1、Designation: E1409 08E1409 13Standard Test Method forDetermination of Oxygen and Nitrogen in Titanium andTitanium Alloys by the Inert Gas Fusion Technique1This standard is issued under the fixed designation E1409; the number immediately following the designation indicates the year oforiginal adoptio
2、n 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 oxygen in titanium and titaniu
3、m alloys in concentrations mass fractions from0.01 % to 0.5 % and the determination of nitrogen in titanium and titanium alloys in concentrations mass fractions from 0.003 %to 0.11 %.1.2 The values stated in both inch-pound and SI units are to be regarded separately as the standard. The values given
4、 inparentheses are for information only.1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatoryli
5、mitations prior to use. Specific warning statements are given in 8.8.2. Referenced Documents2.1 ASTM Standards:2E50 Practices forApparatus, Reagents, and Safety Considerations for ChemicalAnalysis of Metals, Ores, and Related MaterialsE135 Terminology Relating to Analytical Chemistry for Metals, Ore
6、s, and Related MaterialsE173 Practice for Conducting Interlaboratory Studies of Methods for Chemical Analysis of Metals (Withdrawn 1998)3E882 Guide for Accountability and Quality Control in the Chemical Analysis LaboratoryE1019 Test Methods for Determination of Carbon, Sulfur, Nitrogen, and Oxygen i
7、n Steel, Iron, Nickel, and Cobalt Alloys byVarious Combustion and Fusion TechniquesE1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical MethodE1914 Practice for Use of Terms Relating to the Development and Evaluation of Methods for Chemical Analysis3. T
8、erminology3.1 DefinitionsFor definitions of terms used in this method, refer to Terminology E135 and Practice E1914.4. Summary of Test Method4.1 This test method is intended for use with automated, commercially available, inert gas fusion analyzers. These analyzerstypically measure both oxygen and n
9、itrogen simultaneously or sequentially utilizing parallel measurement systems.4.2 The test sample, plus flux, is fused in a graphite crucible under a flowing inert gas stream (argon, helium) at a temperaturesufficient to release oxygen and nitrogen. Oxygen combines with carbon to form carbon monoxid
10、e (CO) and nitrogen is releasedas N2. Depending on instrument design, the CO is may be oxidized to carbon dioxide (CO2) or left). The CO or CO2 as CO and,or both, are swept by the inert gas stream into either an infrared or thermal conductivity detector. The detector output responsegenerated by anal
11、ysis of the test sample is compared to that the response generated by analysis of reference materials and the resultis displayed as percent oxygen. The nitrogen is swept by the inert gas stream (helium gas) into a thermal conductivity detector.The detector response generated by analysis of the test
12、sample is compared to that the response generated by analysis of referencematerials and the result is displayed as percent nitrogen.1 E01 on 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, Re.Current e
13、dition approved June 15, 2008Oct. 1, 2013. Published July 2008November 2013. Originally approved in 1991. Last previous edition approved in 20052008 asE1409 05.E1409 08. DOI: 10.1520/E1409-08.10.1520/E1409-13.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Custome
14、r Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last approved version of this historical standard is referenced on www.astm.org.This document is not an ASTM standard and is intended only to prov
15、ide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the
16、standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14.3 In a typical instrument for the determination of nitrogen, the sample gases are swept with inert gas through h
17、eated rareearth/copper oxide that converts CO to CO2 and hydrogen (H2) to water (H2O). The CO2 is absorbed on sodium hydroxideimpregnated on clay, and the H2O is removed with magnesium perchlorate. The nitrogen, as N2, enters the measuring cell and thethermistor bridge output is integrated and proce
18、ssed to display percent oxygen.nitrogen.5. Significance and Use5.1 This test method is primarily intended as a test for compliance with compositional specifications. It is assumed that all whouse this test method will be trained analysts capable of performing common laboratory procedures skillfully
19、and safely. It isexpected that the work will be performed in a properly equipped laboratory.6. Interferences6.1 The elements usually present in titanium and its alloys do not interfere but there is some evidence to suggest that low purityflux can cause some adsorption of the released oxygen.7. Appar
