ASTM D2332-84(1999)
(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
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.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 2332 – 84 (Reapproved 1999)
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 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
1.1 This practice covers X-ray spectrochemical analysis of
elements numbered 51 or higher depends on the available
water-formed deposits.
instrumentation.
1.2 The practice is applicable to the determination of
elements of atomic number 11 or higher that are present in
5. Significance and Use
significant quantity in the sample (usually above 0.1 %).
5.1 Certain elements present in water-formed deposits are
1.3 This standard does not purport to address all of the
identified. Concentration levels of the elements are estimated.
safety concerns, if any, associated with its use. It is the
5.2 Deposit analysis assists in providing proper water con-
responsibility of the user of this standard to establish appro-
ditioning.
priate safety and health practices and determine the applica-
5.3 Deposits formed from or by water in all its phases may
bility of regulatory limitations prior to use.
be further classified as scale, sludge, corrosion products, or
2. Referenced Documents biological deposits. The overall composition of a deposit or
some part of a deposit may be determined by chemical or
2.1 ASTM Standards:
spectrographic analysis; the constituents actually present as
D 887 Practices for Sampling Water-Formed Deposits
chemical substances may be identified by microscope or X-ray
D 1129 Terminology Relating to Water
diffraction studies. Organisms may be identified by micro-
E 11 Specification for Wire-Cloth Sieves for Testing Pur-
scopical or biological methods.
poses
6. Apparatus
3. Terminology
6.1 Sample Preparation Equipment:
3.1 Definitions— For definitions of terms used in this
6.1.1 Fusion Crucibles, prepared from 25-mm (1-in.)
practice, refer to Terminology D 1129.
commercial-grade graphite rods. The dimensions shall be 29
1 3
4. Summary of Practice
mm (1 ⁄8 in.) high, an inside diameter of 19 mm ( ⁄4in.), and a
cavity 22 mm ( ⁄8 in.) deep.
4.1 The sample or its fusion with a suitable flux is powdered
6.1.2 Pulverizers, including an agate or mullite mortar and
and the powder is compacted (mounted). The mount is then
pestle, minimum capacity 25 ml.
irradiated by an X-ray beam of short wavelength (high energy).
6.1.3 Sieves—No. 100 (150-μm) and No. 270 (53-μm) as
The characteristic X rays of the atom that are emitted or
specified in Specification E 11.
fluoresced upon absorption of the primary or incident X rays
6.1.4 Compactors—A press, equipped with a gage enabling
are dispersed, and intensities at selected wavelengths are
reproducible pressure, is recommended.
measured by sensitive detectors. Detector output is related to
6.2 Excitation Source (X-ray Tube:)
concentration by calibration curves or charts.
6.2.1 Stable Electrical Power Supply (61 %).
6.2.2 Source of high-intensity, short-wave-length X rays.
This practice is under the jurisdiction of ASTM Committee D-19 on Water and
6.3 Sample Housing (Turret).
is the direct responsibility of Subcommittee D19.03 on Sampling of Water and
6.4 Spectrometer—Best resolution of the spectrometer and
Water-Formed Deposits, Surveillance of Water and Flow Measurement of Water.
best sensitivity are not simultaneously attainable; a compro-
Current edition approved Dec. 28, 1984. Published March 1985. Originally
published as D 2332 – 65 T. Last previous edition D 2332– 79. mise is effected to give adequate values for each.
Annual Book of ASTM Standards, Vol 11.02.
6.4.1 Collimating System.
Annual Book of ASTM Standards, Vol 11.01.
6.4.2 Spectrogoniometer.
Annual Book of ASTM Standards, Vol 14.02.
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 2332
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/g of sample) to present a reproducible surface composition
be determined; for example, a gypsum or an ammonium to the X-ray beam.
dihydrogen phosphate crystal can be used for determining
NOTE 1—At least semiquantitative results can be obtained more quickly
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
general use, being applicable over a broad range and producing
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
assembly, conditioning, and preparation of the fluorescent
7.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that X-ray apparatus.
10.2 Follow the manufacturer’s instructions with respect to
all reagents shall conform to the specifications of the Commit-
tee on Analytical Reagents of the American Chemical So
...
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