ASTM D5544-16
(Test Method)Standard Test Method for On-Line Measurement of Residue After Evaporation of High-Purity Water
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 and health practices and determine the applicability of regulatory limitations prior to use. For specific hazards statements, see Section 8.
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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: D5544 − 16
Standard Test Method for
On-Line Measurement of Residue After Evaporation of High-
1
Purity Water
This standard is issued under the fixed designation D5544; 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 D2777Practice for Determination of Precision and Bias of
Applicable Test Methods of Committee D19 on Water
1.1 This test method covers the determination of dissolved
D3370Practices for Sampling Water from Closed Conduits
organic and inorganic matter and colloidal material found in
D3864Guide for On-Line Monitoring Systems for Water
high-purity water used in the semiconductor, and related
Analysis
industries. This material is referred to as residue after evapo-
D3919Practice for Measuring Trace Elements in Water by
ration (RAE).The range of the test method is from 0.001 µg/L
Graphite Furnace Atomic Absorption Spectrophotometry
(ppb) to 60 µg/L (ppb).
D5127Guide for Ultra-Pure Water Used in the Electronics
1.2 Thistestmethodusesacontinuous,realtimemonitoring
and Semiconductor Industries
technique to measure the concentration of RAE.Apressurized
E1184Practice for Determination of Elements by Graphite
sample of high-purity water is supplied to the test method’s
Furnace Atomic Absorption Spectrometry
apparatus continuously through ultra-clean fittings and tubing.
Contaminants from the atmosphere are therefore prevented
3. Terminology
from entering the sample. General information on the test
methodandaliteraturereviewonthecontinuousmeasurement
3.1 Definitions—For definitions of terms used in this test
2
of RAE has been published.
method, refer to Terminology D1129.
1.3 The values stated in SI units are to be regarded as
3.2 Definitions of Terms Specific to This Standard:
standard. The values given in parentheses are mathematical
3.2.1 aerosol, n—any solid or liquid particles, with a nomi-
conversions to inch-pound units that are provided for informa-
nal size range from 10 nm to 100 µm, suspended in a gas
tion only and are not considered standard.
(usually air).
1.4 This standard does not purport to address all of the
3.2.2 colloidal suspension, n—any material in suspension
safety concerns, if any, associated with its use. It is the
(for example, silica) with a nominal particle size less than 100
responsibility of the user of this standard to establish appro-
nm.
priate safety and health practices and determine the applica-
bilityofregulatorylimitationspriortouse.Forspecifichazards 3.2.3 Water-based condensation particle counter (WCPC),
statements, see Section 8.
n—instrument for detecting very small aerosol particles in a
size range from approximately 7 nm to 2 to 3 µm.
2. Referenced Documents
3.2.3.1 Discussion—The WCPC cannot differentiate among
3
2.1 ASTM Standards:
particles of varying size within this size range; the counter
D1129Terminology Relating to Water
reports the number of particles with a size greater than that
definedbythedetection-efficiencycurve.Detectionisindepen-
1 dent of particle composition.
This test method is under the jurisdiction ofASTM Committee D19 on Water
and is the direct responsibility of Subcommittee D19.03 on Sampling Water and
3.2.4 detection effıciency, n—in this test method, detection
Water-Formed Deposits,Analysis of Water for Power Generation and Process Use,
efficiencyrepresentsacurverelatingparticlesizetoacounter’s
On-Line Water Analysis, and Surveillance of Water.
Current edition approved June 1, 2016. Published June 2016. Originally
ability to detect that size.
approved in 1994. Last previous edition approved in 2011 as D5544–11. DOI:
10.1520/D5544-16. 3.2.5 polydisperse, adj—a type of size population, in this
2
Blackford, D. B., “Use of Nonvolatile Residue Monitoring in Semiconductor
caseofaerosolparticles,composedofmanydifferentsizes;the
Water Applications” Ultrapure Water Journal, Tall Oaks Publishing, November
opposite of monodisperse, which is a type of size distribution
2008, pp. 16–23.
3
of just one size.
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
3.2.6 realtime, n—the time that an event is occurring plus
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. the response time.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ------
...
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: D5544 − 11 D5544 − 16
Standard Test Method for
On-Line Measurement of Residue After Evaporation of High-
1
Purity Water
This standard is issued under the fixed designation D5544; 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 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) 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
2
a literature review on the continuous measurement of RAE has been published.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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 and health practices and determine the applicability of regulatory
limitations prior to use. For specific hazards statements, see Section 8.
2. Referenced Documents
3
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
D3370 Practices for Sampling Water from Closed Conduits
D3864 Guide for On-Line Monitoring Systems for Water Analysis
D3919 Practice for Measuring Trace Elements in Water by Graphite Furnace Atomic Absorption Spectrophotometry
D5127 Guide for Ultra-Pure Water Used in the Electronics and Semiconductor Industries
E1184 Practice for Determination of Elements by Graphite Furnace Atomic Absorption Spectrometry
3. Terminology
3.1 Definitions—For definitions of terms used in this test method, refer to Terminology D1129.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 aerosol, n—any solid or liquid particles, with a nominal size range from 10 nm to 100 μm, suspended in a gas (usually
air).
