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1、BRITISH STANDARD BS EN ISO 10280:1995 Incorporating Amendment No. 1 Steel and iron Determination of titanium content Diantipyrylmethane spectrophotometric method The European Standard EN ISO 10280:1995 has the status of a British Standard ICS 77.080 Licensed Copy: sheffieldun sheffieldun, na, Sun No
2、v 19 15:59:17 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 10280:1995 This British Standard, having been prepared under the direction of the Iron and Steel Standards Policy Committee, was published under the authority of the Standards Board and comes into effect on 29 November 1991 BSI 03-20
3、00 The following BSI references relate to the work on this standard: Committee reference ISM/18 Draft for comment 90/36028 DC ISBN 0 580 20276 3 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Iron and Steel Standards Policy Committee (I
4、SM/-) to Technical Committee ISM/18, upon which the following bodies were represented: BICRA British Steel Industry Department of Trade and Industry (Laboratory of the Government Chemist) Ferro Alloys and Metals Producers Association Ministry of Defence Amendments issued since publication Amd. No.Da
5、teComments 8697December 1995 Indicated by a sideline in the margin Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:59:17 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 10280:1995 BSI 03-2000i Contents Page Committees responsibleInside front cover National forewordii Foreword2 1Scope3
6、 2Normative references3 3Principle3 4Reagents3 5Apparatus4 6Sampling4 7Procedure4 8Expression of results6 9Special case7 10Test report7 Annex A (informative) Additional information on the international cooperative tests8 Annex B (informative) Graphical representation of precision data9 Figure B.1 Lo
7、garithmic relationships between titanium content () and repeatability (r) and reproducibility (R and Rw)9 Table 15 Table 25 Table 37 Table A.18 Publication(s) referred toInside back cover wTi Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:59:17 GMT+00:00 2006, Uncontrolled Copy, (c) BSI B
8、S EN ISO 10280:1995 ii BSI 03-2000 National foreword This Subsection of BS 6200 has been prepared under the direction of the Iron and Steel Standards Policy Committee. It supersedes BS 6200-3.32.1:1986, which is withdrawn. It is identical with ISO 10280:1991 “Steel and iron Determination of titanium
9、 content Diantipyrylmethane spectrophotometric method”, published by the International Organization for Standardization (ISO). In 1995 the European Committee for Standardization (CEN) has accepted ISO 10280:1991 as European Standard EN ISO 10280:1995. As a consequence of implementing the European St
10、andard this British Standard is renumbered as BS EN ISO 10280 and any reference to BS 6200-3.32.1 should be read as a reference to BS EN ISO 10280. The Technical Committee has reviewed the provisions of ISO 377-2, ISO 385-1 and ISO 648, to which reference is made in the text, and has decided that th
11、ey are acceptable for use in conjunction with this standard. Related British Standards for ISO 377-2:1989, ISO 385-1:1984 and ISO 648:1977 are, respectively, BS 6200-2 “Sampling and sample preparation” Section 2.1:1993 “Methods for iron and steel”, BS 846:1985 “Specification for burettes” and BS 158
12、3:1986 “Specification for one-mark pipettes”. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligati
13、ons. Cross-references International StandardCorresponding British Standard ISO 1042:1983BS 1792:1982 Specification for one-mark volumetric flasks (Identical) ISO 3696:1987BS 3978:1987 Specification for water for laboratory use (Identical) ISO 5725:1986BS 5497 Precision of test methods Part 1:1987 Gu
14、ide for the determination of repeatability and reproducibility for a standard test method by inter-laboratory tests (Identical) Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the EN ISO title page, pages 2 to 10, an inside back cover and a back cover.
