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2、nductively coupled plasma atomic emission spectrometric methodICS 73.060.10Iron ores Determination of various elements BRITISH STANDARDBS ISO 11535:2006BS ISO 11535:2006Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 20/11/2009 02:50, Uncontrolled Copy, (c) BSIThis British Standard was publis
3、hed under the authority of the Standards Policy and Strategy Committee on 31 January 2007 BSI 2007ISBN 978 0 580 50110 4Amendments issued since publicationAmd. No. Date Commentscontract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunity from
4、legal obligations. National forewordThis British Standard was published by BSI. It is the UK implementation of ISO 11535:2006.The UK participation in its preparation was entrusted to Technical Committee ISE/58, Iron ores.A list of organizations represented on ISE/58 can be obtained on request to its
5、 secretary.This publication does not purport to include all the necessary provisions of a Reference numberISO 11535:2006(E)INTERNATIONAL STANDARD ISO11535Second edition2006-12-15Iron ores Determination of various elements Inductively coupled plasma atomic emission spectrometric method Minerais de fe
6、r Dosage de divers lments Mthode par spectromtrie dmission atomique avec plasma induit par haute frquence BS ISO 11535:2006Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 20/11/2009 02:50, Uncontrolled Copy, (c) BSIii Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 20/11/2009 02:50, Un
7、controlled Copy, (c) BSIiiiContents Page Foreword iv 1 Scope . 1 2 Normative references . 1 3 Principle. 2 4 Reagents 2 5 Apparatus 4 6 Sampling and samples. 4 6.1 Laboratory sample 4 6.2 Preparation of predried test samples . 5 7 Procedure 5 7.1 Number of determinations . 5 7.2 Test portion . 5 7.3
8、 Blank test and check test. 5 7.4 Determination 5 7.4.1 Decomposition of the test portion 5 7.4.2 Adjustment of spectrometer 6 7.4.3 Measurements. 7 8 Calculation of results . 7 8.1 Calibration graph 7 8.2 Correction of spectral interference. 7 8.3 Standardization of calibration graph (drift correct
9、ion). 9 8.4 General treatment of results 10 8.4.1 Repeatability and permissible tolerances10 8.4.2 Determination of analytical result. 10 8.4.3 Check for trueness . 11 8.4.4 Calculation of final result. 11 8.5 Oxide factors . 12 9 Test report . 12 Annex A (informative) Suggested calibration solution
10、s 13 Annex B (normative) Plasma-spectrometer performance tests 15 Annex C (normative) Flowsheet of the procedure for the acceptance of analytical values for test samples 18 Annex D (informative) Derivation of repeatability and permissible tolerance equations . 19 Annex E (informative) Precision data
11、 obtained by international analytical trials 20 BS ISO 11535:2006Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 20/11/2009 02:50, Uncontrolled Copy, (c) BSIiv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member
12、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 organizations, governmental
13、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 given in the ISO/IEC Directive
14、s, 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 75 % of the member bodies c
15、asting 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 11535 was prepared by Technical Committee ISO/TC 102, Iron ore and direct reduced
16、iron, Subcommittee SC 2, Chemical analysis. This second edition cancels and replaces the first edition (ISO 11535:1998), which has been technically revised. It has been updated to alter the manner in which the precision data are presented. BS ISO 11535:2006Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA
17、 STANDARDS, 20/11/2009 02:50, Uncontrolled Copy, (c) BSI1Iron ores Determination of various elements Inductively coupled plasma atomic emission spectrometric method WARNING This International Standard may involve hazardous materials, operations and equipment. This International Standard does not pur
18、port to address all of the safety problems associated with its use. It is the responsibility of the user of this International Standard to establish appropriate health and safety practices and determine the applicability of regulatory limitations prior to use. 1 Scope This International Standard spe
19、cifies a method for the determination of aluminium, calcium, phosphorus, magnesium, manganese, silicon and titanium in iron ores by inductively coupled plasma atomic emission spectrometry (ICP-AES). This method is applicable to the mass-fraction ranges given in Table 1, in natural iron ores, iron or
