1、BRITISH STANDARDBS ISO 22960:2008Titanium and titanium alloys Determination of iron Molecular absorption spectrometry using 1, 10-phenanthrolineICS 77.120.50g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55
2、g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS ISO 22960:2008This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 May 2008 BSI 2008ISBN 978 0 580 57633 1National forewordThis British Standard is the UK implementation of ISO 22960:2
3、008.The UK participation in its preparation was entrusted to Technical Committee NFE/35, Light metals and their alloys.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 cont
4、ract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunity from legal obligations. Amendments/corrigenda issued since publicationDate CommentsReference numberISO 22960:2008(E)INTERNATIONAL STANDARD ISO22960First edition2008-01-15Titanium and tit
5、anium alloys Determination of iron Molecular absorption spectrometry using 1, 10-phenanthroline Titane et alliages de titane Dosage du fer Spectromtrie dabsorption molculaire par la 1,10-phnanthroline BS ISO 22960:2008ii iiiContents Page Foreword iv 1 Scope . 1 2 Normative references . 1 3 Principle
6、. 1 4 Reagents 1 5 Apparatus 2 6 Sample . 3 7 Procedure 3 8 Expression of results . 4 9 Precision 5 BS ISO 22960:2008iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International St
7、andards 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 and non-governmental, in liaison with ISO, also
8、 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, Part 2. The main task of technical committee
9、s 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 casting a vote. Attention is drawn to the possib
10、ility 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 22960 was prepared by Technical Committee ISO/TC 79, Light metals and their alloys, Subcommittee SC 11, Titanium. BS ISO 22960:20
11、081Titanium and titanium alloys Determination of iron Molecular absorption spectrometry using 1, 10-phenanthroline 1 Scope This International Standard specifies a molecular absorption spectrometric method using 1, 10-phenanthroline for the determination of the mass fraction of iron in titanium and t
12、itanium alloys. The method is applicable to titanium and titanium alloys with a mass fraction of iron in the range from 0,005 % to 2,0 %. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited app
13、lies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 384:1978, Laboratory glassware Principles of design and construction of volumetric glassware ISO 648:1), Laboratory glassware Single volume pipettes ISO 1042:1998, Laboratory glassware
14、 One-mark volumetric flasks ISO 3696:1987, Water for analytical laboratory use Specifications and test methods ISO 4787:1984, Laboratory glassware Volumetric glassware Methods for use and testing of capacity 3 Principle Dissolve the test portion in hydrochloric acid and hydrofluoric acid. Add nitric
15、 acid to oxidize titanium. Then add boric acid, tartaric acid, ammonium acetate and hydroxyl ammonium chloride. Add 1, 10-phenanthroline to make a 1,10-phenanthroline-iron complex. Determine the iron concentration in the test portion using a spectrophotometer. 4 Reagents 4.1 General During the analy
16、sis, use only reagents of recognized analytical grade and water that complies with grade 2 of ISO 3696. 1) To be published. (Revision of ISO 648:1977) BS ISO 22960:20082 4.2 Hydrochloric acid (1+1) Add slowly 500 ml of hydrochloric acid ( 201,16 g/ml to 1,19 g/ml) to 500 ml of water. 4.3 Nitric acid
17、 (1+1) Add slowly 500 ml of nitric acid ( 201,42 g/ml) to 500 ml of water. 4.4 Hydrofluoric acid (1+1) Add, carefully and slowly, 100 ml of hydrofluoric acid ( 201,14 g/ml) to 100 ml of water. 4.5 Boric acid 4.6 Tartaric acid solution (200 g/l) 4.7 Ammonium acetate solution (500 g/l) 4.8 Hydroxyl am
18、monium chloride solution (100 g/l) 4.9 1, 10-phenanthroline solution (100 g/l) Dissolve 2,4 g of 1,10-phenanthrolinium chloride monohydrate in 1 000 ml of water, or dissolve 2,0 g of 1,10-phenanthroline monohydrate in 100 ml of ethanol minimum purity 95 % (volume fraction) and dilute to 1 000 ml wit
19、h water. 4.10 Iron standard solution 4.10.1 Iron standard stock solution (0,500 mg Fe/ml) Weigh, to the nearest 0,1 mg, 0,500 g of iron metal minimum purity 99,9 % (mass fraction) into a 300 ml beaker, heat and decompose with 30 ml of hydrochloric acid (4.2). Add 5 ml of nitric acid (4.3) to oxidize
20、 iron and heat to evaporate nitrogen oxides. After cooling, transfer to a 1 000 ml volumetric flask, make up to the mark with water and mix. 4.10.2 Iron standard solution (0,050 mg Fe/ml) Pipette 10,00 ml of iron standard stock solution (4.10.1) to a 100 ml volumetric flask, make up to the mark with
21、 water and mix. Prepare this solution on the day of use. 5 Apparatus 5.1 General. Use normal laboratory apparatus. 5.2 Volumetric glassware, of class A complying with ISO 384, ISO 648 and ISO 1042. Use in accordance with ISO 4787. 5.3 Analytical balance, sensitive to 0,1 mg. 5.4 Spectrophotometer. B
