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1、BRITISH STANDARD BS ISO 22963:2008 Titanium and titanium alloys Determination of oxygen Infrared method after fusion under inert gas ICS 77.120.50 ? Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Licensee=Boeing Co/5910770001 Not for Resale, 08/14/
2、2008 22:30:03 MDTNo reproduction or networking permitted without license from IHS -,-,- BS ISO 22963:2008 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 May 2008 BSI 2008 ISBN 978 0 580 57636 2 National foreword This British Standard is t
3、he UK implementation of ISO 22963:2008. 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
4、all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations. Amendments/corrigenda issued since publication DateComments Copyright British Standards Institution Provided by IHS under l
5、icense with BSI - Uncontrolled Copy Licensee=Boeing Co/5910770001 Not for Resale, 08/14/2008 22:30:03 MDTNo reproduction or networking permitted without license from IHS -,-,- Reference number ISO 22963:2008(E) INTERNATIONAL STANDARD ISO 22963 First edition 2008-01-15 Titanium and titanium alloys De
6、termination of oxygen Infrared method after fusion under inert gas Titane et alliages de titane Dosage de loxygne Mthode par infrarouge aprs fusion sous gaz inerte BS ISO 22963:2008 Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Licensee=Boeing Co/
7、5910770001 Not for Resale, 08/14/2008 22:30:03 MDTNo reproduction or networking permitted without license from IHS -,-,- ii Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Licensee=Boeing Co/5910770001 Not for Resale, 08/14/2008 22:30:03 MDTNo repro
8、duction or networking permitted without license from IHS -,-,- iii Contents Page Foreword iv 1 Scope . 1 2 Principle. 1 3 Reagents 1 4 Apparatus 2 5 Sample . 3 6 Procedure 3 7 Precision 6 BS ISO 22963:2008 Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled
9、Copy Licensee=Boeing Co/5910770001 Not for Resale, 08/14/2008 22:30:03 MDTNo reproduction or networking permitted without license from IHS -,-,- iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work o
10、f 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 and non-governmenta
11、l, 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, Part 2. The main
12、 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 casting a vote. Atte
13、ntion 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 22963 was prepared by Technical Committee ISO/TC 79, Light metal and their alloys, Subcommittee SC 11
14、, Titanium. BS ISO 22963:2008 Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Licensee=Boeing Co/5910770001 Not for Resale, 08/14/2008 22:30:03 MDTNo reproduction or networking permitted without license from IHS -,-,- 1 Titanium and titanium alloys
15、Determination of oxygen Infrared method after fusion under inert gas 1 Scope This International Standard specifies an infrared method after fusion under inert gas for the determination of the mass fraction of oxygen in titanium and titanium alloys. The method is applicable to titanium and titanium a
16、lloys with a mass fraction of oxygen in the range from 0,02 % to 0,4 %. 2 Principle The test portion, plus flux (platinum or nickel metal) is fused in a graphite crucible under an inert gas stream (He or Ar) using an impulse furnace. The released oxygen combines with carbon to form carbon monoxide.
