ASTM D6323-98(2003)
(Guide)Standard Guide for Laboratory Subsampling of Media Related to Waste Management Activities (Withdrawn 2012)
Standard Guide for Laboratory Subsampling of Media Related to Waste Management Activities (Withdrawn 2012)
ABSTRACT
This guide covers common techniques for laboratory subsampling of media related to waste management activities. This guide includes several sample homogenization techniques, including mixing and grinding, as well as information on how to obtain a specimen or split laboratory samples. The limitations and advantages of sample preparation options are presented in details. The matrix specific subsampling procedures are presented in detail.
SIGNIFICANCE AND USE
This guide discusses options for taking a subsample from a sample submitted to a laboratory. If followed, it will minimize the bias and variance of the characteristic of interest of the laboratory sample prior to analysis.
The guide will describe appropriate instructions to be submitted to the laboratory with the field sample.
This guide is intended for use in the laboratory to take a representative subsample or specimen of the whole field sample for direct analysis or sample preparation for analysis. It is intended for field personnel, data users, laboratory sample reception personnel, analysts, and managers.
To obtain a representative subsample, layer analysis, grinding, mixing, and changing the physical state such as digesting, drying, melting or freezing may be required. This guide considers cone and quartering, riffle splitting, and particle size reduction.
SCOPE
1.1 This guide covers common techniques for obtaining representative subsamples from a sample received at a laboratory for analysis. These samples may include solids, sludges, liquids, or multilayered liquids (with or without solids).
1.2 The procedures and techniques discussed in this guide depend upon the sample matrix, the type of sample preparation and analysis performed, the characteristic(s) of interest, and the project specific instructions or data quality objectives.
1.3 This guide includes several sample homogenization techniques, including mixing and grinding, as well as information on how to obtain a specimen or split laboratory samples.
1.4 This guide does not apply to air or gas sampling.
1.5 The values stated in SI units are to be regarded as the standard.
1.6 This standard does not purport to address all of the safety concerns, 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.
WITHDRAWN RATIONALE
This guide covers common techniques for obtaining representative subsamples from a sample received at a laboratory for analysis. These samples may include solids, sludges, liquids, or multilayered liquids (with or without solids).
Formerly under the jurisdiction of Committee D34 on Waste Management, this guide was withdrawn in June 2012 in accordance with section 10.5.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D6323–98 (Reapproved 2003)
Standard Guide for
Laboratory Subsampling of Media Related to Waste
Management Activities
This standard is issued under the fixed designation D6323; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope D4823 Guide for Core Sampling Submerged, Unconsoli-
dated Sediments
1.1 This guide covers common techniques for obtaining
D5743 Practice for Sampling Single or Multilayered Liq-
representative subsamples from a sample received at a labora-
uids, With or Without Solids, in Drums or Similar Con-
tory for analysis. These samples may include solids, sludges,
tainers
liquids, or multilayered liquids (with or without solids).
D5792 Practice for Generation of Environmental Data Re-
1.2 The procedures and techniques discussed in this guide
lated to Waste Management Activities: Development of
depend upon the sample matrix, the type of sample preparation
Data Quality Objectives
andanalysisperformed,thecharacteristic(s)ofinterest,andthe
D5956 Guide for Sampling Strategies for Heterogeneous
project specific instructions or data quality objectives.
Wastes
1.3 This guide includes several sample homogenization
D6051 Guide for Composite Sampling and Field Subsam-
techniques, including mixing and grinding, as well as informa-
pling for Environmental Waste Management Activities
tion on how to obtain a specimen or split laboratory samples.
1.4 This guide does not apply to air or gas sampling.
3. Terminology
1.5 The values stated in SI units are to be regarded as the
3.1 contaminant unit, n—the largest particle size that con-
standard.
tains the contaminant of interest
1.6 This standard does not purport to address all of the
3.1.1 Discussion—The contaminant of concern, as defined
safety concerns, if any, associated with its use. It is the
by the project objectives, may be associated with all the
responsibility of the user of this standard to establish appro-
particle sizes or associated with only a certain particle size or
priate safety and health practices and determine the applica-
sizes. At the time of waste generation, discharge or spill, the
bility of regulatory limitations prior to use.
particle size of this contaminant of concern may be on the
2. Referenced Documents atomic or molecular scale, such as solvent spill into sand, or a
macro scale, such as lead acid batteries at a dump site. The
2.1 ASTM Standards:
contaminant unit may also be in-between these scales, such as
C702 Practice for Reducing Samples of Aggregate to Test-
leadparticlesencapsulatedincoal.Inpractice,thecontaminant
ing Size
unit may change if the contaminant unit becomes absorbed or
C859 Terminology Relating to Nuclear Materials
adsorbed to particles larger than the contaminant unit. It is the
D346 Practice for Collection and Preparation of Coke
size of the contaminant unit at the time of subsampling, not at
Samples for Laboratory Analysis
the time of generation, that is referred to as the contaminant
D2234/D2234M Practice for Collection of a Gross Sample
unit.
of Coal
3.2 maximum allowable particle size, n—the largest lineal
D4547 Guide for Sampling Waste and Soils for Volatile
dimension of a sample’s individual particles accepted for a
Organic Compounds
given sample mass.
