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ASTM D5788-95(2011)

(Guide)

Standard Guide for Spiking Organics into Aqueous Samples

Standard Guide for Spiking Organics into Aqueous Samples

SIGNIFICANCE AND USE
Matrix spiking of samples is commonly used to determine the bias under specific analytical conditions, or the applicability of a test method to a particular sample matrix, by determining the extent to which the added spike is recovered from the sample matrix under these conditions. Reactions or interactions of the analyte or component of interest with the sample matrix may cause a significant positive or negative effect on recovery and may render the chosen analytical, or monitoring, process ineffectual for that sample matrix.
Matrix spiking of samples can also be used to monitor the performance of a laboratory, individual instrument, or analyst as part of a regular quality assurance program. Changes in spike recoveries from the same or similar matrices over time may indicate variations in the quality of analyses and analytical results.
Spiking of samples may be performed in the field or in the laboratory, depending on what part of the analytical process is to be tested. Field spiking tests the recovery of the overall process, including preservation and shipping of the sample and may be considered a measure of the stability of the analytes in the matrix. Laboratory spiking tests the laboratory process only. Spiking of sample extracts, concentrates, or dilutions will be reflective of only that portion of the process subsequent to the addition of the spike.
Special precautions shall be observed when nonlaboratory personnel perform spiking in the field. It is recommended that all spike preparation work be performed in a laboratory by experienced analysts so that the field operation consists solely of adding a prepared spiking solution to the sample matrix. Training of field personnel and validation of their spiking techniques are necessary to ensure that spikes are added accurately and reproducibly. Consistent and acceptable recoveries from duplicate field spikes can be used to document the reproducibility of sampling and the spiking technique. When environmental...
SCOPE
1.1 This guide covers the general technique of “spiking” aqueous samples with organic analytes or components. It is intended to be applicable to a broad range of organic materials in aqueous media. Although the specific details and handling procedures required for all types of compounds are not described, this general approach is given to serve as a guideline to the analyst in accurately preparing spiked samples for subsequent analysis or comparison. Guidance is also provided to aid the analyst in calculating recoveries and interpreting results. It is the responsibility of the analyst to determine whether the methods and materials cited here are compatible with the analytes of interest.
1.2 The procedures in this guide are focused on “matrix spike” preparation, analysis, results, and interpretation. The applicability of these procedures to the preparation of calibration standards, calibration check standards, laboratory control standards, reference materials, and other quality control materials by spiking is incidental. A sample (the matrix) is fortified (spiked) with the analyte of interest for a variety of analytical and quality control purposes. While the spiking of multiple sample test portions is discussed, the method of standard additions is not covered.
1.3 This guide is intended for use in conjunction with the individual analytical test method that provides procedures for analysis of the analyte or component of interest. The test method is used to determine an analyte or component's background level and, again after spiking, its now elevated level. Each test method typically provides procedures not only for samples, but also for calibration standards or analytical control solutions, or both. These procedures include preparation, handling, storage, preservation, and analysis techniques. These procedures are applicable by extension, using the analyst's judgement on a case-by-case basis, to spiking solutions, an...

General Information

Status
Historical
Publication Date
30-Apr-2011
ICS
71.040.40 - Chemical analysis
Technical Committee
D19 - Water
Drafting Committee
D19.06 - Methods for Analysis for Organic Substances in Water
Current Stage
Ref Project

Relations

Replaces
ASTM D5788-95(2005) - Standard Guide for Spiking Organics into Aqueous Samples
Effective Date
01-May-2011
Replaced By
ASTM D5788-95(2017) - Standard Guide for Spiking Organics into Aqueous Samples
Effective Date
15-Dec-2017
Referred By
ASTM D2036-09(2022) - Standard Test Methods for Cyanides in Water
Effective Date
01-May-2011
Referred By
ASTM D4282-15(2022) - Standard Test Method for Determination of Free Cyanide in Water and Wastewater by Microdiffusion
Effective Date
01-May-2011
Referred By
ASTM D2330-20 - Standard Test Method for Methylene Blue Active Substances
Effective Date
01-May-2011
Referred By
ASTM D4193-08(2020)e1 - Standard Test Method for Thiocyanate in Water
Effective Date
01-May-2011

