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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 1090 (2002): Compressed Hydrogen [CHD 6: Industrial Gases] “!ा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 1090:2002 Indian Standard COMPRESSED HYDROGEN —SPECIFICATION ( Third Revision) I ICS 71.100.20 I 1, I 0 BIS2002 1 BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG 1 NEW DELHI 110002 I i > ] September 2002 Price Group 1I f Industrial Gases Sectional Committee, CHD 6 FOREWORD This Indian Standard (Third Revision) was adopted bythe Bureau of Indian Standards, after the draft finalized by the Industrial Gases Sectional Committee had been approved by the Chemical Division Council. The second revision was prepared to upgrade the quality of the gas required by the Electric Lamp Industry by incorporating the limits of impurities, like carbon monoxide, hydrocarbons and oxides of nitrogen etc, which were not described earlier. This high purity hydrogen of 99.9 percent purtiy isalso used in the production of butane], octanol, polyurethane, polyamides, aniline and hydrogenation of fats and oils. Since the specification calls for high purity standards, the analysis demand instruments having high sensitivity and precision. Hence, the classical glass test sets, orsat apparatus, etc, have been discarded for high purity gas for which only instrumental methods involving electrochemical analyzer, gas chromatography,etc, have been prescribed. This third revision has been undertaken since ithas beennow technically possible toproduce still higher purity ~{~radcof 99,999 percent which finds itsuse inElectronic Industry, necessity hasbeen felt to revise the standard for incorporating the ultra pure grade of the hydrogen gas. Since this grade requires stricter control of impurities, analysis of impurities aredone with adifferent approach. 7’heimpurities are concentrated by absorption and determining by chromatography. The composition of the Committee responsible for formulation of this standard isgiven at Annex N. For the purpose of deciding whether aparticular requirement ofthis standard iscomplied with, the final value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with IS2: 1960‘Rules forrounding off numerical values (revised’. The number ofsignificant places retained inthe rounded off value should be the same asthat of the specified value inthis standard. .-$ ,. Is 1090:2002 Indian Standard COMPRESSED HYDROGEN — SPECIFICATION (Third l?evision) 1 SCOPE 5.2 For Grade 1and Grade 2 This standard prescribes therequirements andmethods The material shall aIsocomply with the requirements of sampling and test for compressed hydrogen. given in Table 1when tested in accordance with the methods prescribed in referred Annex. Instrumental 2 NORMATIVE REFERENCES methods as well as classical methods have been prescribed for determination of impurities in The following Indian Standards contain provisions which, through reference in this text, constitute compressed hydrogen. For Grade 1, instrumental provisions ofthis standard. Atthetime ofpublication, methods shall be employed. For Grade 2, classical the editions indicated were valid. All standards are methods, wherever specified, shall be adopted. subject to revisions, and parties to agreements based However, for routine analysis, instrumental methods on this standard are encouraged to investigate the may be adopted for Grade 2also. possibility of applying the most recent editions ofthe standards indicated below: Table 1Requirements for Compressed Hydrogen (Clause 5.2) IS No. Title 265:1993 Hydrochloric acid ~ourth revision) sl Characteristic Requirements Methodsof 266:1993 Sulphuric acid (third revision) 308:1988 Dissolved acetylene (gas) (third revision) 1260 Pictorial marking for handling and i)HydrogenPercent 99.98 99.6 A (Part 1): 1973 labelling ofgoods: Part 1Dangerous byvolume, &fin ii) Oxygen, ppm by 4 0.3 (percent B