ASTM D2332-13(2021)

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: D2332 − 13 (Reapproved 2021)
Standard Practice for
Analysis of Water-Formed Deposits by Wavelength-
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 3.1.1 For definitions of terms used in this standard, refer to
Terminology D1129.
1.1 This practice covers X-ray spectrochemical analysis of
water-formed deposits.
4. Summary of Practice
1.2 The practice is applicable to the determination of
4.1 Thesampleoritsfusionwithasuitablefluxispowdered
elements of atomic number 11 or higher that are present in
and the powder is compacted (mounted). The mount is then
significant quantity in the sample (usually above 0.1 %).
irradiatedbyanX-raybeamofshortwavelength(highenergy).
1.3 The values stated in SI units are to be regarded as
The characteristic X rays of the atom that are emitted or
standard. The values given in parentheses after SI units are
fluoresced upon absorption of the primary or incident X rays
provided for information only and are not considered standard.
are dispersed, and intensities at selected wavelengths are
1.4 This standard does not purport to address all of the measured by sensitive detectors. Detector output is related to
safety concerns, if any, associated with its use. It is the concentration by calibration curves or charts.
responsibility of the user of this standard to establish appro-
4.2 The K spectral lines are used for elements of atomic
priate safety, health, and environmental practices and deter-
numbers 11 to 50. Whether the K or L lines are used for the
mine the applicability of regulatory limitations prior to use.
elements numbered 51 or higher depends on the available
1.5 This international standard was developed in accor-
instrumentation.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
5. Significance and Use
Development of International Standards, Guides and Recom-
5.1 Certain elements present in water-formed deposits are
mendations issued by the World Trade Organization Technical
identified. Concentration levels of the elements are estimated.
Barriers to Trade (TBT) Committee.
5.2 Deposit analysis assists in providing proper water con-
2. Referenced Documents
ditioning.
2.1 ASTM Standards:
5.3 Deposits formed from or by water in all its phases may
D887 Practices for Sampling Water-Formed Deposits
be further classified as scale, sludge, corrosion products, or
D1129 Terminology Relating to Water
biological deposits. The overall composition of a deposit or
D1193 Specification for Reagent Water
some part of a deposit may be determined by chemical or
E11 Specification for Woven Wire Test Sieve Cloth and Test
spectrographic analysis; the constituents actually present as
Sieves
chemical substances may be identified by microscope or X-ray
diffraction studies. Organisms may be identified by micro-
3. Terminology
scopical or biological methods.
3.1 Definitions:
6. Apparatus
1 6.1 Sample Preparation Equipment:
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
6.1.1 Fusion Crucibles, prepared from 25-mm (1-in.)
Water-Formed Deposits, Analysis of Water for Power Generation and Process Use,
commercial-grade graphite rods. The dimensions shall be 29
On-Line Water Analysis, and Surveillance of Water.
1 3
mm (1 ⁄8 in.) high, an inside diameter of 19 mm ( ⁄4 in.), and a
Current edition approved Dec. 1, 2021. Published December 2021. Originally
cavity 22 mm ( ⁄8 in.) deep.
approved in 1965. Last previous edition approved in 2013 as D2332 – 13. DOI:
10.1520/D2332-13R21.
6.1.2 Pulverizers, including an agate or mullite mortar and
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
pestle, minimum capacity 25 ml.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6.1.3 Sieves—No. 100 (150-µm) and No. 270 (53-µm) as
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. specified in Specification E11.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2332 − 13 (2021)
6.1.4 Compactors—A press, equipped with a gauge en- 7.5 Helium Gas, commercial grade, for the spectrometer
abling reproducible pressure, is recommended. flushing system, when vacuum or air paths are not used.
6.2 Excitation Source (X-ray Tube): 7.6 Sodium and Lithium Borates—(Na B O and Li B O ),
2 4 7 2 4 7
6.2.1 Stable Electrical Power Supply (61 %). commonly used as fluxes for the sample.
6.2.2 Source of high-intensity, short-wave-length X rays.
8. Sampling
6.3 Sample Housing (Turret).
8.1 Collect the sample in accordance with Practices D887.
6.4 Spectrometer—Best resolution of the spectrometer and
best sensitivity are not simultaneously attainable; a compro-
9. Preparation of Sample
mise is effected to give adequate values for each.
9.1 Reduce the entire sample of deposits to about 100 g
6.4.1 Collimating System.
(drying, degreasing, and crushing if necessary) and grind this
6.4.2 Spectrogoniometer.
subsampletoapowderthatwillpassaNo.100(150-µm)sieve.
6.4.3 Analyzing Crystal and Holder—The choice of the
analyzing crystal is made on the basis of what elements must 9.2 Mix the powdered sample thoroughly and remove about
be determined; for example, a gypsum or an ammonium
10 g for X-ray fluorescence testing (Note 1). Fuse a weighed
dihydrogen phosphate crystal can be used for determining amount with a weighed amount of a suitable flux (2 to 10 g of
magnesium but lithium fluoride is much superior for copper
flux/gofsample)topresentareproduciblesurfacecomposition
and iron (high-intensity diffracted secondary rays and conse- to the X-ray beam.
quently greater sensitivity and potential precision). A salt,
NOTE1—Atleastsemiquantitativeresultscanbeobtainedmorequickly
sodium chloride (NaCl), crystal is frequently employed for
by compacting (mounting) the test portion (9.3 and 9.4) and proceeding in
generaluse,beingapplicableoverabroadrangeandproducing
accordance with Sections 10, 11, and 12. The decrease in sample
preparation will actually result in improved accuracy in some instances.
intense lines and medium broadening.
6.4.4 Counter-Tube Support.
9.3 Grind not more than 10 g of the material prepared for
X-ray analysis (sample or fusion) to pass a No. 270 (53-µm
6.5 Evacuating or Flushing System.
sieve).
6.6 Measuring System:
9.4 Make duplicate wafers (or suitable mounts for the
6.6.1 Detector (of which the principal types are the Geiger
particular equipment that will be used) by compacting the
counter, scintillation counter, and flow-proportional
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