इंटरनेट मानक Disclosure to Promote the Right To Information Whereas the Parliament of India has set out to provide a practical regime of right to information for citizens to secure access to information under the control of public authorities, in order to promote transparency and accountability in the working of every public authority, and whereas the attached publication of the Bureau of Indian Standards is of particular interest to the public, particularly disadvantaged communities and those engaged in the pursuit of education and knowledge, the attached public safety standard is made available to promote the timely dissemination of this information in an accurate manner to the public. “जान1 का अ+धकार, जी1 का अ+धकार” “प0रा1 को छोड न’ 5 तरफ” Mazdoor Kisan Shakti Sangathan Jawaharlal Nehru “The Right to Information, The Right to Live” “Step Out From the Old to the New” IS 228-22 (2003): Methods of Chemical Analysis of Steels, Part 22: Determination of Total Hydrogen in Steel by Thermal Conductivity Method (Hydrogen 0.1 ppm to 50 ppm) [MTD 4: Wrought Steel Products] “!ान $ एक न’ भारत का +नम-ण” Satyanarayan Gangaram Pitroda ““IInnvveenntt aa NNeeww IInnddiiaa UUssiinngg KKnnoowwlleeddggee”” “!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता हहहहै””ै” Bhartṛhari—Nītiśatakam “Knowledge is such a treasure which cannot be stolen” IS 228( Part 22 ) :2003 mT22mfh=mmn wfhR-lma~*4wm (m#Fi=romfh$hf@irh5$0m) Indian Standard METHODS OF CHEMICAL ANALYSIS OF STEELS PART 22 DETERMINATION OF TOTAL HYDROGEN IN STEEL BY THERMAL CONDUCTIVITY METHOD ( HYDROGEN 0.1 ppm TO 50 ppm ) lCS 77.080.20 0 BIS 2003 BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG NEW DELHI 110002 May 2003 Price Group 1 Methods of Chemical Analysis of Ferrous Metals Sectional Committee, MTD 2 FOREWORD This Indian Standard ( Part 22 ) was adopted by the Bureau of Indian Standards, after the draft finalized by the Methods of Chemical Analysis of Ferrous Metals Sectional Committee had been approved by the Metallurgical Engineering Division Council. IS228, which was first published in 1952 and subsequently revised in 1959, covered the chemical analysis of plain carbon and low alloy steels, alongwith pig iron and cast iron. It was revised again to make it comprehensive in respect of steel analysis and to exclude pig iron and cast iron which were being covered in separate standards. During its second revision the standard has been split up in several parts. This part covers the method for determination of total hydrogen in steel by thermal conductivity method. The other parts of this series are: (Partl ): 1987 Determination of carbon by volumetric method ( for carbon 50 percent ) ( third revision ) (Part 2): 1987 Determination of manganese in plain carbon and low alloy steels by arsenite method ( third revision ) (Part 3): 1987 Determination of phosphorus by alkali-metric method (third revision ) (Part 4): 1987 Determination of total carbon by gravimetric method (for carbon greater than or equal to 0.1 percent ) (third revision ) (Part 5):1987 Determination of nickel by dimethyl glyoxime (gravimetric )method (for nickel greater than or equal to 0.1 percent ) ( third revision ) (Part 6): 1987 Determination of chromium by persulphate oxidation method (for chromium greater than or equal to 0.1 percent ) (third revision ) (Part 7): 1990 Determinant ion of molybdenum by alphabenzoinoxime method (for molybdenum greater than 1percent ) ( third revision ) (Part 8): 1989 Determination of silicon by gravimetric method (for silicon 0.05 to 0.50 percent )(third revis ion ) (Part 9): 1989 Determination of sulphur in plain carbon steels by evolution method (for sulphur 0.01 to 0.25 percent ) ( third revision ) (Part O): 1989 Determination of molybdenum by thiocyanate ( photometric ) method in low and high alloy steels (for molybdenum 0.01 to 1.5 percent) (third revision) (Part 1):1990 Determination of total silicon by reduced molybdosilicate spectrophotometric method in carbon steels and low alloy steels ( for silicon 0.01 to 0.05 percent) ( third revision ) (Part 2): 1988 Determination of mangtmese by periodate spectrophotometric method in low and high alloy steels ( for manganese 0.01 to 2.0 percent ) (third revision ) (Part 13):1982 Determination of arsenic (Part 14):1988 Determination of carbon by thermal conductivity method ( for carbon 0.005 to 2.000 percent) (Part 15):1992 Determination of copper by thiosulphate iodide method (for copper 0.05 to 5percent ) (Part 16):1992 Determination of tungsten by spectrophotometric method ( for tungsten O.1 to 2 percent ) ( Continued on third cover) IS 228( Part 22 ): 2003 Indian Standard METHODS OF CHEMICAL ANALYSIS OF STEELS PART 22 DETERMINATION OF TOTAL HYDROGEN IN STEEL BY THERMAL CONDUCTIVITY METHOD ( HYDROGEN 0.1 ppm TO 50 ppm ) 1 SCOPE 5.4 Sodium Hydroxide on Asbestos ( Commonly known as Ascarite ) This standard ( Part 22 ) covers the determination of total ( diffusible and residual ) hydrogen in steel 5.5 Copper Turnings (0.1 ppmto 50 ppm ). 