ASTM E1552-93(2002)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:E1552–93 (Reapproved2002)
Standard Test Method for
Determining Hafnium in Zirconium and Zirconium Alloys
Using the D-C Argon Plasma Spectrometer
This standard is issued under the fixed designation E 1552; 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 E 1097 Guide for Direct Current Plasma Emission Spec-
trometry Analysis
1.1 This test method covers the determination of hafnium in
zirconium and zirconium alloys in concentrations greater than
3. Terminology
0.003 %.
3.1 For definitions of terms used in this test method, refer to
1.2 This standard does not purport to address all of the
Terminology E 135.
safety problems, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
4.1 The sample, in the form of drillings, chips, milling,
bility of regulatory limitations prior to use. Specific precau-
turnings or powder, is dissolved in dilute hydrofluoric acid
tionary statements are given in Section 8.
(HF). The hafnium content is measured using a d-c argon
plasma spectrometer which is calibrated with reference solu-
2. Referenced Documents
tions of hafnium in the presence of zirconium. The micropro-
2.1 ASTM Standards:
cessor is programmed to display the results in micrograms per
B 349 SpecificationforZirconiumSpongeandOtherForms
millilitre (µg/mL).
of Virgin Metal for Nuclear Application
B 350 Specification for Zirconium and Zirconium Alloy
5. Significance and Use
Ingots for Nuclear Application
5.1 When zirconium materials are used in nuclear applica-
B 351 Specification for Hot-Rolled and Cold-Finished Zir-
tions, it is necessary that hafnium, a neutron absorber, be
conium and Zirconium Alloy Bars, Rod and Wire for
2 present only at very low concentrations.
Nuclear Application
5.2 This method is useful in testing materials for compli-
B 352 Specification for Zirconium and Zirconium Alloy
ance with the compositional requirements as given in Specifi-
Sheet, Strip, and Plate for Nuclear Application
cations B 349, B 350, B 351, B 352, and B 353.
B 353 Specification for Wrought Zirconium and Zirconium
Alloy Seamless and Welded Tubes for Nuclear Service
6. Apparatus
B 614 Practice for Descaling and Cleaning Zirconium and
6.1 Plastic Labware:
Zirconium Alloy Surfaces
6.1.1 Beakers, 100-mL, disposable, polypropylene, or
E50 Practices for Apparatus, Reagents, and Safety Precau-
125-mL polytetrafluoroethylene (PTFE) are satisfactory.
tions for Chemical Analysis of Metals
6.1.2 Volumetric Flasks—Linear polyethylene (LPE) or
E 135 Terminology Relating to Analytical Chemistry for
polymethylpentene (PMP) are satisfactory.
Metals, Ores, and Related Materials
E 1060 Practice for Interlaboratory Testing of Spectro- NOTE 1—Plastic volumetric flasks change dimension as they age and
therefore must be recalibrated periodically.
chemical Methods of Analysis
6.2 Spectrometer —Modified Czerny-Turner, using an
Echelle grating with 30° prism for order separation providing
This test method is under the jurisdiction of ASTM Committee E01 on
˚
areciprocallineardispersionofabout1Amminthe80to85th
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
responsibility of Subcommittee E01.06 on Ti, Zr, W, Mo, Ta, Nb, Hf. order. The instrument is operated in the sequential mode.
Current edition approved Oct. 10, 2002. Published September 1993.
6.3 Excitation Source :
Annual Book of ASTM Standards, Vol 02.04.
Annual Book of ASTM Standards, Vol 3.05.
4 6
Discontinued, See, 1997 Annual Book of ASTM Standards, Vol 03.05. Spectrometer system manufactured by Applied Research Laboratories, Inc.,
Annual Book of ASTM Standards, Vol 03.06. Valencia, CA 91355, has been found satisfactory.
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E1552–93 (2002)
6.3.1 D-C Argon Plasma, formed by a tungsten cathode and
Exit slits, µm 25 wide by 300 high
two carbon anodes in an inverted “Y” configuration, having a
current output of 7 A at 40 V. 10. Preparation of Calibration Solutions and Specimens
6.3.2 Glassspraytubeshallbereplacedwithonemadefrom
10.1 Preparation of Calibration Solutions:
PTFE or pyrolytic graphite to prevent hydrofluoric acid attack
10.1.1 Weigh 1.0 g SRM to the nearest 1 mg into a plastic
on the glass.
beaker.Add 20 mLwater and, in small increments, add 10 mL
6.4 Argon—Commercially available as prepurified gas or
HF (48 %) and cover with a plastic cover. When the reaction
liquid is satisfactory.
subsides,add2mLHNO andplacethebeakeronasteambath
for 10 min to assure complete dissolution of the specimen.
7. Reagents and Materials
10.1.2 Cool the solution, transfer to a 100-mL plastic
7.1 Purity and Concentration of Reagents—The purity and
volumetric flask, dilute to volume and mix.
concentration of chemical reagents shall conform to the re-
10.2 Preparation of Hafnium Solution (1 mg/mL):
quirements prescribed in PracticesE50.
10.2.1 Hafnium Metal—Weigh 0.1 g of the pure hafnium to
7.2 Pure Metals:
the nearest 0.1 mg, into a plastic beaker.Add 20 mLwater and,
7.2.1 Hafnium Metal or Hafnium Dioxide, of highest purity
in small increments, add 10 mLHF. Cover with a plastic cover
available and having a known impurity content.
and place beaker on a steam bath until dissolution is complete.
Cool the beaker, transfer to a 100-mL plastic volumetric flask,
NOTE 2—Many hafnium materials contain residual zirconium in quan-
dilute to volume, and mix.
tity sufficient to affect the hafnium value.
10.2.2 Hafnium Dioxide—Weigh 0.1179 g of the pure HfO
7.2.2 Zirconium Metal, of the highest purity available and
to the nearest 1 mg into a plastic beaker.Add 30 mLHF, cover
having a known hafnium content.
with a plastic cover and place the beaker on a steam bath until
7.3 Reference Materials:
dissolution is complete. Cool the beaker, transfer to a 100-mL
7.3.1 Standard Reference Materials (SRM) : Three unal-
plastic volumetric flask, dilute to volume, and mix.
loyed zirconium materials—SRM 1234, 1235, and 1236 con-
taining 46, 95, and 198 ppm hafnium, respectively, and three NOTE 3—Hafnium metal and HfO weights must be correspondin
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