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 ENISO10280:1995 has the status of a British Standard ICS 77.080BSENISO10280:1995 This British Standard, having been
2、prepared under the directionof the Iron and Steel Standards Policy Committee, waspublished under the authorityof the Standards Boardand comes into effect on 29November1991 BSI 03-2000 The following BSI references relate to the work on this standard: Committee reference ISM/18 Draft for comment 90/36
3、028 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 (ISM/-) to Technical Committee ISM/18, upon which the following bodies were represented: BICRA British Steel Industry Dep
4、artment of Trade and Industry (Laboratory of the Government Chemist) Ferro Alloys and Metals Producers Association Ministry of Defence Amendments issued since publication Amd. No. Date Comments 8697 December 1995 Indicated by a sideline in the marginBSENISO10280:1995 BSI 03-2000 i Contents Page Comm
5、ittees responsible Inside front cover National foreword ii Foreword 2 1 Scope 3 2 Normative references 3 3 Principle 3 4 Reagents 3 5 Apparatus 4 6 Sampling 4 7 Procedure 4 8 Expression of results 6 9 Special case 7 10 Test report 7 Annex A (informative) Additional information on the international c
6、ooperative tests 8 Annex B (informative) Graphical representation of precision data 9 Figure B.1 Logarithmic relationships between titanium content () and repeatability (r) and reproducibility (R and R w ) 9 Table 1 5 Table 2 5 Table 3 7 Table A.1 8 Publication(s) referred to Inside back cover w TiB
7、SENISO10280:1995 ii BSI 03-2000 National foreword This Subsection of BS6200 has been prepared under the direction of the Iron and Steel Standards Policy Committee. It supersedes BS6200-3.32.1:1986, which is withdrawn. It is identical with ISO10280:1991 “Steel and iron Determination of titanium conte
8、nt Diantipyrylmethane spectrophotometric method”, published by the International Organization for Standardization (ISO). In1995 the European Committee for Standardization (CEN) has accepted ISO10280:1991 as European Standard ENISO10280:1995. As a consequence of implementing the European Standard thi
9、s British Standard is renumbered as BSENISO10280 and any reference to BS6200-3.32.1 should be read as a reference to BSENISO10280. The Technical Committee has reviewed the provisions of ISO377-2, ISO385-1 and ISO648, to which reference is made in the text, and has decided that they are acceptable fo
10、r use in conjunction with this standard. Related British Standards for ISO377-2:1989, ISO385-1:1984 and ISO648:1977 are, respectively, BS 6200-2 “Sampling and sample preparation” Section2.1:1993 “Methods for iron and steel”, BS846:1985 “Specification for burettes” and BS1583:1986 “Specification for
11、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 obligations. Cross-references Inte
12、rnational Standard Corresponding British Standard ISO 1042:1983 BS 1792:1982 Specification for one-mark volumetric flasks (Identical) ISO 3696:1987 BS 3978:1987 Specification for water for laboratory use (Identical) ISO 5725:1986 BS 5497 Precision of test methods Part1:1987 Guide for the determinati
13、on 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, pagesi andii, theEN ISO title page, pages2 to10, an inside back cover and a back cover. This standard has been updat
14、ed (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 10280 September 1995 ICS 77.080 Descriptors: Steels, iron, cast iron, chemical analysis, determination of
15、 content, titanium, spectrometric method English version Steel and iron Determination of titanium content Diantipyrylmethane spectrophotometric method (ISO 10280:1991) Aciers et fontes Dosage du titane Mthodespectrophotomtrique au diantipyrylmthane (ISO10280:1991) Stahl und Eisen Bestimmung von Tita
16、n Photometrische Methode mit Diantipyrylmethan (ISO10280:1991) This European Standard was approved by CEN on1995-08-06. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without
17、 any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made
18、 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 versions. CEN members are the national standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy,
19、Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1995 Copyright reserved to CEN members Ref. No.
