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ASTM D5673-16

(Test Method)

Standard Test Method for Elements in Water by Inductively Coupled Plasma—Mass Spectrometry

Standard Test Method for Elements in Water by Inductively Coupled Plasma—Mass Spectrometry

SIGNIFICANCE AND USE
5.1 The test method is useful for the determination of element concentrations in many natural waters, metallurgical process cyanide solutions and wastewaters. It has the capability for the determination of up to 21 elements. High analysis sensitivity can be achieved for some elements that are difficult to determine by other techniques.
SCOPE
1.1 This test method covers the determination of dissolved elements in ground water, surface water, and drinking water. It may also be used for the determination of total-recoverable elements in these waters as well as wastewater.2  
1.2 This test method should be used by analysts experienced in the use of inductively coupled plasma—mass spectrometry (ICP-MS), the interpretation of spectral and matrix interferences and procedures for their correction.  
1.3 It is the user's responsibility to ensure the validity of the test method for waters of untested matrices.  
1.4 Table 1 lists elements for which the test method applies, with recommended masses and typical estimated instrumental detection limits using conventional pneumatic nebulization. Actual working detection limits are sample dependent and, as the sample matrix varies, these detection limits may also vary. In time, other elements may be added as more information becomes available and as required. (A) Instrument detection limits (3σ) estimated from seven replicate scans of the blank (1 % v/v HNO3) and three replicate integrations of a multi-element standard.  
1.4.1 This method covers the analysis of mine dewatering groundwater and wastewater effluent in the range of 2–120 μg/L dissolved antimony and 3–200 μg/L dissolved arsenic.  
1.4.2 This method covers the analysis of metallurgical processing cyanide solutions in the range of 1–500 µg/L dissolved gold.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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.

General Information

Status
Published
Publication Date
31-Jan-2016
ICS
13.060.50 - Examination of water for chemical substances
Technical Committee
D19 - Water
Drafting Committee
D19.05 - Inorganic Constituents in Water
Current Stage
Ref Project

Relations

Refers
ASTM D1066-18 - Standard Practice for Sampling Steam
Effective Date
01-Aug-2018
Refers
ASTM D1066-18e1 - Standard Practice for Sampling Steam
Effective Date
01-Aug-2018
Refers
ASTM E1601-19 - Standard Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method
Effective Date
01-Nov-2019

