BS ISO 9683-2-2009 Iron ores - Determination of vanadium content - Flame atomic absorption spectrometric methods《铁矿石 钒含量的测定 火焰原子吸收光谱法》.pdf

1、BS ISO ICS 73.060 .10 NO COP YING WIT HOUTB SI PER MISSI ON EX CE PT AS PER MITTED BY COPY RI GHT LAW BR ITISHS TANDA RD Ir on or es Det erm ina ti on of vanadi um Part2 :F lame atomica bs or pti on sp ect ro me tr ic me th ods 9683 -2:2009 Incorporating corrigendum September 2015This Brit ish Sta n

2、da rd was pub lishedu ndert he aut horityo ft he Sta nda rds Policy and Stra te gy Co mm itt ee on 31 July 20 09 ISBN9780580914928 BS ISO 96 83 -2 :20 09 National for ew ord This Bri tishS tandardi st he UK imp lem ent at ion of ISO 96 83 -2 :20 09. The UK pa rti cipa tioni ni ts prepar ation was en

3、tr us ted to Tec hn ic al Committee ISE/ 58, Iron ores. Al ist of or ga nizat ionsr epr esen ted on thisc ommi ttee canb eo btain ed on requ est to its sec retar y. Th is publ ic ation does not pur port to in cl ude all the nec ess ary provi si ons of ac ontr ac t. Us ers arer esp ons ib le for itsc

4、 orr ect appl ic ati on. Co mp lia nce withaB ritish St and ard cannotc onf er immu ni ty fr om le gal obli gation s. The British Standards Institution 2015. Published by BSI Standards Limited 2015 Amendments/corrigenda issued since publication Date Comments 30 September 2015 Implementation of ISO c

5、orrected text 1 October 2009: ISO foreword updated Reference number ISO 9683-2:2009(E) ISO 2009INTERNATIONAL STANDARD ISO 9683-2 First edition 2009-06-15 Corrected version 2009-10-01 Iron ores Determination of vanadium Part 2: Flame atomic absorption spectrometric methods Minerais de fer Dosage du v

6、anadium Partie 2: Mthodes par spectromtrie dabsorption atomique dans la flamme ISO 9683-2:2009(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedde

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10、g photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published

11、in Switzerland ii ISO 2009 All rights reservedBS ISO 9683-2:2009ISO 9683-2:2009(E) ISO 2009 All rights reserved iiiContents Page Foreword iv 1 Scope1 2 Normative references1 3 Principle1 3.1 Dissolution .1 3.2 Determination 2 3.2.1 Extraction (Method 1 only) .2 3.2.2 Measurement (Methods 1 and 2)2 4

12、 Reagents.2 5 Apparatus.3 6 Sampling and samples4 6.1 Laboratory sample 4 6.2 Preparation of predried test samples4 7 Procedure.5 7.1 Number of determinations5 7.2 Safety precautions 5 7.3 Test portion5 7.4 Blank test and check test .5 7.5 Determination Method 1 (mass fraction of vanadium between 0,

13、004 % and 0,06 %).5 7.5.1 Decomposition of the test portion.5 7.5.2 Dissolution of salts and residue treatment.5 7.5.3 Extraction of vanadium.6 7.5.4 Adjustment of the atomic absorption spectrometer6 7.5.5 Atomic absorption measurements 6 7.6 Determination Method 2 (mass fraction of vanadium between

14、 0,06 % and 0,5 %).7 7.6.1 Decomposition of the test portion.7 7.6.2 Dissolution of salts and residue treatment.7 8 Expression of results7 8.1 Calculation of mass fraction of vanadium7 8.2 General treatment of results.8 8.2.1 Repeatability and permissible tolerance.8 8.2.2 Determination of analytica

15、l result8 8.2.3 Between-laboratories precision.9 8.2.4 Check for trueness 9 8.2.5 Calculation of final result10 8.3 Oxide factor10 9 Test report10 Annex A (normative) Flowsheet of the procedure for the acceptance of analytical values for test samples 11 Annex B (informative) Derivation of repeatabil

16、ity and permissible tolerance equations12 Annex C (informative) Precision data obtained by international analytical trials13 BS ISO 9683-2:2009ISO 9683-2:2009(E) iv ISO 2009 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national sta

17、ndards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International or

18、ganizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules give

19、n in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 7

20、5 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 9683-2 was prepared by Technical Committee ISO/TC 102, I

21、ron ore and direct reduced iron, Subcommittee SC 2, Chemical analysis. This first edition cancels and replaces ISO 9684:1991. ISO 9683 consists of the following parts, under the general title Iron ores Determination of vanadium: Part 1: BPHA spectrophotometric method Part 2: Flame atomic absorption

