Designation:E1447−09(Reapproved2016)
Standard Test Method for
Determination of Hydrogen in Titanium and Titanium Alloys by Inert Gas Fusion Thermal Conductivity/Infrared Detection Method1
This standard is issued under thefixed designation E1447;the number immediately following the designation indicates the year of original adoption or,in the ca of revision,the year of last revision.A number in parenthes indicates the year of last reapproval.A superscript epsilon(´)indicates an editorial change since the last revision or reapproval.
1.Scope
1.1This test method applies to the determination of hydro-gen in titanium and titanium alloys in concentrations from
0.0006%to0.0260%.
1.2The values stated in SI units are to be regarded as standard.No other units of measurement are included in this standard.
1.3This standard does not purport to address all of the safety concerns,if any,associated with its u.It is the responsibility of the ur of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to u.For specific hazards,e Section9.
相遇那一刻
2.Referenced Documents
2.1ASTM Standards:2
C696Test Methods for Chemical,Mass Spectrometric,and Spectrochemical Analysis of Nuclear-Grade Uranium Di-oxide Powders and Pellets
E50Practices for Apparatus,Reagents,and Safety Consid-erations for Chemical Analysis of Metals,Ores,and Related Materials
E135Terminology Relating to Analytical Chemistry for Metals,Ores,and Related Materials
E1601Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method
E1914Practice for U of Terms Relating to the Develop-ment and Evaluation of Methods for Chemical Analysis (Withdrawn2016)33.Terminology
3.1Definitions—For definitions of terms ud in this test method,e Terminology E135and E191
4.
4.Summary of Test Method
散文小说4.1The specimen,contained in a small,single-u graphite crucible,is fud under aflowing carrier gas atmosphere. Hydrogen prent in the sample is relead as molecular hydrogen into theflowing gas stream.The hydrogen is pa-rated from other liberated gas such as carbon monoxide and finally measured in a thermal conductivity cell.
4.2Alternatively,hydrogen is converted to water by passing the gas stream over heated copper oxide and subquently measuring in an appropriate infrared(IR)cell.
4.3This test method is written for u with commercial analyzers equipped to perform the above operations automati-cally and is calibrated using reference materials of known hydrogen content.
5.Significance and U
5.1This test method is intended to test for compliance with compositional specifications.It is assumed that all who u this test method will be trained analysts capable of performing common laboratory procedures skillfully and safely.It is expected that the work will be performed in a properly equipped laboratory.
6.Interferences
6.1The elements ordinarily prent in titanium and its alloys do not interfere.
7.Apparatus
手机相册里的照片误删怎么恢复
7.1Fusion and Measurement Apparatus—Automatic hydro-gen determinator,consisting of an electro
de furnace or induc-tion furnace;analytical gas stream impurity removal systems; auxiliary purification systems and either a thermal conductivity cell hydrogen measurement system or an infrared hydrogen measurement system(Note1).
N OTE1—The apparatus and analysis system have been previously described in the Apparatus and Apparatus and Equipment ctions of Test
1This test method is under the jurisdiction of ASTM Committee E01on
Analytical Chemistry for Metals,Ores,and Related Materials and is the direct
responsibility of Subcommittee E01.06on Ti,Zr,W,Mo,Ta,Nb,Hf,Re.
Current edition approved Aug.1,2016.Published August2016.Originally
六下语文书人教版approved in1992.Last previous edition approved in2009as E1447–09.DOI:
10.1520/E1447-09R16.
2For referenced ASTM standards,visit the ASTM website,www.astm,or
contact ASTM Customer Service at rvice@astm.For Annual Book of ASTM
Standards volume information,refer to the standard’s Document Summary page on
the ASTM website.
3The last approved version of this historical standard is referenced on
www.astm.
Copyright©ASTM International,100Barr Harbor Drive,PO Box C700,West Conshohocken,PA19428-2959.United States
Methods C696.Several models of commercial analyzers are available and prently in u in industry.Each has its own unique design characteristics and operational requirements.Consult the instrument manufacturer’s instructions for operational details.
7.2Graphite Crucibles—The crucibles are machined from high-purity graphite.U the size crucibles recommended by the manufacturer of the instrument.
7.3Crucible Tongs—Capable of handling recommended crucibles.