20、atus7.1 InstrumentFusion and measurement apparatus, automatic oxygen and nitrogen determinator consisting of an electrodefurnace, provision for scrubbing impurities from analytical gas stream; infrared or thermal conductivity measurement system(s),or both, and auxiliary gas purification systems (Not
21、e 1).NOTE 1The apparatus and analysis systems have been previously described in Test Method E1019. Several models of commercial oxygen andnitrogen determinators are available and presently in use by industry. Each has its own unique design characteristics and operational requirements. Consultthe ins
22、trument manufacturers instruction manual for operational details.7.2 Graphite CruciblesThe crucibles must be made of high-purity graphite and be of the dimensions recommended by theinstrument manufacturer.7.3 FluxWire baskets Flux must be made of high-purity nickel and nickel. If nickel baskets are
23、used, the dimensions mustmeet the requirements of the automatic sample drop, if present, on the instrument. (See Note 2.) Ultra high-purity nickel flux iscommercially available and may eliminate the need to clean the flux before using it.NOTE 2In some instruments, nitrogen and oxygen are run sequent
24、ially and platinum is the required flux for nitrogen. High-purity platinum can besubstituted for nickel in the same ratio of flux to sample.7.4 TweezersTweezers or Crucible Tongs, Six-inch tweezers made of solvent and acid-resistant plastic.acid resistant material.8. Reagents8.1 AcetoneResidue after
25、 evaporation must be 0.0005 %.Low residue reagent grade or higher purity.8.2 Graphite PowderPowder (optional)High-purity as specified by the instrument manufacturer.8.3 Inert GasUse the purity and type specified by the instrument manufacturer.8.4 Magnesium Perchlorate, Anhydrous4Used in the instrume
26、nt to absorb water. Use the purity specified by the instrumentmanufacturer.8.5 Nickel Flux Cleaning SolutionPrepare a fresh solution An acid solution capable of removing surface contamination fromthe nickel flux.Asolution made by combining 75 mL of acetic acid, 25 mL of nitric acid (HNOHNO3), and 2
27、mL of hydrochloricacid (HCl).HCl has been found suitable for this purpose.8.6 Copper Oxide or Rare Earth/Copper OxideReagent used in some instruments to oxidize CO to CO2 for thermalconductivity detection. Use the purity specified by the instrument manufacturer.8.7 Sodium Hydroxide on Clay5Reagent u
28、sed in some instruments to absorb CO2. Use a purity specified by the instrumentmanufacturer.8.8 Titanium Sample Pickle SolutionPrepare a fresh solution of 3 Three parts 30 % hydrogen peroxide (H2O2) and 1 part 48 %hydrofluoric acid (HF). HNOHF. Other pickle solutions3 may be substituted if there are
29、 data supporting the effectiveness of thesolution on removing contaminants. For example, substituting concentrated HNO3 for 30 % H2O2 has been found effective (seeNote 3). (WarningHF causes serious burns that may not be immediately painful; refer to the paragraph about HF in the SafetyPrecautions Ha
30、zards Section of Practices E50.)NOTE 3In 2004, alternative sample preparation procedures (Section 12) were tested by seven laboratories. Three laboratories processed the samplematerials by pickingpickling their samples in HF-H2O2 (8.8). Two laboratories utilized the HF-HNO3 alternative pickle soluti
31、on (8.8). Two laboratoriesutilized abrasion (in this case diamond saw and shear) in accordance with 12.412.2. The prepared samples were distributed among the laboratories for4 Known commercially as Anhydrone.5 Known commercially as Ascarite II.E1409 132analysis. Six laboratories analyzed these sampl
32、es in random order under a single operator, single-day, single calibration sample run. The results of thistesting are given in Tables X1.1 and X2.1 for oxygen and nitrogen, respectively. In both cases, the analysis of the ANOVAvariance (ANOVA) indicatesthat there is no significant difference at the
33、95 % level of confidence for either oxygen or nitrogen due to the preparation technique.9. Hazards9.1 Use care when handling hot crucibles and operating furnaces to avoid personal injury by either burn or electrical shock.9.2 For precautions to be observed in the use of HF and other reagents in this
34、 test method, refer to Practices E50.10. Preparation of Apparatus10.1 Assemble the apparatus as recommended by the manufacturer. Make the required power, gas, and water connections. Turnon the instrument and allow sufficient time to stabilize the equipment.10.2 Change the chemical trapsreagents and
