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ASTM D5544-16(2023)

(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, 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.

General Information

Status
Published
Publication Date
31-Oct-2023
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 D5544-16 - Standard Test Method for On-Line Measurement of Residue After Evaporation of High-Purity Water
Effective Date
01-Nov-2023
Referred By
ASTM E772-15(2021) - Standard Terminology of Solar Energy Conversion
Effective Date
01-Nov-2023
Referred By
ASTM D5127-13(2018) - Standard Guide for Ultra-Pure Water Used in the Electronics and Semiconductor Industries
Effective Date
01-Nov-2023

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ASTM D5544-16(2023) - Standard Test Method for On-Line Measurement of Residue After Evaporation of High-Purity Water
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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 (Reapproved 2023)
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 2. Referenced Documents
3
2.1 ASTM Standards:
1.1 This test method covers the determination of dissolved
organic and inorganic matter and colloidal material found in D1129 Terminology Relating to Water
D2777 Practice for Determination of Precision and Bias of
high-purity water used in the semiconductor, and related
industries. This material is referred to as residue after evapo- Applicable Test Methods of Committee D19 on Water
D3370 Practices for Sampling Water from Flowing Process
ration (RAE). The range of the test method is from 0.001 μg/L
(ppb) to 60 μg/L (ppb). Streams
D3864 Guide for On-Line Monitoring Systems for Water
1.2 This test method uses a continuous, real time monitoring
Analysis
technique to measure the concentration of RAE. A pressurized
D3919 Practice for Measuring Trace Elements in Water by
sample of high-purity water is supplied to the test method’s
Graphite Furnace Atomic Absorption Spectrophotometry
apparatus continuously through ultra-clean fittings and tubing.
D5127 Guide for Ultra-Pure Water Used in the Electronics
Contaminants from the atmosphere are therefore prevented
and Semiconductor Industries
from entering the sample. General information on the test
E1184 Practice for Determination of Elements by Graphite
method and a literature review on the continuous measurement
2 Furnace Atomic Absorption Spectrometry
of RAE has been published.
3. Terminology
1.3 The values stated in SI units are to be regarded as
standard. The values given in parentheses are mathematical
3.1 Definitions—For definitions of terms used in this test
conversions to inch-pound units that are provided for informa-
method, refer to Terminology D1129.
tion only and are not considered standard.
3.2 Definitions of Terms Specific to This Standard:
1.4 This standard does not purport to address all of the
3.2.1 aerosol, n—any solid or liquid particles, with a nomi-
safety concerns, if any, associated with its use. It is the
nal size range from 10 nm to 100 μm, suspended in a gas
responsibility of the user of this standard to establish appro-
(usually air).
priate safety, health, and environmental practices and deter-
3.2.2 colloidal suspension, n—any material in suspension
mine the applicability of regulatory limitations prior to use.
(for example, silica) with a nominal particle size less than
For specific hazards statements, see Section 8.
100 nm.
1.5 This international standard was developed in accor-
3.2.3 water-based condensation particle counter (WCPC),
dance with internationally recognized principles on standard-
n—instrument for detecting very small aerosol particles in a
ization established in the Decision on Principles for the
size range from approximately 7 nm to 2 μm to 3 μm.
Development of International Standards, Guides and Recom-
3.2.3.1 Discussion—The WCPC cannot differentiate among
mendations issued by the World Trade Organization Technical
particles of varying size within this size range; the counter
Barriers to Trade (TBT) Committee.
reports the number of particles with a size greater than that
defined by the detection-efficiency curve. Detection is indepen-
dent of particle composition.
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
3.2.4 detection effıciency, n—in this test method, detection
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, efficiency represents a curve relating particle size to a counter’s
On-Line Water Analysis, and Surveillance of Water.
ability to detect that size.
Current edition approved Nov. 1, 2023. Published December 2023. Originally
approved in 1994. Last previous edition approved in 2016 as D5544 – 16. DOI:
3
10.1520/D5544-16R23. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
2
Blackford, D. B., “Use of Nonvolatile Residue Monitoring in Semiconductor contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Water Applications” Ultrapure Water Journal, Tall Oaks Publishing, November Standards volume information, refer to the standard’s Document Summary page on
2008, pp. 16–23. the ASTM we
...

