ASTM D5542-16
(Test Method)Standard Test Methods for Trace Anions in High Purity Water by Ion Chromatography
Standard Test Methods for Trace Anions in High Purity Water by Ion Chromatography
SIGNIFICANCE AND USE
4.1 The anions fluoride, chloride, and sulfate have been identified as important contributors to corrosion of high pressure boilers, electric power turbines and their associated heat exchangers. Many electric power utilities attempt to reduce these contaminants in their boiler feed water to less than 1 μg/L.
4.2 In the semiconductor manufacturing process these ions, among others, have been identified as a cause of low product yield and, thus, must be monitored and controlled to levels similar to those required by the electric power industry.
4.3 Low molecular weight organic acids, such as acetate and formate, have been found in many steam generator feed waters and condensates. They are believed to come from the high temperature breakdown of organic matter found in boiler make up water. It is felt that these organic acids promote corrosion by lowering the pH of boiler waters and may even be corrosive themselves.
4.4 Such low molecular weight organics may also be produced when ultraviolet light is used to produce bacteria-free water for semiconductor processing. Such polar organic contaminants are suspected of causing reduced semiconductor yields.
4.5 Phosphates are commonly added to drum boilers in the low mg/L level to precipitate calcium and magnesium and thereby prevent scale formation. Ion chromatography can be used to monitor the concentration of such chemicals in boiler water, as well as detect unwanted carry-over into the steam.
SCOPE
1.1 These test methods cover the determination of trace (μg/L) levels of fluoride, acetate, formate, chloride, phosphate, and sulfate in high purity water using ion chromatography in combination with sample preconcentration. Other anions, such as bromide, nitrite, nitrate, sulfite, and iodide can be determined by this method. However, since they are rarely present in significant concentrations in high purity water, they are not included in this test method. Two test methods are presented and their ranges of application, as determined by a collaborative study, are as follows:
Range Tested
(μg/L Added)
Limit of DetectionA
(Single Operator)
(μg/L)
Sections
Test Method A:
7–16
Chloride
0–24
0.8
Phosphate
0–39
B
Sulfate
0–55
1.8
Test Method B:
17–24
Fluoride
0–14
0.7
Acetate
0–414
6.8
Formate
0–346
5.6
(A) Limit of detection is lowest measurable concentration not reportable as zero at 99 % level of confidence as per EPRI study as cited in Sections 16 and 24.(B) Insufficient data to calculate limit of detection.
1.2 It is the user's responsibility to ensure the validity of these test methods for waters of untested matrices.
1.3 The common practical range of Test Method A is as follows: chloride, 1 to 100 μg/L, phosphate, 3 to 100 μg/L, and sulfate, 2 to 100 μg/L.
1.4 The common practical range of Test Method B is as follows: fluoride, 1 to 100 μg/L, acetate, 10 to 200 μg/L, and formate, 5 to 200 μg/L.
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.
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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: D5542 − 16
Standard Test Methods for
1
Trace Anions in High Purity Water by Ion Chromatography
This standard is issued under the fixed designation D5542; 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 responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
1.1 These test methods cover the determination of trace
bility of regulatory limitations prior to use.
(µg/L) levels of fluoride, acetate, formate, chloride, phosphate,
and sulfate in high purity water using ion chromatography in
2. Referenced Documents
combination with sample preconcentration. Other anions, such
2
as bromide, nitrite, nitrate, sulfite, and iodide can be deter-
2.1 ASTM Standards:
mined by this method. However, since they are rarely present D1066 Practice for Sampling Steam
in significant concentrations in high purity water, they are not
D1129 Terminology Relating to Water
included in this test method. Two test methods are presented D1192 Guide for Equipment for Sampling Water and Steam
3
and their ranges of application, as determined by a collabora-
in Closed Conduits (Withdrawn 2003)
tive study, are as follows: D1193 Specification for Reagent Water
A
D3370 Practices for Sampling Water from Closed Conduits
Limit of Detection
Range Tested
(Single Operator) Sections
D3856 Guide for Management Systems in Laboratories
(µg/L Added)
(µg/L)
Engaged in Analysis of Water
Test Method A: 7–16
Chloride 0–24 0.8
D4210 Practice for Intralaboratory Quality Control Proce-
B
Phosphate 0–39
dures and a Discussion on Reporting Low-Level Data
Sulfate 0–55 1.8
3
(Withdrawn 2002)
Test Method B: 17–24
Fluoride 0–14 0.7
D4453 Practice for Handling of High Purity Water Samples
Acetate 0–414 6.8
D5810 Guide for Spiking into Aqueous Samples
Formate 0–346 5.6
D5847 Practice for Writing Quality Control Specifications
A
Limit of detection is lowest measurable concentration not reportable as zero at
for Standard Test Methods for Water Analysis
99 % level of confidence as per EPRI study as cited in Sections 16 and 24.
B
Insufficient data to calculate limit of detection.
3. Terminology
1.2 It is the user’s responsibility to ensure the validity of
these test methods for waters of untested matrices.
