1、Designation: E 1552 93 (Reapproved 2002)Standard Test Method forDetermining Hafnium in Zirconium and Zirconium AlloysUsing the D-C Argon Plasma Spectrometer1This standard is issued under the fixed designation E 1552; the number immediately following the designation indicates the year oforiginal adop
2、tion or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of hafnium inzirconium and zi
3、rconium alloys in concentrations greater than0.003 %.1.2 This standard does not purport to address all of thesafety problems, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility o
4、f regulatory limitations prior to use. Specific precau-tionary statements are given in Section 8.2. Referenced Documents2.1 ASTM Standards:B 349 Specification for Zirconium Sponge and Other Formsof Virgin Metal for Nuclear Application2B 350 Specification for Zirconium and Zirconium AlloyIngots for N
5、uclear Application2B 351 Specification for Hot-Rolled and Cold-Finished Zir-conium and Zirconium Alloy Bars, Rod and Wire forNuclear Application2B 352 Specification for Zirconium and Zirconium AlloySheet, Strip, and Plate for Nuclear Application2B 353 Specification for Wrought Zirconium and Zirconiu
6、mAlloy Seamless and Welded Tubes for Nuclear Service2B 614 Practice for Descaling and Cleaning Zirconium andZirconium Alloy Surfaces3E 50 Practices for Apparatus, Reagents, and Safety Precau-tions for Chemical Analysis of Metals4E 135 Terminology Relating to Analytical Chemistry forMetals, Ores, and
7、 Related Materials4E 1060 Practice for Interlaboratory Testing of Spectro-chemical Methods of Analysis5E 1097 Guide for Direct Current Plasma Emission Spec-trometry Analysis53. Terminology3.1 For definitions of terms used in this test method, refer toTerminology E 135.4. Summary of Test Method4.1 Th
8、e sample, in the form of drillings, chips, milling,turnings or powder, is dissolved in dilute hydrofluoric acid(HF). The hafnium content is measured using a d-c argonplasma spectrometer which is calibrated with reference solu-tions of hafnium in the presence of zirconium. The micropro-cessor is prog
9、rammed to display the results in micrograms permillilitre (g/mL).5. Significance and Use5.1 When zirconium materials are used in nuclear applica-tions, it is necessary that hafnium, a neutron absorber, bepresent only at very low concentrations.5.2 This method is useful in testing materials for compl
10、i-ance with the compositional requirements as given in Specifi-cations B 349, B 350, B 351, B 352, and B 353.6. Apparatus6.1 Plastic Labware:6.1.1 Beakers, 100-mL, disposable, polypropylene, or125-mL polytetrafluoroethylene (PTFE) are satisfactory.6.1.2 Volumetric FlasksLinear polyethylene (LPE) orp
11、olymethylpentene (PMP) are satisfactory.NOTE 1Plastic volumetric flasks change dimension as they age andtherefore must be recalibrated periodically.6.2 Spectrometer6Modified Czerny-Turner, using anEchelle grating with 30 prism for order separation providinga reciprocal linear dispersion of about 1 A
12、mm in the 80 to 85thorder. The instrument is operated in the sequential mode.6.3 Excitation Source6:1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and is the directresponsibility of Subcommittee E01.06 on Ti, Zr, W, Mo
13、, Ta, Nb, Hf.Current edition approved July 15, 1993. Published September 1993.2Annual Book of ASTM Standards, Vol 02.04.3Annual Book of ASTM Standards, Vol 3.05.4Discontinued, See, 1997 Annual Book of ASTM Standards, Vol 03.05.5Annual Book of ASTM Standards, Vol 03.06.6Spectrometer system manufactur
14、ed by Applied Research Laboratories, Inc.,Valencia, CA 91355, has been found satisfactory.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.3.1 D-C Argon Plasma, formed by a tungsten cathode andtwo carbon anodes in an inverted “Y” co