goods volume, MO-X byvolume) 4905:1968 Methods for random sampling iii) Nitrogen, ppm by 100 0.1 (percent c 7062:1973 Glossary of terms used in gas volume, MUX byvolume) iv) Water vapour, 4 50 D industry mg/m3, Ma v) Carbon dioxide, 5 25 E 3 TERMINOLOGY ppm by volume, Forthe purpose ofthis standard, thedefinitions given Max vi) Carbon monoxide, 1.0 10 F in IS7062 shall apply. ppm by volume, Max 4 GRADES vii) Mercury, mghf, Nil 0.2 G Mar The material shall be of the following three grades: viii) Hydrocarbons, ppm 1.0 — H byvolume, Max a) U[tra Pure Grade — Suitable foruseinsemi- conductor industry andforresearch purposes. b) Grade 1— Suitable for use in electric lamp 5.3 For Ultra Pure Grade industry, manufacture of butanol, octanol, Thematerial shallcomply withtherequirements given polyurethane, polyamides, aniline, hydroge- inTable2whentested inaccordance withthemethods nation of fats and oils and for determining prescribed inreferred Annex. reducibility of sinter, iron ore, etc. c) Grade 2 — Suitable for other purposes like 6PACKING cooling turbogenerator, gas welding, cutting The gas shall be supplied compressed in cylinders. of special steel, filling meteorological The design of cylinders, pressure of gas in cylinders, balloons, etc. andpacking andtransport shall be inaccordance with the Gas Cylinders Rules, 1940 of the Government of 5 REQUIREMENTS Indiawith suchmodifications asmaybe ordered from 5.1 Compressed hydrogen shall be a colourIess, time-to-time by the Chief Controller of Explosives, odourless gasandshallconsistessentiallyofhydrogen. Government of India, or other duly constituted authority. 1 Is 1090:2002 Table 2 Requirements for Compressed Hydrogen shall be in accordance with the Gas Cylinder (Clause 5.3) Rules, 1940withsuchmodifications asmaybe ordered from time-to-time by the Chief Controller of SI Characteristic ~Jltra Methodsof Explosives, Government of India or other duly No. Pure Test (Ref Grade toAnnex) constituted authority. The grade of the gas shall be i) Hydrogen percent by mass, 99.999 Efy stenciled on the cylinder. The cylinders shall also be volume, ktin difference marked with the appropriate symbol specified in ii) Oxygen, ppm by volume, 1.0 J IS 1260 (Part 1). Max iii) Nitrogen, ppm by volume, 2.0 J 7.1.1 The cylinders may also be marked with the 1 Max iv) Water vapour, mg/m~, Max 3.0 L Standard Mark. v) Carbon dioxide, ppm by 0.5 J volume, Max 7.1.1.1 The use of the Standard Mark isgoverned by vi) Carbon monoxide, ppm by 1.0 J theprovisions ofthe Bureau of Indian Standards ACI, volume, Max 1986andtheRules andRegulations made thereunder. vii) Mercury, mg/rn3,Max Nil K viii) Hydrocarbons, ppm by I.0 H The details of conditions under which the Iicence for volume, Max the use of the Standard Mark may be granted to ix) Solphrrr compound, Max 0.1 A-4 of manufacturers orproducers maybe obtained from the 1S308 Bureau of Indian Standards. ~) Argon Nil J 8 SAMPLING 7 MARKING Representative samples of gas shall be drawn and 7.1 The marking, painting and Iabelling of cylinders adjudged asprescribed inAnnex M. ,, ..”. ANNEX A [Table 1,S1 No. (i)] . . 3 DETERMINATION OF HYDROGEN A-1 METHODS c) Drying tube — U-form packed with phosphorus pentoxide; A-1.0 Two methods, namely, the gravimetric method and the volumetric method are prescribed. In case of d) Copper oxide tube — U-form filled with dispute, gravimetric method shallbeconsidered asthe granulated copper oxide; -- referee method. e) Electric furnace — with thermostatic attachment, capable of heating to 400°C. A-1.1 Gravimetric Method o Thermometer — capable of reading up to A known volume of the gas, after removal of carbon 400”C; and monoxide and oxygen isdried andpassed overheated copper oxide. The resulting water formed isabsorbed g) Absorption tube — U-form filled with t’ phosphorus pentoxide. in a phosphorus pentoxide tube and weighed. A-1.l.2 Reagents A-1. 