1、BS ISO 9682-1:2009 ICS 73.060.10 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BRITISH STANDARD Iron ores Determination of manganese content Part 1: Flame atomic absorption spectrometric methodThis British Standard was published under the authority of the Standards Policy an
2、d Strategy Committee on 31 July 2009 BSI 2009 ISBN 978 0 580 62727 9 Amendments/corrigenda issued since publication Date Comments BS ISO 9682-1:2009 National foreword This British Standard is the UK implementation of ISO 9682-1:2009. It supersedes BS 7020-9.2:1993 which is withdrawn. The UK particip
3、ation in its preparation was entrusted to Technical Committee ISE/58, Iron ores. A list of organizations represented on this committee can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its c
4、orrect application. Compliance with a British Standard cannot confer immunity from legal obligations.BS ISO 9682-1:2009Reference number ISO 9682-1:2009(E) ISO 2009INTERNATIONAL STANDARD ISO 9682-1 Second edition 2009-06-15 Iron ores Determination of manganese content Part 1: Flame atomic absorption
5、spectrometric method Minerais de fer Dosage du manganse Partie 1: Mthode par spectromtrie dabsorption atomique dans la flamme BS ISO 9682-1:2009 ISO 9682-1:2009(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or vie
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10、41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2009 All rights reservedBS ISO 9682-1:2009 ISO 9682-1:2009(E) ISO 2009 All rights reserved iiiContents Page Foreword iv 1 Scope1 2 Normative references1 3 Principle1 4 Reagents.2 5 Apparatus.2 6 Sampling and samp
11、les3 6.1 Laboratory sample 3 6.2 Preparation of predried test samples3 7 Procedure.4 7.1 Number of determinations4 7.2 Safety precautions 4 7.3 Test portion4 7.4 Blank test and check test .4 7.5 Determination 4 7.5.1 Decomposition of the test portion.4 7.5.2 Treatment of the test solution5 7.5.3 Adj
12、ustment of the atomic absorption spectrometer6 7.5.4 Atomic absorption measurements 6 8 Expression of results7 8.1 Calculation of mass fraction of manganese.7 8.2 General treatment of results.7 8.2.1 Repeatability and permissible tolerance.7 8.2.2 Determination of analytical result8 8.2.3 Between-la
13、boratories precision.8 8.2.4 Check for trueness 8 8.2.5 Calculation of final result9 8.3 Oxide factor9 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 repeatability and permissible toleranc
14、e equations12 Annex C (informative) Precision data obtained by international analytical trials13 BS ISO 9682-1:2009 ISO 9682-1:2009(E) iv ISO 2009 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member b
15、odies). 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 a
16、nd 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 Directives
17、 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 ca
18、sting 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 9682-1 was prepared by Technical Committee ISO/TC 102, Iron ore and direct reduced
19、iron, Subcommittee SC 2, Chemical analysis. This second edition cancels and replaces the first edition (ISO 9682-1:1991), which has been technically revised. ISO 9682 consists of the following parts, under the general title Iron ores Determination of manganese content: Part 1: Flame atomic absorptio
20、n spectrometric method Part 2: Periodate spectrophotometric method BS ISO 9682-1:2009 INTERNATIONAL STANDARD ISO 9682-1:2009(E) ISO 2009 All rights reserved 1Iron ores Determination of manganese content Part 1: Flame atomic absorption spectrometric method WARNING This part of ISO 9682 may involve ha
21、zardous materials, operations and equipment. This part of ISO 9682 does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this part of ISO 9682 to establish appropriate health and safety practices and determine the applicability of reg
22、ulatory limitations prior to use. 1 Scope This part of ISO 9682 specifies a flame atomic absorption spectrometric method for the determination of the mass fraction of manganese in iron ores. This method is applicable to a mass-fraction range of 0,01 % to 2,5 % of manganese in natural iron ores, iron
23、 ore concentrates and agglomerates, including sinter products. 2 Normative references The following referenced documents are 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
24、 (including any amendments) applies. ISO 648, Laboratory glassware Single-volume pipettes ISO 1042, Laboratory glassware One-mark volumetric flasks ISO 3082, Iron ores Sampling and sample preparation procedures ISO 7764, Iron ores Preparation of predried test samples for chemical analysis 3 Principl
25、e The test portion is decomposed by one of the following methods. a) Fusion of the test portion in sodium carbonate/sodium tetraborate flux and dissolution of the cooled melt in hydrochloric acid. b) Treatment with hydrochloric acid, with the addition of a small amount of nitric acid. Evaporation to
26、 dehydrate silica, addition of hydrochloric acid, dilution and filtration. Ignition of the residue and removal of silica by evaporation with hydrofluoric and sulfuric acids. Fusion with sodium carbonate and sodium tetraborate and dissolution of the cooled melt in the filtrate. The solution obtained,
27、 in both cases, is aspirated into the flame of an atomic absorption spectrometer using a dinitrogen oxide/acetylene flame. The absorbance values obtained are compared with those obtained from the calibration solutions. BS ISO 9682-1:2009 ISO 9682-1:2009(E) 2 ISO 2009 All rights reserved4 Reagents Du
28、ring the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. 4.1 Sodium carbonate (Na 2 CO 3 ), anhydrous. 4.2 Sodium tetraborate (Na 2 B 4 O 7 ), anhydrous. 4.3 Hydrochloric acid, 1,16 g/ml to 1,19 g/ml. 4.4 Hydrochloric acid, 1,16 g/ml
29、 to 1,19 g/ml, diluted 1 + 1. 4.5 Nitric acid, 1,4 g/ml. 4.6 Hydrofluoric acid, 1,13 g/ml, 40 % (by mass), or 1,19 g/ml, 48 % (by mass). 4.7 Sulfuric acid, 1,84 g/ml. 4.8 Sulfuric acid, 1,84 g/ml, diluted 1 + 1. 4.9 Background solution. Dissolve 12 g of metallic iron (wire or powder) or 17 g of iron