7.4Tweezers or Forceps—For contamination-free sample handling.
8.Reagents and Materials
8.1Acetone,low-residue reagent grade or higher purity. 8.2Sodium Hydroxide on Clay Ba,commonly known as Ascarite II.
8.3High-Purity Carrier Gas(99.99%)—Argon,nitrogen, or helium(Note2).
N OTE2—Carrier gas vary by instrument model and include high-purity argon,nitrogen,and helium.Consult instrument manufacturer’s instructions for proper gas recommendation.
8.4High-Purity Tin Metal(Low Hydrogen)—U the purity specified by the instrument manufacturer.
8.5Magnesium Perchlorate,Anhydrone.
8.6Molecular Sieve—Characteristics specified by the in-strument manufacturer.
8.7Schutze Reagent—Iodine pentoxide over silica gel. 8.8Copper Oxide Wire—To convert hydrogen to water in IR-detection instruments.Characteristics specified by the in-strument manufacturer.
9.Hazards
9.1For hazards to be obrved in the u of this test method, refer to Practices E50.手电筒的英文
9.2U care when handling hot crucibles and operating electrical equipment to avoid personal injury by either burn or electrical shock.
10.Preparation of Apparatus
10.1Asmble the apparatus as recommended by the manu-facturer.
10.2Test the furnace and analyzer to ensure the abnce of gas leaks and make the required electrical power and water connections.Prepare the apparatus for operation in accordance with the manufacturer’s instructions.Make a minimum of two determinations using a specimen as directed in13.2before attempting to calibrate the system or to determine the blank.
11.Sample Preparation
11.1U solid form specimens prepared as directed in11.2. Specimens must be of an appropriate size tofit into the graphite crucible and should not exceed0.30g in weight.
11.2Cut the specimen to the approximate size of0.15g to 0.30g(preferably by shearing).For specimens of unknown history or suspected surface contamination,abrade specimen surfaces with a cleanfile to remove contamination.Other methods,such as turning down on a lathe,may be employed for reducing sample size and removing the surface of the sample(Note3).Rin the sample in acetone,and air dry. Weigh to60.001g.Samples shall be handled only with tweezers or forceps after cleaning and weighing to prevent contamination.
N OTE3—Regardless of the method ud,the sample must not be allowed to overheat,as this will adverly affect the results of the analysis. Indications that the sample has overheated while being worked may include discoloration of the metal or the sample becoming too hot to handle without tools.微信视频怎么保存
12.Calibration
12.1Calibration Reference Materials—Select only titanium or titanium alloy reference materials(Note4).
N OTE4—Gas dosing:it is satisfactory to calibrate the unit by dosing known volume(s)of hydrogen gas into the detection system.If the instrument has this feature,refer to the manufacturer’s recommen
ded procedure.In this ca instrument respon must always be verified by analyzing titanium or titanium alloy reference materials.
12.2Determination of Crucible/Tin Blank Reading:
12.2.1If the instrument is equipped with an electronic blank compensator,adjust to zero,and proceed with the determina-tion of the blank value.
12.2.2Make at least three blank determinations as directed in13.2using the weight of tinflux as recommended by the instrument manufacturer(Note5).U a fresh crucible each time.
N OTE5—Flux weight is dependent upon the model of the instrument and the manufacturer’s instruction.Refer to the manufacturer’s instruc-tions and recommendations.
12.2.3If the average blank value exceeds0.0000%6 0.0001%,or a standard deviation for the three concutive values exceeds60.0001%,then determine the cau,make necessary corrections,and repeat12.2.1and12.2.2(Note6).
N OTE6—Refer to the instrument manufacturer’s instructions concern-ing the troubleshooting and correction of blank determinations not meeting the above criterion.
12.2.4Enter the average blank value in the appropriate mechanism of the analyzer(Note7)according to the manu-facturer’s instruction.This mechanism will electronically com-pensate for the blank value.
N OTE7—If the unit does not have this function,the average blank must be subtracted from the total result.
12.3Calibration Procedure:
12.3.1Prepare at least four0.15g to0.30g specimens(at least one specimen if calibrating by gas dosing)of a titanium hydrogen reference material as directed in11.2.This titanium hydrogen reference material should have a hydrogen content greater than or approximately equal to the unknown samples within the scope of this test method(0.0006%to0.0260%).