35、filters as required. Test the furnace and analyzer to ensure the absence of leaks.Makeleaks (Note 4 a). A minimum of two test runs using a sample as directed in 14.3 and 14.4 is recommended to condition thenewly changed filters filters. This should be done before attempting to calibrate the system o
36、r to determine the value of the blank.NOTE 4Typical leak checks should be 0.0 mm Hg to 1.5 mm Hg. The maximum allowable leak check should follow the manufacturersrecommendation.11. Nickel Flux Preparation11.1 Nickel is necessary to flux the titanium fusion reaction but contamination can be present o
37、n the surface of the nickel wirebaskets that must be removed before use.Ultra high-purity nickel is commercially available that does not require the nickel cleaningprocedure below. Its sufficiency must be verified by satisfactory blank determinations. If ultra high-purity nickel is not used, thenick
38、el must be cleaned to remove contamination (11.2).11.2 Immerse the flux in freshly prepared nickel flux cleaning solution for 50 s to 60 s, then rinse in running water for 2 minto 3 min. Pour flux onto paper towels to remove excess water. Place flux in sealable glass container, rinse with acetone an
39、d decant.Replace with fresh acetone and store flux under To prevent new oxidation from forming, the flux may be stored under fresh acetoneuntil used. (See Notes 4 and 5Note 5.)NOTE 4Nickel is necessary to flux the titanium fusion reaction but significant oxidation can be present on the surface of ni
40、ckel wire baskets that cancause interference with the analysis. Ultra high-purity nickel baskets are commercially available that do not require the nickel cleaning procedure above.Their sufficiency must be verified by satisfactory blank determinations.NOTE 5The fluxing agent must be of proper size t
41、o be introduced through the sample drop mechanism and into the graphite crucible.12. Sample Preparation12.1 The optimum test sample is Remove the surface of the sample either mechanically (12.2) or chemically (12.3a pinapproximately). Start with a sample of 18 in. (5 mm) in diameter and nominally we
42、ighing 0.12 g to 0.15 g. Cut the sample to thisapproximate weight range.sufficient size that the final sample after surface removal will be between 0.100 g and 0.150 g.12.2 To mechanically remove the sample surface, abrade with a clean file or similar abrasive device to remove contamination.Other me
43、thods, such as shearing, saw cutting, or turning down on a lathe, may be employed for reducing sample size and removingthe surface of the sample. Regardless of the method used, the sample must not be allowed to overheat, as this will adversely affectthe results of the analysis. Indications that the
44、sample has overheated while being worked may include discoloration of the metalor the sample becoming too hot to handle without tools. Rinse the sample in acetone and air dry. Weight to 60.001 g. Proceedto 12.4.12.3 Leach the test sample in the titanium sample pickle solution (To chemically remove W
45、arningSee 8.8.) (see Note 4) untilthe surface is clean.surface contamination, follow 12.3.1 and 12.3.2This will normally require approximately 5 s from the time ofthe initial vigorous reaction between the sample and the solution12.3.1 Leach the test sample in the titanium sample pickle solution. (Wa
46、rningSee 8.8.) (see Note 3) until the surface is clean.This will normally require approximately 5 s from the time of the initial vigorous reaction between the sample and the solution.12.3.2 Immediately remove the reacting test sample and rinse it twice with water and once with acetone and allow to a
47、ir dry.Weigh to 60.001 g.12.3 Immediately remove the reacting test sample with tweezers and rinse it twice with water and once with acetone and allowto air dry. This test sample should now weigh between 0.100 g and 0.140 g.12.4 Alternatively, clean surfaces may be prepared on the test sample by fili
48、ng or cutting off all outside edges, retaining onlyfresh surfaces, and finishing by rinsing with acetone and air drying. The test sample should now weigh between 0.100 g and 0.140g.12.4 All subsequent operations on the test sample and flux must be done without introducing contamination to either. Us
49、e onlyclean tweezers or crucible tongs and never let the test sample or flux contact the analystsanalysts skin. In the event this doeshappen, rinse the sample plusand nickel basket with acetone and air dry before analysis.E1409 13313. StandardizationCalibration13.1 StandardantsReference MaterialsSelect only titanium or titanium alloy reference materials. Select one containingapproximately 0.2 % oxygen and approximately 0.02 % nitrogen. materials such that the high point on the calibration curves willrepresent an amount of oxygen and nitrogen that
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