30、 oxide (in both cases with a mass fraction of manganese less than 0,003 %) in 100 ml of hydrochloric acid (4.3) by heating in a covered 1 000 ml beaker. If metallic iron is used, oxidize by adding nitric acid (4.5) drop by drop. Cool and add 300 ml of hydrochloric acid (4.3). Dissolve 32 g of sodium
31、 carbonate (4.1) and 16 g of sodium tetraborate (4.2) in 300 ml of water, add carefully to the iron solution and heat to remove carbon dioxide. Cool, transfer to a 1 000 ml one-mark volumetric flask, dilute to volume with water and mix. 4.10 Manganese standard solutions. 4.10.1 Manganese stock solut
32、ion, 500 g Mn/ml. Dissolve 0,500 g of high-purity manganese metal minimum purity 99,9 % (by mass) in 25 ml of hydrochloric acid (4.4) in a covered tall-form beaker, while heating. When dissolution is complete, cool, transfer the solution to a 1 000 ml one-mark volumetric flask, dilute to volume with
33、 water and mix. 4.10.2 Manganese standard solution, 50 g Mn/ml. Transfer 50 ml of manganese stock solution (4.10.1) to a 500 ml one-mark volumetric flask, dilute to volume with water and mix. 4.11 Manganese calibration solutions. To a series of 100 ml one-mark volumetric flasks, transfer 0 ml; 5,0 m
34、l; 10,0 ml; 20,0 ml; 30,0 ml, respectively, of manganese standard solution (4.10.2). Add 25,0 ml of background solution (4.9) to each flask, dilute to volume with water and mix. The range of manganese concentrations that can be covered may vary from one instrument to another. Attention should be pai
35、d to the minimum performance criteria described in 5.5. For instruments with high sensitivity, the solution of highest concentration shown above may be deleted from the series and an additional solution included at the lower end, e.g. 2,0 ml of manganese standard solution (4.10.2). 5 Apparatus Ordin
36、ary laboratory apparatus, including one-mark pipettes and one-mark volumetric flasks complying with the specifications of ISO 648 and ISO 1042, respectively, and the following. BS ISO 9682-1:2009 ISO 9682-1:2009(E) ISO 2009 All rights reserved 35.1 Platinum or suitable platinum alloy crucibles, of m
37、inimum capacity 25 ml. 5.2 Muffle furnace, to provide a minimum temperature of 1 020 C. 5.3 Combined magnetic stirrer/hotplate. 5.4 Stirring bars, polytetrafluoroethylene (PTFE)-coated, 10 mm long. 5.5 Atomic absorption spectrometer, equipped with a dinitrogen oxide/acetylene burner. The atomic abso
38、rption spectrometer used in this method will be satisfactory if it meets the following criteria. a) Minimum sensitivity: the absorbance of the most concentrated manganese calibration solution (4.11) is at least 0,27. b) Graph linearity: the slope of the calibration graph covering the top 20 % of the
39、 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 stability: the standard deviation of the absorbance of the most concentrated calibration solution and that o
40、f 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 the most concentrated calibration solution. The use of a strip-chart recorder and/or digital read-out device
41、 is recommended to evaluate criteria a), b) and c) and for all subsequent measurements. NOTE Instrument parameters can vary with each instrument. The following parameters were successfully used in several laboratories and they can be used as guidelines. Solutions were aspirated into a dinitrogen oxi
42、de/acetylene flame of a premix burner. Hollow cathode lamp, mA 5 Wavelength, nm 279,5 Dinitrogen oxide flow rate, l/min 7,5 Acetylene flow rate, l/min 4,0 In systems where the values shown above for gas flow rates do not apply, the ratio of the gas flow rates can still be a useful guideline. 6 Sampl
43、ing and samples 6.1 Laboratory sample For analysis, use a laboratory sample of minus 100 m particle size which has been taken and prepared in accordance with ISO 3082. In the case of ores with significant contents of combined water or oxidizable compounds, use a particle size of minus 160 m. NOTE Gu
44、idance on significant contents of combined water and oxidizable compounds is incorporated in ISO 7764. 6.2 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
45、 of the container. Dry the test sample at 105 C 2 C, as specified in ISO 7764. (This is the predried test sample.) BS ISO 9682-1:2009 ISO 9682-1:2009(E) 4 ISO 2009 All rights reserved7 Procedure 7.1 Number of determinations Carry out the analysis at least in duplicate in accordance with Annex A, ind
46、ependently, on one predried test sample. NOTE The expression “independently“ means that the second and any subsequent result is not affected by the previous result(s). For this particular analytical method, this condition implies that the repetition of the procedure is carried out either by the same
47、 operator at a different time or by a different operator including, in both cases, appropriate recalibration. 7.2 Safety precautions WARNING Follow the manufacturers instructions for igniting and extinguishing the dinitrogen oxide/acetylene flame to avoid possible explosion hazards. Wear tinted safe
48、ty glasses whenever the flame is in operation. 7.3 Test portion Taking several increments, weigh, to the nearest 0,000 2 g, approximately 0,5 g of the predried test sample obtained in accordance with 6.2. 7.4 Blank test and check test In each run, one blank test and one analysis of a certified refer
49、ence material of the same type of ore shall be carried out in parallel with the analysis of the ore sample(s) under the same conditions. A predried test sample of the certified reference material shall be prepared as specified in 6.2. The certified reference material should be of the same type as the sample to be analysed and the properties of the two materials should be sufficiently similar to ensure that, in both cases, no significant changes in the analytical procedure will become necessary. Wh
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