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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: D5673 − 16
Standard Test Method for
Elements in Water by Inductively Coupled Plasma—Mass
1
Spectrometry
This standard is issued under the fixed designation D5673; 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* 2. Referenced Documents
3
2.1 ASTM Standards:
1.1 This test method covers the determination of dissolved
elements in ground water, surface water, and drinking water. It D1066Practice for Sampling Steam
D1129Terminology Relating to Water
may also be used for the determination of total-recoverable
2
elements in these waters as well as wastewater. D1193Specification for Reagent Water
D2777Practice for Determination of Precision and Bias of
1.2 Thistestmethodshouldbeusedbyanalystsexperienced
Applicable Test Methods of Committee D19 on Water
in the use of inductively coupled plasma—mass spectrometry
D3370Practices for Sampling Water from Closed Conduits
(ICP-MS), the interpretation of spectral and matrix interfer-
D5810Guide for Spiking into Aqueous Samples
ences and procedures for their correction.
D5847Practice for Writing Quality Control Specifications
1.3 Itistheuser’sresponsibilitytoensurethevalidityofthe
for Standard Test Methods for Water Analysis
test method for waters of untested matrices.
E691Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.4 Table1listselementsforwhichthetestmethodapplies,
E1601Practice for Conducting an Interlaboratory Study to
with recommended masses and typical estimated instrumental
Evaluate the Performance of an Analytical Method
detection limits using conventional pneumatic nebulization.
E1763Guide for Interpretation and Use of Results from
Actual working detection limits are sample dependent and, as
the sample matrix varies, these detection limits may also vary. Interlaboratory Testing of Chemical Analysis Methods
4
(Withdrawn 2015)
In time, other elements may be added as more information
becomes available and as required.
3. Terminology
1.4.1 This method covers the analysis of mine dewatering
groundwater and wastewater effluent in the range of 2–120
3.1 Definitions:
µg/L dissolved antimony and 3–200 µg/L dissolved arsenic.
3.1.1 For definitions of terms used in this standard, refer to
1.4.2 This method covers the analysis of metallurgical Terminology D1129.
processing cyanide solutions in the range of 1–500 µg/L
3.2 Definitions of Terms Specific to This Standard:
dissolved gold.
3.2.1 calibration blank, n—a volume of water containing
the same acid matrix as is in the calibration standards (see
1.5 The values stated in SI units are to be regarded as
11.1).
standard. No other units of measurement are included in this
standard. 3.2.2 calibration standards, n—a series of known standard
solutions used by the analyst for calibration of the instrument
1.6 This standard does not purport to address all of the
(that is, preparation of the analytical curve) (see Section 11).
safety concerns, if any, associated with its use. It is the
3.2.3 calibration stock solution, n—a solution prepared
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- from the stock standard solution(s) to verify the instrument
bility of regulatory limitations prior to use. response with respect to analyte concentration.
3.2.4 dissolved, adj—capable of passing through a 0.45-µm
membrane filter.
1
This test method is under the jurisdiction ofASTM Committee D19 on Water
and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents
3
in Water. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Feb. 1, 2016. Published June 2016. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1996. Last previous edition approved in 2015 as D5673–15. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D5673-16. the ASTM website.
2 4
EPATest Method: Determination of Trace Elements in Waters and Wastes by The last approved version of this historical standard is referenced on
Inductively Coupled Plasma—Mass Spectrometry, Method200.8. www.astm.org.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D5
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D5673 − 15 D5673 − 16
Standard Test Method for
Elements in Water by Inductively Coupled Plasma—Mass
1
Spectrometry
This standard is issued under the fixed designation D5673; 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*
1.1 This test method covers the determination of dissolved elements in ground water, surface water, and drinking water. It may
2
also be used for the determination of total-recoverable elements in these waters as well as wastewater.
1.2 This test method should be used by analysts experienced in the use of inductively coupled plasma—mass spectrometry
(ICP-MS), the interpretation of spectral and matrix interferences and procedures for their correction.
1.3 It is the user’s responsibility to ensure the validity of the test method for waters of untested matrices.
1.4 Table 1 lists elements for which the test method applies, with recommended masses and typical estimated instrumental
detection limits using conventional pneumatic nebulization. Actual working detection limits are sample dependent and, as the
sample matrix varies, these detection limits may also vary. In time, other elements may be added as more information becomes
available and as required.
1.4.1 This method covers the analysis of mine dewatering groundwater and wastewater effluent in the range of 2–120 μg/L
dissolved antimony and 3–200 μg/L dissolved arsenic.
1.4.2 This method covers the analysis of metallurgical processing cyanide solutions in the range of 1–500 μg/L dissolved gold.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1
This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents in Water.
Current edition approved July 1, 2015Feb. 1, 2016. Published August 2015June 2016. Originally approved in 1996. Last previous edition approved in 20102015 as
D5673 – 10.D5673 – 15. DOI: 10.1520/D5673-15.10.1520/D5673-16.
2
EPA Test Method: Determination of Trace Elements in Waters and Wastes by Inductively Coupled Plasma—Mass Spectrometry, Method 200.8.
TABLE 1 Recommended Analytical Mass and Estimated
Instrument Detection Limits
Recommended Estimated Instrument
Element
A
Analytical Mass Detection Limit, μg/L
Aluminum 27 0.05
Antimony 121 0.08
Arsenic 75 0.9
Barium 137 0.5
Beryllium 9 0.1
Cadmium 111 0.1
Chromium 52 0.07
Cobalt 59 0.03
Copper 63 0.03
Gold 197 0.01
Lead 206, 207, 208 0.08
Manganese 55 0.1
Molybdenum 98 0.1
Nickel 60 0.2
Selenium 82 5.0
Silver 107 0.05
Thallium 205 0.09
Thorium 232 0.03
Uranium 238 0.02
Vanadium 51 0.02
Zinc 66 0.2
A
Instrument detection limits (3σ) estimated from seven replicate scans of the blank
(1 % v/v HNO ) and three replicate integrations of a multi-element standard.
3
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D5673 − 16
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.
2. Referenced Documents
3
2.1 ASTM Standards:
D1066 Practice for Sampling Steam
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
D3370 Practices for Sampling Water from Closed Conduits
D5810 Guide for Spiking into Aqueous Samples
D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method
E1763 Guide for Interpretation and Use of Results from Interlaboratory Testing of Chemical Analysis Methods (Withdrawn
4
2015)
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.
3.2 Definitions of Terms Specifi
...

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1.1 This test method covers the determination of bisphenol A (BPA) extracted from water utilizing solid phase extraction (SPE), separated using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS). BPA is qualitatively and quantitatively determined by this method. This test method adheres to multiple reaction monitoring (MRM) mass spectrometry.  
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 The method detection limit (MDL) and reporting limit (RL) for BPA are listed in Table 1.  
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.  
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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ASTM
ASTM D8025-23(Test Method)
Standard Test Method for Determination of Select Pesticides in Water by Multiple Reaction Monitoring Liquid Chromatography Tandem Mass Spectrometry

