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ASTM D8456-22

(Test Method)

Standard Test Method for Determination of Nitrosamines in Water by Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS)

Standard Test Method for Determination of Nitrosamines in Water by Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS)

SIGNIFICANCE AND USE
5.1 Nitrosamines are a class of nitrogen-containing compounds with a known occurrence in wastewater. They may also be created in deionization and are a potential contaminant in water for reuse. The World Health Organization has issued a guideline for NDMA in drinking water at 0.1 µg/L. NDMA may occur in chlorinated effluents and other wastewaters. Other methods for nitrosamines employ solid phase extraction, which may not be applicable to wastewaters that contain particulate matter or a high organic load. This method analyses nitrosamines directly using LC-MS/MS.
SCOPE
1.1 This test method covers the liquid chromatography tandem mass spectrometry (LC-MS/MS) detection and quantitation of N-nitrosamines after direct injection. It has been validated for groundwater, surface water, wastewater influents, and wastewater effluents. This test method is not limited to these aqueous matrices; however, the applicability of this test method to other aqueous matrices must be demonstrated.  
1.2 This test method is applicable to nitrosamines that can be chromatographed and detected using a mass spectrometry procedure. Table 1 lists the compounds that have been validated for this test method. This test method is not limited to the compounds listed in Table 1; however, the applicability of the test method to other compounds must be demonstrated.  
1.3 Analyte concentrations from 0.05 µg/L up to approximately 5 µg/L may be determined without dilution of the sample. Analytes with insufficient sensitivity will not be detected, but they can be measured with acceptable accuracy and precision when present in sufficient amounts. In addition, newer instruments, or instruments of improved sensitivity may be used to lower detection limits.  
1.4 Analytes that are not separated chromatographically, but that have different mass spectra and noninterfering quantitation ions, can be identified and measured in the same calibration mixture or water sample. Analytes that have very similar product ions cannot be individually identified and measured in the same calibration mixture or water sample unless they have different retention times.  
1.5 It is the responsibility of the user to ensure the validity of this test method for untested matrices.  
1.6 This test method is restricted to use by or under the supervision of analysts experienced in the use of a liquid chromatograph with tandem mass spectrometry (LC-MS/MS).  
1.7 Depending on data usage, you may modify this test method but limit to modifications that improve performance while still meeting method quality acceptance criteria. Shortening the chromatographic run simply to save time is not allowed. Use Practice E2935 or similar statistical tests to confirm that modifications produce equivalent results on non-interfering samples. In addition, use Guide E2857 or equivalent statistics to re-validate the modified test.  
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.

General Information

Status
Published
Publication Date
30-Apr-2022
ICS
13.060.01 - Water quality in general
Technical Committee
D19 - Water
Drafting Committee
D19.06 - Methods for Analysis for Organic Substances in Water
Current Stage
Ref Project

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ASTM D8456-22 - Standard Test Method for Determination of Nitrosamines in Water by Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS)ASTM D8456-22 - Standard Test Method for Determination of Nitrosamines in Water by Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS)
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ASTM D8456-22 - Standard Test Method for Determination of Nitrosamines in Water by Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS)
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Standards Content (Sample)

