IS 1090 (2002): Compressed Hydrogen [CHD 6: Industrial Gases]

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.

“जान का अधकार, जी का अधकार” “परा को छोड न तरफ” Mazdoor Kisan Shakti Sangathan Jawaharlal Nehru “The Right to Information, The Right to Live” “Step Out From the Old to the New”

“ान एक न भारत का नमण” Satyanarayan Gangaram Pitroda “Invent a New India Using Knowledge”

“ान एक ऐसा खजाना जो कभी चराया नह जा सकताह ै”ै 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

0 BIS 2002 BUREAU OF INDIAN STANDARDS 1 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 by the 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 is also 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 it has been now technically possible to produce still higher purity ~{~radcof 99,999 percent which finds its use in Electronic Industry, necessity has been 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 are done with a different approach. 7’he impurities are concentrated by absorption and determining by chromatography. The composition of the Committee responsible for formulation of this standard is given at Annex N. For the purpose of deciding whether a particular requirement of this standard is complied with, the final value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with IS 2: 1960 ‘Rules for rounding off numerical values (revised’. The number of significant places retained in the rounded off value should be the same as that of the specified value in this standard.

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Is 1090:2002 Indian Standard COMPRESSED HYDROGEN — SPECIFICATION (Third l?evision)

1 SCOPE 5.2 For Grade 1 and Grade 2 This standard prescribes the requirements and methods The material shall aIso comply with the requirements of sampling and test for compressed hydrogen. given in Table 1 when tested in accordance with the methods prescribed in referred Annex. Instrumental 2 NORMATIVE REFERENCES methods as well as classical methods have been The following Indian Standards contain provisions prescribed for determination of impurities in which, through reference in this text, constitute compressed hydrogen. For Grade 1, instrumental provisions of this standard. At the time of publication, 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 2 also. possibility of applying the most recent editions of the standards indicated below: Table 1 Requirements for Compressed Hydrogen (Clause 5.2) IS No. Title 265:1993 Hydrochloric acid ~ourth revision) sl Characteristic Requirements Methods of 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 of goods: Part 1Dangerous by volume, &fin ii) Oxygen, ppm by 4 0.3 (percent B goods volume, MO-X by volume) 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 by volume) iv) Water vapour, 4 50 D industry mg/m3, Ma v) Carbon dioxide, 5 25 E 3 TERMINOLOGY ppm by volume, Max For the purpose of this standard, the definitions given vi) Carbon monoxide, 1.0 10 F in IS 7062 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 by volume, Max a) U[tra Pure Grade — Suitable for use in semi- conductor industry and for research purposes. b) Grade 1 — Suitable for use in electric lamp 5.3 For Ultra Pure Grade industry, manufacture of butanol, octanol, The material shall comply with the requirements given polyurethane, polyamides, aniline, hydroge- in Table 2 when tested in accordance with the methods nation of fats and oils and for determining prescribed in referred Annex. reducibility of sinter, iron ore, etc. c) Grade 2 — Suitable for other purposes like 6 PACKING 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. and packing and transport shall be in accordance with the Gas Cylinders Rules, 1940 of the Government of 5 REQUIREMENTS India with such modifications as maybe ordered from 5.1 Compressed hydrogen shall be a colourIess, time-to-time by the Chief Controller of Explosives, odourless gas and shall consist essentially of hydrogen. 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, 1940 with such modifications as maybe ordered from time-to-time by the Chief Controller of SI Characteristic ~Jltra Methods of No. Pure Test (Ref Explosives, Government of India or other duly Grade to Annex) 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 Max IS 1260 (Part 1). iii) Nitrogen, ppm by volume, 2.0 J 7.1.1 1 Max The cylinders may also be marked with the 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 is governed by vi) Carbon monoxide, ppm by 1.0 J the provisions of the Bureau of Indian Standards ACI, volume, Max 1986 and the Rules and Regulations 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 or producers maybe obtained from the 1S 308 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 as prescribed in Annex 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 shall be considered as the 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 is dried and passed over heated Absorption tube — U-form filled with copper oxide. The resulting water formed is absorbed g) t’ in a phosphorus pentoxide tube and weighed. phosphorus pentoxide. A-1.l.2 Reagents A-1. 1.1 Apparatus The apparatus shall consist of the following parts a) Mercury 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) Glass wool — long fibre

2 IS 1090:2002

4oo”c

N2 —

LEV??LLING BOTTLE = — TEMP 300°-4000C — —

~-=x:. -—- ——. 0 --- LJ

FIG. 1 ASSEMBLYOFAPPARATUSFORTHEDETERMINATIONOF HYDROGEN(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 a sample of the gas freed from carbon dioxide and oxygen in the burette over mercury. Level carefully carbon dioxide and oxygen). 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”C and pass a current of pure dioxide and oxygen is passed overheated 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 in proper 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 of the sample of b) Burette — of 100 ml, graduated into tenths the gas, continue the flow of nitrogen for another of millilitres; 15 to 20 rein, and then remove the absorption tube, c) Copper oxide tube — U-form filled with cool it and weigh, granulated copper oxide (600 –500 microns); A-1. 1.4 Calculation d) Electric furnace — with thermostatic attachment, capable of heating to 400”C; and Hydrogen, percent _ 346200 (273 +t) (1–0.Ola) M by volume – 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 as determined about 350 + 1‘C. Put stopcoks A and B in position I in Annex B, (see Fig. 2) and pass a current of pure nitrogen at the M = mass in g of water formed, rate of 4 to 5 MI for 15 min 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 ASSEMBLYOFTHEAPPARATUSFORTHEDETERMINATIONOF HYDROGEN

Turn stopcock B in position 2 and stopcock A in to the mark on the pipette and close stopcock A. Allow , position 3 and adjust the level of mercury to the mark to cool and note the volume of the residue VIin the on the pipette. Close stopcock A. burette. Put stopcocks A and B in position 1 and switch off the furnace. Turn stopcock A to position 2 and raise the levelling bottle so that the mercury just begins to issue from the 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 by volume= freed from carbon dioxide, oxygen and carbon v monoxide in the burette. Level carefully and note the initial volume V. Then put stopcock A in position 3 where and gradually transfer the sample into the copper oxide a = perentage of oxygen as determined in tube by raising the levelling bottle to the height of Annex B, stopcock A and repeat the above operation 3 to 4 times. V = initial volume of the gas, and Finally, bring the mercury to the mark on the pipette. ~ = final volume of the gas after reaction. Lift again to the height of stopcock A and repeat the NOTE — No corrections for temperature and pressure we above operation 3 to 4 times. Finally bring the mercury necessary, if these remain constant during the test.

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.O Two methods are described, namely, Method I and Method 2. Three methods have been prescribed, namely, the electrochemical analyzer, the oxygen analyzer and the B-1.2.1 Method 1 gas chromatography. B-1.2.1.1 Principle B-1. 1.1 Electrochemical Analyzer A sample of gas is bubbled through an alkaline solution The oxygen in the test gas reacts with the silver cathode of pyrocatechol in complete absence of oxygen. The in the galvanic cell contained in the apparatus to colour developed in the solution due to the reaction of produce hydroxyl ions which oxidize metallic pyrocatechol with oxygen ;n the sample gas is matched cadmium to cadmium hydroxide. This generates a with standard colour discs. current which flows in the external circuit consisting B-1 .2.1.2 Apparatus of a galvanometersconnected across the electrodes. The magnitude of the current is a measure of the amount a) The assembly of apparatus shall be as shown of oxygen in the gas. The procedure to be followed for in Fig. 3, and the determination of oxygen content shall depend on b) Standard colour discs — available from the the type of analyzer used. Manufacturers’ instructions supplters of scientific instruments. in this regard shall be followed. B-1.2.1.3 Reagents B-1. 1.2 Oxygen Analyzer a) Pyracatechol solution — Bubble oxygen-free Oxygen analyzer based on zirconium oxide sensing nitrogen from a tested certified cylinder element measures oxygen concentration in nearly 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. It combines the advance of microprocessor 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 100 ml stabiIized zirconium 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 g of ferrous ammonium this regard shall be followed. sulphate, 1 g of the zinc and 2 ml of concentrated sulphuric acid, still maintaining B-1. 1.3 Gas Chromatography the nitrogen bubbling and warm the solution Gas chromatography is a process of separation gently so that a brisk evolution of hydrogen achieved by means of a partition between a stationary occurs. When most of the zinc has dissolved, phase and a moving phase. A iuitable 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 1 VPM (ppm by volume). coupling M to the set where this solution as well as that in bottle E is kept bubbling with B-1. 1.3.1 Procedure oxygen-free nitrogen continuously to prevent Calibrate the instrument against calibration gas of the entry of atmospheric oxygen. After known composition by measuring the peaks or the leaving the reagents, the nitrogen 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 of distilled water in a beaker and bubble, fairly and compute the concentration of various impurities vigorously, oxygen-fkee nitrogen through it. by comparing the peaks or the areas under peaks with Add 250 g of sodium hydroxide in smal I that of calibration gas. portions to the water while nitrogen is