12.3.2Follow the calibration procedure recommended by the manufacturer.Analyze at least three reference material specimens to determine the calibration slope(Note8).Treat each specimen as directed in13.2before proceeding to the next one(Note9
).
N OTE 8—For calibration by gas dosing,perform at least three gas do analys to determine the calibration slope.Refer to instrument manufac-turer’s instructions.
N OTE 9—Some instruments have expanded computer capabilities that allow multi-point calibration which may improve the accuracy and precision of the calibration over the single-point calibration methodology as tested in the current interlaboratory study (ILS).
12.3.3Confirm the calibration by analyzing a specimen of titanium hydrogen reference material (Note 10).The ILS ud an acceptance criterion where the value fell within the allow-able limits of the certified value.An alternate procedure can be implemented where this value should agree with the certified value within the limits of a prediction interval calculated using Eq 1.The prediction interval is defined as the range of values bounded by the analysis value -p and the analysis value +p .If the prediction interval does not encompass the certified value,determine and correct the cau,and repeat 12.3.1and 12.3.2(Note 11).Either acceptance limit criterion is acceptable for routine operation.
N OTE 10—Confirmation of the calibration does not ensure accuracy.The accuracy of this test method is largely dependent upon the abnce of bias in the hydrogen values assigned to the reference materials and upon the homogeneity of the materials.
N OTE 11—See the instrument manufacturer’s instructions concerning the troubleshooting and correcting of errant calibration.
p 5t ·S
11
1
=n
D
·s (1)
where:
p =one-half the prediction interval,n =number of replicates ud in 12.3.2,
t =student’s t chon for the 95%confidence level for n
replicate measurements (for example:t =2.35when n =3,2.13when n =4,2.02,when n =5),and
s =standard deviation of n replicates in 12.3.2(Note 12).
N OTE 12—Here,s should be comparable to S m ,the repeatability standard deviation,given in Table 1.If s »S m ,there is evidence that the repeatability of the particular instrument is not acceptable for u with this test method.The ur should determine and correct the cau,and repeat 12.3.1through 12.3.3.
12.3.4Confirm calibration linearity by analyzing a mid-range (Note 13)titanium hydrogen reference material,using the limits stated on the certified value as an acceptance range.Alternatively,analyze at least three specimens of a mid-range
(Note 13)titanium hydrogen reference material.Calculate the average and standard deviation(s)of the results.In the abnce of bias among the reference materials,the average result for this reference material should agree with the certified value within a prediction interval defined by the rep
eatability of the measurement system at the mid-range of the calibration (Note 14).This prediction interval may be calculated using Eq 1and the s and n values for the mid-range reference material.If the prediction interval does not encompass the certified value,determine and correct the cau and repeat 12.3.1and 12.3.4(Note 15).
N OTE 13—Commercially available reference materials are not always available at the concentration required to have a true mid-point check.The mid-range material must have a hydrogen concentration that is above the limit of detection,but below that of the high calibration point,preferably as clo to the mid-point of the calibration curve as possible.
N OTE 14—Typically,repeatability standard deviation is a function of the concentration of the analyte.Compare the values labeled ILS Analyzed Mean in Table 1with the values for Minimum SD (S m )to e a typical trend for laboratories using this test method.If your results are not comparable,investigate and correct the cau.
N OTE 15—The prence of bias between the reference material ud in 12.3.2and the reference material ud in 12.3.4may cau the calibration to appear to be non-linear.This cannot be corrected by making adjust-ments to the instrument.
12.3.5One or more continuing calibration verifications must be performed prior to and upon completion of a period of continuous operation,and throughout this period with a pre-determined minimum frequency to be established by each individual test facility.The acceptance range for the verifica-tion material may be the limits stated on the certified value for the reference material,or may be calculated using Eq 1and the s and n values for multiple analys of the verification material.If a continuing calibration verification indicates an out of calibration condition,stop analysis.Results must be supported by acceptable preceding and subquent verifications to be reported.
