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ASTM D3976-92(2005)

(Practice)

Standard Practice for Preparation of Sediment Samples for Chemical Analysis

Standard Practice for Preparation of Sediment Samples for Chemical Analysis

SIGNIFICANCE AND USE
The chemical analysis of sediments, collected from such locations as streams, rivers, ponds, lakes, and oceans can provide information of environmental significance.
Sediment samples are inherently heterogeneous in that they contain occluded water in varying and unpredictable amounts and may contain foreign objects or material not ordinarily considered as sediment, the inclusion of which would result in inaccurate analysis.
Standard methods for separating foreign objects to facilitate homogenization will minimize errors due to poor mixing and inclusion of extraneous material.
Standardized procedures for drying provide a means for reporting analytical values to a common dry weight basis.
SCOPE
1.1 This practice describes standard procedures for preparation of test samples (including the removal of occluded water and moisture) of field samples collected from locations such as streams, rivers, ponds, lakes, and oceans.
1.2 These procedures are applicable to the determination of volatile, semivolatile, and nonvolatile constituents of sediments.
1.3 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. For a specific precautionary statement, see Note 3.

General Information

Status
Historical
Publication Date
30-Jun-2005
ICS
13.060.45 - Examination of water in general
Technical Committee
D19 - Water
Drafting Committee
D19.07 - Sediments, Geomorphology, and Open-Channel Flow
Current Stage
Ref Project

Relations

Replaces
ASTM D3976-92(2001) - Standard Practice for Preparation of Sediment Samples for Chemical Analysis
Effective Date
01-Jul-2005
Replaced By
ASTM D3976-92(2010) - Standard Practice for Preparation of Sediment Samples for Chemical Analysis
Effective Date
15-Jun-2010
Referred By
ASTM D4698-21 - Standard Practice for Total Digestion of Sediment Samples for Chemical Analysis of Various Metals
Effective Date
01-Jul-2005
Referred By
ASTM E1611-21 - Standard Guide for Conducting Sediment Toxicity Tests with Polychaetous Annelids
Effective Date
01-Jul-2005
Referred By
ASTM D5074-90(2022) - Standard Practice for Preparation of Natural-Matrix Sediment Reference Samples for Major and Trace Inorganic Constituents Analysis by Partial Extraction Procedures
Effective Date
01-Jul-2005
Referred By
ASTM D3975-93(2019) - Standard Practice for Development and Use (Preparation) of Samples for Collaborative Testing of Methods for Analysis of Sediments
Effective Date
01-Jul-2005
Referred By
ASTM E1391-03(2023) - Standard Guide for Collection, Storage, Characterization, and Manipulation of Sediments for Toxicological Testing and for Selection of Samplers Used to Collect Benthic Invertebrates
Effective Date
01-Jul-2005
Referred By
ASTM D5765-16 - Standard Practice for Solvent Extraction of Total Petroleum Hydrocarbons from Soils and Sediments Using Closed Vessel Microwave Heating
Effective Date
01-Jul-2005
Referred By
ASTM E2122-22 - Standard Guide for Conducting In-situ Field Bioassays With Caged Bivalves
Effective Date
01-Jul-2005

