ASTM D4327-17
(Test Method)Standard Test Method for Anions in Water by Suppressed Ion Chromatography
Standard Test Method for Anions in Water by Suppressed Ion Chromatography
SIGNIFICANCE AND USE
5.1 Ion chromatography provides for both qualitative and quantitative determination of seven common anions, F−, Cl−, NO2−, HPO4 −2, Br−, NO3−, and SO4−2, in the milligram per litre range from a single analytical operation requiring only a few millilitres of sample and taking approximately 10 to 15 min for completion. Additional anions, such as carboxylic acids, can also be quantified.
Note 2: This test method may be used to determine fluoride if its peak is in the water dip by adding 1 mL of eluent (at 100× the concentration in 8.3) to all 100-mL volumes of samples and standards to negate the effect of the water dip. (See 6.3, and also see 6.4.) The quantitation of unretained peaks should be avoided. Anions such as low molecular weight organic acids (formate, acetate, propionate, etc.) that are conductive coelute with fluoride and would bias fluoride quantitation in some drinking waters and most wastewaters. The water dip can be further minimized if measures are taken to remove carbonic acid which remain in the eluent after suppression using carbonate based eluents. There is no water dip if hydroxide eluents are used.
5.2 Anion combinations such as Cl−/Br − and NO2−/NO3−, which may be difficult to distinguish by other analytical methods, are readily separated by ion chromatography.
SCOPE
1.1 This test method2,3 covers the sequential determination of fluoride, chloride, nitrite, ortho-phosphate, bromide, nitrate, and sulfate ions in water by suppressed ion chromatography.
Note 1: Order of elution is dependent upon the column used; see Fig. 1.
1.3 It is the user's responsibility to ensure the validity of this test method for other matrices.
1.4 Concentrations as low as 0.01 mg/L were determined depending upon the anions to be quantified, in single laboratory work. Utilizing a 50-μL sample volume loop and a sensitivity of 3000 μS/cm full scale, the approximate detection limits shown in Table 1 can be achieved. Lower detection limits have been observed with newer instrumentation, column technology and eluents. The analyst must assure optimum instrument performance to maintain a stable baseline at more sensitive conductivity full-scale settings. (A) Data provided by U.S. EPA/EMSL Laboratory, Cincinnati, OH.(B) Column: as specified in 7.1.4.
Detector: as specified in 7.1.6.
Eluent: as specified in 8.3.
Pump rate: 2.0 mL/min.
Sample loop: 50 μL.
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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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: D4327 − 17
Standard Test Method for
1
Anions in Water by Suppressed Ion Chromatography
This standard is issued under the fixed designation D4327; 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* 1.7 This test method update approves the use of electrolyti-
2,3 cally generated eluent, electrolytically regenerated eluent,
1.1 This test method covers the sequential determination
electrolyticsuppression(notautozeroing),andelectrolytictrap
of fluoride, chloride, nitrite, ortho-phosphate, bromide, nitrate,
columns also known as reagent-free ion chromatography. This
and sulfate ions in water by suppressed ion chromatography.
approvalisbasedonacceptancebytheU.S.EPAasreferenced
NOTE 1—Order of elution is dependent upon the column used; see Fig.
in Appendix X2.
1.
1.8 The values stated in SI units are to be regarded as
1.2 This test method is applicable to drinking and wastewa-
standard. No other units of measurement are included in this
ters.Therangestestedforthistestmethodforeachanionwere
standard.
as follows (measured in mg/L):
1.9 This standard does not purport to address all of the
Fluoride 0.26 to 8.49
safety concerns, if any, associated with its use. It is the
Chloride 0.78 to 26.0
Nitrite-N 0.36 to 12.0
responsibility of the user of this standard to establish appro-
Bromide 0.63 to 21.0
priate safety, health, and environmental practices and deter-
Nitrate-N 0.42 to 14.0
mine the applicability of regulatory limitations prior to use.
o-Phosphate 0.69 to 23.1
Sulfate 2.85 to 95.0
1.10 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.3 Itistheuser’sresponsibilitytoensurethevalidityofthis
ization established in the Decision on Principles for the
test method for other matrices.
Development of International Standards, Guides and Recom-
1.4 Concentrations as low as 0.01 mg/L were determined
mendations issued by the World Trade Organization Technical
depending upon the anions to be quantified, in single labora-
Barriers to Trade (TBT) Committee.
tory work. Utilizing a 50-µL sample volume loop and a
sensitivity of 3000 µS/cm full scale, the approximate detection
2. Referenced Documents
limits shown in Table 1 can be achieved. Lower detection
4
2.1 ASTM Standards:
limitshavebeenobservedwithnewerinstrumentation,column
D1066Practice for Sampling Steam
technology and eluents. The analyst must assure optimum
D1129Terminology Relating to Water
instrument performance to maintain a stable baseline at more
D1193Specification for Reagent Water
sensitive conductivity full-scale settings.
