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IS 5760 (1998): Argon, compressed and liquid [CHD 6:Industrial Gases]

Indian Standard

ARGON, COMPRESSED AND LIQUID — SPECIFICATION

( Second Revision )

ICS 71.100.20

© BIS 1998

B U R E A U O F I N D I A N S T A N D A R D S MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

May 1998 Price Group 4

IS 5760 : 1998

Industrial Gases Sectional Committee, CHD 006

FOREWORD

This Indian Standard (Second 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.

This standard was originally published in 1969 and covered only argon used for welding and other metallurgical operations. In the first revision of this standard in 1983, another grade of argon was incorporated to cover high purity argon for use in lamp industry and in direct reading vacuum spectrograph. Since then, other industrial uses of high purity argon have grown tremendously, particularly, the use of ultra high purity argon in electronics industry This second revision of the standard has been undertaken to incorporate another grade of argon, that is, ultra high purity grade argon for use in electronics industry.

At present, argon is being manufactured and marketed in three grades, namely, Grade 1 Ultra high purity argon for use in electronics and allied industries, Grade 2 High purity argon for use in lamp industry, and Grade 3 Argon for use in welding and for other metallurgical processes. Commercial/industrial users are also accustomed to these grades.

As stringent limits of impurities have been prescribed for ultra high purity argon (Grade 1) and high purity argon (Grade 2) the analysis of these grades of argon demands the employment of sophisticated modern instruments having high degree of sensitivity and precision. In view of this, the conventional forms of glass test sets and apparatus have not been prescribed for Grade 1 and Grade 2 argon. The equipment and the instruments prescribed tor analysis are amongst the latest in the field.

The Committee responsible for formulation of this standard is given in Annex C.

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.

AMENDMENT NO. 1 DECEMBER 2008 TO

IS 5760 : 1998 ARGON, COMPRESSED AND LIQUID — SPECIFICATION

( Second Revision )

(Page 5, Annex B, Table 2) — Substitute the following for the existing:

Table 2 Number of Cylinders to be Selected (Clause B-1.2)

(CHD 6)

Reprography Unit, BIS, New Delhi, India

Lot Size N (1)

Up to 25 26 to 50 51 to 100 101 to 200 201 to 300 301 and above

Number of Cylinders to be Selected n (2)

3 5 8 15 20 25

IS 5760 : 1998

Indian Standard

ARGON, COMPRESSED AND LIQUID — SPECIFICATION

( Second Revision ) 1 SCOPE

This standard prescribes requirements and methods of sampling and test for argon, liquid and compressed.

2 REFERENCES

The Indian Standards listed below contain provisions which through reference in this text, constitute provisions of this Indian Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this Indian Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below:

IS No. Title

4905 : 1968 Methods for random sampling

7062 : 1973 Glossary of terms used in gas industry

3 TERMINOLOGY

For the purpose of this standard, the definitions given in IS 7062 shall apply.

4 GRADES

There shall be three grades of argon, namely:

Grade 1 Ultra high purity argon for use in electronics and allied industries and in direct redding vacuum spectrograph,

Grade 2 High purity argon for use in lamp and allied industries, and

Grade 3 Commercial grade argon for use in weld ing industry and for other metallurgical operations.

5 REQUIREMENTS

5.1 The material shall be compressed gas or liquid for vaporization.

5.2 The material shall comply with the requirements prescribed in Table 1 when tested in accordance with the methods prescribed in Annex A. Reference to the relevant clauses of Annex A is given in col 6 of Table 1.

6 PACKING AND MARKING

6.1 The gas shall be supplied compressed in cylinders or liquid argon tanks. The design of cylinders or liquid argon tanks, the maximum pressure of argon in them. and packing, marking, painting, labelling and transport of cylinders tanks shall be in conformity with the Gas Cylinder Rules, 1981 of the Government of India with modifications as may be ordered from lime to time by the Chief Controller of Explosives or any other authority duly constituted by the Government of India.

Table 1 Requirements for Argon, Compressed and Liquid

(Clauses 5.2 and B-3)

Sl No.

(1)

i)

ii) iii)

iv)

v)

vi)

vii)

Characteristic

(2)

Oxygen, ppm, Max

Nitrogen, ppm, Max

Hydrogen, ppm, Max

Water vapours, ppm, Max

Carbon dioxide, ppm, Max

Carbon monoxide, ppm, Max

Requirement 4

Grade Grade Grade 1

(3)

0 5

2 0

1 0

0 5

0 5

0.5

Hydrocarbons, ppm, Max 0 2

2 (4)

5 0

10 0

2 0

4 0

0 5

0 5

0 5

3 (5)

10 0

300

5 0

7 0

3 0

2 0

–

Method of Test (Ref to Cl No.

in Annex A) (6)

A-2, A 3

A-2, A 4

A-2

A-5

A-2, A-6

A-2, A-7

A-2, A-8

7 SAMPLING

The method of drawing representative samples from a lot, number of tests to be performed and the criteria for conformity of the material to the requirements of this specification shall be as prescribed in Annex B.

1

IS 5760 : 1998

ANNEX A

(Clause 5.2) METHODS OF TEST FOR ANALYSIS OF ARGON, COMPRESSED AND LIQUID

A-1 GENERAL

Only instrumental methods of test have been prescribed for analysis of argon, compressed and liquid.

A-2 DETERMINATION OF OXYGEN, NITROGEN, HYDROGEN, WATER VAPOUR, CARBON DIOXIDE, CARBON MONOXIDE AND HYDROCARBONS

A-2.1 Gas Chromatographic Method

A-2.1.1 Principle

Chromatography is a process of separation achieved by means of a partition between a stationary phase and a moving phase. A suitable synthetic zeolite and suitable detector are used in chromatography.