3.2.1 Discussion—The maximum allowable particle size is
sometimes referred to as the allowable particle size. A simple
This guide is under the jurisdiction of ASTM Committee D34 on Waste
method of measurement is a sieve.
Management and is the direct responsibility of Subcommittee D34.01.01 on
3.3 multilayered sample, n—a sample consisting of two or
Planning for Sampling.
more clearly differentiated components.
Current edition approved Aug. 10, 2003. Published December 1998. DOI:
10.1520/D6323-98R03.
3.3.1 Discussion—Multilayered samples are those with two
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
or more distinct visual layers of material. These layers may be
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
the result of differences in density, such as liquid/liquid layers
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. (for example, chlorinated solvents and water, water and oil),
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6323–98 (2003)
liquid/solid layers (for example, sludge), solid/solid layers (for 5.1.1 Theappropriateinstructionsmustbereviewedbyboth
example, small rocks and large rocks), or combinations of the laboratory receiving personnel and the analyst(s) or super-
these layers (for example water, oil, and soil). These layers visor. If there are no instructions, the appropriate laboratory
may also be the result of depositional layering, such as green personnel should contact the data user. Options should be
clay and silty sand from a coring sample. discussed and clarified prior to initiating any subsampling
3.4 particle size, n—the controlling lineal dimension of procedure. These instructions may include such options as
individual particles (see Terminology C859). those found inTable 1.The limitations and advantages of these
3.5 representative subsample, n—a subsample collected in methods are also found in this table. The data user should be
informed about the limitations and advantages of all subsam-
such a manner that it reflects one or more characteristics of
interest (as defined by the project objectives) of the laboratory pling procedures prior to deciding which one to use.
sample from which it was collected.
5.1.2 If the data user still provides no instructions upon
3.5.1 Discussion—A representative subsample can apply to
being contacted, laboratory personnel should explain to the
a single sample, or a composite sample.
data user that the laboratory’s standard operating procedures,
3.6 sample, n—a portion of material taken from a larger
which reflect the concerns and issues discussed in this stan-
quantity for the purpose of estimating properties or composi-
dard, will be used. The sample should be treated as if the scale
tion of the larger quantity, (see Guide D6051).
of the contamination is on the micro level, and no artifacts can
3.7 sludge, n—Any mixture of solids that settles out of
be removed. Since sample matrices and types and mechanisms
solution. Sludges contain liquids that are not apparent as free
of contamination are infinitely variable and require judgments
liquids, (see Practice D5743). to be made, it is advisable that experienced analysts decide
3.8 subsample, n—a portion of a sample taken for the which subsampling techniques be employed.These procedures
purpose of estimating properties or composition of the whole must be discussed and clarified with the data user prior to
sample, (see Guide D6051).
initiating any subsampling procedure.
3.8.1 Discussion—A subsample is also commonly referred
5.2 If the sample integrity or composition is not as antici-
to by such terms as specimen, aliquot, subsample, or analytical
pated, the data user must be contacted to confirm or clarify the
subsample. To avoid confusion, the term specimen is used to
instructions. An example of when this would be necessary
refer to the final portion of the sample used during analysis.
would be a case where a coring sleeve was received at the
Thematerialreceivedatthelaboratorywillbereferredtoasthe
laboratory.Onopeningthecontainer,theanalystnoticesclayin
laboratory sample.All portions subsampled in-between receipt
one end of the sleeve, and sand at the other end. Before the
at the laboratory and the specimen are referred to as sub-
analyst can proceed, the appropriate instructions from the data
samples. The subsample may be the specimen.
user must be obtained.
5.2.1 Field samples should be collected in appropriate
4. Significance and Use
containers for the analyses requested. If the submitted sample
is improperly collected, the data user should be contacted by
4.1 This guide discusses options for taking a subsample
from a sample submitted to a laboratory. If followed, it will laboratory personnel. If the data user authorizes the laboratory
to continue with the analysis, a note should be made in the
minimize the bias and variance of the characteristic of interest
of the laboratory sample prior to analysis. receival documentation, and also in the case narrative in the
final report.
4.2 The guide will describe appropriate instructions to be
submitted to the laboratory with the field sample.