1.1 Apparatus a) Mercury The apparatus shall consist of the following parts assembled as shown in Fig. 1. b) Copper oxide, granular — 600 to 500 microns a) Levelling bottle — of 200 ml capacity; c) Phosphorus pentoxide b) Burette — of 100 ml graduated into tenths of millilitres; d) Glasswool — long fibre 2 IS 1090:2002 4oo”c N2 — LEV??LLING BOTTLE =— TEMP 300°-4000C — — ~-=x:. —-——-. 0 --- LJ FIG. 1ASSEMBLYOFAPPARATUSFORTHEDETERMINATIOONFHYDROGEN(VOLUMETRICMETHOD) A-1. 1.3 Pt-ocedure P= atmospheric pressure in mm/Hg, and v= initial volume in ml of the gas (free from Collect asample ofthe gas freed from carbon dioxide carbon dioxide and oxygen). andoxygen intheburette overmercury. Levelcarefully and note the volume at atmospheric pressure and A-1.2 Volumetric Method temperature. Switch on the furnace, adjust the A known volume of the gas after removal of carbon temperature to 350+ 10”Cand pass acurrent ofpure dioxideandoxygenispassedoverheated copper oxide. nitrogen at the rate of 4 to 5 I/h through the drying The dimunition in volume indicates the volume of tube, copper oxide tube and absorption tube. After hydrogen in sample. sweeping the apparatus with nitrogen to remove any moisture in the copper oxide tube, remove the A-1.2.1 Apparatus absorption tube, allow it to cool and weigh. Replace The apparatus shall consist of the following parts the absorption tube inproper position and, by raising assembled as shown in Fig. 2. the levelling bottle, introduce the sampIe of the gas slowly into the stream of nitrogen running through a) Levelling bottle — of 200 ml capacity; the apparatus. After the introduction ofthe sample of b) Burette — of 100 ml, graduated into tenths the gas, continue the flow of nitrogen for another of millilitres; 15to 20 rein, and then remove the absorption tube, c) Copper oxide tube — U-form filled with cool itand weigh, granulated copper oxide (600–500 microns); A-1. 1.4 Calculation d) Electric furnace — with thermostatic attachment, capable ofheating to400”C; and Hydrogen, percent _ 346200 (273+t) (1–0.Ola) M byvolume – e) Pipette — Hempel type with three-way pxv stopcock. where A-1.2.2 Procedure t = atmospheric temperature in “C, Switch on the furnace and adjust to a temperature of a = percent oxygen by volume asdetermined about 350 + 1‘C. Put stopcoks A and B in position I in Annex B, (see Fig. 2) and pass acurrent of pure nitrogen atthe M = mass in g of water formed, rate of 4 to 5 MIfor 15min through the apparatus. 3 — i. Is 1090:2002 ‘ /--THERMOMETER f3URETTE~ \ LEVELLING BOTTLE .-----.-—- - LELECTRIC FURNACE --- 4 POSITION OF THREE-WAY STOP-COCKS 1 4 3+ L FIG.2 ASSEMBLYOFTHEAPPARATUSFORTHEDETERMINATIOONFHYDROGEN Turn stopcock B in position 2 and stopcock A in to themark onthepipette andclosestopcock A. Allow , position 3and adjust the level ofmercury tothe mark to cool and note the volume of the residue VIin the on the pipette. Close stopcock A. burette. PutstopcocksA andB inposition 1and switch off the furnace. Turn stopcock A to position 2 and raise the levelling bottle sothat the mercury just begins to issuefromthe A-1.2.3 Calculation outlet near stopcock A.Connect the hydrogen supply at the outlet and admix about 100 ml of the sample (100-a)(V -V,) Hydrogen,percent byvolume= freed from carbon dioxide, oxygen and carbon v monoxide inthe burette. Level carefully and note the where initial volume V. Then put stopcock A in position 3 andgradually transfer thesampleintothecopper oxide a = perentage of oxygen as determined in tube by raising the levelling bottle to the height of Annex B, stopcock A andrepeat theaboveoperation 3to4times. V = initial volume of the gas, and Finally, bring the mercury to the mark onthe pipette. ~ = final volume of the gas after reaction. Lift again to the height of stopcock Aand repeat the NOTE — No corrections for temperature and pressure we above operation 3to4times. Finallybringthemercury necessary, iftheseremain constantduringthetest. Is 1090:2002 ANNEX B [Table 1,S1’lVO(.ii)] DETERMINATION OF OXYGEN B-1 INSTRUMENTAL METHOD B-1.2 Classical Method B-1.1 General B-1.2.OTwomethodsaredescribed, namely,Method I and Method 2. Three methods have been prescribed, namely, the electrochemical analyzer, theoxygen analyzer andthe B-1.2.1 Method 1 gas chromatography. B-1.2.1.1 Principle B-1. 