5 Is 1090:2002

ill

& //

LWASTE ZpvROCATECHOL ‘NoOH SOLUTION ‘Hg

FIG. 3 DIAGRAMMATICLAYOUTOFTHEAPPARATUSFORTHEDETERMINATIONOFOXYGENBY PYROCATECHOL . _-

bubbled through. When the solution is cool, P and allow the gas to pass to the atmosphere through !. > pour it into the bottle E and attach to the set tap R. There should always be a slight excess of gas through the coupling M. bubbling through the mercury in F. Allow the gas to pass until C is thoroughly washed out. By turning taps B-1.2.1.4 Procedure N and Q, force sodium hydroxide solution into C to

Turn taps Q and N off so that liquid does not rise into the 1 ml mark. Turn the tap N to connect C to the C. Turn K so that nitrogen bubbles through mercury pyrocatechol reservoir and force the solution into C to the 10 ml mark. Shut taps Q and N. If the solution in in order to obtain pressure in D and E. Pour water . . into S with tap R open to the atmosphere until water C is only slightly coloured, it is ready for test, but if level isjust below tap R. Half fill bubbler G with water. there is appreciable colour, run it carefully to waste Fill the bubbler L to height of 62 mm with mercury. bottle Jby closing tap P, and opening tap Q to waste. Run mercury into reservoir T and raise T until the Refill C to the 10 ml mark as indicated above. If the mercury reaches the fixed mark on F. ‘I%is height of solution is still appreciably coloured, the process shall mercury gives a speed of approximately 15 ml/min. be repeated until an almost colorless solution is Connect the cylinder or gas supply to be tested to A by obtained. means of a flow adjustment valve and glass or copper Match the colour of the solution in C as quickly as tubing, any connections being made with rubber possible with a suitable standard on the colour disc pressure tubing and as short as possible. Turn B so using the matching plate and turn tap R immediately that the gas from the cylinder will pass to the so that the gas passes into the measuring burette H. atmosphere and carefully open the cylinder valve and When 100 or 200 ml of gas have passed in, rematch C flow adjustment valves. When the connections have against suitable standard. If the gas contains been thoroughly blown out with gas, reduce the rate appreciable quantity of oxygen, it may only be of flow to about 2.5 l/h and turn B so that the gas necessary to use 100 ml of gas to obtain a suitable passes into C through the sintered disc. Open the tap colour change. 6 —A

Is 1090:2002

NOTES charged bottle A with the solutions, fill t The set does not function satisfactorily with oxygen measuring burette C with water by raising concentrations above 50 ppm. Ievelling bottle D, closing one-way tap G and 2 The rate of flow should be approximately 15 ml/min, and this turning three-way tap F, to position 2. When should be checked during a test by noting the time for 200 ml of gas to collect in H. If there is any appreciable deviation from this the water in the burette reaches the zero mark, rate, mercury in Fshould be raised or lowered until the correct turn three-way tap Fto position 1and replace speed is obtained. bottle D in set. 3 The set will function satisfactorily at a temperature of 15 to 20”C. Above this temperature, the ‘blanks’ are likely to be high. NOTE — The burette C shall be capable of measuring k) ;in accuracy of O.05 ml. 4 If after a test the increase in colour of the solution in C is very i slight, further test may be carried out using the same solution. b) Open one-way tap G and lower bottle D to 5 After shutting off F’, refilling H with water, and turning B to draw the liquid into absorption pipette B from connect the gas supply to the atmosphere, the test cylinder shall be removed, the next cylinder connected and the procedure given bottle A. When burette C becomes full of gas, in B-1.2 .1.4 repeated. close one-way tap G and turn three-way tap 6 When the set is not in use, C shall always be empty and isolated Fto position 2 and raise bottle D until burette from the atmosphere and the gas pressure in D and E released by C is full of water again. Turn three-way tap turning K sothat the nitrogen bubbles through the reagents direct F to position 1 and repeat the foregoing to the atmosphere, operations until the level of the solution B-1.2. 1.5 Calculation reaches mark L. Perfect control of the level B–AX, OO may be obtained by raising or lowering bottle Oxygen, ppm . — D SIOWIY. v c) Close tap G and finally expel any gas from where burette C and turn tap F to position 1. B = figure on colour standard used after pass- d) Connect the supply of gas to inlet a of three- ing the gas sample; way tap F, the tap being in position 1, purge A = figure on colour standard used before pass- the inlet tube a with the sample and then turn ing the gas sample; and tap F to position 2. Bring the level of water V = volume of gas passed, that is 100or200 ml. in bottle D in line with graduation mark 100 NOTE — A figure ‘ 8’ on colourstandarddenotes0.0008mlof on burette C. Turn tap to position 3 and raise oxygen. Thus, if 100 ml test gas causes a change from figure ’8’ water bottle D to expel all the gas to to figure ‘12’. atmosphere. Again turn tap F to position 2 ----- and lower water bottle D in line with (12-8) xIW=4 Therefore, ppm, of oxygen in gas= graduation mark 100 on burette C. Repeat 100 this process of purging burette C and the B-1.2.2 Method 2 (Absorption in Pyrogallol Solution) manifold connections up to G and F once again. B-1.2.2. 1 Apparatus e) Turn tap F’to position 1 again. Allow water The assembly of apparatus shall be as shown in Fig. 4. to drain down the sides of burette C and read the volume keeping water level same in B-1.2.2.2 Reagents burette C and bottle D. Open tap G and raise a) Pyrogal/ol solution — Dissolve 350 g of bottle D until burette C is just full of water. pyrogallol in 1000 ml of water. Keep the Close tap G, replace bottle D in set and leave stock solution in amber coloured bottles. gas to be tested in absorption pipette B for a b) Potassium hydroxide solution — Dissolve few minutes so that active contaminants are 1000 g of potassium hydroxide in 1000 ml absorbed from it. of water. o Open tap G and lower bottle D until the level NOTE — Alkali purified by alcohol should not be used since of the solution again reaches mark L. To solutions evolve some carbon monoxide. ensure complete absorption, raise the bottle again until burette C is full of water, close B-1.2.2.3 Procedure tap G, replace bottle D is set for another few a) Pour 140 ml of pyrogallol solution and minutes. Open tap G and lower bottle D unt i I 100 ml of potassium hydroxide solution into the level of the solution again reaches mar+ Woulfes bottle A through its opening J. L. Close tap G and finally allow water to drain Immediately after introducing the solutions, in the burette C and read the volume of gas, close the opening with rubber bung and shake keeping the water level same in burette C and the bottle to mix the solutions. Having bottle D.

7 Is 1090:2002

-fi= o = 5-: :-=------=-= ------WATER LEVEL IN -- 10 : JACKET L i% 20 -

-1- 1--1

WATER JACKET /B Ew-

: 80 90 -- I -- GLASS --: TUBE PACKING z-- E D -. — / ..

99 ---- =-—.=_..-———=————=—___=_=_=_)0 .--—--—-—--:e-——__-- RUBBER BAG CONTAINING .---—_.—__‘Br NITROGEN TECHNICAL -_ WATER -- L 7 U

. c m,.. (=y==y=fl-o . a b INLET a b INLET a b POSITION 1 OF F POSITION 2 OF F POSITION 3 OF F

FIG. 4 ASSEMBLYOFAPPARATUSFORTHEDETERMINATIONOF OXYGENBY PYROGALLOL

Is 1090:2002

g) Repeat the steps outlined in (e) and (~ until where two consecutive readings agree. V = initial volume of gas [see B-1.2.2.3(a)l. B-1.2.2.4 Calculation and V] = volume of gas after absorption ::ng’i:”ty active=(Ml - M,) ~~ [see B-1.2.2.3(g)] ~ v, percent by vo~ume

ANNEX C

[Table 1, SINO. (iii)]

DETERMINATION OF NITROGEN

C-1 INSTRUMENTAL METHOD C-1.2 For Grade 2

C-1.l Gas Chromatograph Method The concentration of nitrogen shall be obtained from difference of the amount of hydrogen and impurities. C-1. 1.1 Procedure namely oxygen and nitrogen. Nitrogen shall be determined by gas chromatography as prescribed in B-1.1.3.

ANNEX D ----

[Table 1, SINO. (iv)]

DETERMINATION OF WATER VAPOUR

D-1 METHODS dew or frost is formed from the moisture content of the gas at a particular pressure which maybe observed D-I.O General optically in the apparatus. The temperature at which Three methods have been prescribed, namely the dew or frost is formed is a measure of moisure electrolytic hygrometers, frost or dew point hygrometer content of the gas. The procedure to be followed for and capacitance hygrometer. determining the moisture content shall depend upon the type of the apparatus to be used. The manufacturer’s D-1. 1 Electrolytic Hygrometer instructions in this regard shall be followed. The instrument is based on the absorption and electrolysis of the water vapour present in the sample D-1.3 Capacitance Hygrometer gas. The electrolysis current gives a direct measurement of water vapour present in the gas The instrument is based on the change of capacitance flowing through the instrument at a steady rate. The of the sensor when a sample gas containing water procedure to be followed for determining the moisture vapour passes through it. The change in capacitance content shall depend on the type of apparatus to be gives a direct measurement of water vapour present used. The manufacturer’s instructions in this regard in the gas. The procedure to be followed for shall be followed. determining the moisture content shall depend upon the type of the apparatus to be used. The D-1.2 Frost or Dew Point Hygrometer manufacturer’s instructions in this regard shal I be A metal surface on the hygrometer is cooled so that followed.

