Standard Practices for Identification of Crystalline Compounds in Water-Formed Deposits By X-Ray Diffraction

SIGNIFICANCE AND USE
The identification of the crystalline structures in water-formed deposits assists in the determination of the deposit sources and mode of deposition. This information may lead to measures for the elimination or reduction of the water-formed deposits.
SCOPE
1.1 These practices provide for X-ray diffraction analysis of powdered crystalline compounds in water-formed deposits. Two are given as follows:
  Sections Practice A—Camera 12 to 21 Practice B—Diffractometer22 to 30
1.2 Both practices yield qualitative identification of crystalline components of water-formed deposits for which X-ray diffraction data are available or can be obtained. Greater difficulty is encountered in identification when the number of crystalline components increases.
1.3 Amorphous phases cannot be identified without special treatment. Oils, greases, and most organic decomposition products are not identifiable.
1.4 The sensitivity for a given component varies with a combination of such factors as density, degree of crystallization, particle size, coincidence of strong lines of components and the kind and arrangement of the atoms of the components. Minimum percentages for identification may therefore range from 1 to 40 %.
1.5 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 consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 8 and Note 20.

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D934 −08
StandardPractices for
Identification of Crystalline Compounds in Water-Formed
1
Deposits By X-Ray Diffraction
This standard is issued under the fixed designation D934; 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
2
1.1 These practices provide for X-ray diffraction analysis of 2.1 ASTM Standards:
powdered crystalline compounds in water-formed deposits. D887 Practices for Sampling Water-Formed Deposits
Two are given as follows: D933 Practice for Reporting Results of Examination and
Analysis of Water-Formed Deposits
Sections
Practice A—Camera 12 to 21
D1129 Terminology Relating to Water
Practice B—Diffractometer 22 to 30
D1193 Specification for Reagent Water
1.2 Both practices yield qualitative identification of crystal-
D2331 Practices for Preparation and Preliminary Testing of
line components of water-formed deposits for which X-ray
Water-Formed Deposits
diffraction data are available or can be obtained. Greater
E11 Specification for Woven Wire Test Sieve Cloth and Test
difficulty is encountered in identification when the number of
Sieves
crystalline components increases.
3. Terminology
1.3 Amorphous phases cannot be identified without special
treatment. Oils, greases, and most organic decomposition 3.1 For definitions of terms used in these practices, refer to
products are not identifiable.
Terminology D1129.
1.4 The sensitivity for a given component varies with a
4. Summary of Practices
combination of such factors as density, degree of
crystallization, particle size, coincidence of strong lines of
4.1 Powdered samples are irradiated with a monochromatic
components and the kind and arrangement of the atoms of the X-ray beam of short wavelength (from about 0.05 to 0.25 nm).
components. Minimum percentages for identification may
The X rays interact with the atoms in the crystal and are
therefore range from 1 to 40 %. scattered in a unique diffraction pattern which produces a
fingerprint of the crystal’s atomic or molecular structure. The
1.5 This standard does not purport to address all of the
analytical instrumentation used in X-ray diffraction includes
safety concerns, if any, associated with its use. It is the
3
the powder camera and the diffractometer (1-5).
responsibility of the user of this standard to consult and
establish appropriate safety and health practices and deter-
5. Significance and Use
mine the applicability of regulatory limitations prior to use.
Specific precautionary statements are given in Section 8 and 5.1 The identification of the crystalline structures in water-
Note 20.
formed deposits assists in the determination of the deposit
1
These practices are under the jurisdiction of ASTM Committee D19 on Water
2
and are the direct responsibility of Subcommittee D19.03 on Sampling Water and For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Water-Formed Deposits, Analysis of Water for Power Generation and Process Use, contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
On-Line Water Analysis, and Surveillance of Water. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Oct. 1, 2008. Published November 2008. Originally the ASTM website.
3
approved in 1947. Last previous edition approved in 2003 as D934 – 80 (2003). The boldface numbers in parentheses refer to the references listed at the end of
DOI: 10.1520/D0934-08. these practices.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D934−08
sources and mode of deposition. This information may lead to
measures for the elimination or reduction of the water-formed
deposits.
6. Purity of Reagents
6.1 Reagent grade chemicals shall be used in all tests.
Unless otherwise indicated, it is intended that all reagents shall
conform to the specifications of the Committee on Analytical
Reagents of the American Chemical Society, where such
1

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D934−08
4
specifications are available. Other grades may be used, pro- 10.2.1 Air-dry moist samples before grinding. If there is
vided it is first ascertained that the reagent is of sufficiently special need to preserve the nature or composition of the
high purity to permit its use without lessening the accuracy of original deposit, special handling must be observed. Handle
the determination. deliquescentdepositsinadry-boxatmosphere.Handlesamples
subject to oxidation in an inert atmosphere.
6.2
...

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 934–80 (Reapproved 2003) Designation: D 934 – 08
Standard Practices for
Identification of Crystalline Compounds in Water-Formed
1
Deposits By X-Ray Diffraction
This standard is issued under the fixed designation D 934; 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 These practices provide for X-ray diffraction analysis of powdered crystalline compounds in water-formed deposits. Two
are given as follows:
Sections
Practice A—Camera 12 to 21
Practice B—Diffractometer 22 to 30
1.2 Both practices yield qualitative identification of crystalline components of water-formed deposits for which X-ray
diffraction data are available or can be obtained. Greater difficulty is encountered in identification when the number of crystalline
components increases.
1.3 Amorphous phases cannot be identified without special treatment. Oils, greases, and most organic decomposition products
are not identifiable.
1.4 Thesensitivityforagivencomponentvarieswithacombinationofsuchfactorsasdensity,degreeofcrystallization,particle
size, coincidence of strong lines of components and the kind and arrangement of the atoms of the components. Minimum
percentages for identification may therefore range from 1 to 40 %.
1.5 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 consult and establish appropriate safety and health practices and determine the applicability of
regulatory limitations prior to use. Specific precautionary statements are given in Section 8 and Note 20.
2. Referenced Documents
2
2.1 ASTM Standards:
D 887 Practices for Sampling Water-Formed Deposits
D 933 Practice for Reporting Results of Examination and Analysis of Water-Formed Deposits
D 1129 Terminology Relating to Water
D 1193 Specification for Reagent Water
D 2331 Practices for Preparation and Preliminary Testing of Water-Formed Deposits
E 11 Specification for Wire Cloth and Sieves for Testing Purposes
3. Terminology
3.1 Definitions—ForFor definitions of terms used in these practices, refer to Terminology D 1129.
4. Summary of Practices
4.1 Powdered samples are irradiated with a monochromatic X-ray beam of short wavelength (from about 0.05 to 0.25 nm).The
X rays interact with the atoms in the crystal and are scattered in a unique diffraction pattern which produces a fingerprint of the
crystal’s atomic or molecular structure. The analytical instrumentation used in X-ray diffraction includes the powder camera and
3
the diffractometer (1), (2), (3), (4), (51-5).
5. Significance and Use
5.1 The identification of the crystalline structures in water-formed deposits assists in the determination of the deposit sources
1
These practices are under the jurisdiction of ASTM Committee D19 on Water and are 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 July 3, 1980.Oct. 1, 2008. Published November 1980.2008. Originally approved in 1947. Last previous edition approved in 19802003 as
D 934 – 80 (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.
3
The boldface numbers in parentheses refer to the references listed at the end of these practices.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D934–08
and mode of deposition. This information may lead to measures for the elimination or reduction of the water-formed deposits.
6. Purity of Reagents
6.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform
to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications are
4
available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use
without lessening the accuracy of the determination.
6.2 Purity
...

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