Standard Practice for Analysis of Water-Formed Deposits by Wavelength-Dispersive X-Ray Fluorescence

SIGNIFICANCE AND USE
Certain elements present in water-formed deposits are identified. Concentration levels of the elements are estimated.
Deposit analysis assists in providing proper water conditioning.
Deposits formed from or by water in all its phases may be further classified as scale, sludge, corrosion products, or biological deposits. The overall composition of a deposit or some part of a deposit may be determined by chemical or spectrographic analysis; the constituents actually present as chemical substances may be identified by microscope or X-ray diffraction studies. Organisms may be identified by microscopical or biological methods.
SCOPE
1.1 This practice covers X-ray spectrochemical analysis of water-formed deposits.
1.2 The practice is applicable to the determination of elements of atomic number 11 or higher that are present in significant quantity in the sample (usually above 0.1 %).
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D2332 − 08
StandardPractice for
Analysis of Water-Formed Deposits by Wavelength-
1
Dispersive X-Ray Fluorescence
This standard is issued under the fixed designation D2332; 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 measured by sensitive detectors. Detector output is related to
concentration by calibration curves or charts.
1.1 This practice covers X-ray spectrochemical analysis of
water-formed deposits. 4.2 The K spectral lines are used for elements of atomic
numbers 11 to 50. Whether the K or L lines are used for the
1.2 The practice is applicable to the determination of
elements numbered 51 or higher depends on the available
elements of atomic number 11 or higher that are present in
instrumentation.
significant quantity in the sample (usually above 0.1 %).
1.3 This standard does not purport to address all of the 5. Significance and Use
safety concerns, if any, associated with its use. It is the
5.1 Certain elements present in water-formed deposits are
responsibility of the user of this standard to establish appro-
identified. Concentration levels of the elements are estimated.
priate safety and health practices and determine the applica-
5.2 Deposit analysis assists in providing proper water con-
bility of regulatory limitations prior to use.
ditioning.
2. Referenced Documents
5.3 Deposits formed from or by water in all its phases may
2
be further classified as scale, sludge, corrosion products, or
2.1 ASTM Standards:
biological deposits. The overall composition of a deposit or
D887 Practices for Sampling Water-Formed Deposits
some part of a deposit may be determined by chemical or
D1129 Terminology Relating to Water
spectrographic analysis; the constituents actually present as
D1193 Specification for Reagent Water
chemical substances may be identified by microscope or X-ray
E11 Specification for Woven Wire Test Sieve Cloth and Test
diffraction studies. Organisms may be identified by micro-
Sieves
scopical or biological methods.
3. Terminology
6. Apparatus
3.1 For definitions of terms used in this practice, refer to
6.1 Sample Preparation Equipment:
Terminology D1129.
6.1.1 Fusion Crucibles, prepared from 25-mm (1-in.)
commercial-grade graphite rods. The dimensions shall be 29
4. Summary of Practice
1 3
mm (1 ⁄8 in.) high, an inside diameter of 19 mm ( ⁄4 in.), and a
4.1 Thesampleoritsfusionwithasuitablefluxispowdered
7
cavity 22 mm ( ⁄8 in.) deep.
and the powder is compacted (mounted). The mount is then
6.1.2 Pulverizers, including an agate or mullite mortar and
irradiatedbyanX-raybeamofshortwavelength(highenergy).
pestle, minimum capacity 25 ml.
The characteristic X rays of the atom that are emitted or
6.1.3 Sieves—No. 100 (150-µm) and No. 270 (53-µm) as
fluoresced upon absorption of the primary or incident X rays
specified in Specification E11.
are dispersed, and intensities at selected wavelengths are
6.1.4 Compactors—A press, equipped with a gauge en-
abling reproducible pressure, is recommended.
1
This practice is under the jurisdiction of ASTM Committee D19 on Water and
6.2 Excitation Source (X-ray Tube):
is the direct responsibility of Subcommittee D19.03 on Sampling Water and
6.2.1 Stable Electrical Power Supply (61 %).
Water-Formed Deposits, Analysis of Water for Power Generation and Process Use,
6.2.2 Source of high-intensity, short-wave-length X rays.
On-Line Water Analysis, and Surveillance of Water.
Current edition approved Oct. 1, 2008. Published November 2008. Originally
6.3 Sample Housing (Turret).
approved in 1965. Last previous edition approved in 2003 as D2332 – 84 (2003).
DOI: 10.1520/D2332-08.
6.4 Spectrometer—Best resolution of the spectrometer and
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
best sensitivity are not simultaneously attainable; a compro-
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
mise is effected to give adequate values for each.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 6.4.1 Collimating System.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D2332 − 08
6.4.2 Spectrogoniometer. 9. Preparation of Sample
6.4.3 Analyzing Crystal and Holder—The choice of the
9.1 Reduce the entire sample of deposits to about 100 g
analyzing crystal is made on the basis of what elements must
(drying, degreasing, and crushing if necessary) and grind this
be determined; for example, a gypsum or an ammonium
subsampletoapowderthat
...