1.1 Electrochemical Analyzer Asampleofgasisbubbledthrough analkalinesolution Theoxygen inthetestgasreactswiththesilvercathode of pyrocatechol in complete absence of oxygen. The in the galvanic cell contained in the apparatus to colour developed inthe solution duetothe reaction of produce hydroxyl ions which oxidize metallic pyrocatechol withoxygen ;nthesamplegasismatched cadmium to cadmium hydroxide. This generates a with standard colour discs. current which flows inthe external circuit consisting B-1.2.1.2 Apparatus ofagalvanometersconnected acrosstheelectrodes.The magnitude of the current is a measure of the amount a) Theassembly ofapparatus shallbeasshown ofoxygen inthegas.Theprocedure tobefollowed for in Fig. 3, and the determination of oxygen content shall depend on b) Standard colour discs — available from the thetype ofanalyzer used. Manufacturers’ instructions supplters of scientific instruments. inthis regard shall be followed. B-1.2.1.3 Reagents B-1. 1.2 Oxygen Analyzer a) Pyracatechol solution — Bubbleoxygen-free Oxygen analyzer based on zirconium oxide sensing nitrogen from a tested certified cylinder element measures oxygen concentration innearly all through 1000 ml of distilled water, for half non-combustible gases and gas mixtures in all an hour, contained in the bottle D. Divide proportions. Itcombinestheadvanceofmicroprocessor the distilled water into two portions, one of technology with trusted cell design. This uses a 900 ml in bottle D, and the other of 100ml stabiIizedzirconium oxide tube, which when hot acts in a small conical flask. Keep both portions ------ as oxygen concentration cell providing an emf bubbling with oxygen-free nitrogen to the proportional to the oxygen according to the Nemst 900 ml of water in bottle D, add 7 g of equation. The procedure to be followed for the pyrocatechol, maintaining the nitrogen determination of oxygen content shall depend on the bubbling. To the 100 ml of water in the type of analyzer used. Manufacturer’s instructions in conical flask, add 6 gof ferrous ammonium this regard shall be followed. sulphate, 1 g of the zinc and 2 ml of concentrated sulphuric acid,stillmaintaining B-1.1.3 Gas Chromatography thenitrogen bubbling andwarm the solution Gas chromatography is a process of separation gently sothat abrisk evolution of hydrogen achieved bymeans of apartition between astationary occurs. Whenmost ofthezinchasdissolved, phase andamoving phase. Aiuitable synthetic zeolite add the solution quickly to the solution in and suitable detector are used in the gas bottle D, transferring the remaining zinc as chromatography. It should be capable to analyzing well. Attach bottle D quickly through the various impurities up to 1VPM (ppm by volume). coupling Mto the set where this solution as well asthat inbottle E iskept bubbling with B-1.1.3.1 Procedure oxygen-free nitrogen continuously toprevent Calibrate the instrument against calibration gas of the entry of atmospheric oxygen. After known composition by measuring the peaks or the leavingthereagents, thenitrogen will escape areas under various peaks of the chromatogram through K atmospheric pressure. following the instructions of the manufacturer. Carry b) Sodium @droxide solution — Take 500 mI out the test according to manufacturer’s instructions ofdistilledwaterinabeakerandbubble, fairly and compute the concentration of various impurities vigorously, oxygen-fkee nitrogen through it. bycomparing the peaks orthe areasunder peaks with Add 250 g of sodium hydroxide in smalI that of calibration gas. portions to the water while nitrogen is 5