ASTM D5996-05(2009)
(Test Method)Standard Test Method for Measuring Anionic Contaminants in High-Purity Water by On-Line Ion Chromatography
Standard Test Method for Measuring Anionic Contaminants in High-Purity Water by On-Line Ion Chromatography
SIGNIFICANCE AND USE
In the power-generation industry, high-purity water is used to reduce corrosion from anions, such as sulfate, chloride, and fluoride. These anions are known to be detrimental to materials of construction used in steam generators, reactor vessel internals and recirculation piping, heat exchangers, connective piping, and turbines. Most electric generating plants try to control these anions to 1.0 μg/L in the steam generator feed water. Some nuclear power plants have been able to control anion contaminants at less than 0.02 μg/L.
These anions and others cause low product yields in semiconductor manufacturing. They are also monitored and controlled at similarly low levels as in the electric power industry.
Low molecular weight organic acids (acetate, formate, propionate) have been detected in steam generator feed water. These low molecular weight organic materials are believed to be high-temperature degradation products of chemicals used to control cycle water pH and organic contaminants in cycle makeup water.
In the semiconductor industry, anion contaminants may come from the breakdown of low molecular weight organic materials by ultraviolet light radiation, which is frequently used to produce bacteria-free water. These organic compounds may also contribute to low product yield.
The production of high-purity water for process makeup and use frequently employs the use of demineralizers to remove unwanted anion contaminants. Also in the electric power industry, demineralizers are used in the process stream to maintain low levels of these contaminants. As such, it is important to monitor this process to ensure that water quality standards are being met. These processes can be monitored for the above-mentioned anions.
On-line measurements of these contaminants provide a greater degree of protection of the processes by allowing for frequent on-line measurement of these species. Early detection of contaminant ingress allows for quicker corrective action to locate, ...
SCOPE
1.1 This test method covers on-line analysis of high-purity water by the ion chromatography technique. This test method is applicable for measuring various anionic contaminants in high-purity water, typically in the range of 0.01 to 100 μg/L. This test method is used to determine the concentration of acetate, formate, chloride, fluoride, phosphate, nitrate, and sulfate in a continuously flowing sample. The range of the test method is only as good as the reagent water available for preparing standards. At extremely low concentrations, 1.0 μg/L, preparing standards is difficult, and extra care must be taken in their preparation. The sample may have to be conditioned from higher pressures and temperatures to conditions that are suitable for use by on-line instruments.
1.2 Online sample analysis of flowing streams does not lend itself to collaborative studies due to the nature of the sample and the possibility of contamination that may result from handling the sample as part of the collaborative study. Therefore this standard test method is not based on the results of a collaborative study but is intended to provide the best possible guidance for doing this type of analysis.
1.3 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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Designation: D5996 − 05(Reapproved 2009)
Standard Test Method for
Measuring Anionic Contaminants in High-Purity Water by
1
On-Line Ion Chromatography
This standard is issued under the fixed designation D5996; 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 D1192Guide for Equipment for Sampling Water and Steam
3
in Closed Conduits (Withdrawn 2003)
1.1 This test method covers on-line analysis of high-purity
D1193Specification for Reagent Water
water by the ion chromatography technique. This test method
D2777Practice for Determination of Precision and Bias of
is applicable for measuring various anionic contaminants in
Applicable Test Methods of Committee D19 on Water
high-purity water, typically in the range of 0.01 to 100 µg/L.
D3370Practices for Sampling Water from Closed Conduits
This test method is used to determine the concentration of
D3864Guide for On-Line Monitoring Systems for Water
acetate, formate, chloride, fluoride, phosphate, nitrate, and
Analysis
sulfate in a continuously flowing sample.The range of the test
D4453Practice for Handling of High Purity Water Samples
method is only as good as the reagent water available for
D5542Test Methods for TraceAnions in High Purity Water
preparing standards. At extremely low concentrations, <1.0
by Ion Chromatography
µg/L, preparing standards is difficult, and extra care must be
D5810Guide for Spiking into Aqueous Samples
taken in their preparation. The sample may have to be
D5847Practice for Writing Quality Control Specifications
conditioned from higher pressures and temperatures to condi-
for Standard Test Methods for Water Analysis
tions that are suitable for use by on-line instruments.
1.2 Onlinesampleanalysisofflowingstreamsdoesnotlend
3. Terminology
itself to collaborative studies due to the nature of the sample
3.1 Fordefinitionsoftermsusedinthistestmethod,referto
and the possibility of contamination that may result from
Terminology D1129.
handling the sample as part of the collaborative study. There-
fore this standard test method is not based on the results of a 3.2 Definitions of Terms Specific to This Standard:
collaborative study but is intended to provide the best possible 3.2.1 analytical column, n—a column used to separate the
guidance for doing this type of analysis.
anions of interest.