20、e concentrates and agglomerates, including sinter products. Table 1 Mass-fraction ranges Element Range of mass fractions % Al Ca Mg Mn P Si Ti 0,07 to 3,30 0,012 to 6,80 0,008 to 1,90 0,012 to 1,70 0,011 to 1,60 0,44 to 9,40 0,018 to 0,17 2 Normative references The following referenced documents are
21、 indispensable for the application of 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 One-mark pipettes ISO 1042, Laboratory glassware One-mark
22、 volumetric flasks ISO 3082, Iron ores Sampling and sample preparation procedures ISO 3696, Water for analytical laboratory use Specification and test methods ISO 7764, Iron ores Preparation of predried test samples for chemical analysis BS ISO 11535:2006Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA S
23、TANDARDS, 20/11/2009 02:50, Uncontrolled Copy, (c) BSI2 3 Principle The test portion is decomposed by fusion in a sodium carbonate/sodium tetraborate flux and the cooled melt is dissolved in hydrochloric acid. The solution is diluted to volume and measured on an ICP spectrometer. Final results are r
24、ead from a calibration graph prepared using standard solutions. 4 Reagents During the analysis, use only reagents of recognized analytical grade and only water that complies with grade 2 of ISO 3696. 4.1 Iron oxide (Fe2O3), of minimum purity 99,99 % (mass fraction). 4.2 Sodium carbonate (Na2CO3), an
25、hydrous. To produce final impurity levels in a solution below the detection limits determined or suggested in the performance test, a high-quality grade is required. 4.3 Sodium tetraborate (Na2B4O7), anhydrous. The same purity criteria as for the sodium carbonate are required. 4.4 Hydrochloric acid,
26、 1,16 g/ml to 1,19 g/ml. The same purity criteria as for the sodium carbonate are required. 4.5 Hydrochloric acid, 1,16 g/ml to 1,19 g/ml, diluted 1 + 1. Add 500 ml of hydrochloric acid (4.4) to 500 ml of water and mix. 4.6 Nitric acid, 1,4 g/ml. The same purity criteria as for the sodium carbonate
27、are required. 4.7 Stock solutions. 4.7.1 Phosphorus, 1 000 g/ml. Dry approximately 10 g of potassium dihydrogen orthophosphate (KH2PO4) at 110 C until a constant mass is reached, and cool in a desiccator. Dissolve 4,393 6 g in about 200 ml of water in a 1 000 ml one-mark volumetric flask. When the d
28、issolution is complete, dilute to volume with water and mix. 4.7.2 Manganese, 1 000 g/ml. Dissolve 1,000 0 g of high-purity manganese metal in 20 ml of hydrochloric acid (4.5) in a covered tall-form beaker while heating. When dissolution is complete, cool, transfer to a 1 000 ml one-mark volumetric
29、flask, dilute to volume with water and mix. 4.7.3 Magnesium, 1 000 g/ml. Dissolve 1,000 0 g of high-purity magnesium metal in 20 ml of hydrochloric acid (4.5) in a covered tall-form beaker while heating. When dissolution is complete, cool, transfer to a 1 000 ml one-mark volumetric flask, dilute to
30、volume with water and mix. BS ISO 11535:2006Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 20/11/2009 02:50, Uncontrolled Copy, (c) BSI34.7.4 Silicon, 1 000 g/ml. Accurately weigh 2,139 3 g of pure silicon oxide (finely ground, previously heated at 1 000 C for 45 min) into a platinum crucibl
31、e (5.2). Mix with 5 g of sodium carbonate (4.2), and melt in a furnace at 1 000 C for 15 min. Dissolve the melt in 100 ml of warm water and transfer to a 1 000 ml one-mark volumetric flask; increase the volume to approximately 500 ml with water, add 20 ml of hydrochloric acid (4.5), dilute to volume
32、 with water and mix. Store in a polyethylene flask. 4.7.5 Aluminium, 1 000 g/ml. Dissolve 1,000 0 g of high-purity aluminium metal in 20 ml of hydrochloric acid (4.5) in a covered tall-form beaker. Add about 4 drops of nitric acid (4.6). When dissolution is complete, add about 20 ml of water and hea
33、t to liberate oxides of nitrogen. Cool and transfer to a 1 000 ml one-mark volumetric flask, dilute to volume with water and mix. 4.7.6 Titanium, 1 000 g/ml. Dissolve 1,000 0 g of high-purity titanium metal in 100 ml of hydrochloric acid (4.5) in a covered tall-form beaker while heating. When dissol
34、ution is complete, cool, transfer to a 1 000 ml one-mark volumetric flask, dilute to volume with hydrochloric acid (4.5) and mix. 4.7.7 Calcium, 1 000 g/ml. Dry approximately 10 g of calcium carbonate (CaCO3) at 110 C until a constant mass is reached, and cool in a desiccator. Dissolve 2,497 2 g in
35、20 ml of hydrochloric acid (4.5) in a covered tall-form beaker while heating. When dissolution is complete, cool, transfer to a 1 000 ml one-mark volumetric flask, dilute to volume with water and mix. 4.8 Calibration and reference solutions Calibration solutions are defined as the solutions required