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5.1 Ion chromatography provides for both qualitative and quantitative determination of seven common anions, F−, Cl−, NO2−, HPO4 −2, Br−, NO3−, and SO4−2, in the milligram per litre range from a single analytical operation requiring only a few millilitres of sample and taking approximately 10 to 15 min for completion. Additional anions, such as carboxylic acids, can also be quantified.
Note 2: This test method may be used to determine fluoride if its peak is in the water dip by adding 1 mL of eluent (at 100× the concentration in 8.3) to all 100-mL volumes of samples and standards to negate the effect of the water dip. (See 6.3, and also see 6.4.) The quantitation of unretained peaks should be avoided. Anions such as low molecular weight organic acids (formate, acetate, propionate, etc.) that are conductive coelute with fluoride and would bias fluoride quantitation in some drinking waters and most wastewaters. The water dip can be further minimized if measures are taken to remove carbonic acid which remain in the eluent after suppression using carbonate based eluents. There is no water dip if hydroxide eluents are used.  
5.2 Anion combinations such as Cl−/Br − and NO2−/NO3−, which may be difficult to distinguish by other analytical methods, are readily separated by ion chromatography.
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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.  
1.3 It is the user's responsibility to ensure the validity of this test method for other matrices.  
1.4 Concentrations as low as 0.01 mg/L were determined depending upon the anions to be quantified, in single laboratory work. Utilizing a 50-μL sample volume loop and a sensitivity of 3000 μS/cm full scale, the approximate detection limits shown in Table 1 can be achieved. Lower detection limits have been observed with newer instrumentation, column technology and eluents. The analyst must assure optimum instrument performance to maintain a stable baseline at more sensitive conductivity full-scale settings. (A) Data provided by U.S. EPA/EMSL Laboratory, Cincinnati, OH.(B) Column: as specified in 7.1.4.
Detector: as specified in 7.1.6.
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Sample loop: 50 μL.  
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1.6 Using alternate separator column and eluents may permit additional anions such as acetate, formate, or citrate to be determined. This is not the subject of this test method.  
1.7 This test method update approves the use of electrolytically generated eluent, electrolytically regenerated eluent, electrolytic suppression (not autozeroing), and electrolytic trap columns also known as reagent-free ion chromatography. This approval is based on acceptance by the U.S. EPA as referenced in Appendix X2.  
1.8 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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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1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.7 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 hazard statements, see 7.3 and Section 9.  
1.8 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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ASTM
ASTM E2160-23(Test Method)
Standard Test Method for Heat of Reaction of Thermally Reactive Materials by Differential Scanning Calorimetry

SIGNIFICANCE AND USE
5.1 This test method is useful in determining the extrapolated onset temperature, the peak heat flow temperature and the heat of reaction of a material. Any onset temperature determined by this test method is not valid for use as the sole information used for determination of storage or processing conditions.  
5.2 This test method is useful in determining the fraction of a reaction that has been completed in a sample prior to testing. This fraction of reaction that has been completed can be a measure of the degree of cure of a thermally reactive polymer or can be a measure of decomposition of a thermally reactive material upon aging.  
5.3 The heat of reaction values may be used in Practice E1231 to determine hazard potential figures-of-merit Explosion Potential and Shock Sensitivity.  
5.4 This test method may be used in research, process control, quality assurance, and specification acceptance.
SCOPE
1.1 This test method determines the exothermic heat of reaction of thermally reactive chemicals or chemical mixtures, using milligram specimen sizes, by differential scanning calorimetry. Such reactive materials may include thermally unstable or thermoset materials.  
1.2 This test method also determines the extrapolated onset temperature and peak heat flow temperature for the exothermic reaction.  
1.3 This test method may be performed on solids, liquids or slurries.  
1.4 The applicable temperature range of this test method is 25 °C to 600 °C.  
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 is related to Test Method E537, but provides additional information.  
1.7 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.  
1.8 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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