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ANNEX E

[Table 1, S1No. (v)]

DETERMINATION OF CARBON DIOXIDE

E-1 INSTRUMENTAL METHOD E-2.3.2 Phenolphthalein Indicator Dissolve 0.50 g of phenolphthalein in 100 ml of E-1. 1 General rectified spirit. Three methods have been prescribed, namely, infra- i E-2.3.3 Barium Hydroxide Solution red analyzer, electrochemical method and the gas chromatography method. Dissolve about 4 g of barium hydroxide in 2000 ml of water in large flask. Close the flask and shake until E-1. 1.1 Infra-Red Analper the crystals have completely disappeared and a light lnfra-red analyzers are used for determining impurities insoluble powder remains. Allow the solution to stand of hetroatomic gases. The hetroatomic gases absorb for two days or until the barium carbonate has energy at characteristic wavelengths when subjected completely settled; siphon it into a bottle through to infra-red radiation. The procedure to be followed which current air (free from carbon dioxide) has been for determining the impurities contents shall depend passed for 2 h previously. Assemble this bottle with a on the type of apparatus to be used. The manufacturer’s soda-lime tube and a burette. instructions in this regard shall be followed. E-2.4 Procedure E-1. 1.2 Electrochemical Method Take 25 ml of barium hydroxide solution in each When a gas containing carbon dioxide is passed absorber, R, and R, and add carbon dioxide-free water through a reactivated liquid, the electrical conductivity to about half thei~ height. Pass the gas through the of the liquid changes depending upon the carbon spiral absorbers at the rate of about 5 I/h. Measure the dioxide content. The measurement of the change in rate of flow of the gas by suitable flowmeter and record electrical conductivity gives a direct measurement of the temperature and atmospheric pressure at regular carbon dioxide. The procedures to be followed for intervals. Pass 30 I of gas keeping temperature and determining carbon dioxide shall depend upon the type pressure of the gas constant. Titrate individual Iy the of apparatus to be used. The manufacturer’s baryta solution in both the absorbers with standard instructions in this regard shall be followed. hydrochloric acid using phenolphthalein indicator and #-- E-1. 1.3 Gas Chromatography find out the total volume of standard hydrochloric acid used in the two titrations. The procedure shall be the same as prescribed under B-1.1.3. E-2.4. 1 Carry out a blank titration with an equal volume of barium hydroxide solution used in the two E-2 CLASSICAL METHOD absorbers.

E-2.1 Principle E-2.5 Calculation

A known volume of the gas is passed through barium Carbon dioxide, 1039 (~– V2)(273–t)N hydroxide solution and the amount of carbon dioxide ppm by volume = absorbed is determined from the amount of barium P hydroxide solution neutralized. where p’, = volume in ml of standard hydrochloric acid E-2.2 Apparatus used for the blank titration of barium The apparatus consists of two spiral absorbers RI and hydroxide solution R, being provided with soda-lime tube as shown in v, = volume in ml of standard hydrochloric acid F:g. 5. used for titrations, average temperature in ‘C. E-2.3 Reagents normality of the standard hydroch Ioric E-2.3.1 Standard Hydrochloric Acid (see 1S 265) acid, and Approximately 0.02 N. P= average pressure in mm Hg.

10 Is 1090:2002

354 t- u u

-7 -.1-

45— r 100 / R, -/ r SODA-LIME

5COMPLETE COILS 7mm DlA TUBE (APPROX) / t @l TD2JET~ 40

L-1 —50-r-

All dimensions in millimetres.

FIG. 5 SPIRALABSORBERSFORTHEDETERMINATIONOF CARBONDIOXIDE

ANNEX F

[Table 1, S1IVO.(vi)]

DETERMINATION OF CARBON MONOXIDE

F-1 INSTRUMENTAL METHOD F-1.1 Gas Chromatography

F-1.0 Three methods have been prescribed, namely, The procedure for carrying out the determination shal I the gas chromatography method, infra-red analyzer be the same as prescribed in B-1.1.3. and the electrochemical method.

11 Is 1090:2002

F-1.2 Infra-Red Analyzer concentrated sulphuric acid. The procedure for carrying out the determination shall F-2.2.5 U-tube — one (F) be the same as prescribed in E-1.1.1. Containing iodine pentoxide.

F-1.3 Electrochemical Method F-2.2.6 Hot Bath (G) The procedure for carrying out the determination shall Either air or oil electrically heated. be the same as prescribed in E-1.1.2 after converting carbon monoxide into carbon dioxide by using suitable F-2.2.7 Thermometer (H) converter, such as, iodine pentoxide. Reading up to 200”C, graduated to 0.5”C.

F-2 CLASSICAL METHOD F-2.2.8 Absorber (J

F-2.1 Method Containing potassium iodine solution. A known volume of the gas is passed through hot F-2.2,9 Carbon Dioxide Absorbers (K) iodine pentoxide. Any carbon monoxide present is thus Two each containing baryta solution and fitted with oxidized to carbon dioxide which is estimated by burette containing standard hydrochloric acid. absorption in baryta solution. F-2.3 Reagents F-2.2 Apparatus F-2.3.1 Standard Hydrochloric Acid (see 1S 266) The apparatus shall consist of the following components assembled as shown in Fig. 6. Approximately 0.02 N.

F-2.2.1 A4ercuty Filled Bye-pass Safe~ Valve (A) F-2.3.2 Bmyta Solution

F-2.2.2 Gas Scrubbers (B) Dissolve about 4 g of barium hydroxidein2000 ml of water in a large flask. Close the flask and shake until Containing 40 percent potassium hydroxide solution. crystals have completely disappeared and a light. F-2.2.3 Gas Bubblers — one (C) insoluble powder of barium carbonate remains. Allow the solution to stand for 2 days, until the barium Containing saturated solution of chromic acid in carbonate has completely settled; siphon it into a bottle concentrated sulphuric acid. through which a current of air (free from carbon F-2.2.4 U-tube — one (D) dioxide) has been passed for 2 h previously. Connect this bottle with a soda-lime tube and with a burette as Containing saturated solution of chromic acid in shown in Fig. 7.

FIG, 6 ASSEMBLYOF IODINEPENTOXIDEAPPARATUSFORTHEDETERMINATIONOF CARBONMONOXIDE

12 Is 1090:2002 n C&

SODA–LIME] ——.————-___—__—______E———.———————____——______————____1 1-——— —__ __ ——— ——. —— __ __ _ ml \ n / I!!I

BOTTLE INTERNAL1.Y 1 ---- COATED WITH PARAFFIN 2 LJ ?, ; 48 —

492

50—

PINCH COCK ..

8 cm LONG TIP

FIG. 7 BOTTLEFORSTORINGBARYTASOLUTION

13 Is 1090:2002

F-2.3.3 Iodine Pentoxide using phenolphthalein as indicator. Find out the total volume of standard hydrochloric acid used in the two F-2.3.4 Potassium Iodine Solulion titrations. Dissolve 5 g of potassium iodine crystals in 100 ml of F-2.4.2 Carry out a blank titration with an equal water. volume of baryta solution used for absorption. F-2.3.5 Phenolphtha[ein Indicator F-2.5 Calculation Dissolve 0.50 g of phenolphthalein in 100 ml of rectified spirit. Carbon monoxide, 3098.0 (~ –Vz) (273 +t)N ppm by volume = F-2.4 Procedure P where F-2.4.1 Take 25 ml of baryta solution in each carbon v, = volume in ml of standard hydrochloric dioxide absorber K and add water to about half its acid used for the blank titration of baryta height. Maintain the temperature of iodine pentoxide solution in F-2.4.2, bath at 150°C. Flush the apparatus with about 5 I of nitrogen. Pass the carbon dioxide mixed with an equal v, = volume in ml of standard hydrochloric volume of pure nitrogen at the rate of about 5 I/h. acid used for titrations of baryta solution Measure the rate of flow of the gas by a suitable device in F-2.4.1, and record the temperature and atmospheric pressure t= average temperature in “C, at regular intervals. pass 1() I of carbon dioxide, normality of the standard hydrochloric keeping the temperature and pressure of the gas N’ acid, and constant. Titrate individually the baryta solution in both the absorbers with standard hydrochloric acid P= average pressure in mm Hg.

ANNEX G -, ___ [Table 1, SINO. (vii)]

DETERMINATION OF MERCURY ,

G-1 INSTRUMENTAL METHOD G-2.2 Apparatus

C-1.1 Drager Tubes G-2.2. 1 Photoelectric Absorptiometer or Spectrophotometer G-1.1.1 This apparatus works on the principle of absorption and change in colour. Sealed tubes G-2.2.2 Gas Flowmeter containing the active chemicals are obtainable for C-2.2.3 Dreschel Bottles determining different impurities present in a gas in VPM range. For the procedure for determination of Two, 250 ml capacity, fitted with sintered discs having mercury, instructions of manufacturer of the apparatus a pore diameter 90 to 150 microns. shall be folIowed. G-2.3 Reagents G-2 CLASSICAL METHOD All the reagent solutions shall be freshly prepared. ,.

G-2.1 Principle G-2.3.1 Sulphuric Acid Mercury is absorbed in acidified potassium Approximately 1 N solution. permanganate solution and the excess permanganate G-2.3.2 Potassium Permanganate Solution is reduced with hydroxyammonium chloride. Mercury is extracted from the solution with dithizone and Dissolve 1.58 g of potassium permanganate in I 000 determined absorptiometrically. ml of 1 N sulphuric acid.