22、spectrometric methods This corrected version of ISO 9683-2:2009 incorporates the following correction: a new sixth paragraph has been added to this foreword. BS ISO 9683-2:2009INTERNATIONAL STANDARD ISO 9683-2:2009(E) ISO 2009 All rights reserved 1Iron ores Determination of vanadium Part 2: Flame at

23、omic absorption spectrometric methods WARNING This part of ISO 9683 may involve hazardous materials, operations and equipment. This part of ISO 9683 does not purport to address all of the safety issues associated with its use. It is the responsibility of the user to establish appropriate health and

24、safety practices and determine the applicability of regulatory limitations prior to use. 1 Scope This part of ISO 9683 specifies two flame atomic absorption spectrometric methods for the determination of the mass fraction of vanadium in iron ores. Method 1 is applicable to mass fractions of vanadium

25、 between 0,004 % and 0,06 %, and Method 2 is applicable to mass fractions of vanadium between 0,06 % and 0,5 %, in natural iron ores, iron ore concentrates and agglomerates, including sinter products. 2 Normative references The following referenced documents are indispensable for the application of

26、this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 648, Laboratory glassware Single-volume pipettes ISO 1042, Laboratory glassware One-mark volumetric flasks ISO 3082, Iron

27、 ores Sampling and sample preparation procedures ISO 7764, Iron ores Preparation of predried test samples for chemical analysis 3 Principle 3.1 Dissolution The test portion is decomposed by digestion with hydrochloric acid in a polytetrafluoroethylene (PTFE) beaker, hydrofluoric and nitric acids are

28、 added and the solution is evaporated to dryness. Hydrochloric and boric acids are added and the solution is again evaporated to dryness. The salts are dissolved in hydrochloric and nitric acids (Method 1), or hydrochloric acid (Method 2), and the solution is filtered. The residue is ignited and fus

29、ed with sodium carbonate and the cooled melt is dissolved in the test solution. BS ISO 9683-2:2009ISO 9683-2:2009(E) 2 ISO 2009 All rights reserved3.2 Determination 3.2.1 Extraction (Method 1 only) The solution is oxidized with cerium(IV) solution, and phosphoric acid and sodium tungstate solution a

30、re added. The vanadium complex is extracted with a 1 + 1 mixture of 1-pentanol and 4-methyl-2-pentanone. The solvent phase is treated with water and then ascorbic acid solution to return the vanadium to an aqueous phase. 3.2.2 Measurement (Methods 1 and 2) Aluminium solution is added to the test sol

31、ution, which is diluted to volume. The solution is aspirated into a dinitrogen oxide/acetylene flame in an atomic absorption spectrometer and the absorbance is measured at a wavelength of approximately 318,5 nm. 4 Reagents During the analysis, use only reagents of recognized analytical grade, and on

32、ly distilled water or water of equivalent purity. 4.1 Hydrochloric acid, 1,16 g/ml to 1,19 g/ml. 4.2 Hydrochloric acid, 1,16 g/ml to 1,19 g/ml, diluted 1 + 1. 4.3 Hydrofluoric acid, 1,13 g/ml, 40 % (by mass) or 1,19 g/ml, 48 % (by mass). 4.4 Nitric acid, 1,4 g/ml. 4.5 Nitric acid, 1,4 g/ml, diluted

33、1 + 1. (Method 1 only.) 4.6 Phosphoric acid, 1,7 g/ml, diluted 1 + 2. (Method 1 only.) 4.7 Sodium carbonate (Na 2 CO 3 ), anhydrous powder. 4.8 Boric acid (H 3 BO 3 ). 4.9 Di-ammonium cerium(IV) nitrate (NH 4 ) 2 Ce(NO 3 ) 6 , 20 g/l solution. (Method 1 only.) Dissolve 2,0 g of di-ammonium cerium(IV

34、) nitrate in a mixture of 15 ml of nitric acid (4.5) and 85 ml of water. 4.10 Sodium tungstate (Na 2 WO 4 2H 2 O), 165 g/l solution. (Method 1 only.) Dissolve 16,5 g of sodium tungstate dihydrate in approximately 70 ml of water, dilute to 100 ml and mix. 4.11 Ascorbic acid (C 6 H 8 O 6 ), 10 g/l sol

35、ution. (Method 1 only.) Prepare freshly for each series of tests. 4.12 1-Pentanol (n-amyl alcohol, 1-pentan-1-ol). (Method 1 only.) 4.13 4-Methyl-2-pentanone (methyl isobutyl ketone, MIBK). (Method 1 only.) 4.14 Mixed solvent. (Method 1 only.) Prepare a 1 + 1 volume ratio mixture of 1-pentanol (4.12

