1、Designation: E1070 11E1070 17Standard Test Method forDetermination of Phosphorus in Iron Ores by Phospho-Molybdenum-Blue Spectrophotometry1This standard is issued under the fixed designation E1070; the number immediately following the designation indicates the year oforiginal adoption or, in the cas
2、e 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 phosphorus in iron ores, concentrates, and agg
3、lomerates in the concentrationrange from 0.005 % to 1.0 % phosphorus.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 This test method has been evaluated in accordance with Practice E1601 and Guide E1763. Unless otherwi
4、se noted in theprecision and bias section, the lower limit in the scope of each method specifies the lowest analyte content that may be analyzedwith acceptable error (defined as a nominal 5 % risk of obtaining a 50 % or larger relative difference in results on the same testsample in two laboratories
5、).1.4 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 regulatorylimitations prior to use.1.5 This intern
6、ational standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Commi
7、ttee.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data to Determine Conformance with SpecificationsE50 Practices forApparatus, Reagents, and Safety Considerations for ChemicalAnalysis of Metals, Ores, and Related Ma
8、terialsE60 Practice for Analysis of Metals, Ores, and Related Materials by SpectrophotometryE135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related MaterialsE877 Practice for Sampling and Sample Preparation of Iron Ores and Related Materials for Determination of ChemicalCompo
9、sition and Physical PropertiesE882 Guide for Accountability and Quality Control in the Chemical Analysis LaboratoryE1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical MethodE1763 Guide for Interpretation and Use of Results from Interlaboratory Testing
10、of Chemical Analysis Methods (Withdrawn2015)33. Terminology3.1 DefinitionsFor definitions of terms used in this test method, refer to Terminology E135.4. Summary of Test Method4.1 The sample is fused in a zirconium crucible with sodium peroxide. peroxide (Na2O2). The melt is dissolved in water andhy
11、drochloric acid. HCl. In a suitable aliquot, the molybdenum blue complex is formed by the addition of ammoniummolybdate-hydrazine sulfate solution. The absorbance of the phospho-molybdenum-blue complex is measured at 725 nm.1 This test method is under the jurisdiction of ASTM Committee E01 on Analyt
12、ical Chemistry for Metals, Ores, and Related Materials and is the direct responsibility ofSubcommittee E01.02 on Ores, Concentrates, and Related Metallurgical Materials.Current edition approved Sept. 1, 2011May 1, 2017. Published September 2011July 2017. Originally approved in 1985. Last previous ed
13、ition approved in 20052011 asE1070 00 (2005). 11. DOI: 10.1520/E1070-11.10.1520/E1070-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summa
14、ry 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 provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not
15、 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 standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Dr
16、ive, PO Box C700, West Conshohocken, PA 19428-2959. United States15. Significance and Use5.1 This test method for the analysis of iron ore concentrates and agglomerates is primarily intended as a referee method to testfor compliance with compositional specifications. It is assumed that users of this
17、 test method will be trained analysts capable ofperforming common laboratory procedures skillfully and safely. It is expected that work will be performed in a properly-equippedlaboratory and that proper waste disposal procedures will be followed.Appropriate quality control practices shall be followe
18、d, suchas those described in Guide E882.5.2 The determination of this element is needed for international trade and primary iron and steel making.6. Interferences6.1 Elements normally found in iron ores do not interfere excepting arsenic giving positive interference (0.01 % As = 0.001 %P).7. Apparat
19、us7.1 Zirconium Crucible, 50 mL capacity.7.2 SpectrophotometerVisible spectrophotometer capable of measuring absorbance at the 725 nm wavelength using a 1-cmpath length cell in accordance with Practice E60.8. Reagents and Materials8.1 Purity of ReagentsReagent grade chemicals shall be used in all te
20、sts. Unless otherwise indicated, it is intended that allreagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where suchspecifications are available.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficie
21、nt high purityto permit its use without lessening the accuracy of the determination.8.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water conforming toType I or II of Specification D1193. Type III or IV may be used if they effect no measurable c
22、hange in the blank or sample.8.3 Ammonium Molybdate Solution (20 g/L)To 500 mL of water, add cautiously and slowly 300 mL of H2SO4 and cool. Add20 g of ammonium molybdate (NH4)6-MoMo7O244H2O. Stir to dissolve and dilute to 1 L with water.8.4 Fusion BlankDissolve 4 g of Na2O2 in 40 mL of water in a 2
23、50-mL beaker. Add 30 mL of HCl. Boil for 2 min. Cool anddilute to 100 mL with water in a volumetric flask. Prepare fresh as needed.8.5 Hydrazine Sulfate (1.5 g/L)Dissolve 0.15 g of hydrazine sulfate NH2NH2H2SO4 in water and dilute to 100 mL withwater. Prepare fresh as needed.8.6 Molybdate (5 g/L) Hy
24、drazine Sulfate (0.15 g/L) SolutionAdd 50 mL of ammonium molybdate solution (20 g/L) to 100mL of water. Add 20 mL of hydrazine sulfate solution (1.5 g/L) and dilute to 200 mL with water.NOTE 1This solution should be prepared within 30 min of use in a quantity appropriate for the number of tests bein
25、g made.8.6.1 This solution should be prepared within 30 min of use in a quantity appropriate for the number of tests being made.8.7 Sodium Peroxide (Na2O2)Use caution when using peroxide.8.8 Sodium Sulfite Solution (100 g/L)Dissolve 10 g of sodium sulfite (Na2SO3) in water and dilute to 100 mL with
26、water.8.9 Standard Phosphorus SolutionDry anhydrous disodium phosphate (Na2HPO4) at 105 C for 2 h and after desiccation,dissolve 0.2292 g of the reagent in 200 mL of water. Dilute to 1 L with water in a volumetric flask and mix. This solution, A,provides 1 mL = 50 g P. Transfer 10.00 mL of solutionA
27、into a 50-mL volumetric flask, dilute to mark with water, and mix. Thissolution, B, provides the standard phosphorus solution for calibration 1 mL = 10 g P.9. Hazards9.1 For precautions to be observed in this method, refer to Practices E50.10. Sampling and Sample Preparation10.1 Collect and prepare
28、gross samples in accordance with Practice E877.10.2 Pulverize the laboratory sample to pass a No. 100 (150-m) sieve.NOTE 1To facilitate decomposition, some ores, such as specular hematite, require grinding to pass a No. 200 (75-m) sieve.4 Reagent Chemicals, American Chemical Society Specifications,
29、American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc
30、. (USPC), Rockville, MD.E1070 17211. Calibration and Standardization11.1 The recommended range of phosphorus content is from 0.005 mg to 0.10 mg phosphorus in 50 mL of color solution usingcell depth of 1 cm.11.2 Into a series of five 150-mL beakers, transfer 10.0 mL of fusion blank solution (8.4) an
31、d then transfer (0, 0.50, 2.50) mLof standard B; B phosphorus solution (8.9); 1.00 mL and 2.00 mL of standard A phosphorus solution (8.9) corresponding to (0,5, 25, 50, and 100) g of phosphorus respectively. To each beaker add 15 mL of sodium sulfite solution (8.8). Mix. Bring to a boil.Add 20 mL of
32、 molybdate-hydrazine sulfate solution (8.6). Bring to a boil. Simmer for 10 min in boiling water bath. Cool. Transferinto a 50-mL volumetric flask and dilute to the mark with water. Mix. This solution is stable for at least 2 h.11.3 PhotometrySpectrophotometryAdjust the spectrophotometer to the init
33、ial setting, using water as the reference solution.While maintaining this setting, measure absorbance of the calibration standard and sample solutions at approximately 725 nm ina 1-cm cell.11.4 Preparation of Calibration CurveSubtract the absorbance of the 0-mLphosphorus standard solution from the a
34、bsorbanceof each standardcalibration solution and plot the net absorbance against g g of phosphorus in the color solution.12. Procedure12.1 Weigh approximately the amount of the prepared sample specified in the following table into a small weighing bottlepreviously dried at 150 C:TABLE 1 Statistical
35、 InformationSample Average Phosphorus Content,% Standard DeviationRelativeStandardDeviation, %Number ofParticipatingLaboratoriesNumber ofReplicatesJapan 830-1 (0.125)A 0.1270 0.0035 2.75 8 24NBS 690 (0.011)A 0.0085 0.0010 11.76 8 24NBS 692 (0.039)A 0.0393 0.0022 5.61 8 24NBS 693 (0.056)A 0.0554 0.00
36、20 3.61 8 24A Certificate ValuePhosphorus content, %.E1070 173P Content, %Mass ofSample, gSampleAliquot, mLFusionBlank, mL0.005 to 0.15 0.300 10.0 None0.15 to 0.50 0.100 10.0 None0.50 to 1.0 0.100 5.0 5.0Dry the contents for 1 h at 105 C to 110 C. Cap the bottle and cool to room temperature in a des
37、iccator. Momentarily releasethe cap to equalize the pressure and weigh the capped bottle and test sample to the nearest 0.1 mg. Repeat the drying and weighinguntil there is no further loss of mass. Transfer the test sample into a zirconium crucible and reweigh the capped bottle to the nearest0.1 mg.