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ASTM D3976-92(2005) - Standard Practice for Preparation of Sediment Samples for Chemical AnalysisASTM D3976-92(2005) - Standard Practice for Preparation of Sediment Samples for Chemical Analysis
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ASTM D3976-92(2005) - Standard Practice for Preparation of Sediment Samples for Chemical Analysis
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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:D3976–92(Reapproved 2005)
Standard Practice for
Preparation of Sediment Samples for Chemical Analysis
This standard is issued under the fixed designation D3976; 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 sis.Largeobjectsaremechanicallyremovedandsmallonesare
eliminated by sieving the sample through a 10-mesh (2-mm
1.1 This practice describes standard procedures for prepa-
openings) sieve.
ration of test samples (including the removal of occluded water
4.2 Wet, sieved samples are mixed for preliminary homog-
and moisture) of field samples collected from locations such as
enization, then allowed to settle to remove most of the
streams, rivers, ponds, lakes, and oceans.
occluded water.
1.2 These procedures are applicable to the determination of
4.3 Moisture determinations are made on separate samples
volatile, semivolatile, and nonvolatile constituents of sedi-
from those analyzed for volatile or semivolatile constituents.
ments.
4.4 Analyses for volatile constituents are made using wet,
1.3 This standard does not purport to address all of the
settled samples from which supernatant liquid has been re-
safety concerns, if any, associated with its use. It is the
moved by decantation. The results are corrected to those that
responsibility of the user of this standard to establish appro-
would have been obtained on samples dried to constant weight
priate safety and health practices and determine the applica-
at 105 6 2°C, on the basis of a moisture determination using
bility of regulatory limitations prior to use. For a specific
a separate sample.
precautionary statement, see Note 3.
4.5 Analyses for semivolatile constituents (for example,
2. Referenced Documents mercury) are made on samples previously dried at a tempera-
ture found to be adequate for the purpose, and specified in the
2.1 ASTM Standards:
corresponding analytical procedure.
D596 Guide for Reporting Results of Analysis of Water
4.6 Analyses for nonvolatile constituents are made on
D1129 Terminology Relating to Water
samples previously dried to constant weight at 105 6 2°C.
D1192 Guide for Equipment for SamplingWater and Steam
4.7 A flow diagram, outlining typical procedures, is shown
in Closed Conduits
in Fig. 1.
D3370 Practices for Sampling Water from Closed Conduits
D4410 Terminology for Fluvial Sediment
5. Significance and Use
3. Terminology
5.1 Thechemicalanalysisofsediments,collectedfromsuch
locations as streams, rivers, ponds, lakes, and oceans can
3.1 Definitions—For definitions of terms used in this prac-
provide information of environmental significance.
tice, refer to Terminologies D1129 and D4410.
5.2 Sediment samples are inherently heterogeneous in that
4. Summary of Practice
they contain occluded water in varying and unpredictable
amounts and may contain foreign objects or material not
4.1 Samples collected (see Practices D3370 and Specifica-
ordinarily considered as sediment, the inclusion of which
tion D1192) in the field are screened to remove foreign objects
would result in inaccurate analysis.
prior to homogenization for chemical examination and analy-
5.3 Standard methods for separating foreign objects to
facilitate homogenization will minimize errors due to poor
This practice is under the jurisdiction of ASTM Committee D19 on Water and
mixing and inclusion of extraneous material.
is the direct responsibility of Subcommittee D19.07 on Sediments, Geomorphology,
5.4 Standardized procedures for drying provide a means for
and Open-Channel Flow.
Current edition approved July 1, 2005. Published August 2005. Originally reporting analytical values to a common dry weight basis.
approved in 1980. Last previous edition approved in 2001 as D3976 – 92 (2001).
DOI: 10.1520/D3976-92R05.
6. Preliminary Treatment of Field Samples
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6.1 Theanalyticalsampleisarbitrarilydefinedasthatwhich
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on passes a 10-mesh (approximately 2-mm openings) sieve. The
the ASTM website.
purpose of this is to provide a basis for discrimination of
Withdrawn.
sediment and foreign objects or materials. Stainless steel or
Withdrawn. The last approved version of this historical standard is referenced
on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D3976–92 (2005)
FIG. 1 Flow diagram for Sediment-Sample Treatment
nylonsievesmaybeusedwheninorganicconstituentsaretobe 6.5.1 Store the material, as prepared above, in contact with
determined. Stainless steel or brass sieves are suitable for use its supernatant liquid, until time of use for chemical examina-
when organic substances are to be determined. tion.
NOTE 1—For inorganic analyses, stainless steel sieves are acceptable NOTE 3—Precaution: Samples intended for both organic and inorganic
provided the mesh is not soldered or welded to the frame. For organic compound analysis may undergo changes in composition during storage.
analyses, organic materials such as rubber or plastics should not be used The analytical method should specify the conditions necessary to assure
in the storage or handling of samples. requisite stability. In the absence of specific instructions, storage at a
temperature of 4°C or lower for a period of time not to exceed 1 week is
6.2 Sieve dry samples without further pretreatment and
recommended, although it is known
...