NOTE — Dithizonates are particularly sensitive to ultra-violet G-2.3.3 Hydroxyammonium Chloride light and shall be shielded from direct sunlight and from fluorescent lighting in the laboratory, 10 percent (w/v) aqueous solution,

14 1s 1090:2002

G-2.3.4 Dithizone Solution about 5 ml in excess. Di!ute to 100 ml and treat the solution from the two bubblers separately as follows. Dissolve 0.010 0 g of dithizone in 100 ml of chloroform. Further, dilute 6 ml of this solution to G-2.5.2 Transfer to a 250 ml separating funnel and 100 ml with chloroform. extract with 10ml of the dithizone solution by shaking vigorously for one min. If the dithizone solution turns G-2.3.5 Standard A4ercury Solution yellow or orange repeat the extraction with further Dissolve 0.135 g of mercuric chloride and dilute to 10 ml portions. Combine the chloroform extracts. 1000 ml in 1 N sulphuric acid. Further dilute 10 ml (Almost all the mercury should be collected in the of this solution to 1 000 ml with 1 N sulphuric acid. first bubbler. If a substantial proportion is found in One millilitre of the resulting solution contains 1 pg the second bubbler the determination shall be repeated of mercury. using three bubblers.) Prepare a blank by treating 20 ml of the quantity of dithizone. G-2.4 Preparation of Colour Standards G-2.5.3 Measure the optical densities of the solution Into seven 250 ml beakers each containing 20 ml of in the spectrophotometer at a wavelength of 495 ~un the 1 N sulphuric acid, transfer known amounts of or in the absorptiometer with a corresponding filter. the mercury varying from nil to 12 micrograms An Ilford No. 603 filter paper is suitable for this increasing by stages of 2 pg and treat each solution in purpose. Determine the number of micrograms of the following manner: mercury present from a calibration graph previous Iy Dilute to 100 ml with water and transfer to a prepared from the colour standards (see G-2.4). If 250 ml separating funnel. Add 10 ml of the more than one extraction with chloroform was made, dithizone solution and shake vigorously for 1min. multiply the number of micrograms of mercury by the Filter the dithizone extract through a dry number of extraction. Whatman No. 1 filter paper or equivalent into G-2.6 Calculation 1 cm glass cell. Mercury content, 2.784x M X(273+T) G-2.5 Procedure expressed as Hg, mg/m3 = VXP Place 20 ml of the potassium permanaganate solution into each of the two 250 ml Dreschel bottles, connected where in series. Connect the bottles to the sampling point ~. mass in micrograms of mercury found; and the exit from the bottles to the flowmeter. Pass gas through the bottles at a rate of not more than 1 I/rein T= temperature in ‘C of the gas at the time of until about 25 1of gas have been passed. Disconnect determination; the bottles and purge by passing filtered compressed v= volume in Iitres of gas taken; and nitrogen for 1 min. P= barometric pressure mm Hg at the time of G-2.5. 1 Add hydroxyammonium chloride solution to the determination. each bottle until the contents are decolourized, adding

ANNEX H

[Table 1, SINO. (viii)]

DETERMINATION OF HYDROCARBONS

H-1 METHODS H-1.2 Infra-Red Analyzer

H-1.O General The procedure for determination shall be the same as prescribed in E-1.l.l. Three methods have been prescribed, namely, the gas chromatography method, infra-red analyzer and total H-1.3 Total Hydrocarbon Analyzer hydrocarbon analyzer. The sample gas containing hydrocarbon impurities is H-1.l Gas Chromatography Method burnt in a jet of hydrocarbon in the flame ionization detector and the organic components present in the The procedure for determination shall be the same as sample gas provide the source of ions. Concentration prescribed in B-1.1.3. of ions is proportional to the concentration of the 15 Is 1090:2002 organic components. Electrodes having considerably H-1.3.1 Calibrate the instrument against calibration potential difference between them are used to measure gas of known concentration of hydrocarbon following the current produced due to ionization and the the instructions of the manufacturer. Then carry instrument is calibrated in terms of concentration of out the test according to the manufacturer’s hydrocarbons. instructions.

ANNEX J

[Table 2, S1No. (ii), (iii), (v), (vi) and(x)]

METHOD FOR THE DETERMINATION OF OXYGEN, ARGON, CARBON DIOXJDE, CARBON MONOXIDE AND NITROGEN IN HYDROGEN BY GAS CHROMATOGRAPHY

J-1 INTRODUCTION J-3.2 Adsorption Packing Material

This method is suitable for the determination of Silica gel, gas chromatographic grade, 250 pm to oxygen, argon, carbon monoxide and nitrogen in 500 pm particle size. electrolytic compressed hydrogen in the concentration range 1 ml to 1000 ml per cubic meter of hydrogen. J-3.3 Column Materials J-3.3.1 Porapak R, 150 pm to 200 pm particle size. J-2 PRINCIPLE J-3.3.2 Molecular Sieve 13 X, 180 pm to 250 pm The impurities in the hydrogen are concentrated by particle size. adsorption on silica gel cooled by liquid nitrogen. The silica gel is warmed to room temperature, the J-3.3.3 Molecular Sieve 5 A, 150 pm to 200 pm impurities desorbed and determined by gas particle size, chromatographyy. J-3.4 Carrier Gas, Helium — 99.995 percent pure. The gas chromatography is fitted with two packed columns and uses katharometer detection. The J-3.5 Calibration Gases hydrogen complies with the specification with respect J-3.5.1 Carbon Dioxide, at least 99.9 percent pure. to oxygen content if the combined argon and oxygen contents are lower than 10 ml/m3 (10 ppm) but, if J-3.5.2 Carbon Monoxide, at least 99 percent pure. they exceed this figure, a further determination should J-3.5.3 Nitrogen, not less than 99 percent pure. be carried out to measure the oxygen content alone. This can be done by the method described in this J-3.5.4 Oxygen, at least 99 percent pure. Annex but using a 9 m molecular sieve 5A column J-3.6 Liquid Nitrogen instead of 2.7 m molecular sieve 13 x column. J-3.7 Dry Air J-3 REAGENTS J-4 APPARATUS The following reagents (all of which shall be of analytical reagent quality) are required. J-4.1 Adsorption System

J-3. 1 Drying Tube Materials J-4.1.1 General Description

J-3. 1.1 Phosphorus Pentoxide The apparatus is shown diagrammatically in Fig. 8. It consists of two adsorption tubes which are immersed J-3. 1.2 Asbestos Fibre in liquid nitrogen to remove impurities from the hydrogen. Adsorption tube (2) is used as the analysis 16 1s 1090:2002

TO COLUMN OF GAS 6AS CHROMATOGRAPHY

HYD Sou

ING LIQUID NITROGEN PRESSURE @ REGULATOR NEEDLE VALVE + @ ON/OFF VALVE

FIG. 8 APPARATUS FORDETERMINATIONOF GASEOUSIMPURITIESINH2

tube which concentrates impurities in the hydrogen. J-4.1.4 Adsorption Tubes Adsorption tube (1) is used as a hydrogen purification Two stainless steel tubes, internal diameter about system in which the impurities are removed to provide 4.5 mm, length 300 mm, each bent into the form of a a pure stream of hydrogen gas for describing the ,x” U with a nominal distance between legs of 60 mm. concentrated impurities from adsorption tube (2) and The tubes are packed as described in J-5.1.2. for the calibration of the gas chromatography. J-4.1.5 Dewar Flasks The impurities are desorbed from adsorption tube (2) by passing 3 ml x 100 ml portions of purified hydrogen Two flasks, each of 1000 ml capacity. gas through the tube at ambient temperature. Each NOTE — Dewar flasks with inner loose fittings, plastics liners 100ml portion of gas is passed into a gas syringe which should not be used as containem for liquid nitrogen and other low acts as a reservoir and part of the gas is transferred to temperature cryogenic fluids. a gas chromatographic column in a sampling valve. J-4.1.6 Injection Point A phosphorus pentoxide drying tube is provided to remove water from the hydrogen so as to ensure that Consisting of a short branch in the line fitted with a the silica gel in the adsorption tubes retains its silicon rubber septum. efficiency for adsorbing the impurities from the J-4, 1.7 Gas-tight Syringe hydrogen stream. Glass construction, graduated to 100 ml fitted with a J-4. 1.2 Pressure Regulator metal connector suitable for connection to a Stainless steel construction with a non-diffusing type compression fitting. diaphragm capable of controlling hydrogen at 100 kPa J-4. 1.8 Volumetric Gas Meter pressure with a discrimination of 10 kPa. Capable of measuring 2001 at 60 l/h to 70 I/h. J-4. 1.3 Drying Tube J-4. 1.9 Connecting Tubing Stainless steel tubing, external diameter 13 mm nominal, length 200 mm, The tube requires repacking Stainless steel tubing, approximate internal diameter at regular intervals, as described in J-5.1.1, the 2 mm, external diameter 3.17 mm. The minimum frequency depending on the concentration of water in length should be used. the hydrogen. 17 [s 1090:2002

$4.1.10 Stainless Steel Compression Fittings chart speed 10 mm/min. Dead band not greater than 0.3 percent of full scale, noise less than 0.2 percent of Stainless steel couplings and T pieces to match tubing full scale and linearity better than 0.4 percent of full specified in J-4.1.9. scale. J-4. 1.11 Fine Control Needle Valves J-5 PROCEDURE Three valves with stainless steel body and small dead volume. J-5.1 Preparation of Apparatus

J-4.1. 12 ON/OFF Valves J-5.1.1 Drying Tube Three valves with stainless steel body and small dead Pack the tube with a mixture of equal parts of the volumes. phosphorus pentoxide (J-3.1.1) and the asbestos fibre (J-3.1.2) plug the ends with glass fibre and stopper J-4.2 Gas Chromatographic System when not in use.