15、nfiguration, having acurrent output of 7 A at 40 V.6.3.2 Glass spray tube shall be replaced with one made fromPTFE or pyrolytic graphite to prevent hydrofluoric acid attackon the glass.6.4 ArgonCommercially available as prepurified gas orliquid is satisfactory.7. Reagents and Materials7.1 Purity and
16、 Concentration of ReagentsThe purity andconcentration of chemical reagents shall conform to the re-quirements prescribed in Practices E 50.7.2 Pure Metals:7.2.1 Hafnium Metal or Hafnium Dioxide, of highest purityavailable and having a known impurity content.NOTE 2Many hafnium materials contain resid
17、ual zirconium in quan-tity sufficient to affect the hafnium value.7.2.2 Zirconium Metal, of the highest purity available andhaving a known hafnium content.7.3 Reference Materials:7.3.1 Standard Reference Materials (SRM)7: Three unal-loyed zirconium materialsSRM 1234, 1235, and 1236 con-taining 46, 9
18、5, and 198 ppm hafnium, respectively, and threealloyed zircoloy materialsSRM 1237, 1238, and 1239 con-taining 31, 178, and 77 ppm hafnium, respectively.7.3.2 Other reference solutions can be prepared by dissolv-ing zirconium metal in HF. A solution of hafnium metaldissolved in HF is added to the zir
19、conium solution to producethe required concentrations.8. Hazards8.1 This method involves the use of concentrated hydrof-luoric acid. Read and follow label precautions carefully beforeusing.8.2 Refer to Practices E 50, 7.4.11, for more information.9. Preparation of Apparatus9.1 Conduct start-up and w
20、avelength adjustment in accor-dance with the manufacturers instructions.9.1.1 Optimize the hafnium wavelength at 2641.41 or2820.22 while introducing the 1-mg/mL solution prepared in10.2.9.1.2 Enter the appropriate concentration values (micro-gram per millilitre) for the high and low reference materi
21、alsinto the microprocessor.9.2 Replication:9.2.1 Set the microprocessor to average three integrations at10 s each.9.3 Direct Current PlasmaInstrument Parameters:Current, A 7Voltage, V 40Gas Argon, 99.9 % minFlow rate, L/min 8Entrance slits, m 50 wide by 300 highExit slits, m 25 wide by 300 high10. P
22、reparation of Calibration Solutions and Specimens10.1 Preparation of Calibration Solutions:10.1.1 Weigh 1.0 g SRM to the nearest 1 mg into a plasticbeaker. Add 20 mL water and, in small increments, add 10 mLHF (48 %) and cover with a plastic cover. When the reactionsubsides, add 2 mL HNO3and place t
23、he beaker on a steam bathfor 10 min to assure complete dissolution of the specimen.10.1.2 Cool the solution, transfer to a 100-mL plasticvolumetric flask, dilute to volume and mix.10.2 Preparation of Hafnium Solution (1 mg/mL):10.2.1 Hafnium MetalWeigh 0.1 g of the pure hafnium tothe nearest 0.1 mg,
24、 into a plastic beaker. Add 20 mL water and,in small increments, add 10 mL HF. Cover with a plastic coverand place beaker on a steam bath until dissolution is complete.Cool the beaker, transfer to a 100-mL plastic volumetric flask,dilute to volume, and mix.10.2.2 Hafnium DioxideWeigh 0.1179 g of the
25、 pure HfO2to the nearest 1 mg into a plastic beaker. Add 30 mL HF, coverwith a plastic cover and place the beaker on a steam bath untildissolution is complete. Cool the beaker, transfer to a 100-mLplastic volumetric flask, dilute to volume, and mix.NOTE 3Hafnium metal and HfO2weights must be corresp
26、ondinglyincreased as total hafnium content decreases because of impurity content.10.3 Preparation of Hafnium Spiking Solutions:10.3.1 Solution (100 g/mL)Transfer 10.0 mL of the1-mg/mL solution, prepared in accordance with 10.2, into a100-mL plastic volumetric flask, dilute to volume, and mix.10.3.2
27、Solution (10 g/mL)Transfer 10.0 mL of the 100-g/mL solution, prepared in accordance with 10.3.1, into a100-mL plastic volumetric flask, dilute to volume and mix.10.4 Preparation of Synthetic Reference Materials:10.4.1 For each calibration point required, weigh 0.5 g ofthe pure zirconium metal to the