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4.1 This practice provides a general procedure for the solvent extraction of volatile and semi-volatile organic compounds from a water matrix. Solvent extraction is used as the initial step in the solvent extraction of organic constituents for the purpose of quantifying extractable organic compounds.  
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SCOPE
1.1 This practice covers standard procedures for extraction of volatile and semi-volatile organic compounds from water using small volumes of solvents.  
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ASTM D7315-17(2023)(Test Method)
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SIGNIFICANCE AND USE
5.1 Turbidity at the levels defined in the scope of this test method are often monitored to help control processes, monitor the health and biology of water environments and determine the impact of changes in response to environmental events (weather events, floods, etc.). Turbidity is often undesirable in drinking water, plant effluent waters, water for food and beverage processing, and for a large number of other water-dependent manufacturing processes. Removal is often accomplished by coagulation, sedimentation, and various levels of filtration. Measurement of turbidity provides an indicator of contamination, and is a vital measurement for monitoring the characteristics and or quality within the sample’s source or process.  
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5.4 The appropriate measurement range for a specific technology or instrument type that should be utilized is at or below 80 % of full-scale capability for the respective instrument or technology. Measurements above this level may not be dependable.  
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SCOPE
1.1 This test method covers the static determination of turbidity in water. Static refers to a sample that is removed from its source and tested in an isolated instrument. (See Section 4.)  
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ASTM D5847-22(Practice)
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5.1 In order to be certain that the end user of analytical results obtained from using an ASTM Committee D19 test method can be confident that the values have been obtained through a competent application of the test method, a demonstration of the proficiency of the analytical system shall be performed. Appropriate proficiency is demonstrated by achievement of performance criteria derived from results of the test method collaborative study. The QC measures specified in this practice shall be included in each ASTM test method, as applicable, to ensure the quality of measurements.  
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SCOPE
1.1 This practice provides specific, mandatory requirements for incorporating quality control (QC) procedures into all test methods under the jurisdiction of Committee D19.  
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Policy on implementation of requirements for a quality control section in standard test methods generated by Committee D19 on Water.  
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NEW COLLABORATIVE TESTING—As of July 29, 1998, each collaborative study design shall include a QC section as part of the method to be tested. Prior to approval of the study design, the Results Advisor or equivalent shall ascertain the appropriateness of the QC section in meeting the requirements of this practice and Practice D2777, and shall advise the designer of the study of any changes needed to fulfill the requirements of these practices. Before a collaborative study may be conducted, approval of the study design by the Results Advisor or equivalent shall be obtained.  
OLDER VALIDATED METHODS—Standard test methods that were validated using Practices D2777 – 77, D2777 – 86, or D2777 – 94, when balloted for reapproval or revision, shall contain a QC section based upon the best information from the historical record. Where appropriate, information derived from the record of the collaborative study shall be utilized for this purpose. The introduction of the QC section into these standard test methods shall not be construed as a requirement for a new collaborative study, though the Subcommittee may opt for such a study. Any information available regarding QC or precision/bias testing shall be included in the appropriate sections of the published test method.  
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SCOPE
1.1 This practice is applicable for sampling condensed steam or water, such as boiler feedwater, for the collection of suspended solids and (optional) ionic solids using a 0.45-μm membrane filter (suspended solids) and ion exchange media (ionic solids). As the major suspended component found in most boiler feedwaters is some form of corrosion product from the preboiler system, the device used for this practice is commonly called a corrosion product sampler.  
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1.1 This test method describes a simple procedure for the detection of Legionella pneumophila (L. pneumophila) in potable water and non-potable waters (cooling towers, for example). This procedure describes a liquid culture method based on a bacterial enzyme technology. The detection of L. pneumophila is signaled through the utilization of a substrate present in the Legiolert reagent. L. pneumophila cells grow rapidly and reproduce using the rich supply of amino acids, vitamins and other nutrients present in the Legiolert reagent. Actively growing strains of L. pneumophila use the added substrate to produce a brown color indicator or produce turbid growth with or without brown coloration. Legiolert can detect this bacterial species at the following minimum concentrations based on the protocol employed:  
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Standard Practice for Estimation of Measurement Uncertainty for Data from Regression-based Methods