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.
Designation: D8456 − 22
Standard Test Method for
Determination of Nitrosamines in Water by Liquid
1
Chromatography Tandem Mass Spectrometry (LC-MS/MS)
This standard is issued under the fixed designation D8456; 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 while still meeting method quality acceptance criteria. Short-
ening the chromatographic run simply to save time is not
1.1 This test method covers the liquid chromatography
allowed. Use Practice E2935 or similar statistical tests to
tandem mass spectrometry (LC-MS/MS) detection and quan-
confirm that modifications produce equivalent results on non-
titation of N-nitrosamines after direct injection. It has been
interferingsamples.Inaddition,useGuideE2857orequivalent
validated for groundwater, surface water, wastewater influents,
statistics to re-validate the modified test.
and wastewater effluents. This test method is not limited to
these aqueous matrices; however, the applicability of this test 1.8 The values stated in SI units are to be regarded as
method to other aqueous matrices must be demonstrated. standard. No other units of measurement are included in this
standard.
1.2 This test method is applicable to nitrosamines that can
1.9 This standard does not purport to address all of the
be chromatographed and detected using a mass spectrometry
safety concerns, if any, associated with its use. It is the
procedure. Table 1 lists the compounds that have been vali-
responsibility of the user of this standard to establish appro-
datedforthistestmethod.Thistestmethodisnotlimitedtothe
priate safety, health, and environmental practices and deter-
compounds listed in Table 1; however, the applicability of the
mine the applicability of regulatory limitations prior to use.
test method to other compounds must be demonstrated.
1.10 This international standard was developed in accor-
1.3 Analyte concentrations from 0.05 µg/L up to approxi-
dance with internationally recognized principles on standard-
mately 5 µg/L may be determined without dilution of the
ization established in the Decision on Principles for the
sample. Analytes with insufficient sensitivity will not be
Development of International Standards, Guides and Recom-
detected, but they can be measured with acceptable accuracy
mendations issued by the World Trade Organization Technical
and precision when present in sufficient amounts. In addition,
Barriers to Trade (TBT) Committee.
newer instruments, or instruments of improved sensitivity may
be used to lower detection limits.
2. Referenced Documents
1.4 Analytesthatarenotseparatedchromatographically,but 2
2.1 ASTM Standards:
thathavedifferentmassspectraandnoninterferingquantitation
D1129Terminology Relating to Water
ions, can be identified and measured in the same calibration
D1193Specification for Reagent Water
mixture or water sample. Analytes that have very similar
D2777Practice for Determination of Precision and Bias of
product ions cannot be individually identified and measured in
Applicable Test Methods of Committee D19 on Water
the same calibration mixture or water sample unless they have
D3370Practices for Sampling Water from Flowing Process
different retention times.
Streams
1.5 It is the responsibility of the user to ensure the validity
D4448GuideforSamplingGround-WaterMonitoringWells
of this test method for untested matrices. D6089Guide for Documenting a Groundwater Sampling
Event
1.6 This test method is restricted to use by or under the
D6538Guide for Sampling Wastewater With Automatic
supervision of analysts experienced in the use of a liquid
Samplers
chromatograph with tandem mass spectrometry (LC-MS/MS).
D6759Practice for Sampling Liquids Using Grab and Dis-
1.7 Depending on data usage, you may modify this test
crete Depth Samplers
method but limit to modifications that improve performance
E2857Guide for Validating Analytical Methods
1
This test method is under the jurisdiction ofASTM Committee D19 on Water
2
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Organic Substances in Water. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved May 1, 2022. Published July 2022. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
D8456-22. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Driv
...

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5.1 This practice is intended for use by samplers, technicians, or analysts to verify that samples are preserved or at the proper pH specified in analytical procedures.  
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Standard Practice for Collection of Water Samples with High, Medium, or Low Suspended Solids for Identification and Quantification of Microplastic Particles and Fibers

SIGNIFICANCE AND USE
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Standard Practice for Preparation of Water Samples with High, Medium, or Low Suspended Solids for Identification and Quantification of Microplastic Particles and Fibers Using Raman Spectroscopy, IR Spectroscopy, or Pyrolysis-GC/MS

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5.1 Large volumes of water are required to be sieved for accurate quantification of microplastics. Water with high to medium content of suspended solids can lead to an excess of inorganic and organic background material which can interfere with the ability to conduct reliable analyses. The presence of this background material can often impede the ability to accurately discern, distinguish and identify the number of microplastic particles in solution.  
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SIGNIFICANCE AND USE
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Standard Guide for Mitigation of Wildfire Impact to Source Water Protection Areas and Risk to Water Utilities