1.3 This standard does not purport to address all of the 3.2.2 analytical column set, n—a combination of one or
safety concerns, if any, associated with its use. It is the
more guard columns followed by one or more analytical
responsibility of the user of this standard to establish appro- columns.
priate safety and health practices and determine the applica-
3.2.3 anion suppressor device, n—a device that is placed
bility of regulatory limitations prior to use.
between the analytical columns and the detector. Its purpose is
to inhibit detector response to the ionic constituents in the
2. Referenced Documents
eluant, so as to lower the detector background and at the same
2
2.1 ASTM Standards:
time enhance detector response to the ions of interest.
D1066Practice for Sampling Steam
3.2.4 breakthrough volume, n—the maximum sample vol-
D1129Terminology Relating to Water
ume that can be passed through a concentrator column before
the least tightly bound ion of interest is eluted. All of the
columns in series contribute to the overall capacity of the
1
This test method is under the jurisdiction ofASTM Committee D19 on Water
analytical column set.
and is the direct responsibility of Subcommittee D19.03 on Sampling Water and
Water-Formed Deposits,Analysis of Water for Power Generation and Process Use,
3.2.5 concentrator column, n—an ion exchange column
On-Line Water Analysis, and Surveillance of Water.
used to concentrate the ions of interest and thereby increase
Current edition approved Oct. 1, 2009. Published November 2009. Originally
method sensitivity.
approved in 1996. Last previous edition approved in 2005 as D5996–05. DOI:
10.1520/D5996-05R09.
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
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D5996 − 05 (2009)
3.2.6 eluant, n—theionicmobileph
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This document is not anASTM standard and is intended only to provide the user of anASTM 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.
An American National Standard Designation: D5996 – 05 (Reapproved 2009)
Designation:D 5996–96 (Reapproved 2000)
Standard Test Method for
Measuring Anionic Contaminants in High-Purity Water by
1
On-Line Ion Chromatography
This standard is issued under the fixed designation D5996; 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
1.1This test method covers on-line analysis of high-purity water by the ion chromatography technique. This test method is
applicable for measuring various anionic contaminants in high-purity water, typically in the range of 0.02 to 100 µg/L. This test
method is used to determine the concentration of acetate, formate, chloride, fluoride, phosphate, nitrate, and sulfate in a
continuously flowing sample.The range of the test method is only as good as the reagent water available for preparing standards.
Atextremelylowconcentrations,<1.0µg/L,preparingstandardsisdifficult,andextracaremustbetakenintheirpreparation.The
sample may have to be conditioned from higher pressures and temperatures to conditions that are suitable for use by on-line
instruments. The range of the test method is only as good as the reagent water available for standard preparation.
1.2
1.1 This test method covers on-line analysis of high-purity water by the ion chromatography technique. This test method is
applicable for measuring various anionic contaminants in high-purity water, typically in the range of 0.01 to 100 µg/L. This test
method is used to determine the concentration of acetate, formate, chloride, fluoride, phosphate, nitrate, and sulfate in a
continuously flowing sample.The range of the test method is only as good as the reagent water available for preparing standards.
Atextremelylowconcentrations,<1.0µg/L,preparingstandardsisdifficult,andextracaremustbetakenintheirpreparation.The
sample may have to be conditioned from higher pressures and temperatures to conditions that are suitable for use by on-line
instruments.
1.2 Online sample analysis of flowing streams does not lend itself to collaborative studies due to the nature of the sample and
thepossibilityofcontaminationthatmayresultfromhandlingthesampleaspartofthecollaborativestudy.Thereforethisstandard
test method is not based on the results of a collaborative study but is intended to provide the best possible guidance for doing this
type of analysis.
1.3 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
D1192 SpecificationGuide for Equipment for Sampling Water and Steam in Closed Conduits
D1193 Specification for Reagent Water
D2777 Practice for the Determination of Precision and Bias of Applicable Test Methods of Committee D-19D19 on Water
D3370 Practices for Sampling Water from Closed Conduits
D3864 Guide for Continual On-Line Monitoring Systems for Water Analysis
D4453 Practice for Handling of Ultra-Pure Water Samples
2
D5542 Test Methods for TraceAnions in High Purity Water by Ion Chromatography Test Methods for TraceAnions in High
Purity Water by Ion Chromatography
D5810 Guide for Spiking into Aqueous Samples
1
This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.03 on Sampling of Water and
Water-Formed Deposits, Surveillance of Water, and Flow Measurement of Water.
Current edition approved July 10, 1996. Published October 1996.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 Oct. 1, 2009. Published November 2009. Originally approved in 1996. Last previous edition approved in 2005 as D5996–05. DOI:
10.1520/D5996-05R09.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.For Annual Book of ASTM Standards
, Vol 11.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Consho
...
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