SIGNIFICANCE AND USE
5.1 Appropriate application of this practice should result in an estimate of the test-method’s uncertainty (at any concentration within the working range), which can be compared with data-quality objectives to see if the uncertainty is acceptable.  
5.2 With data sets that compare recovered concentration with true concentration, the resulting regression plot allows the correction of the recovery data to true values. Reporting of such corrections is at the discretion of the user.  
5.3 This practice should be used to estimate the measurement uncertainty for any application of a test method where measurement uncertainty is important to data use.
SCOPE
1.1 This practice establishes a standard for computing the measurement uncertainty for applicable test methods in Committee D19 on Water. The practice does not provide a single-point estimate for the entire working range, but rather relates the uncertainty to concentration. The statistical technique of regression is employed during data analysis.  
1.2 Applicable test methods are those whose results come from regression-based methods and whose data are intra-laboratory (not inter-laboratory data, such as result from round-robin studies). For each analysis conducted using such a method, it is assumed that a fixed, reproducible amount of sample is introduced.  
1.3 Calculation of the measurement uncertainty involves the analysis of data collected to help characterize the analytical method over an appropriate concentration range. Example sources of data include: (1) calibration studies (which may or may not be conducted in pure solvent), (2) recovery studies (which typically are conducted in matrix and include all sample-preparation steps), and (3) collections of data obtained as part of the method’s ongoing Quality Control program. Use of multiple instruments, multiple operators, or both, and field-sampling protocols may or may not be reflected in the data.  
1.4 In any designed study whose data are to be used to calculate method uncertainty, the user should think carefully about what the study is trying to accomplish and much variation should be incorporated into the study. General guidance on designing studies (for example, calibration, recovery) is given in Appendix X1. Detailed guidelines on sources of variation are outside the scope of this practice, but general points to consider are included in Appendix X2, which is not intended to be exhaustive. With any study, the user must think carefully about the factors involved with conducting the analysis, and must realize that the computed measurement uncertainty will reflect the quality of the input data.  
1.5 Associated with the measurement uncertainty is a user-chosen level of statistical confidence.  
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SIGNIFICANCE AND USE
5.1 The objective of this practice is to provide guidelines for the preparation of samples for use in collaborative tests, to evaluate methods during their development, and for the evaluation of the precision and bias of proposed test methods.  
5.2 Statements of the precision and bias are a mandatory part of ASTM test methods. Such an evaluation is necessary to provide guidance to the user as to the reliability of measurements that can be expected by its use. The statements are developed on the basis of user experience (ordinarily collaborative tests) with the test method.  
5.3 The availability of test samples is a key requirement for collaborative evaluation of test methods.
SCOPE
1.1 This practice establishes uniform general procedures for the development (preparation) and use of samples in the collaborative testing of methods for chemical analysis of sediments and similar materials.  
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Standard Practice for Certificates of Reference Materials for Water Analysis

SIGNIFICANCE AND USE
4.1 This practice is designed to assist suppliers and users of reference materials by identifying the information necessary on the certificate of analysis of materials designated for use in ASTM test methods. This practice is specifically designed to ensure that materials suitable for use as either calibration or quality control standards are available. This practice does not define a specific certification protocol, but rather provides guidance in the development of adequate data to support the use of the material as either a calibration or quality control standard. Suppliers are referred to ISO Guide 35 for guidelines on acceptable certification protocols. End users are referred to ISO Guide 31 for a more complete description of the elements of typical certificates of analysis.
SCOPE
1.1 This practice covers the information that must be provided on certificates of analysis of reference materials designated to support ASTM methods. It provides end users of these materials with a defined set of data that is required to be on a certificate of analysis and provides information to assist the end user in evaluating the independence of the material. Similarly, it provides the suppliers of reference materials with a consistent format for the presentation of certification data.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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ASTM
ASTM D6568-00(2018)(Guide)
Standard Guide for Planning, Carrying Out, and Reporting Traceable Chemical Analyses of Water Samples

SIGNIFICANCE AND USE
4.1 This guide establishes basic requirements which should be met by water and environmental laboratories that generate and report test chemical analyses which the laboratory client desires to be traceable to SI units (Note 1) or certified reference materials traceable to SI units. Traceability of chemical analyses is important because it provides a uniform basis for the comparison of results from different measurement systems and because it relates those results to our current knowledge of physical laws (Note 2).
Note 1: A certified reference material traceable to SI units is a certified reference material whose value can be related with a stated uncertainty through an unbroken change of comparisons to stated references (usually national or international standards) in SI units, such as a primary measurement made in SI units or a national standard certified in SI units.
Note 2: Not all chemical analysis results can be traceable to SI units or to certified reference material’s traceable to SI units, such as turbidity and or total suspended solids.  
4.2 Many waters-related laboratories comply with ISO Guide 17025 and participate in Proficiency Testing Programs. Laboratories that are connected to the same accreditation bodies and Proficiency Test providers can be expected to report statistically similar results on the same sample. However, some test methods and some certified reference materials are not supported with data traceable to SI units. Therefore, fully compliant laboratories that are not connected to the same providers may report statistically different chemical analysis results if they used the same nontraceable test method on the same sample. This problem could be minimized if they used test methods, measurement devices, and certified reference materials that are traceable to SI units, where available.  
4.3 Although some standard test methods and certified reference materials provide evidence of traceability to SI units, many others do not. Therefor...
SCOPE
1.1 This guide sets a protocol for generating and reporting chemical analyses that are traceable to SI units or to certified reference materials in laboratories that serve the water and environmental industry.  
1.2 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.3 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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