3.1 Definitions:
3.1.1 For definitions of terms used in this standard, refer to
1.3 The common practical range of Test Method A is as
Terminology D1129.
follows: chloride, 1 to 100 µg/L, phosphate, 3 to 100 µg/L, and
3.2 Definitions of Terms Specific to This Standard:
sulfate, 2 to 100 µg/L.
3.2.1 analytical columns, n—a combination of one or more
1.4 The common practical range of Test Method B is as
guard columns followed by one or more separator columns
follows: fluoride, 1 to 100 µg/L, acetate, 10 to 200 µg/L, and
used to separate the ions of interest.
formate, 5 to 200 µg/L.
3.2.1.1 Discussion—It should be remembered that all of the
1.5 The values stated in SI units are to be regarded as columns in series contribute to the overall capacity of the
standard. No other units of measurement are included in this analytical column set.
standard.
3.2.2 breakthrough volume, n—the maximum sample vol-
1.6 This standard does not purport to address all of the ume that can be passed through a concentrator column before
the least tightly bound ion of interest is eluted.
safety concerns, if any, associated with its use. It is the
1
These test methods are under the jurisdiction of ASTM Committee D19 on
2
Water and are the direct responsibility of Subcommittee D19.03 on Sampling Water For referenced ASTM standards, visit the ASTM website, www.astm.org, or
and Water-Formed Deposits, Analysis of Water for Power Generation and Process contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Use, On-Line Water Analysis, and Surveillance of Water. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved June 1, 2016. Published June 2016. Originally the ASTM website.
3
approved in 1994. Last previous edition approved in 2009 as D5542 – 04 (2009). The last approved version of this historical standard is referenced on
DOI: 10.1520/D5542-16. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D5542 − 16
detector background and at the same time enhance detec
...
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: D5542 − 04 (Reapproved 2009) D5542 − 16
Standard Test Methods for
1
Trace Anions in High Purity Water by Ion Chromatography
This standard is issued under the fixed designation D5542; 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 These test methods cover the determination of trace (μg/L) levels of fluoride, acetate, formate, chloride, phosphate, and
sulfate in high purity water using ion chromatography in combination with sample preconcentration. Other anions, such as
bromide, nitrite, nitrate, sulfite, and iodide can be determined by this method. However, since they are rarely present in significant
concentrations in high purity water, they are not included in this test method. Two test methods are presented and their ranges of
application, as determined by a collaborative study, are as follows:
A
Limit of Detection
Range Tested
(Single Operator) Sections
(μg/L Added)
(μg/L)
Test Method A: 7–15
Test Method A: 7–16
Chloride 0–24 0.8
B
Phosphate 0–39
Sulfate 0–55 1.8
Test Method B: 16–23
Test Method B: 17–24
Fluoride 0–14 0.7
Acetate 0–414 6.8
Formate 0–346 5.6
A
Limit of detection is lowest measurable concentration not reportable as zero at 99 % level of confidence as per EPRI study as cited in Sections 1516 and 2324.
B
Insufficient data to calculate limit of detection.
1.2 It is the user’s responsibility to ensure the validity of these test methods for waters of untested matrices.
1.3 The common practical range of Test Method A is as follows: chloride, 1 to 100 μg/L, phosphate, 3 to 100 μg/L, and sulfate,
2 to 100 μg/L.
1.4 The common practical range of Test Method B is as follows: fluoride, 1 to 100 μg/L, acetate, 10 to 200 μg/L, and formate,
5 to 200 μg/L.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D1066 Practice for Sampling Steam
D1129 Terminology Relating to Water
3
D1192 Guide for Equipment for Sampling Water and Steam in Closed Conduits (Withdrawn 2003)
D1193 Specification for Reagent Water
D3370 Practices for Sampling Water from Closed Conduits
D3856 Guide for Management Systems in Laboratories Engaged in Analysis of Water
1
These test methods are under the jurisdiction of ASTM Committee D19 on Water and are the direct responsibility of Subcommittee D19.03 on Sampling Water and
Water-Formed Deposits, Analysis of Water for Power Generation and Process Use, On-Line Water Analysis, and Surveillance of Water.
Current edition approved May 1, 2009June 1, 2016. Published June 2009June 2016. Originally approved in 1994. Last previous edition approved in 20042009 as
D5542–04. DOI: 10.1520/D5542-04R09. – 04 (2009). DOI: 10.1520/D5542-16.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D5542 − 16
D4210 Practice for Intralaboratory Quality Control Procedures and a Discussion on Reporting Low-Level Data (Withdrawn
3
2002)
D4453 Practice for Handling of High Purity Water Samples
D5810 Guide for Spiking into Aqueous Samples
D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in these test methods this standard, refer to Terminology D1129.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 analytical columns—columns, n—a combination of one or more guard columns followed by one or more separator
columns used to separate the ions of interest. It should be remembered that all of the columns in series contribute to the overall
capacity
...
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