J-4.2.1 Gas Chromatography J-5.1.2 Adsorption Tubes

With dual katharometer detectors, a gas sampling Pack the adsorption. tubes as follows: valve injection system and an oven capable of being a) Pack one U tube to a height of 150 mm with controlled at 70 + O.l”C. the silica gel-. (J-3.2). J-4.2.2 Pressure Regulator b) Pack the second U tube to a height of 80 mm Capable of controlling helium at 300 kPa pressure with with the silica gel (J-3.2). a discrimination of 30 kPa. Fill the head spaces of the tubes with glass fibre.

J-4.2.3 Flow Controllers J-5. 1.3 Chromatography Columns Two controllers, capable of maintaining flows of Wash the columns with acetone and purge with the 60 ml/min. dry air (J-3.7).

J-4.2.4 Sampling Loop Pack column 1 with the Porapak R (J-3.3.1). Pack Two 2 ml or 5 ml fitted to a gas sampIing valve column 2 with the molecular sieve 13 x (J-3.3.2) and (see J-5.2.3). column 3 with the molecular sieve 5 A (J-3.3.3). Activate the molecular sieve columns before use by J-4.2.5 Co[umns heating at 300°C to 400”C in a stream of the dry nitrogen (J-3.5.3) for 16 h. Install the columns in the Stainless steeI tubing, external diameter 35 mm, gas chromatographyand condition by purging for 16 h internal diameter 4.6 mm (nominal). with the helium (J-3.4) at an oven temperature of a) Column 1: length 1.8 m 100”C using a flow rate of 60 ml/min and with each b) Column 2: length 2.7 m column outlet disconnected from the detector.

c) Column 3: length 9.0 m NOTE — Column 1 should last at least 1 year under normal operating conditions and the packing should be replaced when J-4.2.6 Detector Ancillary Equipment peak shape and component resolution degenerate. Columns 2 and 3canberegeneratedandthisshouldbe done periodically whm The detector power supply system should permit the performance deteriorates. To regenerate, disconnect both columns detect ion of 10ml of carbon monoxide per cubic metre from the katharometer and heat in the chromatography oven at (10 ppm by volume) in 5 ml of sample. This is the 200”C for 12 h with the carrier gas flowing. most critical detection limit. J-5.2 Gas chromatography operating conditions shall An output attenuator is required with a maximum be as follows: sensitivity reduction of 1 000 (nominal) and settings J-5.2. 1 Temperatures in steps such that the peaks, given by the maximum concentration permitted by the specification, can be J-5.2.1.1 Columns kept greater than one-third full scale deflection on the 70°C (nominal) for columns 1and 2; 25°C for column 3. recorder. J-5.2. 1.2 Detectors J-4.2.7 Potentiometric Recorder If separately heated, 70”C to 100”C. I mV full scale deflection, range– O.l mV to + 1.0 mV 1 s (nominal) maximum time for 98 percent full scale J-5.2.2 Gas Flow Rates response, minimum chart width 200 mm, minimum 60 ml/min for columns 1 and 2.

18 Is 1090:2002

J-5.2.3 Sample Volumes J-5.4 Analysis

5 ml for the columns I and 2; 2 ml for column 3. J-5.4.1 Treatment of Sample

J-5.3 Calibration of Gas Chromatography (see Fig. 8) J-5.4.1.1 Purging apparatus Close all the valves in the adsorption system, open With all valves shut and the adsorption tubes at the sample cylinder valve and adjust the pressure ambient temperature, open valves (2), (4) and (6) and regulator to 70 kPa. Immerse adsorption tube control the flow at 60 l/h to 70 l/h with valve (2). (I) (J-4.1 .4) in liquid nitrogen. Open valves (4) and Purge for 5 min. Close valves (2) and (4), open valves (6) to allow hydrogen to pass through the gas (1) and (3) and control the flow at 60 I/h to 70 1/11 meter (J-4. 1.8) to atmosphere. Control the purified with valve (1). Purge for 5 min. hydrogen flow at 60 I/h to 70 I/h with valve(1). Purge J-5.4.1.2 Concentration of impurities for 5 min and then reduce the hydrogen flow to 5 I/h with valve (1). Inject a sample of hydrogen on to the Reduce the flow to 10 l/h with valve (1) and place the required columns to check that the hydrogen is free Dewar flask (J-4.1.5) containing liquid nitrogen, from impurities. Close valve (6) and open valve (5). around adsorption tube (2) (J-4.1.4) with the si1ica gel (J-3.2) well below the surface of the liquid Inject via the injection point (J-4.1 .6) a known volume nitrogen (J-3.6). Note the reading on the volumetric of the pure gas to be detected using the gas gas meter (J-4.1.8), close valve (l), open valve (2) syringe (J-4.1 .7) fitted with a hypodermic needle. Air and adjust the flow to 60 l/h to 70 I/h and pass can be used to calibrate oxygen and nitrogen approximately 200 1 of gas through the adsorption simultaneously. tube.

When the 100 ml gas syringe is tilled with hydrogen J-5.4.1.3 Collection and injection of impurity plus the gas to be detected shut valve (4) and allow concentrate 30 s for the gases to mix. Place a second Dewar flask containing liquid nitrogen Open valve (6) and pass the gas from the syringe into around adsorption tube (1) with the silica gel well the gas chromatography (J-4.2.1) and sample below the surface of the liquid nitrogen. Note the loop (J-4.2.4) and inject the sample onto the required reading on the volumetric gas meter, close valves (2) column (see J-5.4.3 for typical relative retention and (3) and open valves (1) and (4). times). Check that the gas syringe is free from impurities as Measure the peak heights of the components, to the follows: close valve (6), open valve (5) and fill the nearest millimetre, and multiply by the attenuation syringe to the 100 ml mark, controlling the flow with setting to give the peak height in millimetres at valve (1). Close valve (1) open valves (5) and (6) and attenuation x 1. pass the gas from the syringe through the Repeat the injection of the calibration gas at two further chromatography sample valve and inject onto the levels covering the expected concentrated range in the chromatography (J-4.2.1). Repeat this syringe check sample. until no air is detected by the chromatographydetector, using maximum sensitivity. Calculate the factor F, in millilitres of component equivalent to 1 mm peak height at attenuation x 1, for Close valves (4) and (6), open valves (3) and (5), each component from the following formula: remove the liquid nitrogen from around adsorption tube (2) and allow to warm to ambient temperature. Open valve (1) and fill the syringe to the 100 ml mark, close valve (1) and allow 30s for the gas in the syringe to mix. Open valve (6) and pass the gas from the where syringe into the sample valve of the chromatography and inject on to the appropriate column of the VI = volume of component injected (ml), and chromatography.Fill the syringe twice more and inject HI = peak height of component at attenuation x onto the chromatography,to give three chromatograms 1 (mm). for the samples. The factors obtained at the three concentration levels J-5.4.2 Operation of Gas Chromatography and should not differ by more than 10 percent of the Associated Equipment median. Attenuation changes should be made to give, where Repeat this procedure for each gas to be detected. possible peaks of at least one-third full scale.

19 Is 1090:2002

J-5.4.3 Evaluation of Chromatographic Record The sensitivities and retention times of oxygen and argon are almost identical on this column. Typical relative retention times are as follows: J-6 EXPRESSION OF RESULTS Colum.~ Component Typical Relative Retention Time The component content in ml/n13of hydrogen, is given by the following formula: Porapak R Hydrogen 0.84 Air 1,00 H1x Fx103 Carbon dioxide 2.66 v, Molecular Sieve Hydrogen 0.42 13X Oxygen plus argon 0.72 where Nitrogen 1.00 Hz = aggregate peak height of the component Carbon monoxide 1.90 at attenuation X 1 (minimum attenuation Molecular Sieve Hydrogen 1.00 maximum sensitivity) (mm); 5A Argon 2.73 F= amount of component equivalent to I mm Oxygen 2.91 peak height attenuation x 1 (ml); and Nitrogen 8.28 v, = volume of the sample passed through J-5.4.4 Measurement of Peak Size adsorption tube (2) (1). Report the concentration, in millilitres per cubic metre Draw in peak bases and measure the peak heights, to of hydrogen, of each component to the nearest the nearest millimetre, each component on each of 0.1 ml/m3, if greater than 1ml/m3 and to the nearest the three chromatography. 0.02 ml/m3 if lower than 1 ml/m3.

