ASTM D4793-93
(Test Method)Standard Test Method for Sequential Batch Extraction of Waste with Water
Standard Test Method for Sequential Batch Extraction of Waste with Water
SCOPE
1.1 This test method is a procedure for the sequential leaching of a waste containing at least five % solids to generate solutions to be used to determine the constituents leached under the specified testing conditions.
1.2 This test method calls for the shaking of a known weight of waste with water of a specified purity and the separation of the aqueous phase for analysis. The procedure is conducted ten times in sequence on the same sample of waste and generates ten aqueous solutions.
1.3 This test method is intended to describe the procedure for performing sequential batch extractions only. It does not describe all types of sampling and analytical requirements that may be associated with its application.
1.4 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D 4793 – 93
Standard Test Method for
Sequential Batch Extraction of Waste with Water
This standard is issued under the fixed designation D 4793; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Terminology
1.1 This test method is a procedure for the sequential 3.1 Definitions:
leaching of a waste containing at least five % solids to generate 3.1.1 For definitions of terms used in this test method, see
solutions to be used to determine the constituents leached Terminology D 1129.
under the specified testing conditions. 3.2 Symbols:Symbols:
1.2 This test method calls for the shaking of a known weight 3.2.1 Variables listed in this test method are defined in the
of waste with water of a specified purity and the separation of individual sections where they are discussed. A list of defined
the aqueous phase for analysis. The procedure is conducted ten variables is also given in Section 11.
times in sequence on the same sample of waste and generates 3.2.2 Explanation of Variables:
ten aqueous solutions.
1.3 This test method is intended to describe the procedure
¯
X = total mean value
t
for performing sequential batch extractions only. It does not
¯
X = analytical mean value (calculated using data from
a
describe all types of sampling and analytical requirements that
analysis of standards)
may be associated with its application.
S = total standard deviation
tt
1.4 This standard does not purport to address all of the
S = analytical standard deviation
ta
safety problems, if any, associated with its use. It is the
S = estimated standard deviation due to the extraction
te
responsibility of the user of this standard to establish appro-
procedure
priate safety and health practices and determine the applica-
S = total single operator standard deviation
ot
bility of regulatory limitations prior to use.
S = analytical single operator standard deviation
oa
S = estimated single operator standard deviation due to
oe
2. Referenced Documents
the extraction procedure
2.1 ASTM Standards:
4. Significance and Use
D 75 Practices for Sampling Aggregates
D 420 Practice for Investigating and Sampling Soil and
4.1 This test method is intended as a means for obtaining
Rock for Engineering Purposes
sequential extracts of a waste. The extracts may be used to
D 653 Terminology Relating to Soil, Rock, and Contained
estimate the release of certain constituents of the waste under
Fluids
the laboratory conditions described in this test method.
D 1129 Terminology Relating to Water
4.2 This test method is not intended to provide extracts that
D 1193 Specification for Reagent Water
are representative of the actual leachate produced from a waste
D 2216 Test Method for Laboratory Determination of Water
in the field or to produce extracts to be used as the sole basis
(Moisture) Content of Soil, Rock, and Soil-Aggregate
of engineering design.
Mixtures
4.3 This test method is not intended to simulate site-specific
D 2234 Test Method for Collection of a Gross Sample of
leaching conditions. It has not been demonstrated to simulate
Coal
actual disposal site leaching conditions.
D 2777 Practice for Determination of Precision and Bias of
4.4 An intent of this test method is that the final pH of each
Methods of Committee D-19 on Water
of the extracts reflects the interaction of the extractant with the
D 3370 Practices for Sampling Water
buffering capacity of the waste.
4.5 An intent of this test method is that the water extractions
1 reflect conditions where the waste is the dominant factor in
This test method is under the jurisdiction of ASTM Committee D-34 on Waste
Management and is the direct responsibility of Subcommittee D34.02 on Physical determining the pH of the extracts.
and Chemical Characterization.
4.6 This test method produces extracts that are amenable to
Current edition approved Jan. 15, 1993. Published March 1993. Originally
the determination of both major and minor constituents. When
published as D 4793 – 88. Last previous edition D 4793 – 88.
minor constituents are being determined, it is especially
Annual Book of ASTM Standards, Vol 04.03.
Annual Book of ASTM Standards, Vol 04.08.
important that precautions are taken in sample storage and
Annual Book of ASTM Standards, Vol 11.01.
handling to avoid possible contamination of the samples.
Annual Book of ASTM Standards, Vol 05.05.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 4793
4.7 This test method has been tested to determine its consistent with the analyses to be performed. See Practices
applicability to certain inorganic components in the waste. This D 3370, Section 13.
test method has not been tested for applicability to organic
substances, volatile matter (see Note 3 in 5.15), or biologically 6. Reagents
active samples.
