ASTM E1552-93(1998)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.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: E 1552 – 93 (Reapproved 1998)
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Terminology
1.1 This test method covers the determination of hafnium in 3.1 For definitions of terms used in this test method, refer to
zirconium and zirconium alloys in concentrations greater than Terminology E 135.
0.003 %.
4. Summary of Test Method
1.2 This standard does not purport to address all of the
4.1 The sample, in the form of drillings, chips, milling,
safety problems, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- turnings or powder, is dissolved in dilute hydrofluoric acid
(HF). The hafnium content is measured using a d-c argon
priate safety and health practices and determine the applica-
plasma spectrometer which is calibrated with reference solu-
bility of regulatory limitations prior to use. Specific precau-
tionary statements are given in Section 8. tions of hafnium in the presence of zirconium. The micropro-
cessor is programmed to display the results in micrograms per
2. Referenced Documents
millilitre (μg/mL).
2.1 ASTM Standards:
5. Significance and Use
B 349 Specification for Zirconium Sponge and Other Forms
of Virgin Metal for Nuclear Application 5.1 When zirconium materials are used in nuclear applica-
tions, it is necessary that hafnium, a neutron absorber, be
B 350 Specification for Zirconium and Zirconium Alloy
Ingots for Nuclear Application present only at very low concentrations.
5.2 This method is useful in testing materials for compli-
B 351 Specification for Hot-Rolled and Cold-Finished Zir-
conium and Zirconium Alloy Bars, Rod and Wire for ance with the compositional requirements as given in Specifi-
cations B 349, B 350, B 351, B 352, and B 353.
Nuclear Application
B 352 Specification for Zirconium and Zirconium Alloy
2 6. Apparatus
Sheet, Strip, and Plate for Nuclear Application
6.1 Plastic Labware:
B 353 Specification for Wrought Zirconium and Zirconium
6.1.1 Beakers, 100-mL, disposable, polypropylene, or
Alloy Seamless and Welded Tubes for Nuclear Service
125-mL polytetrafluoroethylene (PTFE) are satisfactory.
B 614 Practice for Descaling and Cleaning Zirconium and
6.1.2 Volumetric Flasks—Linear polyethylene (LPE) or
Zirconium Alloy Surfaces
polymethylpentene (PMP) are satisfactory.
E 50 Practices for Apparatus, Reagents, and Safety Precau-
tions for Chemical Analysis of Metals
NOTE 1—Plastic volumetric flasks change dimension as they age and
E 135 Terminology Relating to Analytical Chemistry for
therefore must be recalibrated periodically.
Metals, Ores, and Related Materials
6.2 Spectrometer —Modified Czerny-Turner, using an
E 1060 Practice for Interlaboratory Testing of Spectro-
Echelle grating with 30° prism for order separation providing
chemical Methods of Analysis
˚
a reciprocal linear dispersion of about 1 A mm in the 80 to 85th
E 1097 Guide for Direct Current Plasma Emission Spec-
order. The instrument is operated in the sequential mode.
trometry Analysis
6.3 Excitation Source :
6.3.1 D-C Argon Plasma, formed by a tungsten cathode and
two carbon anodes in an inverted “Y” configuration, having a
current output of 7 A at 40 V.
This test method is under the jurisdiction of ASTM Committee E-1 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct 6.3.2 Glass spray tube shall be replaced with one made from
responsibility of Subcommittee E01.06 on Ti, Zr, W, Mo, Ta, Nb, Hf.
PTFE or pyrolytic graphite to prevent hydrofluoric acid attack
Current edition approved July 15, 1993. Published September 1993.
on the glass.
Annual Book of ASTM Standards, Vol 02.04.
Annual Book of ASTM Standards, Vol 3.05.
Discontinued, See, 1997 Annual Book of ASTM Standards, Vol 03.05.
Annual Book of ASTM Standards, Vol 03.06.
Spectrometer system manufactured by Applied Research Laboratories, Inc.,
Valencia, CA 91355, has been found satisfactory.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
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.
E 1552
6.4 Argon—Commercially available as prepurified gas or subsides, add 2 mL HNO and place the beaker on a steam bath
liquid is satisfactory. for 10 min to assure complete dissolution of the specimen.
10.1.2 Cool the solution, transfer to a 100-mL plastic
7. Reagents and Materials
volumetric flask, dilute to volume and mix.
7.1 Purity and Concentration of Reagents—The purity and 10.2 Preparation of Hafnium Solution (1 mg/mL):
concentration of chemical reagents shall conform to the re- 10.2.1 Hafnium Metal—Weigh 0.1 g of the pure hafnium to
quirements prescribed in Practices E 50. the nearest 0.1 mg, into a plastic beaker. Add 20 mL water and,
7.2 Pure Metals: in small increments, add 10 mL HF. Cover with a plastic cover
7.2.1 Hafnium Metal or Hafnium Dioxide, of highest purity and place beaker on a steam bath until dissolution is complete.
available and having a known impurity content. Cool the beaker, transfer to a 100-mL plastic volumetric flask,
dilute to volume, and mix.
NOTE 2—Many hafnium materials contain residual zirconium in quan-
10.2.2 Hafnium Dioxide—Weigh 0.1179 g of the pure HfO
tity sufficient to affect the hafnium value.
to the nearest 1 mg into a plastic beaker. Add 30 mL HF, cover
7.2.2 Zirconium Metal, of the highest purity available and
with a plastic cover and place the beaker on a steam bath until
having a known hafnium content.
dissolution is complete. Cool the beaker, transfer to a 100-mL
7.3 Reference Materials:
plastic volumetric flask, dilute to volume, and mix.
7.3.1 Standard Reference Materials (SRM) : Three unal-
NOTE 3—Hafnium metal and HfO weights must be correspondingly
loyed zirconium materials—SRM 1234, 1235, and 1236 con- 2
increased as total hafnium content decreases because of impurity content.
taining 46, 95, and 198 ppm hafnium, respectively, and three
alloyed zircoloy materials—SRM 1237, 1238, and 1239 con- 10.3 Preparation of Hafnium Spiking Solutions:
taining 31, 178, and 77 ppm hafnium, respectively. 10.3.1 Solution (100 μg/mL)—Transfer 10.0 mL of the
7.3.2 Other reference solutions can be prepared by
...