ANNEX K

[Table 2, S1NO. (vii)]

METHOD OF DETERMINATION OF MERCURY CONTENT

/ --- K-1 PRINCIPLE K-2.4 Tin (11)chloride, 100 g/1solution. Dissolve 25 g The mercury vapour is removed from the hydrogen of tin (11) chloride, SnClz.2H20 in 50 ml of warm by scrubbing with potassium permanganate/sulphuric concentrated hydrochloric acid, dilute to 250 m i with acid mixture. water and mix. Discard this solution if it is turbid. After the addition of the hydroxylamine in acid K-2.5 Standard mercury solution, corresponding to solution to decolonize the permanganate and bring in 1 g of mercury (Hg) per Iitre. Dissolve 1.354 g of to the solution any precipitated manganese dioxide, mercury (II) chloride in 25 ml of concentrated an aliquot portion is taken for mercury determination hydrochloric acid, dilute to about 200 ml, add 10 mI by flameless atomic absorption method. of concentrated nitric acid. Dilute to the mark with water in a 1 000 ml one-mark volumetric flask and K-2 REAGENTS mix. Prepare this solution at 2-monthly intervals. The following reagents (all of which shall be of 1 ml of this solution contains 1 mg of Hg. analytical grade) are required, and water complying K-2.6 Standard mercury solution, corresponding to with requirement of BS 3978 : 1987 ‘Water for 10 mg of mercury (Hg) per litre. Measure 10.0 mI of laboratory use’ or water of the equivalent purity shall the standard mercury solution (K-2.5) into a 1000 mI be used. one-mark volumetric flask. Add 25 ml of concentrated K-2. 1 Sulphuric Acid (see IS 266) — 2 percent v/v hydrochloric acid, dilute to the mark with water and solution. mix. Prepare afresh daily, K-2.2 Potassium Permanganate — 40 g/1 solution. One ml of this solution contains 10 pg of Hg.

K-2.3 Hydroxylammonium Chloride — 250 g/1 K-2.7 Standard mercury solution, corresponding to Sollltion. 0.1 mg of mercury (Hg) per litre. Measure 10.0 mI of the standard mercury solution (K-2.6) into a I 000 mI

20 Is 1090:2002

one-mark volumetric flask, Add 25 ml of concentrated K-3.2.3 Trap of about 50 ml volume, or an equivalent hydrochloric acid, dilute to the mark with water and means of preventing entrapped liquid droplets from mix. Prepare afresh daily. entering the spectrophotometer tube.

One ml of this solution contains 0.1 ~g of Hg. K-3.3 Flameless atomic absorption spectrophotometer, which can be either: K-2.8 Absorbing solution, dilute 65 ml of the potassium permanganate solution (K-2.2) and 70 ml a) a conventional atomic absorption spectro- of the sulphuric acid solution (K-2.1) to 250 ml with photometer with mercury hollow cathode water and mix. Prepare immediately before use. lamp and a 100 mm minimum path length cell with silica end windows, which is fitted K-3 APPARATUS in the light path in place of the burner; or AlI glassware should be cleaned before use with aqua b) a mercury vapour detector with enclosed gas regia and thoroughly rinsed with distilled water. The path length, capable of full scale reading use of metals which amalgamate with mercury should equivalent to about 200 pg of mercury per be avoided. cubic metre.

K-3.1 Sampling Apparatus (see Fig. 9) K-3.4 Potentiometric chart recorder, matched to the output of the spectrophotometer. K-3. 1.1 Safety lute, containing water to a depth of 250 mm. K-4 PROCEDURE

K-3. 1.2125 ml sintered glass Dreschsel bottles. Two K-4.1 Preparation of Calibration Graph bottles, connected in series. Set up the apparatus as shown in Fig. 10 with an air K-3. 1.3 Volumetric gas meter, capable of measuring flow of 60 l/h passing through the cell but by passing at least 10 Iitres of hydrogen at a rate of 20 I/h. the aeration flask (K-3.2.2). Adjust the instrument at zero. Into the aeration flask (K-3.2.2) pass 16.0 mI of K-3.2 Aeration Train (see Fig. 10) the absorbing solution (K-2.8) and add from a 10 mI K-3.2.1 Supply of mercury free compressed air, burette, 10.0 ml (containing ) 1 pg of Hg of the purified by passage through activated chemical. standard mercury solution (K-2.7). Add the hydroxylammonium chloride solution (K-2.3) drop by K-3.2.2 Aeration flask of about 100 ml capacity, such drop, until the perrnanganate colour isjust discharged as that illustrated in Fig. 10 which is made from a and dilute to 60 ml with water. Swirl to mix. Add 100 ml graduated cylinder.

SAMPLE

f’

/voLUMETRIC L4u GAS METER LLI’TE

FIG. 9 SAMPLINGAPPARATUSFORDETERMINATIONOF MERCURY

21 1s 1090:2002 m i NEEDLE VALVE 100 ml. CELL WITH SILICA WINDOWS

GLASS WOOL ti FLOWMETER LT~Ap

“* J 1

FIG. 10 AERATIONTRAINFORDETERMINATIONOF MERCURY

2.0 ml of the tin (II) chloride solution (K-2.4) K-4.3 Determination of Mercury in the Sample immediately assemble the apparatus and turn the Solution 4-way tap so that the air passes through the aeration Set up the instrument as in the calibration procedure flask. Observe the height of the peak obtained. If (K-4.1). Into the aeration flask pipette 20.0 ml of the necessary, adjust the instrument gain to obtain an sample solution, dilute to 60 ml with water and mix. adequate response (80 percent to 100 percent full scale Add 2.0 ml of the tin (II) chloride solution (K-2.4) deflection), discharged the solution and repeat the and immediately reassemble the apparatus. Operate operation to confirm that the gain setting is correct. the 4-way tap and record the instrument response. Repeat the operation using 0.20 ml, 4.0 ml, 6.0 ml Carry out a blank on the reagents using 16.0 ml of the and 8.0 ml of the standard mercury solution (K-2.7) absorbing solution (K-2.8) developed by the addition, corresponding to 0.02 pg, 0.4 pg, 0.6 ~g and 0.8 pg drop by drop, of the hydroxylammonium chloride ---- of Hg. Substract the peak height obtained from the solution (K-2.3). solution blank from all the other peak heights !’ (including that corresponding to 1 pg of Hg) and Read off the mercury contents of the sample solution > construct a calibration graph of peak height against and blank from the solution graph. If an off-scale micrograms of Hg. reading is obtained with 20 ml of sample solution, repeat the determination using a smaller aliquot K-4.2 Preparation of Sample Solution portion. Set up the absorption train as shown in Fig. 10. Into K-5 EXPRESSION OF RESULTS each of the Drechsel bottles (K-3.1.2), place 40 ml of the potassium permanganate/sulphuric acid Mercury content, in milligrams per cubic metre of mixture (K-2.8) and attach to the hydrogen sample hydrogen, is given by the following formuIa: supply. Allow hydrogen to pass through the absorption train at a rate of about 20 I/h until a suitable sample (M, -M2)x~ volume has been passed; about 201 to 401. q v, .. Disconnect the Drechsel bottles and add the where hydroxylammonium chloride solution (K-2.3) until the permanganate colour isjust discharged. Swirl, replace &f, . mass of mercury found in the aliquot por- the gas distributors, and allow to stand to dissolve any tion of the test solution (pg), deposits of manganese dioxide. Mz = mass of mercury found in the blank (L:), Transfer the contents of both bottles to a 100 ml one- v, = volume of hydrogen taken as sample (1i- mark volumetric flask using a minimum of wash water, tres), and dilute to mark and mix. v. = volume of the aliquot portion of the test ,! solution (ml).

22 Is 1090:2002

ANNEX L

[~able 2, S1fVO.(iv)]

METHOD FOR THE DETERMINATION OF WATER CONTENT

L-1 PRINCIPLE L-2.3.3 Calibration Gas Hydrogen is passed at a constant rate through a tube Acetylene minimum purity 95 percent. containing calcium carbide where the water reacts to form acetylene. L-2.4 Molecular Sieve 5 A 2 HZO+ CaCz= Ca (OJ-1)2+ Cz H2 3 mm pellets activated before use by heating at 400°C in a stream of dry nitrogen for 16 h. The concenb-ation of acetylene in the hydrogen is then determined by gas chromatography using a Porapak L-3 APPARATUS T column and flame ionization detector. The following apparatus is required: L-2 REAGENTS L-3.1 Pressure Regulator L-2.1 Calcium carbide, particle size 150 pm to Stainless steel construction, with an impermeable 200 pm, essentially free from calcium oxide or diaphragm, capable of controlling hydrogen pressure hydroxide. Carbide granules should be crushed, in with a discrimination of 10 kPa. small quantities, and sieved in a dry atmosphere and care should be taken to minimize contact with L-3.2 Reaction System moisture. Store in a glass container sealed with a rubber bung, having a 6 mm hole drilled through it, This is shown diagrammatically in Fig. 11 and which is sealed with a short length of glass or steel comprises the following. rod. L-3.2.1 Calcium carbide reactor consisting of stainless steel tubing, length 230 mm, internal diameter 4 mm L-2.2 Column Packing packed with calcium carbide. The tube will require Porapak T 150 pm to 200 pm particle size. repacking at regular intervals as described in L-4.1 .2. The frequency of repacking depends on the L-2.3 Process Gases concentration of water in the hydrogen.

L-2.3.1 Carrier Gas L-3.2.2 Connecting Tubing Nitrogen at a presssure of not less than 400 kPa. Stainless steel tubing, internal diameter 1.5 mm, L-2.3.2 Auxiliary Gases external diameter 3 mm. The minimum lengths should be used. L-2.3.2.1 Hydrogen at a pressure not less than 400 kPa, minimum purity 99.999 percent free from L-3.2.3 Stainless Steel Couplings acetylene. Reducing couplings for 6 mm to 3 mm outside L-2.3.2.2 Air, compressed at not less than 400 kPa, diameter tubing. Equal T pieces for 3 mm outside free from oil and water. diameter tubing.