28、 nearest 1 mg into a plasticbeaker. Add 10 mL water and, in small increments, add 5 mLHF (48 %) and cover with a plastic cover. Continue asdescribed in 10.1.1.10.4.2 Cool the solution and transfer to a 50-mL plasticvolumetric flask. Reserve sufficient volume for the hafniumspike.10.4.3 Transfer know
29、n quantities of the appropriate hafniumspiking solution prepared in 10.3 to each flask as given in Table1.10.5 Preparation of Specimens:7Available from National Institute of Standards and Technology, StandardReference Materials Program, Building 202, Room 204, Gaithersburg, MD 20899.TABLE 1 Preparat
30、ion of Synthetic Reference SolutionsConcentrationAConcentration ofSpiking Solution,g/mLVolume of SpikingSolution, mLppm g/mL30 + bB0.3 10 1.550 + b 0.5 10 2.5100 + b 1.0 10 5.0200 + b 2.0 10 10.0500 + b 5.0 100 2.5AValues given in parts per million (ppm) and micrograms per millilitre (g/mL)are only
31、true if the zirconium matrix material is hafnium-free. If hafnium is presentin the matrix material, its value must be added to the spiked value.BThe letter b indicates blank.E 1552 93 (2002)210.5.1 Samples shall be clean and oil free. Refer to PracticeB 614 for cleaning procedures.10.5.2 Weigh dupli
32、cate 1.0-g portions, to the nearest 1 mg,into a plastic beaker. Dissolve the samples as described in10.1.1 and 10.1.2.11. Calibration and Standardization11.1 CalibrationThe system sets a two-point calibrationcurve in the microprocessor.11.1.1 “Auto/Range” will set the intensity of the highreference
33、material into memory while being introduced into theplasma.11.1.2 “Low Standard” will set the intensity of the lowreference material into memory while being introduced into theplasma.11.2 StandardizationThe frequency of standardizationwill depend upon the long term stability of the instrument.11.2.1
34、 To ensure that the instrument is in calibration, intro-duce the high, low, or an intermediate reference material as atest solution. If the reading deviates by more than 5 % from theestablished value, recalibrate as described in 11.1.12. Procedure12.1 Introduce up to four test solutions in a series
35、into theplasma with the instrument set to average three readings for 10s each.12.2 Check the calibration after every four test solutions bymeasuring a reference material as a test solution. If the readingdeviates by less than 5 % from the established value, continuewith the next series of tests. If
36、the standard deviates by morethan 5 %, recalibrate as described in 11.1 and remeasure thetest solutions.12.3 Procedures for “drift correction” are described inGuide E 1097.13. Calculation13.1 Calculate the average of the three readings (microgramper millilitre) as follows:Hafnium, ppm 5 A 3 B/C (1)w
37、here:A = concentration of hafnium in test solution, g/mL,B = volume of final test solution, mL, andC = weight of sample, g.14. Precision and Bias14.1 PrecisionFive laboratories cooperated in testing fourspecimens. Precision data are given in Table 2.14.2 BiasNo bias was detected in the interlaborato
38、ry testresults of the NIST SRMs that were included, nor in the higherconcentration production sample which had been assigned aconcentration value for hafnium.15. Keywords15.1 d-c plasma; hafnium; zirconiumE 1552 93 (2002)3ASTM International takes no position respecting the validity of any patent rig
39、hts asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any
40、 time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments wi
41、ll receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by AS
42、TM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); o
43、r through the ASTM website(www.astm.org).TABLE 2 Statistical InformationTest Sample Certified ppm Hf Assigned Value Amount Found Repeatability (R1 E173) Reproducibility (R2 E173)NIST SRM 1234 46 . 46.1 6.4 9.3NIST SRM 1235 95 . 91.7 7.7 15.5NIST SRM 1236 198 . 195.3 14.3 32.1Production Specimen . 614 612.3 41.0 87.8E 1552 93 (2002)4
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