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ASTM D4327-03

(Test Method)

Standard Test Method for Anions in Water by Chemically Suppressed Ion Chromatography

Standard Test Method for Anions in Water by Chemically Suppressed Ion Chromatography

SIGNIFICANCE AND USE
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.
Note 2—This test method may be used to determine fluoride if its peak is in the water dip by adding one 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.
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 method covers the sequential determination of fluoride, chloride, nitrite,  ortho-phosphate, bromide, nitrate, and sulfate ions in water by chemically suppressed ion chromatography. Note 1Order of elution is dependent upon the column used; see .
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):Fluoride0.26 to 8.49Chloride0.78 to 26.0Nitrite-N0.36 to 12.0Bromide0.63 to 21.0Nitrate-N0.42 to 14.0o-Phosphate0.69 to 23.1Sulfate2.85 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 quantitated, in single laboratory work. Utilizing a 50-μL sample volume loop and a sensitivity of 3 μS/cm full scale, the approximate detection limits shown in Table 1 can be achieved. If lower detection levels are required, the sensitivity may be improved by using a lower scale setting (100 μL). 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 formate or citrate to be determined. This is not the subject of this test method.
1.7 This standard does not purport to address all of the safety problems, 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
Historical
Publication Date
09-Jan-2003
ICS
71.040.40 - Chemical analysis
Technical Committee
D19 - Water
Drafting Committee
D19.05 - Inorganic Constituents in Water
Current Stage
Ref Project

Relations

Replaced By
ASTM D4327-11 - Standard Test Method for Anions in Water by Suppressed Ion Chromatography
Effective Date
01-Mar-2011

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ASTM D4327-03 - Standard Test Method for Anions in Water by Chemically Suppressed Ion Chromatography
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Standards Content (Sample)

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:D4327–03
Standard Test Method for
Anions in Water by Chemically Suppressed Ion
1
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*
2
1.1 Thistestmethod coversthesequentialdeterminationof
fluoride, chloride, nitrite, ortho-phosphate, bromide, nitrate,
and sulfate ions in water by chemically suppressed ion chro-
matography.
NOTE 1—Order of elution is dependent upon the column used; see Fig.
1.
1.2 This test method is applicable to drinking and wastewa-
ters.Therangestestedforthistestmethodforeachanionwere
as follows (measured in mg/L):
FIG. 1 Chromatogram Showing Separation Using the AS4A
Fluoride 0.26 to 8.49
Column
Chloride 0.78 to 26.0
Nitrite-N 0.36 to 12.0
Bromide 0.63 to 21.0
sensitivity of 3 µS/cm full scale, the approximate detection
Nitrate-N 0.42 to 14.0
limits shown in Table 1 can be achieved. If lower detection
o-Phosphate 0.69 to 23.1
levels are required, the sensitivity may be improved by using a
Sulfate 2.85 to 95.0
lowerscalesetting(<3µS/cm)oralargersampleinjectionloop
1.3 Itistheuser’sresponsibilitytoensurethevalidityofthis
(>100 µL). The analyst must assure optimum instrument
test method for other matrices.
performance to maintain a stable baseline at more sensitive
1.4 Concentrations as low as 0.01 mg/L were determined
conductivity full-scale settings.
depending upon the anions to be quantitated, in single labora-
1.5 The upper limit of this test method is dependent upon
tory work. Utilizing a 50-µL sample volume loop and a
total anion concentration and may be determined experimen-
tally as described inAnnexA1. These limits may be extended
byappropriatedilutionorbyuseofasmallerinjectionvolume.
1
This test method is under the jurisdiction ofASTM Committee D19 on Water
1.6 Using alternate separator column and eluents may per-
and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents
mit additional anions such as formate or citrate to be deter-
in Water.
Current edition approved Jan. 10, 2003. Published January 2003. Originally
mined. This is not the subject of this test method.
approved in 1984. Last previous edition approved in 1997 as D4327–97. DOI:
1.7 This standard does not purport to address all of the
10.1520/D4327-03.
2 safety problems, if any, associated with its use. It is the
The following references may be consulted for additional information:
responsibility of the user of this standard to establish appro-
Small, H., Stevens, T. S., and Bauman, W. C., “Novel Ion Exchange Chromato-
graphic Method Using Conductrimetric Detection,” Analytical Chemistry, Vol 47,
priate safety and health practices and determine the applica-
1975, p. 1801.
bility of regulatory limitations prior to use.
Stevens, T. S., Turkelson, V. T., and Alve, W. R., “Determination of Anions in
BoilerBlowDownWaterwithIonChromatography,” Analytical Chemistry,Vol49,
2. Referenced Documents
1977, p. 1176.
Sawicki, E., Mulik, J. D., and Witgenstein, E., Editors, Ion Chromatographic 3
2.1 ASTM Standards:
Analysis of Environmental Pollutants, Ann Arbor Science Publishers, Ann Arbor,
D1066 Practice for Sampling Steam
MI, 1978.
D1129 Terminology Relating to Water
Mulik, J. D., and Sawicki, E., Editors, Ion Chromatographic Analysis of
Environmental Pollutants,Vol/No.2,AnnArborSciencePublishers,AnnArbor,MI,
D1193 Specification for Reagent Water
1979.
Weiss, J., Handbook of Ion Chromatography, Dionex Corp., Sunnyvale, CA,
1986.
3
Waters Innovative Methods forAnionAnalysis,WatersChromatographyDivision
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
of Millipore, Method A 107 and A 116, 1990.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Haddad, P. R., and Jackson, P. E., Ion Chromatography: Principles and
Standards volume information, refer to the standard’s Document Summary page on
Applications, Elsevier Scientific Publishing Co., 1990.
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.
1

---------------------- Page: 1 ----------------------
D4327–03
TABLE 1 Approximate Single Laboratory Detection Limits in
that is continuously regenerated by a flow of dilute sulfuric
A,B
Reagent Water
acid. The suppressor device reduces the background conduc-
Retention MDL
tivity of the eluent to a low or negligible level by replacing the
Analyte Peak No.
Time, min mg/L
cationswiththehydrogenion,therebyconvertingtheanionsin
...

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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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1.3 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, ...

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Standard Test Method for Anions in Water by Suppressed Ion Chromatography

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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.
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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.
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Eluent: as specified in 8.3.
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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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