15、This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:59:17 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EU
16、ROPENNE EUROPISCHE NORM EN ISO 10280 September 1995 ICS 77.080 Descriptors: Steels, iron, cast iron, chemical analysis, determination of content, titanium, spectrometric method English version Steel and iron Determination of titanium content Diantipyrylmethane spectrophotometric method (ISO 10280:19
17、91) Aciers et fontes Dosage du titane Mthode spectrophotomtrique au diantipyrylmthane (ISO 10280:1991) Stahl und Eisen Bestimmung von Titan Photometrische Methode mit Diantipyrylmethan (ISO 10280:1991) This European Standard was approved by CEN on 1995-08-06. CEN members are bound to comply with the
18、 CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat or
19、 to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official versi
20、ons. CEN members are the national standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisat
21、ion Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1995 Copyright reserved to CEN members Ref. No. EN ISO 10280:1995 E Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:59:17 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 10280:1995 BSI 03-2000 2 F
22、oreword The text of the International Standard from ISO/TC 17, Steel, of the International Organization for Standardization (ISO) has been taken over as a European Standard by the Technical Committee ECISS/TC 20, Methods of chemical analysis. This European Standard shall be given the status of a nat
23、ional standard, either by publication of an identical text or by endorsement, at the latest by March 1996, and conflicting national standards shall be withdrawn at the latest by March 1996. According to the CEN/CENELEC Internal Regulations, the following countries are bound to implement this Europea
24、n Standard: Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:59:17 GMT+00:00 2006, Uncontrolled Copy, (c) BSI E
25、N ISO 10280:1995 BSI 03-20003 1 Scope This International Standard specifies a diantipyrylmethane spectrophotometric method for the determination of titanium in steel and iron. The method is applicable to titanium contents between 0,002 % (m/m) and 0,80 % (m/m). 2 Normative references The following s
26、tandards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged
27、 to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 377-2:1989, Selection and preparation of samples and test pieces of wrought steels Part 2: Samples for the
28、determination of the chemical composition. ISO 385-1:1984, Laboratory glassware Burettes Part 1: General requirements. ISO 648:1977, Laboratory glassware One-mark pipettes. ISO 1042:1983, Laboratory glassware One-mark volumetric flasks. ISO 3696:1987, Water for analytical laboratory use Specificatio
29、n and test methods. ISO 5725:1986, Precision of test methods Determination of repeatability and reproducibility for a standard test method by inter-laboratory tests. 3 Principle Dissolution of a test portion in hydrochloric, nitric and sulfuric acids. Fusion of the residue with potassium hydrogen su
30、lfate. Formation of a yellow complex with 4,4- diantipyrylmethane. Spectrophotometric measurement of the coloured complex at a wavelength of about 385 nm. 4 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only grade 2 water as specified in
31、ISO 3696. 4.1 Iron, of high purity containing less than 2 4g Ti/g. 4.2 Potassium hydrogen sulfate (KHSO4). 4.3 Sodium carbonate (Na2CO3), anhydrous. 4.4 Hydrochloric acid, about 1,19 g/ml. 4.5 Nitric acid, about 1,40 g/ml. 4.6 Hydrofluoric acid, about 1,15 g/ml. 4.7 Hydrochloric acid, about 1,19 g/m
32、l, diluted 1 + 1. 4.8 Hydrochloric acid, about 1,19 g/ml, diluted 1 + 3. 4.9 Sulfuric acid, about 1,84 g/ml, diluted 1 + 1. 4.10 Tartaric acid solution, 100 g/l. 4.11 Ascorbic acid solution, 100 g/l. Prepare this solution immediately before use. 4.12 Ammonium oxalate solution Dissolve 6 g of ammoniu
33、m oxalate monohydrate (COONH4)2.H2O in water and dilute to 200 ml. 4.13 Iron solution, 12,5 g/l. Dissolve 1,25 g of iron (4.1) in 10 ml of hydrochloric acid (4.7) while heating gently. Add 5 ml of nitric acid (4.5) and boil until the volume of the solution is approximately 10 ml. Cool, transfer to a
34、 100 ml one-mark volumetric flask, dilute to the mark with water and mix. 4.14 Reagent blank solution Prepare a reagent blank solution in parallel with the determination, using the same quantities of reagents as those used for the determination but no iron. Follow exactly the procedure described in
35、7.3.1 and 7.3.2, diluting to 100 ml with water. 4.15 Diantipyrylmethane solution Dissolve 4 g of 4,4-methylenebis(2,3-dimethyl-1- phenyl-5-pyrazolone) monohydrate, C23H24O2N4.H2O, (diantipyrylmethane) in 20 ml of hydrochloric acid (4.7) and dilute to 100 ml with water. 4.16 Titanium standard solutio
36、n 4.16.1 Titanium stock solution, corresponding to 1 g of Ti per litre. Weigh, to the nearest 0,000 1 g, 0,500 g of high purity titanium metal purity 99,9 % (m/m) and transfer to a 300 ml beaker. Add 180 ml of sulfuric acid, about 1,84 g/ml, diluted 1 + 3, cover with a watchglass, heat gently until
37、the metal has dissolved and oxidize with nitric acid (4.5) added drop by drop. Cool, transfer to a 500 ml one-mark volumetric flask, dilute to the mark with water and mix. 1 ml of this stock solution contains 1,0 mg of Ti. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 19 15:59:17 GMT+00:00 200
38、6, Uncontrolled Copy, (c) BSI EN ISO 10280:1995 4 BSI 03-2000 4.16.2 Titanium standard solution, corresponding to 50 mg of Ti per litre. Transfer 10,0 ml or titanium stock solution (4.16.1) to a 200 ml one-mark volumetric flask. Dilute to the mark with water and mix. Prepare this solution immediatel
39、y before use. 1 ml of this standard solution contains 50 4g of Ti. 5 Apparatus All volumetric glassware shall be class A, in accordance with ISO 385-1, ISO 648 or ISO 1042 as appropriate. Ordinary laboratory apparatus, and 5.1 Crucible, of platinum metal or platinum-gold alloy, of capacity 30 ml. 5.