38、 The difference between the two masses is the weightmass of test sample taken for analysis. Add 2 g of sodiumNa2O2peroxide to the crucible and mix with a dry, stainless steel spatula.NOTE 2As used in this test method (except as related to the term relative standard deviation), “percent or “%” refers
39、 to mass fraction (wt/wt) of theform g/100 g.12.2 Fuse over a burner, swirling the crucible until the melt is cherry red and clear. Remove from the heat and swirl until themelt solidifies on the wall of the crucible.12.3 Place the crucible in a 250-mLdry beaker and cool. Cover with a watch glass and
40、 add about 10 mLof water to the crucible.After the reaction ceases, transfer the crucible contents into the beaker, and wash the crucible with water. Add 15 mL of HCl tothe crucible and transfer to the beaker. Rinse the crucible with water and add the rinsings to the beaker. Boil for 2 min. Cool.Tra
41、nsfer the contents and rinsings into a 50-mL volumetric flask. Dilute to volume with water and mix.12.4 Transfer appropriate aliquot of the test solution and fusion blank aliquot (in accordance with 11.2) into a 150-mL beaker.Add 15 mL of sodium sulfite solution (100 g/L). Mix. Bring to a boil. Add
42、20 mL of molybdate (5 g/L) hydrazine sulfate solution(0.15 g/L). g/L) solution. Bring to a boil. Simmer for 10 min in a boiling water bath. Cool. Transfer into a 50-mL volumetric flaskand dilute to the mark with water. Mix.12.5 Measure absorbance at approximately 725 nm in a 1-cm cell in the same ma
43、nner as the calibration standards.solutions.13. Calculation13.1 Subtract the absorbance of the 0-mL phosphorus standardsolution from the absorbance of the test sample solutions.Determine g phosphorus referring to the calibration curve.13.2 Calculate the phosphorus content as follows:Phosphorus,%5S0.
44、005AB3C D (1)where:A = g of phosphorus determined,B = sample aliquot in millilitres (12.1), andB = sample aliquot in milliliters (12.1), andC = sample mass in grams (12.1).13.3 Rounding of test results obtained using this test method shall be performed in accordance with Practice E29, RoundingMethod
45、, unless an alternative rounding method is specified by the customer or applicable material specification.NOTE 3As used in this test method, “percentage“ or “%“ refers to a mass fraction of the form (wt / wt %) (g / 100 g).14. Precision and Bias514.1 PrecisionTable 1 indicates the precision of the t
46、est method between laboratories and comparison with the certifiedreference materials.14.2 BiasThe results obtained by the 8 laboratories on the certified reference iron ores, of varying composition, agree closelywithin narrow limits with the assigned certified phosphorus values, thus demonstrating a
47、bsence of any measurable bias.5 Supporting data are available from ASTM International Headquarters. Request RR:E16-1009.E1070 17415. Keywords15.1 agglomerates and related materials; concentrates; iron ores; phosphorus contentASTM International takes no position respecting the validity of any patent
48、rights 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
49、any 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 will 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 t
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