ASTM D5542-04

Standard Test Methods for Trace Anions in High Purity Water by Ion Chromatography

SIGNIFICANCE AND USE
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.
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.
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.  
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.
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 (g/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 Detection(Single Operator)(μg/L)SectionsTest Method A:7-15Chloride0-240.8Phosphate0-39 Sulfate0-551.8Test Method B:16-22Fluoride0-140.7Acetate0-4146.8Formate0-346 5.6
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 the 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: Historical
• Publication Date: 31-May-2004
• ICS: 71.040.30 - Chemical reagents
• Technical Committee: D19 - Water
• Drafting Committee: D19.03 - Sampling Water and Water-Formed Deposits, Analysis of Water for Power Generation and Process Use, On-Line Water Analysis, and Surveillance of Water

Relations

• Replaces: ASTM D5542-94(1999)e1 - Standard Test Methods for Trace Anions in High Purity Water by Ion Chromatography
• Effective Date: 01-Jun-2004
• Referred By: ASTM D1193-06(2018) - Standard Specification for Reagent Water
• Effective Date: 01-Jun-2004
• Referred By: ASTM D5196-06(2018) - Standard Guide for Bio-Applications Grade Water
• Effective Date: 01-Jun-2004
• Referred By: ASTM D8149-20 - Standard Practice for Optimization, Calibration, and Validation of Ion Chromatographic Determination of Heteroatoms and Anions in Petroleum Products and Lubricants
• Effective Date: 01-Jun-2004
• Referred By: ASTM D5996-16 - Standard Test Method for Measuring Anionic Contaminants in High-Purity Water by On-Line Ion Chromatography
• Effective Date: 01-Jun-2004
• Referred By: ASTM D5127-13(2018) - Standard Guide for Ultra-Pure Water Used in the Electronics and Semiconductor Industries
• Effective Date: 01-Jun-2004

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:D 5542–04
Standard Test Methods for
1
Trace Anions in High Purity Water by Ion Chromatography
This standard is issued under the fixed designation D 5542; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
4
1.1 These test methods cover the determination of trace 2.1 ASTM Standards:
(µg/L) levels of fluoride, acetate, formate, chloride, phosphate, D 1066 Practice for Sampling Steam
and sulfate in high purity water using ion chromatography in D 1129 Terminology Relating to Water
combination with sample preconcentration. Other anions, such D 1192 Specification for Equipment for Sampling Water
5
as bromide, nitrite, nitrate, sulfite, and iodide can be deter- and Steam in Closed Conduits
mined by this method. However, since they are rarely present D 1193 Specification for Reagent Water
in significant concentrations in high purity water, they are not D 2777 Practice for Determination of Precision and Bias of
included in this test method. Two test methods are presented Applicable Methods of Committee D19 on Water
and their ranges of application, as determined by a collabora- D 3370 Practices for SamplingWater from Closed Conduits
tive study, are as follows: D 3856 Guide for Good Laboratory Practices in Laborato-
2
ries Engaged in Sampling and Analysis of Water
Limit of Detection
Range Tested (Single Operator)
D 4210 Practice for Interlaboratory Quality Control Proce-
(µg/L Added) (µg/L) Sections
5
dures and Discussion on Reporting Low-Level Data
Test Method A: 7–15
Chloride 0–24 0.8 D 4327 Test Method for Anions in Water by Chemically
3
Phosphate 0–39
Suppressed Ion Chromatography
Sulfate 0–55 1.8
D 4453 Practice for Handling of Ultra-Pure Water Samples
Test Method B: 16–22
D 5810 Guide for Spiking Into Aqueous Samples
Fluoride 0–14 0.7
Acetate 0–414 6.8
D 5847 Practice for the Writing of Quality Control Speci-
Formate 0–346 5.6
fications for Standard Test Methods for Water Analysis
1.2 It is the user’s responsibility to ensure the validity of
3. Terminology
these test methods for waters of untested matrices.
1.3 The common practical range of Test Method A is as
3.1 Definitions:
follows: chloride, 1 to 100 µg/L, phosphate, 3 to 100 µg/L, and 3.1.1 For definitions of terms used in these test methods
sulfate, 2 to 100 µg/L.
refer to Terminology D 1129.
1.4 The common practical range of Test Method B is as 3.2 Definitions of Terms Specific to This Standard:
follows: fluoride, 1 to 100 µg/L, acetate, 10 to 200 µg/L, and
3.2.1 analytical columns—a combination of one or more
formate, 5 to 200 µg/L. guard columns followed by one or more separator columns
1.5 The values stated in SI units are to be regarded as the
used to separate the ions of interest. It should be remembered
standard. that all of the columns in series contribute to the overall
1.6 This standard does not purport to address all of the
capacity of the analytical column set.
safety concerns, if any, associated with its use. It is the 3.2.2 breakthrough volume—the maximum sample volume
responsibility of the user of this standard to establish appro-
that can be passed through a concentrator column before the
priate safety and health practices and determine the applica- least tightly bound ion of interest is eluted.
bility of regulatory limitations prior to use.
3.2.3 concentrator column—an ion exchange column used
to concentrate the ions of interest and thereby increase method
sensitivity.
3.2.4 eluant—the ionic mobile phase used to transport the
1
These test methods are under the jurisdiction of ASTM Committee D19 on
sample through the exchange column.
Water and are the direct responsibility of Subcommittee D19.03 on Sampling of
Water and Water-Formed Deposits, Surveillance of Water, and Flow Measurement
of Water.
4
Current edition approved June 1, 2004. Published June 2004. Originally For referenced ASTM standards, visit the ASTM website, www.astm.org, or
e1
approved in 1994. Last previous edition approved in 1994 as D 5542 – 94 (1999) . contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
2
Limit of detection is lowest measurable concentration not reportable as zero at Standards volume information, refer to the standard’s Document Summary page on
99 % level of confidence as per EPRI study as cited in Sections 15 and 22. the ASTM website.
3 5
Insufficient data to calculate limit of detection. Withdrawn.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D 5542–04
3.2.5 guard
...