87
0.19
0.05
BD
-
BD
-
2.021
0.033
BO
1.0
0.2
BD
-
0.754
0.033
BD
-
>300
-
BD
-
BD
-
BD
BO
-
>30
-
12.20
0.16
0.22
0.02
BO
-
BD
-
1.387
0.106
Field Sample Number
16 16 SPLIT 19
38.1
4.2
BO
-
6.2
0.2
0.388
0.145
BD
-
193.2
25.7
0.90
0.07
BD
-
0.27
0.03
BD
-
7.6
1.6
>30
-
0.18
0.03
>30
-
BD
-
>30
-
39.8
0.4
0.8
0.1
5.8
0.1
0.603
0.013
BD
™
212.0
3.2
0.83
0.04
BD
"
0.28
0.002
BD
-
8.2
0.3
>30
-
0.22
0.04
>30
-
BO
-
>30
•
2.8
0.4
1.6
0.1
BD
-
0.337
0.012
BD
~
>300
-
BD
-
BO
•
BO
BO
-
>30
-
>30
-
1.14
0.34
BO
-
BO
-
3.641
0.405
19 SPLIT 20 22
2.2
0.6
1.7
0.1
BD
-
0.366
0.030
BD
™
>300
-
BD
"
80
"
0.14
0.76
BD
"
>30
-
>30
-
0.97
0.09
0.7
0.1
BD
*
3.243
0.093
9.2
0.9
0.9
0.01
0.5
0.3
0.168
0.02?
BD
—
228.0
4.6
BD
•
BD
"
0.23
0.12
BD
•
>30
-
>30
"
3.41
0.31
BD
™
80
"
6.923
0.736
8.2
0.1
80
*
0.2
0.1
0.459
0.015
80
"
213.0
9.8
BD
™
BD
™
0.09
0.03
BO
~
16.0
4.3
9.51
0.38
0.40
0.04
BD
•
BD
*
O.S71
0.089
21
6.6
0.4
BO
™
0.®
0.05
0.&4Q
0.816
n
"
243.4
2. A
BO
™
BD
"
o.iie
O.SM
BO
*
10.2
0.7
19.03
0.20
0.?30
"
>30
"
0.16
0.09
5.6
4.2
B0>
™
9.886
8.126
._& A _.... J\
BD Indicates value Below ^
Sample 8 extract MS not analyzed by ICP.
-------
APPENDIX 12 (Continued). ICP DATA FOR EP EXTRACTS (mg/1)
*~1
00
Element
At
As
B
Bl
Be
C«
Cd
Co
Cr
Cu
Fe
Mg
HI
Pb
V
Zn
AVG
STD OEV
AVG
STO OEV
AVG
STO DEV
AVG
STD DEV
AVG
STD DEV
AVG
STO OEV
AVG
STO DEV
AVG
STO DEV
AVG
STD DEV
AVG
STO DEV
AVG
STD DEV
AVG
STD OEV
AVG
STO DEV
AVG
STO OEV
AVG
STO OEV
AVG
STO OEV
Detection
Unit
0.16
0.42
0.14
0.0084
0.0065
0.14
i
0.030
0.22
0.019
0.025
0.14
0.011
0.028
0.18
0.020
0.0068
34
20.1
0.8
BD
0.8
0.1
0.190
0.028
BD
107.4
6.0
1.51
0.02
BD
0.19
0.01
5.11
0.47
0.9
0.2
>30
4.28
0.07
8.9
1.3
BD
>30
36
6.3
0.2
0.9
0.3
0.4
0.1
0.441
0.024
BO
>300
BD
BD
0.25
0.03
BD
2.7
0.1
>30
0.70
0.08
0.8
0.2
BD
5.194
0.051
40
7.6
0.3
1.6
0.01
BD
0.868
0.050
BO
BO
0.07
0.003
0.2
0.02
BO
0.09
0.002
>30
>30
0.68
0.04
0.9
0.1
BD
15.530
0.780
42
0.4
0.02
0.3
0.03
0.4
0.01
0.555
0.022
BD
122.0
0.5
0.52
0.01
BD
0.15
0.003
BO
4.0
1.1
13.58
0.03
0.24
0.004
0.7
0.04
BD
>30
44
22.6
8.1
2.0
0.6
4.3
0.7
0.687
0.060
BD
146.3
15.1
1.24
0.14
0.4
0.1
1.60
0.26
BD
>30
13.28
0.74
0.72
0.15
1.7
0.5
0.55
0.30
12.147
1.486
Field
46
0.5
0.04
0.4
0.1
BO
0.393
0.010
80
41.8
1.9
BD
BO
BD
BD
>30
2.57
0.06
0.50
0.01
O.I
0.02
BO
3.546
4.034
Sample Number
46 StflY
1.6
0.1
0.3
0.1
BD
0.506
0.041
BD
48.6
1.7
BD
BD
BO
BD
>30
3.06
0.23
0.46
0.03
0.2
0.02
BD
16.114
0.606
50
BD
BD
0.2
0.092
BO
88.6
0.19
BO
0.02
BO
BO
24.23
BD
0.2
BD
6.410
51
BD
BD
0.1
0.072
80
85.9
BO
BO
0.20
BO
BO
23.64
BD
0.3