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ASTM D5788-95(2011) - Standard Guide for Spiking Organics into Aqueous SamplesASTM D5788-95(2011) - Standard Guide for Spiking Organics into Aqueous Samples
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ASTM D5788-95(2011) - Standard Guide for Spiking Organics into Aqueous Samples
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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: D5788 − 95 (Reapproved 2011)
Standard Guide for
1
Spiking Organics into Aqueous Samples
This standard is issued under the fixed designation D5788; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 1.4 Theseproceduresapplyonlytoanalytesthataresoluble
in water at the concentration of the spike plus any background
1.1 This guide covers the general technique of “spiking”
material, or to analytes soluble in a solvent that is itself
aqueous samples with organic analytes or components. It is
water-soluble. The system used in the later case must result in
intended to be applicable to a broad range of organic materials
a homogeneous solution of analyte and sample. Meaningful
in aqueous media. Although the specific details and handling
recovery data cannot be obtained if an aqueous solution or
procedures required for all types of compounds are not
homogeneous suspension of the analyte of interest in the
described,thisgeneralapproachisgiventoserveasaguideline
sample cannot be attained.
to the analyst in accurately preparing spiked samples for
subsequent analysis or comparison. Guidance is also provided
1.5 Matrix spiking may be performed in the field or in the
to aid the analyst in calculating recoveries and interpreting
laboratory,dependingonwhichpartoftheanalyticalprocessis
results. It is the responsibility of the analyst to determine
to be tested. Field spiking tests the recovery of the overall
whether the methods and materials cited here are compatible
process, including preservation and shipping of the sample.
with the analytes of interest.
Laboratoryspikingteststhelaboratoryprocessonly.Spikingof
1.2 The procedures in this guide are focused on “matrix
sample extracts, concentrates, or dilutions will test only that
spike” preparation, analysis, results, and interpretation. The portion of the process subsequent to the addition of the spike.
applicability of these procedures to the preparation of calibra-
1.6 The values stated in SI units are to be regarded as
tion standards, calibration check standards, laboratory control
standard. No other units of measurement are included in this
standards, reference materials, and other quality control mate-
standard.
rials by spiking is incidental.Asample (the matrix) is fortified
(spiked) with the analyte of interest for a variety of analytical
1.7 This standard does not purport to address all of the
and quality control purposes. While the spiking of multiple
safety concerns, if any, associated with its use. It is the
sample test portions is discussed, the method of standard
responsibility of the user of this standard to establish appro-
additions is not covered.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
1.3 This guide is intended for use in conjunction with the
individual analytical test method that provides procedures for
2. Referenced Documents
analysis of the analyte or component of interest. The test
method is used to determine an analyte or component’s
2
2.1 ASTM Standards:
background level and, again after spiking, its now elevated
D1129Terminology Relating to Water
level. Each test method typically provides procedures not only
D1193Specification for Reagent Water
for samples, but also for calibration standards or analytical
D3694Practices for Preparation of Sample Containers and
control solutions, or both. These procedures include
for Preservation of Organic Constituents
preparation, handling, storage, preservation, and analysis tech-
D3856Guide for Management Systems in Laboratories
niques.Theseproceduresareapplicablebyextension,usingthe
Engaged in Analysis of Water
analyst’s judgement on a case-by-case basis, to spiking
D4375Practice for Basic Statistics in Committee D19 on
solutions, and are not reiterated in this guide. See also Practice
Water
E200 for preparation and storage information.
E200Practice for Preparation, Standardization, and Storage
of Standard and Reagent Solutions for ChemicalAnalysis
1
This guide is under the jurisdiction ofASTM Committee D19 on Water and is
the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
2
Organic Substances in Water. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved May 1, 2011. Published June 2011. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1995. Last previous edition approved in 2005 as D5788–95 (2005). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D5788-95R11. the A
...