20、EN ISO 10280:1995 EENISO10280:1995 BSI 03-2000 2 Foreword The text of the International Standard from ISO/TC17, Steel, of the International Organization for Standardization (ISO) has been taken over as a European Standard by the Technical Committee ECISS/TC20, Methods of chemical analysis. This Euro
21、pean Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest byMarch1996, and conflicting national standards shall be withdrawn at the latest byMarch1996. According to the CEN/CENELEC Internal Regulations, the following c
22、ountries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom.ENISO10280:1995 BSI 03-2000 3 1 Scope This International Standard
23、 specifies a diantipyrylmethane spectrophotometric method for the determination of titanium in steel and iron. The method is applicable to titanium contents between0,002% (m/m) and0,80% (m/m). 2 Normative references The following standards contain provisions which, through reference in this text, co
24、nstitute 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 to investigate the possibility of applying the most recent editions
25、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 Part2:Samples for the determination of the chemical composition. ISO 385-1:1984, Laboratory g
26、lassware Burettes Part1: 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 Specification and test methods. ISO 5725:1986, Precision of test methods Determinati
27、on 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 sulfate. Formation of a yellow complex with4,4- diantipyrylmethane. Spectr
28、ophotometric measurement of the coloured complex at a wavelength of about385nm. 4 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only grade2 water as specified in ISO3696. 4.1 Iron, of high purity containing less than24g Ti/g. 4.2 Potassiu
29、m hydrogen sulfate (KHSO 4 ). 4.3 Sodium carbonate (Na 2 CO 3 ), anhydrous. 4.4 Hydrochloric acid, about1,19g/ml. 4.5 Nitric acid, about1,40g/ml. 4.6 Hydrofluoric acid, about1,15g/ml. 4.7 Hydrochloric acid, about1,19g/ml, diluted1+1. 4.8 Hydrochloric acid, about1,19g/ml, diluted1+3. 4.9 Sulfuric aci
30、d, about1,84g/ml, diluted1+1. 4.10 Tartaric acid solution, 100g/l. 4.11 Ascorbic acid solution, 100g/l. Prepare this solution immediately before use. 4.12 Ammonium oxalate solution Dissolve6g of ammonium oxalate monohydrate (COONH 4 ) 2 .H 2 O in water and dilute to200ml. 4.13 Iron solution, 12,5g/l
31、. Dissolve1,25g of iron (4.1) in10ml of hydrochloric acid (4.7) while heating gently. Add5ml of nitric acid (4.5) and boil until the volume of the solution is approximately10ml. Cool, transfer to a100ml one-mark volumetric flask, dilute to the mark with water and mix. 4.14 Reagent blank solution Pre
32、pare 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 in7.3.1 and7.3.2, diluting to100ml with water. 4.15 Diantipyrylmethane solution Dissolve4g of4,4-methylenebi
33、s(2,3-dimethyl-1- phenyl-5-pyrazolone) monohydrate, C 23 H 24 O 2 N 4 .H 2 O, (diantipyrylmethane) in20ml of hydrochloric acid (4.7) and dilute to100ml with water. 4.16 Titanium standard solution 4.16.1 Titanium stock solution, corresponding to1g of Ti per litre. Weigh, to the nearest0,0001g, 0,500g
34、 of high purity titanium metal purity 99,9% (m/m) and transfer to a300ml beaker. Add180ml of sulfuric acid, about1,84g/ml, diluted1+3, cover with a watchglass, heat gently until the metal has dissolved and oxidize with nitric acid (4.5) added drop by drop. Cool, transfer to a500ml one-mark volumetri
35、c flask, dilute to the mark with water and mix. 1 ml of this stock solution contains1,0mg of Ti.ENISO10280:1995 4 BSI 03-2000 4.16.2 Titanium standard solution, corresponding to50mg of Ti per litre. Transfer10,0ml or titanium stock solution (4.16.1) to a200ml one-mark volumetric flask. Dilute to the