D2777Practice for Determination of Precision and Bias of
1.5 The upper limit of this test method is dependent upon
Applicable Test Methods of Committee D19 on Water
total anion concentration and may be determined experimen-
D3370Practices for Sampling Water from Flowing Process
tally as described in AnnexA1. These limits may be extended
Streams
byappropriatedilutionorbyuseofasmallerinjectionvolume.
D5810Guide for Spiking into Aqueous Samples
D5847Practice for Writing Quality Control Specifications
1.6 Using alternate separator column and eluents may per-
for Standard Test Methods for Water Analysis
mit additional anions such as acetate, formate, or citrate to be
determined. This is not the subject of this test method.
3. Terminology
3.1 Definitions:
1
This test method is under the jurisdiction ofASTM Committee D19 on Water
3.1.1 For definitions of terms used in this standard, refer to
and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents
in Water.
Terminology D1129.
Current edition approved Dec. 1, 2017. Published December 2017. Originally
approved in 1984. Last previous edition approved in 2011 as D4327–11. DOI:
4
10.1520/D4327-17. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
2
Refs. (1-7) may be consulted for additional information. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
The boldface numbers in parentheses refer to a list of references at the end of Standards volume information, refer to the standard’s Document Summary page on
this standard. the ASTM website.
*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
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D4327 − 17
3.2
...
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: D4327 − 11 D4327 − 17
Standard Test Method for
1
Anions in Water by Suppressed Ion Chromatography
This standard is issued under the fixed designation D4327; 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*
2,3
1.1 This test method covers the sequential determination of fluoride, chloride, nitrite, ortho-phosphate, bromide, nitrate, and
sulfate ions in water by suppressed ion chromatography.
NOTE 1—Order of elution is dependent upon the column used; see Fig. 1.
1.2 This test method is applicable to drinking and wastewaters. The ranges tested for this test method for each anion were as
follows (measured in mg/L):
Fluoride 0.26 to 8.49
Chloride 0.78 to 26.0
Nitrite-N 0.36 to 12.0
Bromide 0.63 to 21.0
Nitrate-N 0.42 to 14.0
o-Phosphate 0.69 to 23.1
Sulfate 2.85 to 95.0
1.3 It is the user’s responsibility to ensure the validity of this test method for other matrices.
1.4 Concentrations as low as 0.01 mg/L were determined depending upon the anions to be quantified, in single laboratory work.
Utilizing a 50-μL sample volume loop and a sensitivity of 33000 μS/cm full scale, the approximate detection limits shown in Table
1 can be achieved. Lower detection limits have been observed with newer instrumentation, column technology and eluents. The
analyst must assure optimum instrument performance to maintain a stable baseline at more sensitive conductivity full-scale
settings.
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 Electrolyticallyelectrolytically generated eluent, electrolytically regenerated
eluent, electrolytic suppression (not autozeroing)autozeroing), and electrolytic trap columns also known as Reagent Free Ion
Chromatography. reagent-free ion chromatography. This approval is based on acceptance by the USU.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 problems,concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and
determine the applicability of regulatory limitations prior to use.
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 Jan. 15, 2011Dec. 1, 2017. Published March 2011December 2017. Originally approved in 1984. Last previous edition approved in 20032011
as D4327 – 03.D4327 – 11. DOI: 10.1520/D4327-11.10.1520/D4327-17.
2 3
TheRefs. following(1-7) references may be consulted for additional information: information.
Small, H., Stevens, T. S., and Bauman, W. C., “Novel Ion Exchange Chromatographic Method Using Conductrimetric Detection,” Analytical Chemistry, Vol 47, 1975,
p. 1801.
Stevens, T. S., Turkelson, V. T., and Alve, W. R., “Determination of Anions in Boiler Blow Down Water with Ion Chromatography,” Analytical Chemistry, Vol 49, 1977,
p. 1176.
Sawicki, E., Mulik, J. D., and Witgenstein, E., Editors, Ion Chromatographic Analysis of Environmental Pollutants, Ann Arbor Science Publishers, Ann Arbor, MI, 1978.
Mulik, J. D., and Sawicki, E., Editors, Ion Chromatographic Analysis of Environmental Pollutants, Vol/No. 2, Ann Arbor Science Publishers, Ann Arbor, MI, 1979.
Weiss, J., Handbook of Ion Chromatography, Dionex Corp., Sunnyvale, CA, 1986.
Waters Innovative Methods for Anion Analysis, Waters Chromatography Division of Millipore, Method A 107 and A 116, 1990.
Haddad, P. R., and Jackson, P. E., Ion Chromatography: Principles and Applications, Elsevier Scientific Publishing Co., 1990.
3
The boldface numbers in parentheses refer to a list of references at the end of this standard.
*A Summary of Changes section appears at the end of this stan
...
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