NOTE — The carrier and auxiliary gases are purified before use L-3.2.4 Stainless Steel Rod by passage first through gas puri@hrg bottles filled with a 5 A molecular sieve, and then through 5pm sintered metal filters. 3 mm outside diameter.

6m m TO 3mm STAINLESS STEEL COUPLING

)0 ● 0(

L-230mmx 6 mm O/D STAINLESS STEEL TUBE

FIG. 11 CALCKJMCARBIDEREACTOR,DETERMINATIONOF WATER

23 ,, . A

Is 1090:2002

L-3.2 .5 Super-ne Glass Wool L-3.4.1 Glass Vessel

L-3.2.6 Gas-tight Syringe 10 I aspirator fitted with rubber bungs covered with aluminium foil. Glass construction, 2 ml and 100 ml capacity. L-3.4.2 Magnetic Stirrer L-3.3 Volumetric Gas Meter Magnetic ‘follower’ fitted with an aluminium foil vane 0.25 I/rev, capable of measuring 2 l/rein. to increase its stirring efficiency.

L-3.4 Calibration Apparatus L-3.4.3 Glass Tubing

This is shown diagrammatically in Fig. 12 and 6 mm outside diameter (nominal). comprises the following.

SEPTUM ~ RUBBER BUNG COVERED WITH ALUMINIUM FOIL

LGLASS l-uBE \

GLASS ASPIRATOR BOTTLE OF 10LITRE CAPACITY -- --

MAGNETIC FOLLOWER COVERED IN ALUMINIUM FOIL AND SHAPED IN THE RUBBER BUNG FORM OF A PROPELLAR COVERED IN r ALUMINUM FOIL

----- * SEPTUM

LGLASS TUBE

@ MAGNETIC STIRRER

FIG. 12 CALIBRATIONAPPARATUSFORDETERMINATIONOFWATER

24 J%_

Is 1090:2002

L-3.4.4 Septa Dead band not more than 0.15 percent full scale To fit 6 mm outside diameter glass tubing. Noise not more than 0.15 percent L-3.4.5 Gas Syringes full scale

Capacity 10 ml and 100 ml. L-4 PROCEDURE

L-3.5 Gas Chromatographic System L-4.1 Preparation of Apparatus

L-3.5. 1 Gas Chromatography L-4. 1.1 Chromatography Column Gas chromatography with flame ionization detector, a Pack with the Porapak T (L-2.2) and condition by gas sampling valve injection system and an oven heating to 180 ‘C for 16 h with the carrier gas capable of being controlled at 80 + 0.1“C. A facility (L-2.3.1) flowing through it at 60 ml/min. lrtstall the shall be provided for purging the sample valve with column (L-3.5.4) in the gas chromatography (L-3.5) nitrogen between determinations. and further condition by purging for 16h with nitrogen L-3.5.2 Pressure Regulators at an oven temperature of 100”C, using a flow rate of 60 ml/min and with the column outlet disconnected Capable of controlling nitrogen, hydrogen and air at from the detector (L-3.5.5). up to 300 kPa pressure with a discrimination of 30 kPa. L-4. 1.2 Calcium Carbide Reactor (see Fig. 11) L-3.5.3 Injection System Plug one end of the stainless steel tube (L-3.2.1) with a Gas sampling valve fitted with a 5 ml sample loop. small piece of the superfine glass wool (L-3.2.5). Fit a L-3.5.4 Co[umn 6 mm to 3 mm reducing coupling (L-3.2.3) to this end. Remove the plug from the bung of the calciuln Stainless steel tubing, external diameter 6 mm, internal carbide (L-2.1 ) container and insert the open end of diameter 4 mm, length 0.5 m. the stainless steel tube (L-3.2.2) into the hole of the L-3.5.5 Detector Ancillary Equipment bung. Invert the container and tap the tube gently to start the calcium carbide flowing into the tube. Continue L-3.5.5. 1 Ionization ampll~er tapping until the tubes are fill. With the reactor in a Any amplifier/flame ionization detector system horizontal position, carefully ease it away from the capable of giving a full scale response for 0.05 ml of container, avoiding spilling any of the calcium carbide .---- acetylene per cubic metre at maximum sensitivity from the tube or the container, then replace the plug in using the sample size stated. the calcium carbide container bung. Remove calcium

carbide from the end of the reactor tube to a depth :’ > Attenuation In steps such that the size of of 5 mm and plug the end with superfine glass wool the peaks given by the (L-3.2.5). Fit a 6 mm to 3 mm coupling. [f the reactor maximum concentration of isnot to be used immediately, both ends should be sealed the specification can be kept with the 3 mm stainless steel rod (L-3.2.4). greater than one-third full scale deflection on the NOTES 1Theaboveoperations should be carried out as quickly as possible recorder. to minimize contact with atmospheric moisture. Noise Level Less than 1 percent of full 2 The reactor should be repacked with fresh material when the scale deflection at maximum pressure required for a given flow rate increases by more than 20 sensitivity. percent of that required for a new reactor or when the time taken Drift Less than 1 percent of full to reach equilibrium atler a change in gas flow through the reactor exceeds 15 min. scale deflection per hour at maximum sensitivity. L-4.2 Gas Chromatography Operating Conditions Output to recorder 1 mV or 10 mV for full scale deflection. Operating conditions shall be as follows.

L-3.5.5.2 Potentiometric recorder L-4.2.1 Column temperature 80”C. Span 1’mV or 10 mV L-4.2.2 Gas Flow Rates (Approximate) Span step 1 s nominal response time Nitrogen carrier gas 60 ml/min Minimum 200 mm calibrated in 1 Hydrogen to detector 60 ml/min chart width percent full scale divisions Air to detector 900 ml/min minimum Nitrogen 30 ml/min Minimum 10 mm/min (purge to gas sample valve) chart .sDeed 25 1s 1090:2002

L-4.3 Chromatography Calibration determine the acetylene content of the hydrogen by reference to the calibration graph. Report the result to Fill the aspirator (L-3.4.1) with the hydrogen the nearest 0.1 ml/m3. (L-2.3.2.1), stopper and start the stirrer (L-3.4.5) inject a volume of the acetylene (L-2.3.3) into the aspirator L-5 EXPRESSION OF RESULTS via the top septum (L-3.4.4) to give an acetylene concentration in the range required. Continue mixing The water content expressed as millilitres of water for 5 min. Withdraw 50 ml of the calibration mixture vapour (HZO) per cubic litre of hydrogen is equal to via the bottom septum and inject on to the chromato- twice the acetylene content determined. graphy(L-3.5.1 ) via the gas sampling valve. Measure the acetylene peak height to the nearest millimetres. Prepare at least two more mixtures in the concentration range and inject on to the chromatography. Carry out a blank determination on the hydrogen used for preparing the calibration mixture by passing it through the sample loop and injecting on the chromatography. Draw a graph relating acetylene peak height (corrected for the blank) to the acetylene concentration, expressed in ml/m3.

L-4.4 Analysis

Connect the stainless steel diaphragm pressure regulator (L-3.1) to a well purged sample point and purge to atmosphere at about 1 l/rein for a minimum of 15 min.

Connect the calcium carbide reactor tube (L-3.2.1) to ACETYLEN the regulator and adjust the hydrogen flow to within the range 0.5 l/rein to 1.0 Vrnin, using the volumetric gas meter (L-3.3) and a stopwatch and allow to purge for 15 min at constant temperature to establish equilibrium conditions in the tube. Insert the needle of the 100 mm gas syringe (L-3.4.5) through the septum and slowly withdraw 100 ml of gas into the syringe. Purge the syringe twice with the sample. Finally fill the syringe, remove from the septum and purge the gas sample valve and loop with 50 ml of sample. Pause for 1s to allow the gas pressure in the sample to attain atmospheric pressure and inject NJECTION on to the column (L-3.5). Adjust the amplifler attenuation (L-3.5.5.1 ) to give, if possible, an acetylene } peak of at least one-third full scale. Carry out a blank determination on an unreacted sample of hydrogen at the same amplifier attenuation. Purge the sample valve with nitrogen between determination. A typical chromatography is shown in Fig. 13.

Measure the acetylene peak height, to the nearest FIG. 13 TYPICALCHROMATOGRAMFOR millimetre, and after correction for any blank DETERMINATIONOFWATER

26 ,, A

Is 1090:2002

ANNEX M

(Clause 8)

SAMPLING OF COMPRESSED HYDROGEN

M-1 SCALE OF SAMPLING case such a table is not available, the following procedure should be followed: M-1.l Lot Starting from any cylinder in the lot, count them In any consignment all cylinders charged at a time in one order as 1, 2, 3,...... up to r and so on, from one charging manifold shall constitute a lot. where r is the integral part of N/n. Every rth M-1.2 The number of cylinder (n) to be selected from cylinder thus counted shall be withdrawn to give the sample for test. a lot shall depend on the size of the lot (N) and shall be in accordance with co] 1 and 2 of Table 3 M-2 TEST SAMPLE

Table 3 Number of Cylinders to be Selected A sample of gas shall be drawn from each cylinder selected as in M-1.2 and shall be the individual test (Clause M-1.2) sample from each cylinder.