6.1 Purity of Reagents—Reagent grade chemicals shall be
4.8 The agitation technique, rate, liquid-to-solid ratio, and
used in all tests. Unless otherwise indicated, it is intended that
filtration conditions specified in the procedure may not be
all reagents shall conform to the specifications of the American
suitable for extracting all types of wastes (see Sections 7, 8,
Chemical Society, where such specifications are available.
and the discussion in Appendix X1).
Other grades may be used, provided it is first ascertained that
the reagent is of sufficiently high purity to permit its use
5. Apparatus
without lessening the accuracy of the determination.
5.1 Straightedge (such as a thin-edged yard stick).
6.2 Purity of Water—Unless otherwise indicated, references
5.2 Impermeable Sheet, of glazed paper, oil cloth, or other
to water shall be understood to mean Type IV reagent water at
flexible material of a composition suitable to the analytes of
18 to 27°C (Specification D 1193). The method by which the
interest.
water is prepared, that is, distillation, ion exchange, reverse
5.3 Drying Pans or Dishes—Two per waste (for example,
osmosis, electrodialysis, or a combination thereof, should
aluminum tins, porcelain dishes, or glass weighing pans),
remain constant throughout testing.
suitable to the waste being tested and the instructions given in
9.2.
7. Sampling
5.4 Drying Oven—Any thermostatically controlled drying
7.1 Obtain a representative sample of the waste to be tested
oven capable of maintaining a steady temperature of 62°C in
using ASTM sampling methods developed for the specific
a range from 100 to 110°C.
industry where available (see Practices D 75 and D 420,
5.5 Desiccator, having the capacity to hold the drying pans
Terminology D 653, and Test Method D 2234).
described in 5.3 and the crucibles described in 5.8.
7.2 Where no specific methods are available, sampling
5.6 Laboratory Balance, capable of weighing to 0.1 g.
methodology for material of similar physical form shall be
5.7 Pipet, 10-mL capacity.
used.
5.8 Crucibles—Two per waste, porcelain, 20-mL capacity
7.3 The amount of sample to be sent to the laboratory
each.
should be sufficient to perform the solids content determination
5.9 Analytical Balance, capable of weighing to 0.1 mg.
as specified in 9.2 and to provide 100 g of sample on a dry
5.10 Large Glass Funnel.
weight basis for each extraction.
5.11 Wash Bottle, 500-mL capacity.
7.4 It is important that the sample of the waste be represen-
5.12 pH Meter—Any pH meter with a readability of 0.01
tative with respect to surface area, as variations in surface area
units and an accuracy of 60.05 units at 25°C is acceptable.
would directly affect the leaching characteristics of the sample.
5.13 Agitation Equipment, of any type that rotates the
Waste samples should contain a representative distribution of
extraction vessel in an end-over-end fashion at a rate of 30 6 2
particle sizes.
r/min such that the axis of rotation is horizontal and it goes
through the center of the bottle, (see Fig. 1 and the discussion NOTE 4—Information on obtaining representative samples can also be
found in Pierre Gy’s Sampling Theory and Sampling Practice, Volumes I
of agitation in Appendix X1).
and II, by F. Picard, CRC Press, 1989.
NOTE 1—Similar devices having a different axial arrangement may be
7.5 In order to prevent sample contamination or constituent
used if equivalency can be demonstrated.
loss prior to extraction, keep samples in closed containers
5.14 Pressure Filtration Assembly—A pressure filtration
appropriate to the sample type and desired analysis. See
device of a composition suitable to the nature of the analyses
Practices D 3370 for guidance. Record the storage conditions
to be performed and equipped with a 0.45 or 0.8-μm pore-size
and handling procedures in the report.
filter (see Note 7, pertaining to 9.4).
7.6 The time between collection and extraction of the
5.15 Extraction Vessels, cylindrical, wide-mouth, of a com-
sample should be determined by the nature of the sample and
position suitable to the nature of the waste and analyses to be
the information desired. See Practices D 3370 for guidance.
performed, constructed of materials that will not allow sorption
Report the length of time between sample collection and
of constituents of interest, and sturdy enough to withstand the
extraction.
impact of the falling sample fragments. Container size should
be selected so that the sample plus extraction fluid occupy
8. Sample Preparation
approximately 95 % of the container. Containers must have
8.1 For free-flowing particulate solid wastes, obtain a
water-tight closure. Containers for samples where gases may
be released should be provided with a venting mechanism.