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.
Designation:D 2332–84 (Reapproved 2003) Designation:D2332–08
Standard Practice for
Analysis of Water-Formed Deposits by Wavelength-
1
Dispersive X-Ray Fluorescence
This standard is issued under the fixed designation D 2332; 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 practice covers X-ray spectrochemical analysis of water-formed deposits.
1.2 The practice is applicable to the determination of elements of atomic number 11 or higher that are present in significant
quantity in the sample (usually above 0.1 %).
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:
D 887 Practices for Sampling Water-Formed Deposits
D1129Terminology Relating to Water 1129 Terminology Relating to Water
D 1193 Specification for Reagent Water
E 11 Specification for Wire Cloth and Sieves for Testing Purposes
3. Terminology
3.1 Definitions—ForFor definitions of terms used in this practice, refer to Terminology D 1129.
4. Summary of Practice
4.1 The sample or its fusion with a suitable flux is powdered and the powder is compacted (mounted). The mount is then
irradiated by an X-ray beam of short wavelength (high energy).The characteristic X rays of the atom that are emitted or fluoresced
upon absorption of the primary or incident X rays are dispersed, and intensities at selected wavelengths are measured by sensitive
detectors. Detector output is related to concentration by calibration curves or charts.
4.2 The K spectral lines are used for elements of atomic numbers 11 to 50. Whether the K or L lines are used for the elements
numbered 51 or higher depends on the available instrumentation.
5. Significance and Use
5.1 Certain elements present in water-formed deposits are identified. Concentration levels of the elements are estimated.
5.2 Deposit analysis assists in providing proper water conditioning.
5.3 Deposits formed from or by water in all its phases may be further classified as scale, sludge, corrosion products, or
biological deposits. The overall composition of a deposit or some part of a deposit may be determined by chemical or
spectrographic analysis; the constituents actually present as chemical substances may be identified by microscope or X-ray
diffraction studies. Organisms may be identified by microscopical or biological methods.
6. Apparatus
6.1 Sample Preparation Equipment:
1
6.1.1 Fusion Crucibles, prepared from 25-mm (1-in.) commercial-grade graphite rods.The dimensions shall be 29 mm (1 ⁄8 in.)
3 7
high, an inside diameter of 19 mm ( ⁄4 in.), and a cavity 22 mm ( ⁄8 in.) deep.
1
This practice 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, Analysis of Water for Power Generation and Process Use, On-Line Water Analysis, and Surveillance of Water.
Current edition approved Dec. 28, 1984.Oct. 1, 2008. Published March 1985.November 2008. Originally published approved in 1965. Last previous edition approved in
19842003 as D 2332 – 84 (2003).
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM 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 ----------------------
D2332–08
6.1.2 Pulverizers, including an agate or mullite mortar and pestle, minimum capacity 25 ml.
6.1.3 Sieves—No. 100 (150-µm) and No. 270 (53-µm) as specified in Specification E 11.
6.1.4 Compactors—A press, equipped with a gauge enabling reproducible pressure, is recommended.
6.2 Excitation Source (X-ray Tube:) X-ray Tube):
6.2.1 Stable Electrical Power Supply (61 %).
6.2.2 Source of high-intensity, short-wave-length X rays.
6.3 Sample Housing (Turret).
6.4 Spectrometer—Best resolution of the spectrometer and best sensitivity are not simultaneously attainable; a compromise is
effected to give adequat
...

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