1、Designation: E 1552 08Standard Test Method forDetermining Hafnium in Zirconium and Zirconium Alloys ByDirect Current PlasmaAtomic Emission Spectrometry1This standard is issued under the fixed designation E 1552; the number immediately following the designation indicates the year oforiginal adoption
2、or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of hafnium inzirconium and zirconiu
3、m alloys in concentrations greater than0.003 %.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety problems, if any, associated with its use. It is theresponsibility
4、 of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific precau-tionary statements are given in Section 8.2. Referenced Documents2.1 ASTM Standards:2B 349/B 349M Specification for Zirconium S
5、ponge andOther Forms of Virgin Metal for Nuclear ApplicationB 350/B 350M Specification for Zirconium and ZirconiumAlloy Ingots for Nuclear ApplicationB 351/B 351M Specification for Hot-Rolled and Cold-Finished Zirconium and Zirconium Alloy Bars, Rod, andWire for Nuclear ApplicationB 352/B 352M Speci
6、fication for Zirconium and ZirconiumAlloy Sheet, Strip, and Plate for Nuclear ApplicationB 353 Specification for Wrought Zirconium and ZirconiumAlloy Seamless and Welded Tubes for Nuclear Service(Except Nuclear Fuel Cladding)B 493 Specification for Zirconium and Zirconium AlloyForgingsB 494/B 494M S
7、pecification for Primary ZirconiumB 495 Specification for Zirconium and Zirconium AlloyIngotsB 523/B 523M Specification for Seamless and Welded Zir-conium and Zirconium Alloy TubesB 550/B 550M Specification for Zirconium and ZirconiumAlloy Bar and WireB 551/B 551M Specification for Zirconium and Zir
8、coniumAlloy Strip, Sheet, and PlateB 614 Practice for Descaling and Cleaning Zirconium andZirconium Alloy SurfacesB 653/B 653M Specification for Seamless and Welded Zir-conium and Zirconium Alloy Welding FittingsB 658/B 658M Specification for Seamless and Welded Zir-conium and Zirconium Alloy PipeB
9、752 Specification for Castings, Zirconium-Base, Corro-sion Resistant, for General ApplicationB811 Specification for Wrought Zirconium Alloy SeamlessTubes for Nuclear Reactor Fuel CladdingE50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelat
10、ed MaterialsE 135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE 1097 Guide for Direct Current Plasma-Atomic EmissionSpectrometry Analysis3. Terminology3.1 For definitions of terms used in this test method, refer toTerminology E 135.4. Summary of Test Method4.1
11、The 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 direct currentplasma (DCP) spectrometer, which is calibrated with referencesolutions of hafnium in the presence of zirconium. Themicroproces
12、sor is programmed to display the results in micro-grams per millilitre (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.1This test method is under the jurisdiction
13、 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, Ta, Nb, Hf, Re.Current edition approved July 15, 2008. Published August 2008. Originallyapproved in 1993. Last previous edition approved in 2
14、002 as E 1552 93 (2002).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Ba
15、rr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.2 This test method is useful in testing materials forcompliance with the compositional requirements as given inSpecifications B 349/B 349M, B 350/B 350M, B 351/B 351M,B 352/B 352M, B 353, B 493, B 494/B 494M, B 495, B 52
16、3/B 523M, B 550/B 550M, B 551/B 551M, B 653/B 653M,B 658/B 658M, B 752, and B811.6. 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) orpolymethylpentene (PMP) are s
17、atisfactory.NOTE 1Plastic volumetric flasks change dimension as they age andtherefore must be recalibrated periodically.6.2 SpectrometerModified Czerny-Turner, using anEchelle grating with 30 prism for order separation providinga reciprocal linear dispersion of about 0.1 nm/mm in the 80 to85th order
18、. The instrument is operated in the sequential mode.6.3 Excitation Source:36.3.1 D-C Plasma, formed by a tungsten cathode and twocarbon anodes in an inverted “Y” configuration, 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
19、 to prevent hydrofluoric acid attackon the glass.6.4 ArgonCommercially available as prepurified gas orliquid is satisfactory.7. Reagents and Materials7.1 Purity and Concentration of ReagentsThe purity andconcentration of chemical reagents shall conform to the re-quirements prescribed in Practices E5
20、0.7.2 Pure Metals:7.2.1 Hafnium Metal or Hafnium Dioxide, of highest purityavailable and having a known impurity content.NOTE 2Many hafnium materials contain residual zirconium in quan-tity sufficient to affect the hafnium value.7.2.2 Zirconium Metal, of the highest purity available andhaving a know
21、n hafnium content.7.3 Reference Materials:7.3.1 Standard Reference Materials (SRM):4OneZircaloy-4, SRM 360b, containing 80 ppm hafnium, is avail-able.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 zirco
22、nium 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 E50, 7.4.11, for more information.9. Preparation of Apparatus9.1 Conduct start-up and wave
23、length adjustment in accor-dance with the manufacturers instructions.9.1.1 Optimize the hafnium wavelength at 264.14 nm or282.02 nm 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 mater
24、ialsinto 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.
25、Preparation 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 nitric acid (H
26、NO3) and place the beaker ona steam bath for 10 min to assure complete dissolution of thespecimen.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
27、nearest 0.1 mg, 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
28、0.1179 g of the 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
29、must be correspondinglyincreased 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,
30、and mix.10.3.2 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:3The sole source of supply of the apparatus known to the committee at this
31、 timeis Applied Research Laboratories, Inc., 5371 NW 161 St., Miami, FL 33014,http:/www.arl-. If you are aware of alternative suppliers, please providethis information to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical commit
32、tee,1whichyou may attend.4Available from National Institute of Standards and Technology (NIST), 100Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http:/www.nist.gov.E155208210.4.1 For each calibration point required, weigh 0.5 g ofthe pure zirconium metal to the nearest 1 mg into a plasticbeake
33、r. 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 known quantities of the appropriate h
34、afniumspiking solution prepared in 10.3 to each flask as given in Table2.10.5 Preparation of Specimens:10.5.1 Samples shall be clean and oil free. Refer to PracticeB 614 for cleaning procedures.10.5.2 Weigh duplicate 1.0-g portions, to the nearest 1 mg,into a plastic beaker. Dissolve the samples as
35、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 material into memory while being introduced into theplasma.11.1.2 “Low Standard” will se
36、t 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 To ensure that the instrument is in calibration, intro-duce the high, low, or an interm
37、ediate 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 into theplasma with the instrument set to average three readings for10 s each.12.2 Check
38、 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 the standard deviates by morethan 5 %, recalibrate as described in 11.1 and remeasure th
39、etest 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)where:A = concentration of hafnium in test solution, g/mL,B = volume of final test soluti
40、on, mL, andC = weight of sample, g.14. Precision and Bias14.1 PrecisionFive laboratories cooperated in testing fourspecimens. Precision data are given in Table 1.14.2 BiasNo bias was detected in the interlaboratory testresults of the NIST SRMs that were included, nor in the higherconcentration produ
41、ction sample that had been assigned aconcentration value for hafnium.15. Keywords15.1 d-c plasma; hafnium; zirconiumASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly a
42、dvised 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 time by the responsible technical committee and must be reviewed every five years andif not revised, eith
43、er 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 will receive careful consideration at a meeting of theresponsible technical committee, which you may attend.
44、 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 ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Indi
45、vidual 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); or through the ASTM website(www.astm.org).TABLE 1 Statistical InformationTest Sample Certified ppm Hf Assig
46、ned 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 87.8TABLE 2 Preparation of Synthetic Reference SolutionsConcentrationAConcentration ofSpiking
47、 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 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.E1552083
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