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ASTM D5544-05

(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
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.
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’calibration. This test method is not different from many other analytical test methods in this respect.
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).
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 immediately to correct a conta...
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
31-Dec-2004
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(2004) - Standard Test Method for On-Line Measurement of Residue After Evaporation of High-Purity Water
Effective Date
01-Jan-2005
Replaced By
ASTM D5544-11 - Standard Test Method for On-Line Measurement of Residue After Evaporation of High-Purity Water
Effective Date
01-May-2011
Referred By
ASTM E772-15(2021) - Standard Terminology of Solar Energy Conversion
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
01-Jan-2005

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ASTM D5544-05 - Standard Test Method for On-Line Measurement of Residue After Evaporation of High-Purity WaterASTM D5544-05 - Standard Test Method for On-Line Measurement of Residue After Evaporation of High-Purity Water
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ASTM D5544-05 - 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
Designation:D5544–05
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 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 Continual On-Line Monitoring Systems
high-purity water used in the semiconductor, and related
for Water 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 0.01
Graphite Furnace Atomic Absorption Spectrophotometry
µg/L(ppb) to 20 mg/L (ppm).
D5127 Guide for Ultra-Pure Water Used in the Electronics
1.2 Thistestmethodusesacontinuous,realtimemonitoring
and Semiconductor Industries
technique to measure the concentration of RAE.Apressurized
E1184 Practice for Electrothermal (Graphite Furnace)
sample of high-purity water is supplied to the test method’s
Atomic Absorption Analysis
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
3.1 Definitions—For definitions of terms used in this test
methodandaliteraturereviewonthecontinuousmeasurement
2 method, refer to Terminology D1129.
of RAE has been published.
3.2 Definitions of Terms Specific to This Standard:
1.3 The values stated in SI units are to be regarded as the
3.2.1 aerosol, n—any solid or liquid particles, with a
standard. The values given in parentheses are for information
nominal size range from 10 nm to 100 µm, suspended in a gas
only.
(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-
3.2.3 condensation particle counter (CPC), n—instrument
bility of regulatory limitations prior to use.Forspecifichazards
for detecting very small aerosol particles in a size range from
statements, see Section 8.
approximately 10 nm to 2 to 3 µm. The CPC cannot differen-
2. Referenced Documents tiate between particles of varying size within this size range; it
3
reports the number of particles with a size greater than that
2.1 ASTM Standards:
defined by its detection efficiency curve. Detection is indepen-
D1129 Terminology Relating to Water
dent of particle composition.
3.2.4 detection effıciency, n—in this test method, detection
1
This test method is under the jurisdiction ofASTM Committee D19 on Water
efficiencyrepresentsacurverelatingparticlesizetoacounter’s
and is the direct responsibility of Subcommittee D19.03 on Sampling of Water and
ability to detect that size.
Water-Formed Deposits,Analysis of Water for Power Generation and Process Use,
3.2.5 diffusion screen, n—a fine mesh screen used to filter
On-Line Water Analysis, and Suveillance of Water.
Current edition approved Jan. 1, 2005. Published January 2005. Originally residue particles of a particular size.
approved in 1994. Last previous edition approved in 2004 as D5544–94 (2004).
3.2.6 high-purity water, n—within the context of this test
DOI: 10.1520/D5544-05.
method, high-purity water is defined as water containing
2
Blackford, D. B., and Kerrick, T. A., Proceeding of Microcontamination ’91,
residue after evaporation in the range from 0.1 µg/L to 20
San Jose, CA, 1991, pp. 39–51. Published by Canon Communications Inc., 3340
Ocean Park Blvd., Suite 1000, Santa Monica, CA 90405.
mg/L.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3.2.7 polydisperse, adj—a size population, in this case of
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
aerosol particles, composed of many different sizes; the oppo-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. site of monodisperse, a distribution of just one size.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D5544–05
3.2.8 realtime, n—t
...