Lot Size Number of Cylinders to be Selected M-3 NUMBER OF TESTS

(!) (;) All the individual test samples from each lot prepared up to 50 5 as in M-1.1 and shall be tested separately for alI the 51 to 100 8 requirements given in Tables 1 and 2. 101 to 150 15 151 to300 20 M-4 CRITERIA FOR CONFORMITY 301 and above 25 A lot shall be declared as conforming to the M-1 .2.1 The cylinders shall be selected at random and requirements of the specification if all individual in order to ensure the randomness of selection, a samples tested pass the requirements prescribed in random number table (see IS 4905) shall be used. In Table 3.

----

27 1s 1090:2002

ANNEX N

(Foreword)

COMMITTEE COMPOSITION Industrial Gases Sectional Committee, CHD 6

Organization Representative(s) Praxair India Pvt Limited, Bangalore SHSUR. S. DHULXHED(Char”rrnarr)

All India Industrial Gases Manufacturers Association, New Delhi DRP. L. BHAm Srmr B. N. QANUNGO(Alternate)

Association ofAutomobile Manufacturers of IndiA New Delhi ~AISVS

Bharat Heavy ElectricaJs Limited, Hyderabad SHSUN.V. S. - Smu A. RAJAMOHAN(Alternate)

BOC India Ltd, Kolkata SHRIF’.AMARNATH

Central Electronics Ltd, Ghaziabad SHRSM. I. ALAM

Chief Controller of Explosives, Nagpur SHIUR. H. BHALEKAR Smrr S. K. BHARDWAS(Alternate)

Department of Electronics, New Delhi DR U. C. PANDEY

Department of Industrial Development, Ministry of Industry, New Delhi SW P. K. Jm Smu N. C. TrWASU(Alternate)

Gujarat State Fertilizer Corporation Ltd, Vadodara SmuM. C. SHAH Smr R. C. MATHUR(Alternate)

Indian Space Research Organization, Shriharikota ~A~

Industrial Oxygen Co Ltd, Mumbai Smr R. R. SINGANFORIA

Laxman & Sylvania Ltd, New Delhi WrU S. K. KAPOOR SHRINAVEENSKXA (Alternate)

Mahahrsa Gases&Chemical Pvt Ltd, Barrgalore SmuM. G. SuaHARAO

Ministry of Defence (DGQA), New Delhi sNruY. v. vArLrms Smu SurrTGHOSH(Alternate)

Mohan Meakins Ltd, Ghaziabad DR E. K. JAYANARAYARAN

National Physical Laboratory, New Delhi ~AINS

National Test House, Kolkata DRB. B. PAL Ordnance Factory, Bhandara DR S. K. DESHMUKH SHRIV. SRINSVASAN(Alternate)

Rashtriya Chemicals and Fertilizers Ltd, Mumbai DR R. N.TRIVEDI

Semi Conductor Complex Ltd, SAS Nagar (Panjab) SHSUS. S. N. PRASAO

Steel Authority of India Ltd, New Delhi Smu A. NAWAN Srmr S. G. K. MuRmY (Alternate)

Steel Fumance Association of IndiA New Delhi Smr M. K. GUPTA

The Asiatic Oxygen & Acetate Co Ltd, Kolkata Smu B. N. SrNHA

The Industrial Gases Ltd, Kolkata Smr T. GARG SHSUL. R. GARG(Alternate)

BIS Directorate General SHRILAJINDERSSNGH,Director (Chem) [Representing Director GeneraI (Er-oflcio)] MemberSecretary SHRSN.K. PAL Director (Chem), BIS

(Continuedonpage 29)

Is 1090:2002

(Con~inuedfrompage 28)

Oxygen, Argon, Acetylene, Hydrogen, Nitrogen, Carbon Dioxide, Helium Subcommittee, CHD 6: I

Organization Representative(s) Praxair lndiaLtd, Bangalore SmoLMOOXHEWEE(Convener)

Air Liquide Indi% New Delhi Smo SAIISHKGCHHAR Sm VSINL4TESHPIWAO (Alternate)

All India Industrial Gas Manufacturers Association, New Delhi lhP. L. Bwmm Smu B. N. QANUNGO(Alternate)

Asiatic Oxygen Ltd, Kolkata SsnuR. C. BHAITAWYA Smu M. P. Dw%rwna (Alternate)

BOC India Ltd, Kolkata %tUp. AhtARNAIH

Electric Lamp Manufacturers (India) Ltd, Kolkata SmuK. SW Smu S. B. BHATTACHARY(Alternate)

Hindustan Lever Ltd, Pune SrmrV.K. Sr+mm

Hydrogas Indi& Mumbai R51HWDWATlVS

GSFC, Vadodara Srnu M.C.SW SmuR.C.MAmuR(Alternate)

hrdostrial Gases Ltd, Kolkata SmrrT. GARG

Industrial Oxygen Co Ltd, Mumbai .%auR R. SINGANPGRIA

Kamrup industrial Gases Ltd, Kolkata Smr N. K. GARG %rru D. K. GARG(Alternate)

Laxman & Sylvania Ltd, New Delhi Stau-D KW SHRINAVEENSaw (Alternate)

Mahalasa Gases&Chemicals Pvt Ltd, Bangalore SmoA. N. PWW SrmrM. G. SUBHAMO (Alternate)

Modi Gas& Chemical Ltd, Modi Nagar smr PRAMOD Km

Mohan Meakins Ltd, Mohan Nagar DR E.R.JAYANARAYAIW Smu B.K. B.mru (Alternate)

National Test House, Kolkata DRB. B. PAL .----’ DR S. ILum (Alternate)

NTPC, New Delhi SruuP. K. Vrntrm Smu P. K. B~ (Alternate) i, .;

Praxair India Ltd, Bangalorc SHSUm SARXAR

Rashtriya Chemicals& Fertilizers Ltd, Kolkata Mu S.S.AMWW Smu B. P. Rm’r?m (Alternate)

RDSO, Lucknow ~ ~R(h’l@ ASSISTANIIkm.4rm @mom (A&r-Iv)(Alternate)

South India Carbonic Gas Industries Ltd, Chennai SmrrF. L. D@ABHOY SmuT.JAGDEESAN(Alternate)

The Asiatic Oxygen &Acetylene Co Ltd, Kolkatrr SmuB. N. Sw

29 Bureau of Indian Standards

BIS is a statutory institution established under the f3ureuu of Indian Standards Act, 1986 to promote harmonious development of the activities of standardization, marking and quality certification of goods and attending to connected matters in the country.

B1S has the copyright of all its publications. No part of these publications may be reproduced in any forlm without the prior permission in writing of BIS. This does not preclude the free use, in the course of implementing the standard, of necessary details, such as symbols and sizes, type or grade designations. Enquiries relating to copyright be addressed to the Director (Publications), BIS.

Review of Indian Standards

Amendments are issued to standards as the need arises on the basis of comments. Standards are also reviewed periodically; a standard along with amendments is reaffirmed when such review indicates that no changes are needed; if the review indicates that changes are needed, it is taken up for revision. Users of Indian Standards should ascertain that they are in possession of the latest amendments or edition by referring to the latest issue of ‘BIS Catalogue’ and ‘Standards: Monthly Additions’.

This Indian Standard has been developed from Doc : No. CHD 6 (698).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

BUREAU OF INDIAN STANDARDS Headquarters : Manak Bhavan, 9 Bahadur Shah Zafar Marg, New Delhi 110002 Telegrams : Manaksanstha Telephones :3230131, 3233375, 3239402 (Common to all offices)

Regional Offices : Telephone Central : Manak Bhavan, 9 Bahadur Shah Zafar Marg 3237617 NEW DELHI 110002 { 3233841 Eastern : I/14 C.I.T. Scheme VII M, V. 1.P. Road, Kankurgachi 3378499,3378561 KOLKATA 700054 { 3378626,3379120 Northern : SCO 335-336, Sector 34-A, CHANDIGARH 160022 603843 { 602025 Southern : C.I.T. Campus, IV Cross Road, CHENNAI 600113 2541216,2541442 { 2542519,25413 15 Western : Manakalaya, E9 MIDC, Marol, Andheri (East) 8329295, 8327858 MUMBAI 400093 { 8327891,8327892 Branches : AHMEDABAD. BANGALORE. BHOPAL. BHUBANESHWAR. COIMBATORE. FARIDABAD. GHAZIABAD. GUWAHATI. HYDERABAD. JAIPUR. KANPUR. LUCKNOW. NAGPUR. hIALAGARH. PATNA. PUNE. RAJKOT, THIRUVANANTHAPURAM. VISAKHAPATNAM.

PrintedatPrabhatOffsetPress,NewDelhi-2 ,“

AMENDMENT NO. 1 DECEMBER 2008 TO IS 1090:2002 COMPRESSED HYDROGEN — SPECIFICATION

( Third Revision)

(Page 27, Annex M, clause M-1.2, Table 3) — Substitute the following for the existing table:

Table 3 Number of Cylinders to be Selected (Clause M-1 .2)

Lot Size Number of Cylinders to be Selected

(’Y) ($

Up to 25 3 26 to 50 5 51 to 100 8 101to200 15 201 to 300 20 301 nndabove 25

ReprographyUnit,BIS,New Delhi,India

,,, . \’