BD
0.690
52
38.7
0.8
3.0
0.03
10.1
0.2
1.760
O.OB4
BD
230.2
13.4
1.80
0.24
0.6
0.01
2.23
0.02
BO
>30
>30
0.57
0.02
21.6
5.0
0.99
0.01
BD
54
B.B
1.4
0.7
0.1
2.1
0.3
1.692
0.300
BO
>300
0.25
0.04
BD
0.13
0.01
0.56
0.14
6.4
1.0
B.53
1.41
0.21
0.04
17.2
2.6
BD
>30
54 SPLIT 56
7.3
0.1
0.7
0.01
2.4
0.1
1.986
0.050
BD
>300
0.20
0.01
BD
0.15
0.01
80
17.0
2.3
9.23
0.14
0.28
'0.05
8.0
0.4
m
>30
4.7
0.1
0.6
0.02
0.2
0.04
0.700
0.008
BD
>300
BD
BO
0.14
0.01
0.10
0.01
>30
12.62
0.10
0.26
0.02
0.5
0.02
BD
8.068
0.118
BO indicates value ielow Detection Unit (3 slgma) shown In first column
(continued)
-------
APPENDIX 12 (Continued). ICP DATA FOR EP EXTRACTS (mg/1)
10
Element
Al AVG
STO DEM
As AVG
STD DEV
B AVG
STO DEV
Ba AVC
STD DEV
Be AVG
STO DEV
Ca AVG
STO DEV
Cd AVG
STD DEV
Co AVG
STO DEV
Cr AVG
STO OEV
Cu AVG
STO OEV
Fe AVG
STO OEV
Mg AVG
STD OEV
Ni AVG
STO DEV
f>b AVG
STD DEV
V AVG
STO DEV
Zn AVG
STO OEV
Detection
Malt
0.16
0.42
0.14
0.0084
0.0065
0.14
0.030
0.22
0.019
0.02S
0.14
0.011
0.02B
0.18
0.020
0.0068
56 SPLIT
12.1
11.4
1.4
1.2
1.1
2.3
0.64S
0.19B
BO
>300
BD
BO
0.66
1.06
0.06
0.02
>30
16.61
S.24
0.23
0.05
0.6
0.1
0.27
0.46
10.401
2.B41
58-2-S
2.7
0.4
0.9
0.04
0.2
0.04
0.535
0.61S
BO
>300
BO
BD
0.34
0.02
0.06
0.04
10.9
8.0
>30
0.16
0.01
0.3
0.03
BO
5.835
0.423
li "A^ 1* -
ft
5.8
0.7
1.1
0.02
BO
0.826
0.007
BO
>300
0.08
0.01
BD
BO
0.07
0.01
>30
28.27
0.48
0.40
O.OS
2.0
0.2
BD
H.1SS
0.262
64
13.0
0.5
BD
0.7
0.04
0.116
O.OOS
BO
9.1
0.2
BO
BD
0.12
O.OOS
0.08
0.10
4.5
0.3
9.50
0.23
0.12
0.004
60
BO
1.232
0.659
Field Sample Number
66
30.8
0.4
1.6
0.05
2.2
0.4
BO
24.276
0.624
2.0
0.1
0.22
0.03
0.8
0.04
0.38
0.001
14.5
0.3
5.0
0.1
BD
0.18
0.01
12.4
0.3
0.75
0.02
1.727
0.078
66 SPLIT
30.5
1.1
0.5
0.05
2.4
0.3
0.158
O.OOS
BO
24.5
0.8
1.91
0.07
0.3
0.01
0.80
0.01
0.38
0.02
14.0
0.6
5.15
0.16
2.67
0.08
0.2
0.02
0.75
0.03
1.778
0.071
68
10.9
0.1
BO
1.0
0.01
0.243
0.003
BD
15.7
0.1
0.07
0.004
BO
0.29
0.01
0.43
0.01
2.7
0.04
2.72
0.04
1.50
0.02
0.2
0.02
0.11
0.002
1.102
0.016
68 SH.lt
11,9
1.0
0.3
0.1
E.I
0.2
0.374
0.167
BD
37.7
37.S
0.07
0.01
BO
0.33
0.01
0.47
0.05
3.4
0.6
3.26
0.87
1.57
0.04
1.2
i.8
0.12
0.02
4.564
5.650
?0
19.4
0.2
J.I
0.02
BD
0.729
0.013
BD
>300
0.54
0.04
0.2
0.01
BO
80
>30
>30
0.74
0.07 '
10.3 ,
0.9
BO
BD
74
5.9
0.1
0.7
0.01
BO
0.723
0.012
BO
>300
BD
BO
BO
BD
>30
J3.84
0.42
0.29
0.03
0.4
0.01
BO
8.580
0.19S
, 78
3.6
0.8
BO
ffi.2
0.2
0.329
JU66
BD
138.7
34 .S
BD
BO
0.12
(0.002)
0.12
ffi.09
ffl.9
0.6
9.05
0.72
0.78
0.04
. i.i
; ; 1.7
,, m
, , 4.622
4.794
-------
APPENDIX 13. ICP DATA FOR WASTE DIGESTS (mg/kg)
