ASTM D6508-15
(Test Method)Standard Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte
Standard Test Method for Determination of Dissolved Inorganic Anions in Aqueous Matrices Using Capillary Ion Electrophoresis and Chromate Electrolyte
SIGNIFICANCE AND USE
5.1 Capillary ion electrophoresis provides a simultaneous separation and determination of several inorganic anions using nanolitres of sample in a single injection. All anions present in the sample matrix will be visualized yielding an anionic profile of the sample.
5.2 Analysis time is less than 5 minutes with sufficient sensitivity for drinking water and wastewater applications. Time between samplings is less than seven minutes allowing for high sample throughput.
5.3 Minimal sample preparation is necessary for drinking water and wastewater matrices. Typically, only a dilution with water is needed.
5.4 This test method is intended as an alternative to other multi-analyte methods and various wet chemistries for the determination of inorganic anions in water and wastewater. Compared to other multi-analyte methods the major benefits of CIE are speed of analysis, simplicity, and reduced reagent consumption and operating costs.
SCOPE
1.1 This test method covers the determination of the inorganic anions fluoride, bromide, chloride, nitrite, nitrate, ortho-phosphate, and sulfate in drinking water, wastewater, and other aqueous matrices using capillary ion electrophoresis (CIE) with indirect UV detection. See Figs. 1-6.
1.2 The test method uses a chromate-based electrolyte and indirect UV detection at 254 nm. It is applicable for the determination or inorganic anions in the range of 0.1 to 50 mg/L except for fluoride whose range is 0.1 to 25 mg/L.
1.3 It is the responsibility of the user to ensure the validity of this test method for other anion concentrations and untested aqueous matrices.
Note 1: The highest accepted anion concentration submitted for precision and bias extend the anion concentration range for the following anions: Chloride to 93 mg/L, Sulfate to 90 mg/L, Nitrate to 72 mg/L, and ortho-phosphate to 58 mg/L.
1.4 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.
1.5 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 and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 9.
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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: D6508 − 15
Standard Test Method for
Determination of Dissolved Inorganic Anions in Aqueous
Matrices Using Capillary Ion Electrophoresis and Chromate
1
Electrolyte
This standard is issued under the fixed designation D6508; 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* D1129Terminology Relating to Water
D1193Specification for Reagent Water
1.1 This test method covers the determination of the inor-
D2777Practice for Determination of Precision and Bias of
ganic anions fluoride, bromide, chloride, nitrite, nitrate, ortho-
Applicable Test Methods of Committee D19 on Water
phosphate,andsulfateindrinkingwater,wastewater,andother
D3370Practices for Sampling Water from Closed Conduits
aqueous matrices using capillary ion electrophoresis (CIE)
D3856Guide for Management Systems in Laboratories
with indirect UV detection. See Figs. 1-6.
Engaged in Analysis of Water
1.2 The test method uses a chromate-based electrolyte and
D5810Guide for Spiking into Aqueous Samples
indirect UV detection at 254 nm. It is applicable for the
D5847Practice for Writing Quality Control Specifications
determination or inorganic anions in the range of 0.1 to 50
for Standard Test Methods for Water Analysis
mg/L except for fluoride whose range is 0.1 to 25 mg/L.
D5905Practice for the Preparation of SubstituteWastewater
F488Test Method for On-Site Screening of Heterotrophic
1.3 It is the responsibility of the user to ensure the validity
3
of this test method for other anion concentrations and untested Bacteria in Water (Withdrawn 2005)
aqueous matrices.
3. Terminology
NOTE 1—The highest accepted anion concentration submitted for
3.1 Definitions:
precision and bias extend the anion concentration range for the following
anions: Chloride to 93 mg/L, Sulfate to 90 mg/L, Nitrate to 72 mg/L, and 3.1.1 For definitions of terms used in this standard, refer to
ortho-phosphate to 58 mg/L.
Terminology D1129.
1.4 The values stated in SI units are to be regarded as
3.2 Definitions of Terms Specific to This Standard:
standard. The values given in parentheses are mathematical
3.2.1 capillary ion electrophoresis, n—an electrophoretic
conversions to inch-pound units that are provided for informa-
techniqueinwhichaUV-absorbingelectrolyteisplacedina50
tion only and are not considered standard.
µm to 75 µm fused-silica capillary.
