ASTM E1917-2002 Standard Test Method for Determination of Phosphorous in Nickel Ferronickel and Nickel Alloys by the Phosphovanadomolybdate Molecular Absorption Spectrometric Metho.pdf
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1、Designation: E 1917 02Standard Test Method forDetermination of Phosphorus in Nickel, Ferronickel, andNickel Alloys by the Phosphovanadomolybdate MolecularAbsorption Spectrometric Method1This standard is issued under the fixed designation E 1917; the number immediately following the designation indic
2、ates the year oforiginal adoption 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
3、of phospho-rus in nickel, ferronickel, and nickel alloys in the 0.0007 %through 0.05 % range.1.2 Arsenic, chromium, hafnium, niobium, silicon, tanta-lum, titanium, and tungsten interfere, but the interference canbe avoided by complexation or volatilization (for Cr). Thelowest phosphorus content (0.0
4、007 %) can be reached only insamples with low contents of interfering elements.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and dete
5、rmine the applica-bility of regulatory limitations prior to use. For specific hazardsassociated with the use of this practice see Practices E50.Refer to specific warning notes given throughout this testmethod.2. Referenced Documents2.1 ASTM Standards:2E50 Practices for Apparatus, Reagents, and Safet
6、y Precau-tions for Chemical Analysis of MetalsE 882 Guide for Accountability and Quality Control in theChemical Analysis LaboratoryE 1452 Practice for Preparation of Calibration Solutions forSpectrophotometric and for Spectroscopic Atomic Analy-sisE 1601 Practice for Conducting Interlaboratory Study
7、 toEvaluate the Performance of an Analytical Method2.2 ISO Standards:ISO 5725:1986 Precision of Test MethodsDeterminationof Repeatability and Reproducibility for a Standard TestMethod by Inter-laboratory Tests3ISO 11400:1992(E) Nickel, Ferronickel and NickelAlloysDetermination of Phosphorus ContentP
8、hosphovanadomolybdate Molecular Absorption Spectro-metric Method33. Summary of Test Method3.1 The sample is dissolved in a mixture of hydrochloricacid and nitric acid. The solution is evaporated to perchloricacid fumes and chromium is removed as volatile chromylchloride. Silicon and refractory eleme
9、nts are complexed withfluoride ions. The phosphorus is converted to phosphovanado-molybdic acid in a perchloric and nitric acid solution. Thephosphovanadomolybdic acid is extracted with 2-methyl-2-pentanone in the presence of citric acid to complex arsenic.Absorbance is measured at 355 nm.4. Signifi
10、cance and Use4.1 This test method is used for the analysis of nickel,ferronickel, and nickel base alloy samples by molecular ab-sorption spectrometry to check compliance with compositionalspecifications. It is assumed that all who use the procedure willbe trained analysts capable of performing commo
11、n laboratoryprocedures skillfully and safely. It is expected that the workwill be performed in a properly equipped laboratory and thatproper waste disposal procedures will be followed.Appropriatequality control practices must be followed, such as thosedescribed in Guide E 882.5. Apparatus5.1 Spectro
12、photometerCapable of measuring absorbanceat a wavelength of 355 nm.5.2 CellsTo fit spectrophotometer, having an optical pathof 1 cm.NOTE 1Cells having other dimensions can be used, provided suitableadjustments can be made in the amount of sample and reagents used.1This practice is under the jurisdic
13、tion of ASTM Committee E01 on AnalyticalChemistry of Metals, Ores and Related Materials and is the direct responsibility ofSubcommittee E01.08 on Nickel, Cobalt and High Temperature Alloys.Current edition approved Sept 10, 2002. Published June 2003. Originallyapproved in 1997. Last previous edition
14、approved in 1997 as E 1917-97.2For 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.3Available from American Nation
15、al Standards Institute, 11 West 42nd Street,New York, NY 10036.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.3 Plastic separatory funnels, 250 mL capacity.6. Reagents6.1 Purity and Concentration of ReagentsThe purity andconcentra
16、tion of common chemical reagents shall conform toPractices E50. The reagents should be free of or contain onlyminimal amounts (0.1 g/g) of phosphorus. Calibration solu-tions shall be prepared in accordance with Practice E 1452.6.1.1 Verify the absence of phosphorus in the reagents usingthe blank tes
17、t (9.6.1). Reagents giving high blank values areunsuitable and should not be used. The blank value for allreagents should be below 0.0005 % P calculated fora1gsample.6.2 Ammonium Metavanadate SolutionDissolve 2.5 g ofammonium metavanadate (NH4VO3) in water and dilute to 1 L.6.3 Citric Acid SolutionD
18、issolve 500 g citric acid mono-hydrate (C6H8O7H2O) in water and dilute to 1 L. Warm thesolution if necessary to facilitate dissolution.6.4 Fluoroboric Acid SolutionDisperse 75 g of boric acid(H3BO3) in 600 mLof hot water in a plastic beaker.Add 50 mLHF (40 %) and dilute to 1 L. Digest over medium he
19、at until theboric acid is dissolved. Store in plastic bottle. The solutionshould be gently heated if the boric acid forms crystals.NOTE 2Warning: HF and fluoroboric acid are extremely irritatingand corrosive to skin and mucous membranes, producing severe skinburns that are slow to heal. In case of c
20、ontact with skin, wash well withwater and seek medical advice. When using HF and fluoroboric acid,always wear appropriate safety gear, such as goggles and gloves.6.5 Hexaammonium Heptamolybdate SolutionDissolve15 g of hexaammonium heptamolybdate tetrahydrate(NH4)6Mo7O244H2O in warm water and dilute
21、to 100 mL.Prepare fresh solution each day. If high and unstable blankvalues appear, there might be a problem with the salt used. Insuch a case, switch to another lot.6.6 4-methyl-2-pentanonemethylisobutyl ketone.6.7 Phosphorus Stock Calibration Solution (1.000 g/L)Transfer 4.3942 g of potassium dihy
22、drogenorthophosphate(KH2PO4) (which has been previously dried at 110C toconstant weight and cooled in a desiccator) toa1Lvolumetricflask. Dissolve in water, dilute to the mark and mix.6.8 Phosphorus Calibration Solution (10 mg/L)Transfer10.0 mL of the phosphorus stock calibration solution toa1Lvolum
23、etric flask. Dilute to the mark with water and mix.6.9 Sodium Nitrite Solution (50 g/L)Dissolve 50 g ofsodium nitrite (NaNO2) in water and dilute to 1 L.7. Interlaboratory Studies (ILS)7.1 This test method was evaluated by a subcommitteewithin ISO Technical Committee 155 (ISO/TC 155/SC 4) onanalysis
24、 of nickel alloys, in accordance with ISO Standard5725. It was published as ISO Standard 11400. ILS test datawere not available for recalculation.8. Sampling and Sample Preparation8.1 The sampling shall be carried out by normal proceduresagreed upon between the parties, or in the event of a dispute,
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