36、 mark with water and mix. Prepare this solution immediately before use. 1 ml of this standard solution contains504g of Ti. 5 Apparatus All volumetric glassware shall be class A, in accordance with ISO385-1, ISO648 or ISO1042 as appropriate. Ordinary laboratory apparatus, and 5.1 Crucible, of platinu
37、m metal or platinum-gold alloy, of capacity30ml. 5.2 Spectrophotometer The spectrophotometer shall be equipped to measure absorbance at a wavelength of385nm. Wavelength measurement shall be accurate to2nm or less. In the absorbance range0,05 to0,85, absorbance measurements shall be repeatable to 0,0
38、03 or better. 6 Sampling Carry out sampling in accordance with ISO377-2 or appropriate national standards for steel and iron. 7 Procedure 7.1 Test portion Weigh, to the nearest0,000 5g, a test portion according to the presumed titanium content as follows: a) for titanium contents in the range0,002%
39、(m/m) to0,125% (m/m), a testportion of1,00g; b) for titanium contents in the range0,125% (m/m) to0,80% (m/m), a testportion of0,50g. 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 c
40、ell as in the determination, 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 a250ml beaker. Add20ml of hydrochloric acid (4.4), cover the beaker with a watchglass and digest at70 C to90 C un
41、til the solvent action ceases. Add5ml of nitric acid (4.5) and boil until the volume of the solution is approximately10ml. Cool the solution, add20ml 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
42、 required to avoid spurting. Once fuming begins the mixture becomes stable andmay be fumed briefly at a higher temperature. Avoid overfuming, particularly with chromium-bearing alloys, as the chromium salts deposited are difficult to redissolve. Cool, add20ml of hydrochloric acid (4.8) and warm to r
43、edissolve the salts. Filter through a low ash, medium texture filter paper and wash with hot water. Wash with10ml 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
44、 as low a temperature as possible until all carbonaceous matter is removed and finally maintain at about700 C for at least15min. Cool, add several drops of sulfuric acid(4.9) and2ml of hydrofluoric acid (4.6), evaporate to dryness and ignite at700 C. NOTE 1For test portions containing tungsten proce
45、ed as specified in clause9. Fuse the residue with1,0g of potassium hydrogen sulfate (4.2) over a Bunsen burner and cool. Dissolve by heating with10ml of tartaric acid solution (4.10) and add to the original filtrate. Transfer to a100ml or200ml one-mark volumetric flask according toTable 1, dilute to
46、 the mark with water and mix. 7.3.3 Colour development Transfer two aliquots according toTable 1 to separate50ml 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) Tes
47、t solution: iron solution (4.13) if required (seeTable 1); reagent blank solution (4.14) if required (seeTable 1); 2,0 ml of ammonium oxalate solution (4.12); 6,0 ml of hydrochloric acid (4.7); 8,0 ml of ascorbic acid solution (4.11), allow to stand for5min; 10,0 ml of diantipyrylmethane solution(4.
48、15). b) Compensating solution: iron solution (4.13) if required (seeTable 1); reagent blank solution (4.14) if required (seeTable 1); 2,0 ml of ammonium oxalate solution (4.12);ENISO10280:1995 BSI 03-2000 5 Table 1 Table 2 Titanium content Mass of test portion (m) Dilution volume of testsolution (7.
49、3.2) (V 0 ) Volume of aliquot (V 1 ) Volume of iron solution (4.13) added Volume of reagent blank solution (4.14) added Cell optical path length % (m/m) g ml ml ml ml cm 0,002 to 0,050 1,0 100 10,0 2 0,050 to 0,125 1,0 100 10,0 1 0,125 to 0,50 0,5 200 10,0 6,0 5,0 1 0,50 to 0,80 0,5 200 5,0 7,0 7,5 1 Titanium content Titanium standard solution (4.16.2) Concentration of titanium in the coloured calibration solutions Corresponding titanium content in the test portion % (m/m) ml 4g/ml %
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