1.5 This standard does not purport to address all of the 3.2.1.1 Discussion—Voltage is applied across the capillary
safety concerns, if any, associated with its use. It is the
causing electrolyte and anions to migrate towards the anode
responsibility of the user of this standard to establish appro- and through the capillary’s UV detector window. Anions are
priate safety and health practices and determine the applica-
separated based upon the differential rates of migration in the
bility of regulatory limitations prior to use. For specific hazard electrical field. Anion detection and quantitation are based
statements, see Section 9.
upon the principles of indirect UV detection.
3.2.2 electrolyte, n—a combination of a UV-absorbing salt
2. Referenced Documents
and an electroosmotic-flow modifier placed inside the
2
2.1 ASTM Standards:
capillary, used as a carrier for the analytes, and for detection
D1066Practice for Sampling Steam
and quantitation.
3.2.2.1 Discussion—The UV-absorbing portion of the salt
1
This test method is under the jurisdiction ofASTM Committee D19 on Water
mustbeanionicandhaveanelectrophoreticmobilitysimilarto
and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents
the analyte anions of interest.
in Water.
Current edition approved Oct. 1, 2015. Published October 2015. Originally
3.2.3 electroosmotic flow (EOF), n—the direction and ve-
approved in 2000. Last previous edition approved in 2010 as D6508–10. DOI:
locityofelectrolyte-solutionflowwithinthecapillaryunderan
10.1520/D6508-15.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. 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 ----
...
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: D6508 − 10 D6508 − 15
Standard Test Method for
Determination of Dissolved Inorganic Anions in Aqueous
Matrices Using Capillary Ion Electrophoresis and Chromate
1
Electrolyte
This standard is issued under the fixed designation D6508; 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 the inorganic anions fluoride, bromide, chloride, nitrite, nitrate, ortho-
phosphate, and sulfate in drinking water, wastewater, and other aqueous matrices using capillary ion electrophoresis (CIE) with
indirect UV detection. See Figs. 1-6.
1.2 The test method uses a chromate-based electrolyte and indirect UV detection at 254 nm. It is applicable for the
determination or inorganic anions in the range of 0.1 to 50 mg/L except for fluoride whose range is 0.1 to 25 mg/L.
1.3 It is the responsibility of the user to ensure the validity of this test method for other anion concentrations and untested
aqueous matrices.
NOTE 1—The highest accepted anion concentration submitted for precision and bias extend the anion concentration range for the following anions:
Chloride to 93 mg/L, Sulfate to 90 mg/L, Nitrate to 72 mg/L, and ortho-phosphate to 58 mg/L.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this The values
given in parentheses are mathematical conversions to inch-pound units that are provided for information only and are not
considered 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 and health practices and determine the applicability of regulatory
limitations prior to use. For specific hazard statements, see Section 9.
2. Referenced Documents
2
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
D3856 Guide for Management Systems in Laboratories Engaged in Analysis of Water
D5810 Guide for Spiking into Aqueous Samples
D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
D5905 Practice for the Preparation of Substitute Wastewater
3
F488 Test Method for On-Site Screening of Heterotrophic Bacteria in Water (Withdrawn 2005)
3. Terminology
3.1 Definitions—Definitions: For definitions of terms used in this test method, refer to Terminology D1129.
3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.
3.2 Definitions of Terms Specific to 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 Sept. 1, 2010Oct. 1, 2015. Published October 2010October 2015. Originally approved in 2000. Last previous edition approved in 20052010 as
ε2
D6508 – 00D6508 – 10. (2005) . DOI: 10.1520/D6508-10.10.1520/D6508-15.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 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 the ASTM website.
3
The last approved version of this historical standard is referenced on 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 ----------------------
D6508 − 15
FIG. 1 Electropherogram of Mixed Anion Working Solution and Added Common Organic Acids
FIG. 2 Electropherogram of 0.2 mg/L Anions Used to Determine MDL
FIG. 3 Electropherogram of Substitute Wastewater
3.2.1 capillary ion electrophoresis, n—an electrophoretic technique in which a UV-absorbing electrolyte is placed in a 50 μm
to 75 μm fused-silica capillary.
3.2.1.1 Discussion—
2
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D6508 − 15
FIG. 4 Electropherogram of Drinking Water
FIG. 5 Electropherogram of Municipal Wastewater Treatment Plant
...
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