40、2 Spectrophotometer The spectrophotometer shall be equipped to measure absorbance at a wavelength of 385 nm. Wavelength measurement shall be accurate to 2 nm or less. In the absorbance range 0,05 to 0,85, absorbance measurements shall be repeatable to 0,003 or better. 6 Sampling Carry out sampling i
41、n accordance with ISO 377-2 or appropriate national standards for steel and iron. 7 Procedure 7.1 Test portion Weigh, to the nearest 0,000 5 g, a test portion according to the presumed titanium content as follows: a) for titanium contents in the range 0,002 % (m/m) to 0,125 % (m/m), a test portion o
42、f 1,00 g; b) for titanium contents in the range 0,125 % (m/m) to 0,80 % (m/m), a test portion of 0,50 g. 7.2 Blank test In parallel with the determination and following the same procedure, carry out a blank test using the same quantities of all the reagents and the same cell as in the determination,
43、 substituting an equivalent amount of iron (4.1) for the test portion. 7.3 Determination 7.3.1 Dissolution of the test portion Place the test portion (7.1) in a 250 ml beaker. Add 20 ml of hydrochloric acid (4.4), cover the beaker with a watchglass and digest at 70 C to 90 C until the solvent action
44、 ceases. Add 5 ml of nitric acid (4.5) and boil until the volume of the solution is approximately 10 ml. Cool the solution, add 20 ml of sulfuric acid (4.9) and evaporate until fumes of sulfur trioxide appear. Just before fuming occurs, solids will begin to form and gentle heating is required to avo
45、id spurting. Once fuming begins the mixture becomes stable and may be fumed briefly at a higher temperature. Avoid overfuming, particularly with chromium-bearing alloys, as the chromium salts deposited are difficult to redissolve. Cool, add 20 ml of hydrochloric acid (4.8) and warm to redissolve the
46、 salts. Filter through a low ash, medium texture filter paper and wash with hot water. Wash with 10 ml of hydrochloric acid (4.7) and again with hot water. Retain the filtrate. 7.3.2 Treatment of insoluble residue Transfer the filter paper and residue to a crucible (5.1), dry and ignite at as low a
47、temperature as possible until all carbonaceous matter is removed and finally maintain at about 700 C for at least 15 min. Cool, add several drops of sulfuric acid (4.9) and 2 ml of hydrofluoric acid (4.6), evaporate to dryness and ignite at 700 C. NOTE 1For test portions containing tungsten proceed
48、as specified in clause 9. Fuse the residue with 1,0 g of potassium hydrogen sulfate (4.2) over a Bunsen burner and cool. Dissolve by heating with 10 ml of tartaric acid solution (4.10) and add to the original filtrate. Transfer to a 100 ml or 200 ml one-mark volumetric flask according to Table 1, di
49、lute to the mark with water and mix. 7.3.3 Colour development Transfer two aliquots according to Table 1 to separate 50 ml one-mark volumetric flasks, to prepare the test solution and the compensating solution. Make the following additions by means of burettes or pipettes, swirling after each addition. a) Test solution: iron solution (4.13) if required (see Table 1); reagent blank solution (4.14) if required (see Table 1); 2,0 ml of ammonium oxalate solution (4.12); 6,0 ml of hydrochloric acid (4.7)