SIGNIFICANCE AND USE
5.1 Pesticides may be used in various agricultural and household products. These products may enter waterways at low levels through run-off or misuse near water resources. Hence, there is a need for quick, easy and robust method to determine pesticide concentration in water matrices for understanding the sources and concentration levels in affected areas.  
5.2 This method has been single-laboratory validated in reagent water and surface waters (Tables 12-14).
SCOPE
1.1 This test method covers a method for analysis of selected pesticides in a water matrix by filtration followed with liquid chromatography/electrospray ionization tandem mass spectrometry analysis. The samples are prepared in 20 % methanol, filtered, and analyzed by liquid chromatography/tandem mass spectrometry. This method was developed for an agricultural run-off study, not for low level analysis of pesticides in drinking water. This method may be modified for lower level analysis. The analytes are qualitatively and quantitatively determined by this method. This method adheres to multiple reaction monitoring (MRM) mass spectrometry.  
1.2 A full collaborative study to meet the requirements of Practice D2777 has not been completed. This standard contains single-operator precision and bias based on single-operator data. Publication of standards that have not been fully validated is done to make the current technology accessible to users of standards, and to solicit additional input from the user community.  
1.3 A reporting limit check sample (RLCS) is analyzed during every batch to ensure that if an analyte was present in a sample at or near the reporting limit it would be positively identified and accurately quantitated within set quality control limits. A method detection limit (MDL) study was not done for this method, the method detection limits would be much lower than the reporting limits in this method and would be irrelevant. A RLCS was determined to be more applicable for this standard. If this method is adapted to report much lower or near the MDL then a MDL study would be warranted.  
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 The Reporting Range for the target analytes are listed in Table 1.  
1.5.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. The reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 6 after taking into account an 8 mL water sample volume and a final diluted sample volume of 10 mL (80 % water/20 % methanol).  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.7 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 D7485-23(Test Method)
Standard Test Method for Determination of Nonylphenol, p-tert-Octylphenol, Nonylphenol Monoethoxylate and Nonylphenol Diethoxylate in Environmental Waters by Liquid Chromatography/Tandem Mass Spectrometry

SIGNIFICANCE AND USE
5.1 NP and OP have been shown to have toxic effects in aquatic organisms. The source of NP and OP is prominently from the use of common commercial surfactants. The most widely used surfactant is nonylphenol ethoxylate (NPEO) which has an average ethoxylate chain length of nine. The ethoxylate chain is readily biodegraded to form NP1EO, NP2EO, nonylphenol carboxylate (NPEC) and, under anaerobic conditions, NP. NP will also biodegrade, but may be released into environmental waters directly at trace levels. This method has been investigated and is applicable for environmental waters, including seawater.
SCOPE
1.1 This test method covers the determination of nonylphenol (NP), nonylphenol ethoxylate (NP1EO), nonylphenol diethoxylate (NP2EO), and octylphenol (OP), extracted from water utilizing solid phase extraction (SPE), separated using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS). These compounds are qualitatively and quantitatively determined by this method. This method adheres to single reaction monitoring (SRM) mass spectrometry.  
1.2 The method detection limit (MDL) and reporting limit (RL) for NP, NP1EO, NP2EO, and OP are listed in Table 1.    
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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.  
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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ASTM
ASTM D7645-23(Test Method)
Standard Test Method for Determination of Aldicarb, Aldicarb Sulfone, Aldicarb Sulfoxide, Carbofuran, Methomyl, Oxamyl, and Thiofanox in Water by Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)

SIGNIFICANCE AND USE
5.1 This test method has been developed by U.S. EPA Region 5 Chicago Regional Laboratory (CRL).  
5.2 The N-methyl carbamate (NMC) pesticides: aldicarb, carbofuran, methomyl, oxamyl, and thiofanox have been identified by EPA as working through a common mechanism. These affect the nervous system by reducing the ability of enzymes. Enzyme inhibition was the primary toxicological effect of regulatory concern to EPA in assessing the NMC’s food, drinking water, and residential risks. In most of the country, NMC residues in drinking water sources are at levels that are not likely to contribute substantially to the multi-pathway cumulative exposure. Shallow private wells extending through highly permeable soils into shallow, acidic ground water represent what the EPA believes to be the most vulnerable drinking water. Aldicarb sulfone and aldicarb sulfoxide are breakdown products of aldicarb and should also be monitored due to their toxicological effects.4  
5.3 This test method has been investigated for use with reagent, surface, and drinking water for the selected carbamates: aldicarb, aldicarb sulfone, aldicarb sulfoxide, carbofuran, methomyl, oxamyl, and thiofanox.
SCOPE
1.1 This test method covers the determination of aldicarb, aldicarb sulfone, aldicarb sulfoxide, carbofuran, methomyl, oxamyl, and thiofanox (referred to collectively as carbamates in this test method) in water by direct injection using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS). These analytes are qualitatively and quantitatively determined by this test method. This test method adheres to multiple reaction monitoring (MRM) mass spectrometry.  
1.2 The Detection Verification Level (DVL) and Reporting Range for the carbamates are listed in Table 1.    
1.2.1 The DVL is required to be at a concentration at least 3 times below the Reporting Limit (RL) and have a signal/noise ratio greater than 3:1. Fig. 1 displays the signal/noise ratios of the primary single reaction monitoring (SRM) transitions, and Fig. 2 displays the confirmatory SRM transitions at the DVLs for the carbamates.  
1.3 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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.  
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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