17、Depending on the instrument design, the carbon monoxide is oxidized into carbon dioxide or left as carbon monoxide and swept by the inert gas stream into an infrared detector. Infrared absorption of the carbon monoxide or dioxide is measured, against a calibration curve made of titanium standard sam
18、ple. 3 Reagents 3.1 General During the analysis, unless otherwise stated, use only reagents of recognized analytical grade. 3.2 Magnesium perchlorate, Mg(ClO4) 2 (commercial designation: anhydrone) This is used in the instrument to absorb water. Use the purity specified by the instrument manufacture
19、r. 3.3 Sodium hydroxide on clay (commercial designation: ascarite) Used in some instruments to absorb carbon dioxide. Use purity specified by the instrument manufacturer. 3.4 Copper oxide Used in some instruments to oxidize carbon monoxide to carbon dioxide. Use the purity specified by the instrumen
20、t manufacturer. 3.5 Helium or argon Use the purity and type (He or Ar) specified by the instrument manufacturer. BS ISO 22963:2008 Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Licensee=Boeing Co/5910770001 Not for Resale, 08/14/2008 22:30:03 MDTN
21、o reproduction or networking permitted without license from IHS -,-,- 2 3.6 Nickel cleaning solution Mix 75 ml of acetic acid, 25 ml of nitric acid and 2 ml of hydrochloric acid. 3.7 Titanium cleaning solution 3.7.1 Titanium cleaning solution (A) Mix 100 ml of nitric acid (1+1) and 5 ml of hydrofluo
22、ric acid. 3.7.2 Titanium cleaning solution (B) Mix 90 ml of nitric acid (1+1) and 30 ml of hydrofluoric acid. 3.8 Acetone 3.9 Nickel Capsule, wire or baskets of minimum purity 99 % (mass fraction), with a mass fraction of oxygen less than 0,005 %. Nickel is immersed in the warm nickel cleaning solut
23、ion (3.6) for 30 s. Then rinse with water, ethanol, and acetone, each for 30 s, and store the nickel in acetone until used. Just before use, it should be dried with air. 3.10 Platinum Sheet (thickness 1 mm), wire ( 3 mm) or foil (thickness from 0,01 to 0,03 mm) of minimum purity 99 % (mass fraction)
24、 and the mass fraction of oxygen is less than 0,005 %. Platinum is washed with acetone and stored in a desiccator until used. 3.11 Titanium standard sample Select only titanium and titanium alloy standards. Select one containing approximately from 0,2 % to 0,35 % (mass fraction) oxygen. The accuracy
25、 of the test method is largely dependent upon the oxygen values assigned to the reference materials and upon the homogeneity of these materials. Thus, the titanium standard sample should be used with standard reference materials or certified reference materials. 4 Apparatus 4.1 Instrument. The instr
26、ument required for fusion of the test portion under an inert gas stream (He or Ar), using an impulse furnace and measurement of the carbon monoxide or dioxide extracted, may be obtained commercially from a number of manufacturers. 4.2 Graphite crucible, use high-purity crucibles suitable for the ins
27、trument. 4.3 Glass-wool filters. 4.4 Tweezer, made of solvent- and acid-resistant plastic (used during the sample preparation process). BS ISO 22963:2008 Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Licensee=Boeing Co/5910770001 Not for Resale, 0
28、8/14/2008 22:30:03 MDTNo reproduction or networking permitted without license from IHS -,-,- 3 5 Sample 5.1 Sampling The sampling procedure for titanium and titanium alloys shall be agreed upon until a corresponding standard method has been published. 5.2 Preparation of test portions The optimum tes
29、t portion is a pin (approximately 5 mm in diameter and nominally weighing from 0,06 g to 0,14 g) or a cube (of sides approximately 3 mm and nominally weighing from 0,06 g to 0,14 g). Cut off a test portion (from 0,08 g to 0,14 g) from the laboratory sample. The test portion shall be cut off by machi
30、ning, using no lubricating fluid and avoiding test-portion over-heating. Clean the sample surface in accordance with method a), b) or c). a) Method a) Leach the test portion in the titanium cleaning solution (3.7.1) at about 20 C until the surface is clean. This will normally require approximately 5
31、0 s. Immediately remove the reacting test portion with tweezers and rinse it twice with water and once with ethanol and acetone, and allow to air dry. This test portion should now weigh between 0,05 g and 0,13 g. The test portion should be reserved in a desiccator. b) Method b) Leach the test portio
32、n in the titanium cleaning solution (3.7.2) for 5 s from the start of a violent reaction of the test portion with the solution. Immediately remove the reacting test portion with tweezers and rinse it twice with water and once with ethanol and acetone, and allow to air dry. This test portion should n