NOTE 2—Suitable container sizes range from 4.0 to 4.5 in. (102 to 114
“Reagent Chemicals, American Chemical Society Specifications,” Am. Chemi-
mm) in diameter and 8.5 to 13.0 in. (216 to 330 mm) in height.
cal Soc., Washington, DC. For suggestions on the testing of reagents not listed by
NOTE 3—The venting of the container has the potential to affect the
the American Chemical Society, see “Reagent Chemicals and Standards,” by Joseph
concentration of volatile compounds in the extracts.
Rosin, D. Van Nostrand Co., Inc., New York, NY, and the “United States
5.15.1 Extraction vessels should be cleaned in a manner Pharmacopeia.”
D 4793
FIG. 1 Extractors
sample of the approximate size required in the test by quarter- merely slide along. Continue the operation with each corner,
ing the sample (Section 7) received for testing on an imper- proceeding in a clockwise direction. Repeat this operation ten
meable sheet of glazed paper, oil cloth, or other flexible times.
material as follows: 8.1.4 Lift all four corners of the sheet towards the center
8.1.1 Empty the sample container into the center of the and, holding all four corners together, raise the entire sheet into
sheet. the air to form a pocket for the sample.
8.1.2 Flatten out the sample gently with a suitable straight- 8.1.5 Repeat 8.1.2.
edge until it is spread uniformly to a depth at least twice the 8.1.6 With a straightedge (such as a thin-edged yard stick),
maximum particle diameter. one at least as long as the flattened mound of sample, gently
8.1.3 Remix the sample by lifting a corner of the sheet and divide the sample into quarters. Make an effort to avoid using
drawing it across, low down, to the opposite corner in a manner pressure on the straightedge sufficient to cause damage to the
that the material is made to roll over and over and does not particles.
D 4793
8.1.7 Discard alternate quarters. weight basis to the extraction vessel. Calculate the amount of
8.1.8 If further reduction of sample size is necessary, repeat waste as received to add using the following equation:
8.1.3-8.1.7. Use a sample size to give 100 g of solid for each
M 5 (2)
extraction. Provide additional samples for determination of
S
solids content. If smaller samples are used in the test, report
where:
this fact.
M = mass of waste as received to add to the extraction
NOTE 5—For other acceptable methods for mixing and subsampling
vessel to give 100 g (weighed to 60.1 g) of solid
free-flowing solid particulate wastes, see Pierre Gy’s Sampling Theory
waste.
and Sampling Practice, Volumes I and II, by F. Picard, CRC Press, 1989.
9.3.2.1 If a mass of solid waste on a dry weight basis other
The method of subsampling should be determined by the physical
than 100 g is used, (Eq 2) through (4) must be modified to
properties of the waste, analytes of interest, and equipment available.
reflect the use of a mass other than 100 g. Replace 100 in these
8.2 For field-cored solid wastes or castings produced in the
equations with the mass used. Use of a mass other than 100 g
laboratory, cut a representative section weighing approxi-
is not recommended.
mately 100 g for testing plus samples for determination for
9.3.3 Add a volume in millilitres, V , of test water (see 6.2)
vl
solids content. Shape the sample so that the leaching solution
to the extraction vessel determined using the following equa-
will cover the material to be leached.
tions:
8.3 For multiphasic wastes, mix thoroughly to ensure that a
M 5 M 2 100 (3)
representative sample will be withdrawn. Take samples for
sw
determination of solids content at the same time as the test
samples.
where:
M = mass of moisture in the sample added to the
sw
9. Procedure
extraction vessel, g.
9.1 Record the physical description of the sample to be
V 5 ~20! ~100! 2 M . (4)
v sw
tested, including particle size so far as it is known.
9.2 Solids Content—Determine the solids content of two
separate portions of the sample as follows: 9.3.4 Agitate continuously for 18 6 0.25 h at 18 to 27°C.
9.2.1 Dry to a constant weight at 104 6 2°C two dishes or Record the agitation time and temperature.
pans of size suitable to the solid waste being tested. Cool in a
9.3.5 Open the extraction vessel. Observe and record any
desiccator and weigh. Record the values to 60.1 g.
visible physical changes in the sample and leaching solution.
9.2.2 Put an appropriately sized portion of sample of the
Record the pH of the waste/leaching solution slurry.
waste to be tested into each pan. Scale the weight used to the
9.4 Filtration—Transfer as much of the waste/leaching
physical form of the waste tested. Use a minimum of 50 g, but
solution as possible through a large glass funnel to a pressure
use larger samples where particles larger than 10 mm in
filtration device equipped with a 0.45 or 0.8-μm filter. Transfer
average diameter
...
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