3.2.2 colloidal suspension, n—any material in suspension (for example, silica) with a nominal particle size less than 100 nm.
3.2.3 Water-based condensation particle counter (WCPC), n—instrument for detecting very small aerosol particles in a size
range from approximately 7 nm to 2 to 3 μm.
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 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, 2011June 1, 2016. Published May 2011June 2016. Originally approved in 1994. Last previous edition approved in 20052011 as
D5544 – 05.D5544 – 11. DOI: 10.1520/D5544-11.10.1520/D5544-16.
2
Blackford, D. B., “Use of Nonvolatile Residue Monitoring in Semiconductor Water Applications” Ultrapure Water Journal, November 2008 pp 16-23 Published by Tall
Oaks PublishingBlackford, D. B., “Use of Nonvolatile Residue Monitoring in Semiconductor Water Applications” Ultrapure Water Journal, Tall Oaks Publishing, November
2008, pp. 16–23.
3
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D5544 − 16
3.2.3.1 Discussion—
The WCPC cannot differentiate among particles of varying size within this size range; the counter reports the number of particles
with a size greater than that defined by the detection-efficiency curve. Detection i
...
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: D5544 − 16
Standard Test Method for
On-Line Measurement of Residue After Evaporation of High-
1
Purity Water
This standard is issued under the fixed designation D5544; 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 D2777 Practice for Determination of Precision and Bias of
Applicable Test Methods of Committee D19 on Water
1.1 This test method covers the determination of dissolved
D3370 Practices for Sampling Water from Closed Conduits
organic and inorganic matter and colloidal material found in
D3864 Guide for On-Line Monitoring Systems for Water
high-purity water used in the semiconductor, and related
Analysis
industries. This material is referred to as residue after evapo-
D3919 Practice for Measuring Trace Elements in Water by
ration (RAE). The range of the test method is from 0.001 µg/L
Graphite Furnace Atomic Absorption Spectrophotometry
(ppb) to 60 µg/L (ppb).
D5127 Guide for Ultra-Pure Water Used in the Electronics
1.2 This test method uses a continuous, real time monitoring
and Semiconductor Industries
technique to measure the concentration of RAE. A pressurized
E1184 Practice for Determination of Elements by Graphite
sample of high-purity water is supplied to the test method’s
Furnace Atomic Absorption Spectrometry
apparatus continuously through ultra-clean fittings and tubing.
Contaminants from the atmosphere are therefore prevented
3. Terminology
from entering the sample. General information on the test
method and a literature review on the continuous measurement
3.1 Definitions—For definitions of terms used in this test
2
of RAE has been published.
method, refer to Terminology D1129.
1.3 The values stated in SI units are to be regarded as
3.2 Definitions of Terms Specific to This Standard:
standard. The values given in parentheses are mathematical
3.2.1 aerosol, n—any solid or liquid particles, with a nomi-
conversions to inch-pound units that are provided for informa-
nal size range from 10 nm to 100 µm, suspended in a gas
tion only and are not considered standard.
(usually air).
1.4 This standard does not purport to address all of the
3.2.2 colloidal suspension, n—any material in suspension
safety concerns, if any, associated with its use. It is the
(for example, silica) with a nominal particle size less than 100
responsibility of the user of this standard to establish appro-
nm.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific hazards 3.2.3 Water-based condensation particle counter (WCPC),
statements, see Section 8. n—instrument for detecting very small aerosol particles in a
size range from approximately 7 nm to 2 to 3 µm.
2. Referenced Documents
3.2.3.1 Discussion—The WCPC cannot differentiate among
3
2.1 ASTM Standards:
particles of varying size within this size range; the counter
D1129 Terminology Relating to Water
reports the number of particles with a size greater than that
defined by the detection-efficiency curve. Detection is indepen-
1 dent of particle composition.
This test method is under the jurisdiction of ASTM Committee D19 on Water
and is the direct responsibility of Subcommittee D19.03 on Sampling Water and
3.2.4 detection effıciency, n—in this test method, detection
Water-Formed Deposits, Analysis of Water for Power Generation and Process Use,
efficiency represents a curve relating particle size to a counter’s
On-Line Water Analysis, and Surveillance of Water.
Current edition approved June 1, 2016. Published June 2016. Originally
ability to detect that size.
approved in 1994. Last previous edition approved in 2011 as D5544 – 11. DOI:
10.1520/D5544-16. 3.2.5 polydisperse, adj—a type of size population, in this
2
Blackford, D. B., “Use of Nonvolatile Residue Monitoring in Semiconductor
case of aerosol particles, composed of many different sizes; the
Water Applications” Ultrapure Water Journal, Tall Oaks Publishing, November
opposite of monodisperse, which is a type of size distribution
2008, pp. 16–23.
3
of just one size.
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
3.2.6 realtime, n—the time that an event is occurring plus
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. the response time.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D5544 − 16
3.2.6.1 Discussion—In this case, the response time is
...
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