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Standard Test Method for On-Line Measurement of Residue After Evaporation of High-Purity Water

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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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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).  
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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).  
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  
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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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1.1 This guide provides concepts, terminology, symbols, and recommendations for the evaluation and expression of the uncertainty of radiochemical measurements of water and other environmental media by testing laboratories. It applies to measurements of radionuclide activities, including gross activities, regardless of whether they involve chemical preparation of the samples.  
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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.  
5.2 Matrix spiking of samples can also be used to monitor the performance of a laboratory, individual instrument, or analyst as part of a regular quality assurance program. Changes in spike recoveries from the same or similar matrices over time may indicate variations in the quality of analyses and analytical results.  
5.3 Spiking of samples may be performed in the field or in the laboratory, depending on what part of the analytical process is to be tested. Field spiking tests the recovery of the overall process, including preservation and shipping of the sample and may be considered a measure of the stability of the analytes in the matrix. Laboratory spiking tests the laboratory process only. Spiking of sample extracts, concentrates, or dilutions will be reflective of only that portion of the process subsequent to the addition of the spike.  
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 guide covers the general technique of “spiking” aqueous samples with organic analytes or components. It is intended to be applicable to a broad range of organic materials in aqueous media. Although the specific details and handling procedures required for all types of compounds are not described, this general approach is given to serve as a guideline to the analyst in accurately preparing spiked samples for subsequent analysis or comparison. Guidance is also provided to aid the analyst in calculating recoveries and interpreting results. It is the responsibility of the analyst to determine whether the methods and materials cited here are compatible with the analytes of interest.  
1.2 The procedures in this guide are focused on “matrix spike” preparation, analysis, results, and interpretation. The applicability of these procedures to the preparation of calibration standards, calibration check standards, laboratory control standards, reference materials, and other quality control materials by spiking is incidental. A sample (the matrix) is fortified (spiked) with the analyte of interest for a variety of analytical and quality control purposes. While the spiking of multiple sample test portions is discussed, the method of standard additions is not covered.  
1.3 This guide is intended for use in conjunction with the individual analytical test method that provides procedures for analysis of the analyte or component of interest. The test method is used to determine an analyte or component's background level and, again after spiking, its now elevated level. Each test method typically provides procedures not only for samples, but also for calibration standards or analytical control solutions, or both. These procedures include preparation, handling, storage, preservation, and analysis techniques. These procedures are applicable by extension, using the analyst's judgement on a case-by-case basis, to spiking solutions, ...

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Standard Test Method for Anions in Water by Suppressed 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.  
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Detector: as specified in 7.1.6.
Eluent: as specified in 8.3.
Pump rate: 2.0 mL/min.
Sample loop: 50 μL.  
1.5 The upper limit of this test method is dependent upon total anion concentration and may be determined experimentally as described in Annex A1. These limits may be extended by appropriate dilution or by use of a smaller injection volume.  
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.  
1.10 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 D5808-23(Test Method)
Standard Test Method for Determining Chloride in Aromatic Hydrocarbons and Related Chemicals by Microcoulometry

SIGNIFICANCE AND USE
5.1 Organic as well as inorganic chlorine compounds can prove harmful to equipment and reactions in processes involving hydrocarbons.  
5.2 Maximum chloride levels are often specified for process streams and for hydrocarbon products.  
5.3 Organic chloride species are potentially damaging to refinery processes. Hydrochloric acid can be produced in hydrotreating or reforming reactors and this acid accumulates in condensing regions of the refinery.
SCOPE
1.1 This test method covers the determination of organic chloride in aromatic hydrocarbons, their derivatives, and related chemicals.  
1.2 This test method is applicable to samples with chloride concentrations to 25 mg/kg. The limit of detection (LOD) is 0.2 mg/kg and the limit of quantitation (LOQ) is 0.7 mg/kg. With careful analytical technique or the measurement of replicates, or both, this method can be used to successfully analyze concentrations below the LOD.
Note 1: The maximum is the highest concentration from the interlaboratory study and the LOD and LOQ were calculated from Performance Testing Program (PTP) data. See Table 1.  
1.3 This test method is preferred over Test Method D5194 for products, such as styrene, that are polymerized by the sodium biphenyl reagent.  
1.4 In determining the conformance of the test results using this method to applicable specifications, results shall be rounded off in accordance with the rounding-off method of Practice E29.  
1.5 Organic chloride values of samples containing inorganic chlorides will be biased high due to partial recovery of inorganic species during combustion. Interference from inorganic species can be reduced by water washing the sample before analysis. This does not apply to water soluble samples.  
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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