5.3 Documentation during the subsampling process is criti-
4.3 This guide is intended for use in the laboratory to take a
cal. Since subsampling techniques may bias the results, the
representative subsample or specimen of the whole field subsampling method used must be noted in the analytical
sample for direct analysis or sample preparation for analysis. It
logbook.
is intended for field personnel, data users, laboratory sample
5.3.1 Anytime the analytical result will be biased, it must be
reception personnel, analysts, and managers.
documented, and the data user should be notified prior to
4.4 To obtain a representative subsample, layer analysis,
beginning any subsampling technique. For example, if head-
grinding, mixing, and changing the physical state such as
space exists in a container arriving at the laboratory, some
digesting, drying, melting or freezing may be required. This
volatile components will have partitioned into that headspace.
guide considers cone and quartering, riffle splitting, and
However, if the data user decides to proceed with the analysis,
particle size reduction.
the analytical logbook and the case narrative on the final report
should indicate this condition.
5. General Considerations
5.4 Particle size is the physical dimension of an object’s
5.1 Successful implementation of this standard depends on pieces or parts. The maximum particle size contained within a
effective communication between the data user and the labo- laboratory sample is the largest of these pieces. The contami-
ratory staff. The selection of optimal subsampling procedures, nant of concern, as defined by the project objectives, may be
techniques, and strategy by the laboratory depends on the associated with all particle sizes or associated with only a
intended use of the data. The data user should submit appro- certain particle size or sizes. The largest of these particle sizes,
priate instructions with all samples and, when necessary, the that contain the contaminant of interest, would be the contami-
laboratory staff shouldcontactthedatauserforconfirmationor nant unit. The contaminant unit, at the time of waste genera-
further clarification of these instructions. tion, discharge or spill, may be on the atomic or molecular
D6323–98 (2003)
TABLE 1 Limitations and Advantages of Sample Preparation Options
Instruction Limitations Advantages
Remove artifacts, such as rocks and twigs, from the (1) May bias analytical results by altering contaminant (1) May be easier to subsample, (2) May be easier to
sample prior to subsampling concentration, (2) May bias sample if results are not analyze, (3) Appropriate if the target population is
properly weight averaged. material minus artifacts.
Digest or extract the contaminant from the outside May bias sample if contaminant is within the large (1) May be easier to analyze, (2) May prevent need
A
of the large particles particles. for weight average calculation.
A
Digest or extract particle sizes separately (1) Separation of particle sizes may be difficult, (1) Allows some particle size consistency during
(2) May bias sample if results are not properly weight analysis, (2) May be easier to subsample within
averaged, (3) Higher cost. portions after separation.
Form an emulsion layer so that the material may May bias the sample if a complete emulsion is not (1) May be easier to subsample as a homogeneous
A
be treated as homogeneous liquid achieved. liquid,
Separate liquid layers (1) Separation of layers may be difficult, especially (1) May be easier to analyze, (2) May be easier to
at the interface, (2) May bias sample if results are subsample within portions after separation, (3) Allows
not properly weight averaged. different preparation methods within each layer.
Dry sample May alter chemistry or change stability of some (1) Allows for consistency of subsampling for liquid/
A
compounds. solid mixtures, (2) Analytes reported unbiased by
moisture content.
Change the physical state, such as freeze the May be difficult to achieve complete freezing or Allows for consistency of subsampling.
material so that it may be treated as a solid, or melting and maintain it long enough to get a
A
melt the material so that it may be treated as a subsample.
liquid
Analyze only one layer of multilayered samples, May bias the sample if there is cross-contamination (1) Possible cost savings to customer, (2) May be
such as analyze only the oil portion of an oil/water between layers easier to subsample from a single layer, (3) May be
mixture for PCBs easier to analyze.
Composite portions of the sample for volatile (1) May overload gas chromatography columns if (1) May prevent losses of volatile because the sample
analysis directly in a purge unit vs. individual sample has high amounts of solvents in each portion, is handled only once, (2) Possible cost savings to
analysis of these portions (2) Separation of portions may be difficult. customer, (3) May prevent need for weight average
calculation.
Reduce particle size (1) Increasing surface area may effect data in some Allows for consistency of subsampling.
procedure with particle digestion or extraction, such
A
as TCLP, (2) May be difficult, depending on matrix.
A
Use standard methods for solids (for example, Dependent on method. See 7.1.5 for more Dependent on method. See 7.1.5 for more information.
cone and quarter, grind, riffle, sieve) information.
A
May be unsuitable for samples to be analyzed for volatile constituents.
scale, such as a solvent spill into sand, or a macro scale, such dated by the sample preparation procedure, multiple sub-
as lead acid batteries at a dump site.The contaminant unit may samples (of equal mass) can be extracted/digested, and the
also be in-between these scales, such as lead particles encap- extracts/digests combined and mixed prior to removal of the
sulated in coal. In practice, the contaminant unit may change if standard volume specimen needed for analysis. Another alter-
the contamin
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