00
o
Element
Al AVG
STD OEV
As AVG
STD DEV
B AVG
STO OEV
B* AVG
STO OEV
Be AVG
STO OEV
Ci AVG
STD DEV
Cd AVG
STD DEV
Co AVG
STO DEV
Cr AVG
STD OEV
Cu AVG
STD DEV
Fe AVG
STO DEV
89 AVG
STO OEV
Nt AVG
STO DEV
Pb AVG
STD DEV
V AVG
STO OEV
Zn AVG
STO DEV
Detection
Unit
16
42
14
0.84
0.65
14
3.0
22
1.9
2.S
14
1.1
2.8
18
2.0
0.68
1
3800
150
90
2
30
2
219.9
3.9
BO
8820
170
9
1
40
2
299
60
193
28
>3000
>3000
385
26
2010
40
48
1
694.0
11.6
2
2910
150
80
10
60
10
95.5
6.2
BO
16630
1380
BO
40
4
183
2
72
5
>3000
>3000
243
34
210
(0.8)
78
8
189.4
9.7
6
15400
300
120
1
660
10
177
4
2.5
0.4
11620
160
84
2
40
10
279
4
1425
25
> 30000
23140
170
51
4
20500
200
BO
> 30000
8
40
10
BO
80
BD
BO
80
10
BD
BO
BD
BO
BD
38
4
BO
BD
BD
26.0
8.6
Field Sample Number
12
300
20
BO
480
40
131.9
9.8
BO
14B40
1500
14
1
40
3
773
97
334
52
>3000
1138
180
81
6
360
60
BO
355.4
54.8
12 SPLIT
750
100
BD
420
30
145.8
25.3
BD
14170
1490
12
1
BO
617
32
338
72
>3000
1000
81
69
6
330
80
.
354.4
19.1
16
13200
90
BO
510
20
248
81
BO
16140
230
40
2
BD
210
2
335
5
> 30000
5071
42
46
2
18780
1830
BD
12720
250
1* Sfc.fi
>6000
BO
170
3
325.7
9.3
BD
17310
390
37
12
BO
157
7
296
10
>3000
>3000
124
7
>3000
30
9
>3000
' 19
2390
420
90
30
340
40
157.6
58.7
BD
> 30000
12
4
40
3
241
13
389
209
>3000
>3000
247
26
BOO
220
BO
436.0
135.5
14 sw.lt 20
2800
470
80
10
370
10
155.0
50.0
BD
>30000
13
4
40
2
262
2
353
90
>3000
>3000
317
16
790
380
BD
407.7
57.6
4000
380
BD
270
no
135.7
3.5
BD
7840
240
10
2
BO
185
38
225
60
>3000
>3000
IBS
11 •
930
30
BD
1003.0
15.5
(continued)
-------
APPENDIX 13 (Continued). ICP DATA FOR WASTE DIGESTS (mg/kg)
00
tleoent
Al
As
B
Ba
Be
Ca
Cd
Co
Cr
Cu
Fe
Hg
HI
Pb
V
Zn
AVG
STO 0£¥
AVG
STO DEV
AVG
STO OEV
AVG
STO DEV
AVG
STO DEV
AVG
STD OEV
AVG
STO OEV
AVG
STD DEV
AVG
STO DEV
AVG
STD DEV
AVG
STO/lfcV
AVG
STD DEV
AVG
STO DEV
AVG
STD DEV
AVG
STO OEV
AVG
STO DEV
22
2310
140
BD
40
4
96.3
7.1
BO
-
7330
160
7
1
BO
80
7
SO
1
>3000
-
613
38
52
S
40
4
5
0.3
131.1
15.0
*4
1540
230
BO
480
20
123.8
l.S
^
-
8030
80
16
3
40
4
299
8
362
3
>3000
-
1698
27
101
2
300
10
BD
1013.7
47.3
28
>6000
-
60
10
600
10
198.5
10.3
2.0
0.1
>30000
-
28
3
30
1
328
4
455
64
>3000
-
>3000
-
76
3
>3000
BD
>3000
-
34
>6000
-
230
3
800
4
148.9
1.0
BO
-
19000
140
90
1
60
4
2014
16
1985
12
>3000
-
1952
1
1361
7
>3000
47
I
>3000
-
36
>6000
-
BO
-
400
20
151.6
6.4
BD
-
17120
850
12
1
30
5
404
16
369
4
>3000
-
>3000
-
183
3
870
50
BO
-
691.3
11.8
Field
40
5780
700
320
30
370
40
146.3
6.0
BO
-
> 30000
-
11
5
60
3
316
26
200
27
>3000
-
>3000
-
134
13
600
20
107
38
