ASTM D2332-13

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

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.
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 The values stated in SI units are to be regarded as 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.

General Information

• Status: Historical
• Publication Date: 31-Dec-2012
• ICS: 13.060.30 - Sewage water
• 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

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 − 13
Standard Practice 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 fluoresced upon absorption of the primary or incident X rays
are dispersed, and intensities at selected wavelengths are
1.1 This practice covers X-ray spectrochemical analysis of
measured by sensitive detectors. Detector output is related to
water-formed deposits.
concentration by calibration curves or charts.
1.2 The practice is applicable to the determination of
4.2 The K spectral lines are used for elements of atomic
elements of atomic number 11 or higher that are present in
numbers 11 to 50. Whether the K or L lines are used for the
significant quantity in the sample (usually above 0.1 %).
elements numbered 51 or higher depends on the available
1.3 The values stated in SI units are to be regarded as
instrumentation.
standard.
1.4 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-
bility of regulatory limitations prior to use.
5.2 Deposit analysis assists in providing proper water con-
ditioning.
2. Referenced Documents
5.3 Deposits formed from or by water in all its phases may
2
2.1 ASTM Standards:
be further classified as scale, sludge, corrosion products, or
D887 Practices for Sampling Water-Formed Deposits
biological deposits. The overall composition of a deposit or
D1129 Terminology Relating to Water
some part of a deposit may be determined by chemical or
D1193 Specification for Reagent Water
spectrographic analysis; the constituents actually present as
E11 Specification for Woven Wire Test Sieve Cloth and Test
chemical substances may be identified by microscope or X-ray
Sieves
diffraction studies. Organisms may be identified by micro-
scopical or biological methods.
3. Terminology
3.1 For definitions of terms used in this practice, refer to
6. Apparatus
Terminology D1129.
6.1 Sample Preparation Equipment:
4. Summary of Practice
6.1.1 Fusion Crucibles, prepared from 25-mm (1-in.)
commercial-grade graphite rods. The dimensions shall be 29
4.1 Thesampleoritsfusionwithasuitablefluxispowdered
1 3
mm (1 ⁄8 in.) high, an inside diameter of 19 mm ( ⁄4 in.), and a
and the powder is compacted (mounted). The mount is then
7
cavity 22 mm ( ⁄8 in.) deep.
irradiatedbyanX-raybeamofshortwavelength(highenergy).
6.1.2 Pulverizers, including an agate or mullite mortar and
The characteristic X rays of the atom that are emitted or
pestle, minimum capacity 25 ml.
6.1.3 Sieves—No. 100 (150-µm) and No. 270 (53-µm) as
1
This practice is under the jurisdiction of ASTM Committee D19 on Water and
specified in Specification E11.
is the direct responsibility of Subcommittee D19.03 on Sampling Water and
Water-Formed Deposits, Analysis of Water for Power Generation and Process Use,
6.1.4 Compactors—A press, equipped with a gauge en-
On-Line Water Analysis, and Surveillance of Water.
abling reproducible pressure, is recommended.
Current edition approved Jan. 1, 2013. Published February 2013. Originally
approved in 1965. Last previous edition approved in 2008 as D2332 – 08. DOI:
6.2 Excitation Source (X-ray Tube):
10.1520/D2332-13.
2 6.2.1 Stable Electrical Power Supply (61 %).
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
6.2.2 Source of high-intensity, short-wave-length X rays.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 6.3 Sample Housing (Turret).
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D2332 − 13
6.4 Spectrometer—Best resolution of the spectrometer and 9. Preparation of Sample
best sensitivity are not simultaneously attainable; a compro-
9.1 Reduce the entire sample of deposits to about 100 g
mise is effected to give adequate values for each.
(drying, degreasing, and crushing if necessary) and grind this
6.4.1 Collimating System.
subsampletoapowderthatwillpassaNo.100(150-µm)sieve.
6.4.2 Spectrogoniometer.
9.2 Mix the powdered sample thoroughly and remove about
6.4.3 Analyzing Crys
...

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: D2332 − 08 D2332 − 13
Standard Practice 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
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 The values stated in SI units are to be regarded as 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D887 Practices for Sampling Water-Formed Deposits
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
E11 Specification for Woven Wire Test Sieve Cloth and Test Sieves
3. Terminology
3.1 For definitions of terms used in this practice, refer to Terminology D1129.
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.
1
This practice 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 Oct. 1, 2008Jan. 1, 2013. Published November 2008 February 2013. Originally approved in 1965. Last previous edition approved in 20032008
as D2332 – 84 (2003).D2332 – 08. DOI: 10.1520/D2332-08.10.1520/D2332-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. 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 − 13
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.
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 E11.
6.1.4 Compactors—A press, equipped with a gauge enabling reproducible pressure, is recommended.
6.2 Excitation Source (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
effe
...