6 CALIBRATION 2 SAMPLING k} &Mih-a%nrdy&’%u%ru’ 2.1 The sample should be collected in a suitable 43, }. ql%yw,%wA”fc&li,-&’hm’nKmmmfL”a~k metal sampler as prescribed by the instrument instructions laid down by the manufacturer. manufacturer. 6.1.2 Use certified reference materials of the desired 2.2 Immerse the sampler in the molten metal for concentration range for calibration. 2 to 4s to allow the sample to be drawn into the inner 6.1.3 Weigh the sample and follow the calibration chamber. Excessive immersion time may cause procedure as laid down in the operation manual of misleading results. Immersion depth mustbeaminimum the instrument and establish the instrument response. of51 mm into the molten metal. 6.1.4 Verify the response of the instrument by 2.3 Immediately after removing the sampler from the analyzing a standard sample after calibration. The molten metal, plunge the end of the sampler into cold value should bewithin the allowable limits of certified water. Agitate it to hasten cooling. value of the standard. If not, repeat the calibration 3 PRINCIPLE and verification. NOTE— Repeat the calibration when the carrier gas In steel the total hydrogen is present in two supply has been changed or when the system has not forms as diffusible hydrogen and the residual been used for long time. hydrogen. The diffusible hydrogen is the hydrogen which diffuses out during the solidification of the 6.2 Calibration by Gas Dosing sample. This is contained within the sample tube. Some instruments have provision for calibration During the analysis for the diffusible hydrogen, by hydrogen gas dosing. Follow the procedure the sample tube is pierced and the diffused suggested by the manufacturer of the instrument for hydrogen is swept out with nitrogen and measured. calibration by analyzing acertified reference standard The residual hydrogen is the hydrogen which is sample. remaining after the solidification of sample. This hydrogen is released by heating the sample in a 7 ANALYSIS nitrogen atmosphere. Carbon dioxide and moisture 7.1 Analyze the samples collected using the released along with hydrogen are removed by patented sampler for diffusible and residual hydrogen suitable absorbent. Hydrogen is then measured by content. thermal conductivity method. 7.2 Diffusible Hydrogen 4 APPARATUS 7.2.1 Insert the sample tube into the pierc~ng unit Any commercial analyzer can be used consisting of of the instrument. The analysis cycle starts essentially furnace and a measurement unit. automatically. The diffused hydrogen contained in the sample tube is carried by the carrier gas to the 5 REAGENTS detector and displayed as diffused hydrogen. 5.1 Nitrogen Gas (Above 99.99 Percent Purity) 7.3 Residual Hydrogen 5.2 Hydrogen Gas (Above 99.99 Percent Purity) 7.3.1 After the completion ofthe diffusible hydrogen 5.3 Anhydrous Magnesium Perchlorate (Commonly analysis, take out the sample tube from the piercing known asAnhydrone ) unit and cut it to get out the pin sample, following IS 228( Part 22 ) :2003 the manufacturer’s recommendations. start the analysis. The sample isheated to atemperature of 1000”C to 1050”C ‘and the residual hydrogen NOTE —Theresidual hydrogen isdetermined byheating liberated is carried by the carrier gas and measured. the samole in a furnace in nitrozen atmosr)here. The furnace;ormally isatubularfurnac; capableif generating atemperature of 11OO°C.Itshallbeprovidedwithproper 8 REPRODUCIBILITY temperature measurement and control devices. 7.3.2 Weigh the pin sample and enter the weight in The reproducibility/precision of,analysis should be the system. Put the sample in the reaction tube and within * 10percent. 2 ( Continuedfrom second cover) (Part 17):1998 Determination of nitrogen by thermal conductivity method (Part 18):1998 Determination of oxygen by instrumental method (Part 19):1998 Determination of nitrogen by steam distillation (Part 20):1987 Determination of carbon and sulphur by infra-red absorption method (Part21 ): 1987 Determination of copper by spectrometric method ( for copper 0.02 to 0.5 percent ) ( third revision) (Part 23 ): 2003 Determination of nitrogen in steel by optical emission spectrometer (nitrogen 0.002 to 1.0 percent ) (Part 24 ): 2003 Determination of nitrogen in steel by inert gas fusion — Thermal conductivity method (nitrogen 0.001 to 0.2 percent) In reporting the result of a test or analysis made in accordance with this standard, if the final value, observed or calculated, isto be rounded off, it shall be done in accordance with IS 2: 1960 ‘Rules for rounding off numerical values (revised )’. 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