12.4Calibration Frequency:
12.4.1It is the responsibility of the ur to document the frequency of blank determination (12.2.1–12.2.4),routine calibration and confirmation (12.3.2and 12.3.3)and linearity confirmation (12.3.4),and the conditions under which blank determination or recalibration,or both,beyond this frequency
1348年
TABLE 1Hydrogen in Titanium Metal Statistical Information A
Material
#Labs Certified Value (µg/g)ILS Analyzed Mean (µg/g)Difference (µg/g)Certified Precision (µg/g)Minimum SD (S m ,Practice E1601)Reproducability SD (S R ,Prac-tice
E1601)Reproducability
商业景观Index (R,Practice E1601)R rel %BCR 318B 1012.211.40.80.80.44 1.01 2.8324.9CEZUS LH 1.64 2.637.3636.3NBS 352D
113227.4 4.62 1.43 1.96 5.4720.0CEZUS 1.44 5.3114.9016.5NBS 353D 119895.8 2.25 3.42 4.0011.1911.7NBS 354D 11215213.2 1.86 3.36 3.6610.24 4.80NIST 5.8011.3531.7814.5CEZUS HH C
10
...
260.1
...
...
4.45
11.7232.8012.6
A ILS conducted in accordance with Practice E1601,Plan A.
B
Certified Reference Material:Commission of the European Communities,Community Bureau of Reference.C
Reference Material:CEZUS,Ugine,France.D
Standard Reference Material:National Institute of Standards and Technology,formerly National Bureau of Standards.E
Standard Reference Material (under development):
National Institute of Standards and Technology.Material is in chip form.
is required (examples may include changing reagents,chang-ing gas cylinders or a personnel shift change).13.Procedure
13.1Asmble the apparatus and condition it as directed in Section 10.
13.2Procedure for Operation:
13.2.1Set the analyzer to operate mode.
13.2.2Prepare a 0.15-g to 0.30-g specimen as directed in 11.2.
13.2.3Place a 0.15-g to 0.30-g specimen in the loading device.If the instrument does not have this feature,refer to the manufacturer’s recommended procedure regarding entry of sample.
13.2.4Enter the sample weight as recommended by the manufacturer.
13.2.5Place a crucible containing high-purity tin as mea-sured in 12.2.2on the furnace electrode/pedestal asmbly and clo the furnace.
13.2.6Start the analysis cycle according to the manufactur-er’s recommended procedure.14.Calculation
14.1The reading will be direct if the blank and weight have been entered correctly into the appropriate portion of the analyzer (Note 16).
N OTE 16—If the analyzer does not offer the functions,calculate the hydrogen content by the following method:Dial the sample weight or a multiple of the sample weight on the weight compensator and u the
following formula (Eq 2)for the calculation of the result:
Hydrogen,%5
~A 2B !3C
D
(2)
where:A =sample digital volt meter (DVM)reading,B =blank DVM reading,
C =weight compensator tting,and
D =
sample weight,g.
15.Precision and Bias
15.1Precision 4—Eleven laboratories cooperated in testing eight samples in triplicate.The data are prented in Table 1.The testing and statistical analysis were performed in accor-dance with the provisions of Practice E1601,Plan A.Six instruments were of the thermal conductivity hydrogen mea-surement system configuration and five instruments were of the infrared hydrogen measurement system configuration.Calibra-tion was performed utilizing a single calibration material (NBS 354,215µg ⁄g 66µg ⁄g).
15.2Bias—Information on the accuracy of this test method is incomplete at this time.The accuracy of this test method may be judged by comparing the results obtained from certified reference materials with their certified values for hydrogen.16.Keywords
16.1hydrogen;inert gas fusion;titanium;titanium alloys
ASTM International takes no position respecting the validity of any patent rights asrted in connection with any item mentioned in this standard.Urs of this standard are expressly advid that determination of the validity of any such patent rights,and the risk of 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 and if not revid,either reapproved or withdrawn.Your comments are invited either for revision of this standard or for additional standards and should be addresd to ASTM International Headquarters.Your comments will receive careful consideration at a meeting of the responsible technical committee,which you may attend.If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards,at the address shown below.
This standard is copyrighted by ASTM International,100Barr 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 above address or at 610-832-9585(phone),610-832-9555(fax),or rvice@astm (e-mail);or through the ASTM website (www.astm).Permission rights to photocopy the standard may also be cured from the Copyright Clearance Center,222Rowood Drive,Danvers,MA 01923,Tel:(978)/
4
Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Rearch Report
RR:E01-1004.