36、) and MIBK (4.13). BS ISO 9683-2:2009ISO 9683-2:2009(E) ISO 2009 All rights reserved 34.15 Aluminium chloride (AlCl 3 6H 2 O), 220 g/l solution. Dissolve 220 g of aluminium chloride hexahydrate in water, add 50 ml of hydrochloric acid (4.1), dilute to 1 000 ml with water and mix. 4.16 Iron oxide, hi

37、gh purity (containing less than 0,002 % V). 4.17 Iron background solution. (Method 2 only.) Dissolve 90 g of high-purity iron oxide (4.16) in 750 ml of hydrochloric acid (4.1) while heating. Cool and carefully add a solution of 30 g of sodium carbonate (4.7) in 200 ml of water. Dilute with water to

38、a final volume of approximately 1 000 ml and mix. NOTE The use of an equivalent quantity of metallic iron (of similarly low vanadium content), in conjunction with a suitable oxidant, is permissible. 4.18 Vanadium standard solution, 1 mg V/ml. Dry ammonium monovanadate (NH 4 VO 3 ) in an air oven at

39、100 C for 1 h and cool to room temperature. Dissolve 2,296 g of the dried product in approximately 600 ml of water, transfer to a 1 000 ml one-mark volumetric flask, dilute to volume with water and mix. 4.19 Diluted vanadium standard solution, 0,2 mg V/ml. (Method 1 only.) Transfer 20,0 ml of vanadi

40、um standard solution (4.18) to a 100 ml one-mark volumetric flask, dilute to volume with water and mix. 4.20 Vanadium calibration solutions. (Method 1 only.) Transfer 1,8 g of high-purity iron oxide (4.16) to each of five 100 ml PTFE beakers (5.1). Proceed according to 7.5.1, incorporating the opera

41、tion in 7.5.2 to dissolve the evaporated salts. Transfer 0 ml; 1,00 ml; 2,00 ml: 4,00 ml and 6,00 ml of the diluted vanadium standard solution (4.19), respectively, to the beakers. Omit the residue-processing steps and add 10 ml of nitric acid (4.5) and 25 ml of water. Evaporate to 50 ml and proceed

42、 as specified in 7.5.3. 4.21 Vanadium calibration solutions. (Method 2 only.) Transfer 0 ml; 1,00 ml; 2,00 ml; 4,00 ml and 6,00 ml of vanadium standard solution (4.18), respectively, to five 100 ml one-mark volumetric flasks. Add 10 ml of iron background solution (4.17), 4,0 ml of aluminium chloride

43、 solution (4.15) and 0,5 g of boric acid (4.8) to each flask. Dilute to volume with water and mix. 5 Apparatus Ordinary laboratory apparatus, including one-mark pipettes and one mark-volumetric flasks complying with the specifications of ISO 648 and ISO 1042, respectively (unless otherwise indicated

44、), and the following. 5.1 Polytetrafluoroethylene (PTFE) beakers, of capacity 100 ml, preferably low form. 5.2 Platinum crucibles, of minimum capacity 20 ml. 5.3 Muffle furnace. 5.4 Separating funnels, 100 ml (preferably graduated). BS ISO 9683-2:2009ISO 9683-2:2009(E) 4 ISO 2009 All rights reserved

45、5.5 Atomic absorption spectrometer, equipped with a dinitrogen oxide/acetylene burner. The atomic absorption spectrometer used in this method is satisfactory if it meets the following criteria. a) Minimum sensitivity: the absorbance of the most concentrated vanadium calibration solution (4.21) is at

46、 least 0,25 (see Note 2). b) Graph linearity: the slope of the calibration graph covering the top 20 % of the concentration range (expressed as a change in absorbance) is not less than 0,7 of the value of the slope for the bottom 20 % of the concentration range determined in the same way. c) Minimum

47、 stability: the standard deviation of the absorbance of the most concentrated calibration solution and that of the zero calibration solution, each being calculated from a sufficient number of repetitive measurements, are less than 1,5 % and 0,5 %, respectively, of the mean value of the absorbance of

48、 the most concentrated solution. The use of a strip-chart recorder and/or digital read-out device is recommended to evaluate criteria a), b) and c) and for all subsequent measurements. NOTE 1 Instrument parameters: V-hollow cathode lamp, mA 10 Wavelength, nm 318,5 Dinitrogen oxide flow rate, l/min 9

49、,5 Acetylene flow rate, l/min 3,8 In systems where the values shown above for gas flow rates do not apply, the given ratio of the flow rates (5:2) can still be a useful guideline. The slit width should be sufficiently narrow to substantially reject the stronger emitting but weaker absorbing line at 318,4 nm. NOTE 2 To check the instrument criteria when only Method 1 is involved, prepare the highest calibration solution specified for Method 2, omitting the iron background solution. 6 Sampling and samples 6