36、 for plotting the calibration graphs of the elements analysed. Their concentration ranges in solution, expressed in micrograms per millilitre, are determined with reference to the performance parameter values and the linearity response of the instrument. A minimum of 10 solutions is necessary to cov
37、er the mass-fraction ranges given in Table 1. For test samples having narrower concentration ranges, calibration solutions shall be prepared to cover the region of interest. If the element concentration in solution exceeds 5 000 detection limit (DL), a separate calibration graph shall be prepared to
38、 cover the range. In the case of non-linearity, either a less sensitive line is to be used or appropriate dilutions of sample and calibration solutions are to be carried out. NOTE For the suggested lines shown in Table 2, the calibration solutions prepared as recommended in Annex A will be in agreem
39、ent with the performance test figures. To comply with the requirements of similarity between the test sample and the calibration solutions, iron, flux and acids must be added (see Note 1 to Table A.1). For each calibration solution, the procedure recommended in 7.4.1 is followed, replacing the test
40、sample with the equivalent amount of iron oxide (4.1). Prior to the final dilution to 200 ml, the stock solutions and hydrochloric acid (4.5) are added in sufficient amounts to retain the final acid concentration (40 ml of HCl diluted 1+1) suggested in Annex A. In addition, to comply with the requir
41、ements of similarity, calibration solutions and test samples are prepared from reagents taken from the same containers to minimize purity differences between batches. BS ISO 11535:2006Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 20/11/2009 02:50, Uncontrolled Copy, (c) BSI4 5 Apparatus Ord
42、inary laboratory equipment, including one-mark pipettes and one-mark volumetric flasks complying with the specifications of ISO 648 and ISO 1042 respectively, and the following. 5.1 Analytical balance, capable of weighing to the nearest 0,000 1 g. 5.2 Platinum or suitable platinum-alloy crucibles, h
43、aving a minimum volume of 40 ml. 5.3 Bunsen burner, having an appropriate fuel/oxidant ratio to provide a minimum temperature of 500 C. 5.4 Muffle furnace, to provide a minimum temperature of 1 020 C. 5.5 Combined hotplate/magnetic stirrer. 5.6 Stirring bars, PTFE-coated, 10 mm long. 5.7 ICP spectro
44、meter. Any conventional ICP spectrometer may be used, provided that the instrument has been initially set up according to the manufacturers recommendations, and that it complies with the performance test (7.4.2.2) carried out prior to the measurements. Suggested analytical lines are shown in Table 2
45、. These lines were found to be relatively free of significant interferences from the matrix elements, but they shall be carefully evaluated for spectral interference, background and ionization prior to their adoption. Failure to attain the recommended performance parameters may indicate an interfere
46、nce. For the analysis of samples having concentrations in the background equivalent concentration (BEC) region or lower, as defined in Table 3, careful assessment of the need for background correction for the particular line chosen is recommended prior to calibration and analysis Table 2 Suggested a
47、nalytical lines Element Wavelength nm Al Ca Mg Mn P Si Ti 396,15 or 308,22 393,36 or 317,93 279,55 or 279,08 257,61 178,29 a251,61 or 288,16 334,94 or 336,12 aCheck and correct, if necessary, for interference by Mn. 6 Sampling and samples 6.1 Laboratory sample For analysis, use a laboratory sample o
48、f minus 100 m particle size which has been taken and prepared in accordance with ISO 3082. In the case of ores having significant contents of combined water or oxidizable compounds, use a particle size of minus 160 m. NOTE A guideline on significant contents of combined water and oxidizable compound
49、s is incorporated in ISO 7764. BS ISO 11535:2006Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 20/11/2009 02:50, Uncontrolled Copy, (c) BSI56.2 Preparation of predried test samples Thoroughly mix the laboratory sample and, taking multiple increments, extract a test sample in such a manner that it is representative of the whole contents of the container. Dry the test sample at 105 C 2 C as specified in ISO 7764. (This is the predried test sample.) 7 Procedure 7.1 Number of determinations Carry out the analysis at least in