1605.1
30.2
Samnle Number
42
>6000
-
70
10
80
-
75.9
1.0
1.3
0.5
7290
80
40
2
BD
-
BO
-
265
3
>3000
-
2225
56
33
1
2130
40
7
2
>3000
-
44
4620
80
300
3
1320
20
96.4
2.2
BO
-
1210
190
145
3
110
10
1865
26
>3000
-
>3000
-
2452
27
367
4
>3000
-
32
5
>3000
-
46
>6000
-
520
80
80
-
962.9
81.2
5.6
1.5
BO
-
8
3
40
2
302
94
138
89
>30QO
-
>3000
-
36
13
ISO
20
7
8
655.5
209.6
46 SPLIT
>6000
-
460
100
BO
-
921.5
76.9
5.2
0.4
BD
-
8
1
40
3
279
42
214
42
>3000
-
>3000
-
37
10
160
10
14
2
675.2
85.9
52
>6000
•
380
360
870
20
807.8
46 .S
BO
-
13830
200
901
4
90
3
406
14
>3000
-
>30QO
1 — '
>3000
-
186
IS
>3000
-
216
196
BD
-
54
4060
SO
100
2
BD
•
306.1
24.3
BD
"
13530
260
18
0.4
BD
-
BO
-
388
9
>3000
"
1223
18
44
I
2340
20
33
1
>3000
-
64 SPLlt
3740
60
100
2
80
~
281.4
224. 2
BD
™
12020
310
16
1
BD
"
BD
"
359
4
>3000
~
1133
27
45
2
2080
'30
32
S
>3000
-
-------
APPENDIX 13 (Continued). ICP DATA FOR WASTE DIGESTS (mg/kg)
00
ro
Field Sample Number
Etc
A1
As
8
e*
Be
C*
Cd
Co
Cr
Cu
Fe
Hg
HI
Pb
V
In
«ent
AVG
STD OEV
AVG
STO OEV
AVG
STO DEV
AVG
STO OEV
AVG
STO OEV
AVG
STO DEV
AVG
STD OEV
AVG
STD DEV
AVG
STO OEV
AVG
STD DEV
AVG
STD DEV
AVG
STO DEV
AVG
STD DEV
AVG
STO DEV
AVG
STO DEV
AVG
STO OEV
56
4030
210
no
10
230
10
105. 1
10.2
BO
12850
S10
5
0.1
BO
199
1
193
a
>3000
1212
17
56
4
340
10
41
4
774.1
27.4
56 SPLIT
3080
180
170
10
1010
20
53.6
5.3
BO
4090
140
32
1
70
1
714
9
467
S
>3000
791
23
190
3
720
10
24
1
857.8
12.8
58
5310
40
90
10
BO
50.4
2.9
BO
14220
470
6
1
BO
BO
174
23
>3000
1741
24
36
3
230
10
24
2
546.9
29.9
60
5650
520
220
10
300
10
143.4
12.0
BO
27040
930
13
0.2
60
3
389
28
362
23
>3000
2234
80
121
6
1670
60
129
10
1015.6
56.5
64
>6000
90
1
60
72.8
4.6
60
19360
430
60
BO
78
3
191
6
>3000
8564
110
77
1
90
1
20
0.3
103.2
0.8
66
3130
110
220
10
820
60
116.1
5.4
BO
2290
80
163
7
70
4
2562
210
556
19
>3000
1004
34
1036
44
380
5
58
3
588.8
8.3
66 SPLIT
3020
100
210
10
790
20
113.3
1.3
60
2260
60
158
a
60
1
2367
63
528
IS
>3000
981
32
937
20
360
10
55
2
547.5
12.7
68
1940
60
200
10
800
60
136.9
0.5
BD
1170
4
21
6
70
3
2151
265
629
28
>3000
513
16
711
52
400
10
107
11
544.8
21.5
70
>6000
160
10
280
2
123.0
1.9
1.2
0.8
10740
110
104
3
30
1
22
3
662
21
>3000
2937
96
66
S
2910
170
44
4
>3000
74
5900
40
200
10
300
4
299.8
18.2
BD
18260
140
13
4
30
10
252
6
661
14
>3000
1663
37
124
12
1540
5
66
5
1423.2
46.5
78
4080
110
100
20
240
2
105.8
2.0
BD
13780
620
10
0.1
BD
198
92
218
49
>3000
1215
40
52
2
320
10
39
3
819.B
19.2
-------
TECHNICAL REPORT DATA
ffletue read Instructions on the reverse before completing)
1, REPORT NO.