33、ow weigh between 0,05 g and 0,13 g. The test portion should be reserved in a desiccator. c) Method c) File or cut off all outside edges, retaining only fresh surfaces, and finishing by rinsing with acetone and air drying. This test portion should now weigh between 0,05 g and 0,13 g. Weigh the test p
34、ortion to the nearest 0,1 mg. 6 Procedure 6.1 Number of determinations Carry out the determination at least in duplicate and, as far as possible, under repeatability conditions. 6.2 Preparation of instrument Assemble the apparatus as recommended by the manufacturer. Make the required power, gas and
35、water connections. Place a graphite crucible (4.2) on the furnace pedestal and then degas by heating above the degassing temperature of the sample. Continuously heat at the oxygen-extraction temperature and record the analyzer reading signal. Repeat this operation until the stable value of the analy
36、zer reading signal is obtained. Check that the glass-wool filters (4.3) are clean and change them as often as necessary. If the electricity supply has been switched off for a long time, allow the instrument to stabilize for the time recommended by manufacturer. BS ISO 22963:2008 Copyright British St
37、andards Institution Provided by IHS under license with BSI - Uncontrolled Copy Licensee=Boeing Co/5910770001 Not for Resale, 08/14/2008 22:30:03 MDTNo reproduction or networking permitted without license from IHS -,-,- 4 After changing the filter (4.3) and/or reagents (3.2, 3.3 and 3.4), or when the
38、 apparatus has been inoperative for a period, stabilize the instrument by carrying out trial analyses, the results of which are to be disregarded. Then proceed with blank, calibration and preparation tests as indicated in 6.3, 6.4, and 6.5 before analyzing the sample. NOTE The appropriate degas temp
39、erature of the sample and oxygen extraction temperature are determined by the manufacturers instruction. When using devices for a computer system preparation of a working curve, standardization (drift correction, normalization, recalibration) and measurement of the oxygen concentration shall be in a
40、ccordance with the operating manual for the devices computer system software. 6.3 Blank test Prior to the determination, carry out the following blank test in duplicate. Proceed as directed in 6.5 with the graphite crucible, and analyze the nickel or platinum (same kind of metal and same mass during
41、 sample analysis) without the test portion. Obtain the reading of the blank test. The mean value of the blank test must be sufficiently low when compared to the content to be determined in the test portion. If the blank values are abnormally high, investigate and eliminate the source of contaminatio
42、n. If the mean value of the blank is satisfactory, it may then be introduced into the blank subtraction device of the instrument. 6.4 Calibration Prior to the determination, carry out the following calibration. Proceed as directed in 6.5, using a titanium standard sample (3.11) instead of the test p
43、ortion. Subtract the mean of the blank value (6.3) from the analyzer reading signal. Repeat the process above several times. Calculate the intermediate oxygen equivalence factor ( f ) of the analyzer reading signal and calculate the oxygen equivalence factor (F) using Equations (1) and (2), ii fmS=
44、O/ (1) Iln= n i i f F n = = 1 (2) BS ISO 22963:2008 Copyright British Standards Institution Provided by IHS under license with BSI - Uncontrolled Copy Licensee=Boeing Co/5910770001 Not for Resale, 08/14/2008 22:30:03 MDTNo reproduction or networking permitted without license from IHS -,-,- 5 where F
45、 is the oxygen equivalence factor, expressed in mg, of the oxygen analyzer reading signal; f is the intermediate oxygen equivalence factor, expressed in mg, of the oxygen analyzer reading signal; mO is the mass of oxygen in the weighted titanium standard sample, expressed in mg (calculated in Equati
46、on (3); S is the intermediate analyzer reading signal after subtracting the mean value of the blank. NOTE 1 Calculate the mass of oxygen in the weighted titanium standard sample as follows: ()/mGP 3 O 10010 = (3) where mO is the mass of oxygen in the weighted titanium standard sample, expressed in m
47、g; G is the mass of titanium standard sample, expressed in g; P is the mass fraction of oxygen in the titanium standard sample, expressed in percent. NOTE 2 Refer to the manufacturers instructions for proper blanking procedures. 6.5 Procedure Assemble the apparatus, calibrate it, and test the perfor
48、mance as directed in 6.2, 6.3 and 6.4. Clean the electrode with a brush and vacuum cleaner before each determination. Wrap a test portion (5.2) in nickel (3.9) or platinum (3.10) and place it in the sample drop-port. NOTE The mass of nickel or platinum must exceed the mass of the test portion by at least a factor of ten. Place a graph