22、S ISO 22960:200836 Sample 6.1 Sampling The sampling procedure for titanium and titanium alloys shall be agreed upon until a corresponding standard method has been published. 6.2 Test portion Extract a test portion from the test sample as specified in Table 1 and weigh to the nearest 0,1 mg. Table 1
23、Recommended test portion masses and aliquot volume taken in 7.4 Mass fraction of iron Mass of test portion Volume of aliquot taken in 7.4 c) % g ml W 0,005 0,1 1,0 20,0 W 0,1 0,4 1,0 10,0 W 0,4 0,8 0,50 10,0 W 0,8 u 2,0 0,20 10,0 7 Procedure 7.1 Number of determinations Carry out the determination a
24、t least in duplicate, as far as possible under repeatability conditions, on each sample. 7.2 Blank test Carry out a blank test in parallel with the analysis, using the same quantities of all reagents but omitting the test portion. 7.3 Preparation of working curve Pipette 0 ml, 2 ml, 4 ml, 6 ml and 8
25、 ml of iron standard solution (4.10.2) into five 100 ml volumetric flasks. Add 15 ml of tartaric acid solution (4.6), 25 ml of ammonium acetate solution (4.7) and 5 ml of hydroxyl ammonium chloride solution (4.8) to each volumetric flask. Dilute to about 80 ml with water and mix. Add 10 ml of 1,10-p
26、henanthroline solution (4.9) to each volumetric flask, make up to the mark with water and mix. After allowing to stand for about 20 min at room temperature, transfer a part of the solution into an absorption cell (10 mm), and measure the absorbance at a wavelength of 510 nm using water as a contrast
27、 solution. Prepare the curve showing the relation between the obtained absorbance and the iron concentration, in milligrams per 100 ml. Ensure that the graph achieves better than 0,999 correlation and is suitably linear. Prepare the working curve for a sample by parallel shifting of the relation cur
28、ve so as to let the curve pass the origin of the coordinate axes. BS ISO 22960:20084 7.4 Preparation of test solution for presentation to spectrophotometer Carry out the following steps. a) Transfer the test portion to a polyethylene beaker (200 ml). b) Add 10 ml of hydrochloric acid (4.2) and 5 ml
29、of hydrofluoric acid (4.4), cover with a polyethylene watch glass and heat gently on a water bath to decompose the test portion. Add 3 ml of nitric acid (4.3) and continue heating until nitrogen oxides evaporate. Then add 3 g of boric acid (4.5), stir to dissolve the boric acid and cool to room temp
30、erature. c) Transfer the solution into a 100 ml volumetric flask and make up to the mark with water. Pipette a test solution into two volumetric flasks (A and B) (specified volume in Table 1) according to the mass fractions of iron in the sample. d) Add 15 ml of tartaric acid solution (4.6), 25 ml o
31、f ammonium acetate solution (4.7) and 5 ml of hydroxyl ammonium chloride solution (4.8) to the volumetric flasks A and B. Dilute to about 80 ml with water and mix. e) Add 10 ml of 1,10-phenanthroline solution (4.9) to volumetric flask A, and make up to the mark with water. To the volumetric flask B,
32、 add water to make up to the mark and mix. 7.5 Determination of iron concentration After allowing to stand for about 20 min at room temperature, transfer a part of the solution into an absorption cell (10 mm), and measure the absorbance at a wavelength of 510 nm using the solution in flask B as the
33、contrast solution. Determine the iron concentration of the test solution from the working curve (7.3). 8 Expression of results The mass fraction of iron in the test portion, wFe, expressed as a percentage, is given by the following equation: wV=312Fe100 10m100(1) where 1is the concentration of iron
34、in the aliquot solution, expressed in mg/100 ml; 2is the concentration of iron in the blank solution, expressed in mg/100 ml; V is the volume of aliquot solution, expressed in ml; m is the mass of test portion, expressed in g. Calculate the mass fraction of iron in the test portion to the third deci
35、mal place. The difference in results of two parallel determinations of the mass fraction of iron in the same sample shall not be greater than the tolerance Equation (2), (3), or (4). If the difference exceeds the tolerance, the analysis shall be repeated. BS ISO 22960:200859 Precision The tolerance
36、of this analytical method is expressed by the following equations: Repeatability limit 2,8 0,005 5 (WFe) + 0,001 0 % (mass fraction) (2) Within-laboratory-reproducibility limit 2,8 0,008 3 (WFe) + 0,001 0 % (mass fraction) (3) Between-laboratory-reproducibility limit 2,8 0,023 3 (WFe) + 0,000 8 % (m
37、ass fraction) (4) BS ISO 22960:2008BS ISO 22960:2008BSI389 Chiswick High RoadLondonW4 4ALBSI British Standards InstitutionBSI is the independent national body responsible for preparing British Standards. It presents the UK view on standards in Europe and at the international level. It is incorporate
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