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ASTM D5544-94(2004)

(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

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, aerospace, and other industries. This material is referred to as residue after evaporation (RAE). The range of the test method is from 0.1 g/L(ppb) to 20 mg/L (ppm).
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.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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.

General Information

Status
Historical
Publication Date
14-Sep-1994
ICS
71.040.40 - Chemical analysis
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
Current Stage
Ref Project

Relations

Replaces
ASTM D5544-94(1999)e1 - Standard Test Method for On-Line Measurement of Residue After Evaporation of High-Purity Water
Effective Date
15-Sep-1994
Replaced By
ASTM D5544-05 - Standard Test Method for On-Line Measurement of Residue After Evaporation of High-Purity Water
Effective Date
01-Jan-2005
Referred By
ASTM D5127-13(2018) - Standard Guide for Ultra-Pure Water Used in the Electronics and Semiconductor Industries
Effective Date
15-Sep-1994
Referred By
ASTM E772-15(2021) - Standard Terminology of Solar Energy Conversion
Effective Date
15-Sep-1994

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ASTM D5544-94(2004) - Standard Test Method for On-Line Measurement of Residue After Evaporation of High-Purity WaterASTM D5544-94(2004) - Standard Test Method for On-Line Measurement of Residue After Evaporation of High-Purity Water
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ASTM D5544-94(2004) - Standard Test Method for On-Line Measurement of Residue After Evaporation of High-Purity Water
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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
An American National Standard
Designation:D5544–94(Reapproved2004)
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope Applicable Methods of Committee D19 on Water
D3370 PracticesforSamplingWaterfromClosedConduits
1.1 This test method covers the determination of dissolved
D3864 Practice for Continual On-line Monitoring Systems
organic and inorganic matter and colloidal material found in
for Water Analysis
high-purity water used in the semiconductor, aerospace, and
D3919 Practice for Measuring Trace Elements in Water by
other industries. This material is referred to as residue after
Graphite Furnace Atomic Absorption Spectrophotometry
evaporation (RAE). The range of the test method is from 0.1
E 1184 Practice for Electrothermal (Graphite Furnace)
µg/L(ppb) to 20 mg/L (ppm).
Atomic Absorption Analysis
1.2 Thistestmethodusesacontinuous,realtimemonitoring
technique to measure the concentration of RAE.Apressurized
3. Terminology
sample of high-purity water is supplied to the test method’s
3.1 Definitions—For definitions of terms used in this test
apparatus continuously through ultra-clean fittings and tubing.
method, refer to Terminology D1129.
Contaminants from the atmosphere are therefore prevented
3.2 Definitions of Terms Specific to This Standard:
from entering the sample. General information on the test
3.2.1 aerosol, n—any solid or liquid particles, with a
methodandaliteraturereviewonthecontinuousmeasurement
2 nominal size range from 10 nm to 100 µm, suspended in a gas
of RAE has been published.
(usually air).
1.3 The values stated in SI units are to be regarded as the
3.2.2 colloidal suspension, n— any material in suspension
standard. The values given in parentheses are for information
(for example, silica) with a nominal particle size less than 100
only.
nm.
1.4 This standard does not purport to address all of the
3.2.3 condensation nucleus counter (CNC), n—instrument
safety concerns, if any, associated with its use. It is the
for detecting very small aerosol particles in a size range from
responsibility of the user of this standard to establish appro-
approximately 10 nm to 2 to 3 µm. The CNC cannot differen-
priate safety and health practices and determine the applica-
tiate between particles of varying size within this size range; it
bility of regulatory limitations prior to use.Forspecifichazards
reports the number of particles with a size greater than that
statements, see Section 8.
defined by its detection efficiency curve. Detection is indepen-
2. Referenced Documents dent of particle composition.
3
3.2.4 detection effıciency, n— in this test method, detection
2.1 ASTM Standards:
efficiencyrepresentsacurverelatingparticlesizetoacounter’s
D1129 Terminology Relating to Water
ability to detect that size.
D1193 Specification for Reagent Water
3.2.5 diffusion screen, n—a fine mesh screen used to filter
D2777 Practice for Determination of Precision and Bias of
residue particles of a particular size.
3.2.6 high-purity water, n—within the context of this test
method, high-purity water is defined as water containing
1
This test method is under the jurisdiction ofASTM Committee D19 on Water
residue after evaporation in the range from 0.1 µg/L to 20
and is the direct responsibility of Subcommittee D19.03 on Sampling of Water and
Water-Formed Deposits,Analysis of Water for Power Generation and Process Use,
mg/L.
On-Line Water Analysis, and Suveillance of Water.
3.2.7 polydisperse, adj—a size population, in this case of
Current edition approved Sept. 15, 1994. Published November 1994.
2 aerosol particles, composed of many different sizes; the oppo-
Blackford, D. B., and Kerrick, T. A., Proceeding of Microcontamination ’91,
site of monodisperse, a distribution of just one size.
San Jose, CA, 1991, pp. 39–51. Published by Canon Communications Inc., 3340
Ocean Park Blvd., Suite 1000, Santa Monica, CA 90405.
3.2.8 realtime, n—the time that an event is occurring plus
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
the response time; in this case, the response time is 3 to 5 min.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Therefore,contaminationisrecorded3to5minafteritoccurs.
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

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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.  
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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).  
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5.1 This guide is intended to help testing laboratories and the developers of methods and software for those laboratories to apply the concepts of measurement uncertainty to radiochemical analyses.  
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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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1.1 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.  
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Eluent: as specified in 8.3.
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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.  
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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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