ASTM D2332-84(2003)
(Practice)Standard Practice for Analysis of Water-Formed Deposits by Wavelength-Dispersive X-Ray Fluorescence
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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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D 2332–84 (Reapproved 2003)
Standard Practice for
Analysis of Water-Formed Deposits by Wavelength-
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 (e) 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
4.2 The K spectral lines are used for elements of atomic
water-formed deposits.
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
be further classified as scale, sludge, corrosion products, or
2.1 ASTM Standards:
biological deposits. The overall composition of a deposit or
D 887 Practices for Sampling Water-Formed Deposits
some part of a deposit may be determined by chemical or
D 1129 Terminology Relating to Water
spectrographic analysis; the constituents actually present as
E11 Specification for Wire Cloth Sieves for Testing Pur-
chemical substances may be identified by microscope or X-ray
poses
diffraction studies. Organisms may be identified by micro-
3. Terminology
scopical or biological methods.
3.1 Definitions—For definitions of terms used in this prac-
6. Apparatus
tice, refer to Terminology D 1129.
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
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.
fluoresced upon absorption of the primary or incident X rays
6.1.3 Sieves—No. 100 (150-µm) and No. 270 (53-µm) as
are dispersed, and intensities at selected wavelengths are
specified in SpecificationE11.
6.1.4 Compactors—Apress, equipped with a gage enabling
This practice is under the jurisdiction of ASTM Committee D19 on Water and reproducible pressure, is recommended.
is the direct responsibility of Subcommittee D19.03 on Sampling of Water and
6.2 Excitation Source (X-ray Tube:)
Water-Formed Deposits, Analysis of Water for Power Generation and Process Use,
6.2.1 Stable Electrical Power Supply (61 %).
On-Line Water Analysis, and Surveillance of Water.
6.2.2 Source of high-intensity, short-wave-length X rays.
Current edition approved Dec. 28, 1984. Published March 1985. Originally
publishedapprovedin1965.Lastpreviouseditionapprovedin1984asD 2332–84.
6.3 Sample Housing (Turret).
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6.4 Spectrometer—Best resolution of the spectrometer and
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
best sensitivity are not simultaneously attainable; a compro-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. mise is effected to give adequate values for each.
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D 2332–84 (2003)
6.4.1 Collimating System. 9.2 Mix the powdered sample thoroughly and remove about
6.4.2 Spectrogoniometer. 10 g for X-ray fluorescence testing (Note 1). Fuse a weighed
6.4.3 Analyzing Crystal and Holder—The choice of the amount with a weighed amount of a suitable flux (2 to 10 g of
analyzing crystal is made on the basis of what elements must flux/gofsample)topresentareproduciblesurfacecomposition
be determined; for example, a gypsum or an ammonium to the X-ray beam.
dihydrogen phosphate crystal can be used for determining
NOTE 1—Atleastsemiquantitativeresultscanbeobtainedmorequickly
magnesium but lithium fluoride is much superior for copper
by compacting (mounting) the test portion (9.3 and 9.4) and proceeding in
and iron (high-intensity diffracted secondary rays and conse-
accordance with Sections 10, 11, and 12. The decrease in sample
quently greater sensitivity and potential precision). A salt,
preparation will actually result in improved accuracy in some instances.
sodium chloride (NaCl), crystal is frequently employed for
9.3 Grind not more than 10 g of the material prepared for
generaluse,beingapplicableoverabroadrangeandproducing
X-ray analysis (sample or fusion) to pass a No. 270 (53-µm
intense lines and medium broadening.
sieve).
6.4.4 Counter-Tube Support.
9.4 Make duplicate wafers (or suitable mounts for the
6.5 Evacuating or Flushing System.
particular equipment that will be used) by compacting the
6.6 Measuring System:
powdered sample (precision and accuracy are improved by
6.6.1 Detector (of which the principal types are the Geiger
briquetting).An internal standard is frequently added by fusion
counter, scintillation counter, and flow-proportional counter).
to the material to be compacted. Some samples may require a
6.6.2 Amplifiers (Including Preamplifier), Rate Meter, Re-
binder (generally organic and added in minimum concentra-
corder, Scaler, and Printout.
tion) for reproducible packing and a smooth surface.
6.6.3 Zeroing, Gain, and Sequence Controls.
10. Preparation of Apparatus
7. Reagents
10.1 Follow the manufacturer’s instructions for the initial
7.1 Purity of Reagents—Reagent grade chemicals shall be
assembly, conditioning, and preparation of the fluorescent
used in all tests. Unless otherwise indicated, i
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