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5.1 Matrix spiking of samples is commonly used to determine the bias under specific analytical conditions, or the applicability of a test method to a particular sample matrix, by determining the extent to which the added spike is recovered from the sample matrix under these conditions. Reactions or interactions of the analyte or component of interest with the sample matrix may cause a significant positive or negative effect on recovery and may render the chosen analytical, or monitoring, process ineffectual for that sample matrix.  
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5.4 Special precautions shall be observed when nonlaboratory personnel perform spiking in the field. It is recommended that all spike preparation work be performed in a laboratory by experienced analysts so that the field operation consists solely of adding a prepared spiking solution to the sample matrix. Training of field personnel and validation of their spiking techniques are necessary to ensure that spikes are added accurately and reproducibly. Consistent and acceptable recoveries from duplicate field spikes can be used to document the reproducibility of sampling and the spiking technique....
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1.1 This guide covers the general technique of “spiking” aqueous samples with organic analytes or components. It is intended to be applicable to a broad range of organic materials in aqueous media. Although the specific details and handling procedures required for all types of compounds are not described, this general approach is given to serve as a guideline to the analyst in accurately preparing spiked samples for subsequent analysis or comparison. Guidance is also provided to aid the analyst in calculating recoveries and interpreting results. It is the responsibility of the analyst to determine whether the methods and materials cited here are compatible with the analytes of interest.  
1.2 The procedures in this guide are focused on “matrix spike” preparation, analysis, results, and interpretation. The applicability of these procedures to the preparation of calibration standards, calibration check standards, laboratory control standards, reference materials, and other quality control materials by spiking is incidental. A sample (the matrix) is fortified (spiked) with the analyte of interest for a variety of analytical and quality control purposes. While the spiking of multiple sample test portions is discussed, the method of standard additions is not covered.  
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1.5 The upper limit of this test method is dependent upon total anion concentration and may be determined experimentally as described in Annex A1. These limits may be extended by appropriate dilution or by use of a smaller injection volume.  
1.6 Using alternate separator column and eluents may permit additional anions such as acetate, formate, or citrate to be determined. This is not the subject of this test method.  
1.7 This test method update approves the use of electrolytically generated eluent, electrolytically regenerated eluent, electrolytic suppression (not autozeroing), and electrolytic trap columns also known as reagent-free ion chromatography. This approval is based on acceptance by the U.S. EPA as referenced in Appendix X2.  
1.8 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.9 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.  
1.10 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 D5544-16(2023)(Test Method)
Standard Test Method for On-Line Measurement of Residue After Evaporation of High-Purity Water

SIGNIFICANCE AND USE
5.1 Even so-called high-purity water will contain contaminants. While not always present, these contaminants may contribute one or more of the following: dissolved active ionic substances such as calcium, magnesium, sodium, potassium, manganese, ammonium, bicarbonates, sulfates, nitrates, chloride and fluoride ions, ferric and ferrous ions, and silicates; dissolved organic substances such as pesticides, herbicides, plasticizers, styrene monomers, deionization resin material; and colloidal suspensions such as silica. While this test method facilitates the monitoring of these contaminants in high-purity water, in real time, with one instrument, this test method is not capable of identifying the various sources of residue contamination or detecting dissolved gases or suspended particles.  
5.2 This test method is calibrated using weighed amounts of an artificial contaminant (potassium chloride). The density of potassium chloride is reasonably typical of contaminants found in high-purity water; however, the response of this test method is clearly based on a response to potassium chloride. The response to actual contaminants found in high-purity water may differ from the test method's calibration. This test method is not different from many other analytical test methods in this respect.  
5.3 Together with other monitoring methods, this test method is useful for diagnosing sources of RAE in ultra-pure water systems. In particular, this test method can be used to detect leakages such as colloidal silica breakthrough from the effluent of a primary anion or mixed-bed deionizer. In addition, this test method has been used to measure the rinse-up time for new liquid filters and has been adapted for batch-type sampling (this adaptation is not described in this test method).  
5.4 Obtaining an immediate indication of contamination in high-purity water has significance to those industries using high-purity water for manufacturing components; production can be halted immediate...
SCOPE
1.1 This test method covers the determination of dissolved organic and inorganic matter and colloidal material found in high-purity water used in the semiconductor, and related industries. This material is referred to as residue after evaporation (RAE). The range of the test method is from 0.001 μg/L (ppb) to 60 μg/L (ppb).  
1.2 This test method uses a continuous, real time monitoring technique to measure the concentration of RAE. A pressurized sample of high-purity water is supplied to the test method's apparatus continuously through ultra-clean fittings and tubing. Contaminants from the atmosphere are therefore prevented from entering the sample. General information on the test method and a literature review on the continuous measurement of RAE has been published.2  
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses are mathematical conversions to inch-pound units that are provided for information only and are not considered standard.  
1.4 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. For specific hazards statements, see Section 8.  
1.5 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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