; EPA-600/4-81-028
3. RECIPIENT'S ACCESSION NO.
,4. TITLE AND SUBTITLE
SAMPLING AND ANALYSIS OF WASTES GENERATED
;BY GRAY IRON FOUNDRIES
8. REPORT DATE
April 1981
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
Werner F. Beckert, Thomas A. Hlnners,
Llewellyn R. Williams, Eugene P. Meier, EMSL-LV
Thomas E. Gran. NSI
8. PERFORMING ORGANIZATION REPORT NO
9. PERFORMING ORGANIZATION NAMK AND ADDRESS
Environmental Monitoring Systems Laboratory
Office of Research and Development
UeS. Environmental Protection Agency
Las Vegas, Nevada 89114
1O. PROGRAM ELEMENT NO.
ABSD1A/CBSD1A
11. CONTRACT/GRANT NO.
12. SPONSORING AGENCY NAME AND ADDRESS
U.S. Environmental Protection Agency—Las Vegas, NV
Office of Research and Development
Environmental Monitoring Systems Laboratory
Las Vegas, Nevada 89114
13. TYPE OF REPORT AND PERIOD COVERED
Tffiff
14. SPONSORING AGENCY CODE
EPA/600/07
16. SUPPLEMENTARY NOTES
thirty (30) wastes generated by 21 gray iron foundries in Pennsylvania and
Michigan were sampled and analyzed. The samples were collected by Northrop Services,
Inc., in accordance with strict chain-of-custody procedures, and sent to the
Environmental Monitoring Systems Laboratory, Las Vegas (EMSL-LV). Three aliquots of
each sample were extracted in accordance with the EPA Extraction Procedure (EP)
(45CFR261.24). A second set of three aliquots of each sample was digested with nitric
acid/hydrogen peroxide. Both the extracts and digests were analyzed, for 16 elements by
ICP and for cadmium, chromium and lead by atomic absorption speetrophotometry0
At the request of the American Foundrymen Society, aliquots of all raw samples, as
well as nine extracts and nine digests, were sent to Dr. W. Boyle, University of
Wisconsin, for independent analysis. Twelve aliquots of raw samples, nine extracts and
nine digests were analyzed by an analytical laboratory under contract to EMSL-LV.
Excellent agreement was obtained between the three laboratories.
Of the 30 samples evaluated for EP toxicity, a total of 9 (30%) exceeded the
criteria levels for cadmium and/or lead. None of the extracts exceeded the hazardous
waste criterion level for chromium.
16. A8STI
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.lOENTIFIERS/OPEN ENDED TERMS
e. COSATI Field/Group
18. DISTRIBUTION STATEMENT
RELEASE TO PUBLIC
19. SECURITY CLASS (Tilts Report)
UNCLASSIFIED
21. NO. OF PAGES
90
20. SECURITY CLASS (This page)
I IMP!
22. PRICE
EPA Form 2220-1 (R«v. 4—77) PHKVIOU* COITION is ossoLCrc
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