SIGNIFICANCE AND USE
4.1 This guide addresses issues related solely to strategies and the development of a plan to address wildfire-related physical and chemical changes to water resources in Source Water Protection Areas. This guide does not include specific advice on risk assessment. Mitigation strategies and planning may consist of a wide variety of actions by individuals, communities, or organizations to prepare for the impacts of wildfires on water quality and quantity in Source Water Protection Areas (see Guide E3136).  
4.2 Source water protection activities not only help the utility identify risk, but they are also necessary to educate regulatory agencies, permitting authorities, and the community about the impacts that their actions can have on source water quality or quantity of the drinking water.  
4.3 Example Users:  
4.3.1 Federal, tribal, state, or municipal facility staff and regulators, including departments of health, water, sewer, and fire;  
4.3.2 Financial and insurance institutions;  
4.3.3 Federal, tribal, state, or local land managers;  
4.3.4 Public works staff, including water systems, groundwater supplies, surface water supplies, stormwater systems, wastewater systems, publicly owned treatment works, and agriculture water management agencies;  
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FIG. 1 Place-based characteristics for consideration when assessing threats to water supplies and treatment due to a wildfire (adapted from (3)).  
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SIGNIFICANCE AND USE
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5.4 Microplastic particles/fibers retained on the sieves are suitable for characterization in terms of size, shape, quantity, and composition (polymer type), dependent upon the chosen analytical method.
SCOPE
1.1 This practice provides for the collection of water samples with high, medium, or low suspended solids to determine the presence, count, polymer type, and physical characteristics of microplastic particles and fibers. This collection practice has been validated for the collection of samples from drinking water, surface waters, wastewater influent and effluent (secondary and tertiary), and marine waters. This practice is not limited to these particular water matrices; however, the applicability of this practice to other aqueous matrices must be demonstrated.  
1.2 Water samples are passed through filters or sieves of adequate mesh size to enable capture of the smallest desired particle size. For waters with high or medium suspended solids content, a series of sieves with increasingly smaller mesh size should be used to prevent clogging and allow for the collection of desired particle size fractions.  
1.3 Subsequent sample preparation followed by analysis utilizing either Pyrolysis gas chromatography/mass spectrometry (Py-GC/MS), IR spectroscopy, or Raman spectroscopy may be used to identify the quantity (mass or number count) and composition (polymer type) of microplastic particles/fibers. The spectroscopic methods can provide a count of the number of particles and fibers present in a sample, and Py-GC/MS can provide the mass present in a sample. When desired, microplastic particle/fiber size, shape and surface characteristics can be ascertained with appropriate instruments such as a scanning electron microscope (SEM).  
1.4 Units—The values stated in SI units are to be regarded as the standard except where standard U.S. equipment is specified in imperial units, for example, inches and gallons. No other units of measurement are included in this standard.  
1.5 Standard Practice—This practice offers a set of instructions for performing one or more specific operations. This practice cannot replace education or experience and should be used in conjunction with professional judgment. Not all aspects of this practice may be applicable in all circumstances. This practice is not intended to represent or replace the standard of care by which the adequacy of a given professional service must be judged, nor should this practice be applied without consideration of a project’s many unique aspects.  
1.6 This standard does not purport to addre...

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ASTM
ASTM D8333-20(Practice)
Standard Practice for Preparation of Water Samples with High, Medium, or Low Suspended Solids for Identification and Quantification of Microplastic Particles and Fibers Using Raman Spectroscopy, IR Spectroscopy, or Pyrolysis-GC/MS

SIGNIFICANCE AND USE
5.1 Large volumes of water are required to be sieved for accurate quantification of microplastics. Water with high to medium content of suspended solids can lead to an excess of inorganic and organic background material which can interfere with the ability to conduct reliable analyses. The presence of this background material can often impede the ability to accurately discern, distinguish and identify the number of microplastic particles in solution.  
5.2 The digestion described in this procedure allows for significant reduction of interfering substances and contaminants, rendering a sample suitable for particle and fiber characterization and identification using either Raman and IR spectroscopic analysis or for polymeric quantification and identification by Pyrolysis-GC/MS.  
5.3 For water samples with medium to low suspended solids, the oxidation and digestion steps necessary will be dependent upon the type and nature of interfering substances and contaminants and may be determined through simple trial efforts.
SCOPE
1.1 This practice provides for the sample preparation of collected water samples with high, medium, or low suspended solids to determine the presence, count, polymer type, and physical characteristics of microplastic particles and fibers. It has been designed for the preparation of samples collected from drinking water, surface waters, wastewater influent and effluent (secondary and tertiary), and marine waters using collection practice (Practice D8332). This practice is not limited to these particular water matrices; however, the applicability of this practice to other aqueous matrices must be demonstrated.  
1.2 This practice consists of a wet peroxide oxidation followed by progressive enzymatic digestion to the extent necessary to remove interfering organic constituents such as cellulose, lipids and chitin that are typically found in abundance in water matrices of samples with high to medium suspended solids such as wastewater influent. For water samples with low suspended solids, such as but not limited to drinking water and tertiary treated wastewater, the oxidation and digestion steps may not be necessary.  
1.3 Water samples prepared using this practice are suitable for analysis utilizing either Pyrolysis-GC/MS methods for qualitative identification and mass quantitation, or IR spectroscopy or Raman spectroscopy for identifying the quantity (number count) and composition (polymer type) of microplastic particles. If desired, microplastic particle size and shape may be ascertained with appropriate instruments such as a scanning electron microscope (SEM) and microscopy techniques.  
1.4 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 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.  
1.6 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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