When the accuracy of analysis is to be achieved at the level of 1 vpm, the results obtained are always relative to the impurities of carrier gas and are not absolute values. Hence, the ultra high purity carrier gas, that is, Grade 1 argon is to be purified further by a suitable rare gas purifier to achieve zero impurity carrier gas.

The purifier system consists of titanium granules at 700°C for removal of nitrogen and oxygen, a copper oxide furnace for removal of hydrogen and carbon monoxide, and molecular sieve to remove carbon dioxide and moisture.

The construction of the gas chromatograph is the same as that of any gas chromatograph with a gas sampling value and a loop of known volume. The column material is molecular sieve 5 A filled in stainless steel column of 4 m length and 4.6 mm internal diameter. The column is regenerated at 250°C in a stream of argon for about 4 h. The detector is the most important part of the whole assembly and is called argon discharge detector. Purified carrier argon gas, which

passes through the detector chamber, is subjected to a strong electromagnetic field maintained between two electrodes by a high frequency generator. The resulting luminescense is modified subsequently by any other element passing through the chamber.

The high frequency generator is operated on a stabilized voltage. The luminous intensity of the gas discharge tube is measured by means of a photo­resistive cell, which is one of the branches of the bridge whose unbalanced voltage is the output signal for recording or integrating.

A-2.1.2 Procedure

Calibrate the instrument against calibration gas of known composition by measuring the peak heights or areas under various peaks of the chromatograph following the instructions of the manufacturer. Carry out the test according to the manufacturer 's instructions and compute the concentration of the various impurities by comparing the peaks or the areas under peaks with that of the calibration gas.

The nature of chromatograph of a calibration gas mixture in argon is depicted in Fig. 1.

A-3 DETERMINATION OF OXYGEN

A-3.1 General

Two methods have been prescribed, namely electrochemical analyser method and gas chromatrographic method.

A-3.1.1 Electrochemical Analyser Method

A-3.1.1.1 Principle

The oxygen detection element consists of a number of silver disc arranged around a central helix to form a spiral through which the test gas passes. The spiral is contained within a porous vyon tube immersed in a

CONCENTRATION IN pprn BY VOLUME

FIG. 1 CALIBRATION GAS

2

IS 5760 : 1998

pool of potassium hydroxide electrolyte to keep the tube moist. The silver acts as the cathode of the cell. Where oxygen molecules in the test gas are absorbed on its surface and go into the solution in the electrolytes as hydroxyl ions. These ions migrate through the electrolyte to the cadmium anode which is oxidized to cadmium hydroxide, the ions having given up their negative charge causing a current to flow in the external circuit consisting of a galvanometer connected across the electrodes. The magnitude of the current is a measure of the amount of oxygen in the gas.

A-3.1.1.2 Apparatus

The instrument should be capable of determining oxygen in the range of 0 to 1 vpm, 0 to 10 vpm, 0 to 100 vpm and 0 to 1 000 vpm.

A-3.1.1.3 Procedure

The procedure to be followed for the determination shall depend on the type of analyser used. The manufacturer's instructions in this regard shall be followed.

A-3.1.2 Gas Chromatographic Method

The procedure for carrying out the determination shall be the same as prescribed under A-2.

A-4 DETERMINATION OF NITROGEN

A-4.1 General

Two methods have been prescribed, namely, gas chromatographic method and spectra analysis method.

A-4.1.1 Spectra Analysis Method

A-4.1.1.1 Principle

The spectra analyser determines nitrogen in argon in the range of 0 to 100 vpm. The analyser is based around a pyrex/quartz cell through which the test gas is passed. A high a.c. Voltage is applied to this cell which causes ionization of the gas and consequent emission of light. A particular and proportionate fraction of this light results from the ionization of nitrogen which is present in the sample. The intensity of emission of light is proportional to the nitrogen concentration. The emitted light through a chopper and narrow band interference filter. The transmitted light, which is proportional to the nitrogen present in the test gas, is detected by a photo-multiplier tube and converted into electrical signal. The signal is pre-amplified and measured. The analyser is to be calibrated by a standard gas mixture.

A-4.1.1.2 Procedure

It shall depend on the type of analyser used. The instrument manufacturer's instructions in this regard shall be followed.

A-4.1.2 Gas Chromatographic Method

The procedure for carrying out the determination shall be the same as prescribed under A-2.

A-5 DETERMINATION OF WATER VAPOUR

A-5.1 General

Four methods have been prescribed. Three methods are instrumental namely, electrolytic hygrometer, frost or dew point hygrometer and capacitance hygrometer. Fourth one is absorption method. For routine analysis any of the methods may be employed. However, in case of any dispute in the determination of water vapour, absorption method shall be used as a referee method.

A-5.1.1 Electrolytic Hygrometer

The method is based on the absorption and electrolysis of the water vapour present in the sample gas. The electrolytic current gives a direct measurement of water vapour present in the gas flowing through the instrument at a steady rate. The exact procedure to be followed shall depend on the type of apparatus to be used. The instrument manufacturer's instructions in this regard shall be followed.

A-5.1.2 Frost or Dew Point Hygrometer

A metal surface on the hygrometer is cooled so that dew or frost is formed from the water vapour content of the gas at a particular pressure which may be observed optically in the apparatus. The temperature at which the dew or frost is formed is a measure of water vapour content of the gas. The exact procedure to be followed shall depend upon the type of apparatus to be used. The instrument manufacturer's instructions in this regard shall be followed.

A-5.1.3 Capacitance Hygrometer

The method is based on the change of capacitance of the sensor when a sample gas containing water vapour passes through it. The change in capacitance gives a direct measurement of water vapour present in the gas. The procedure to be followed shall depend upon the type of apparatus to be used. The instrument manufacturer's instructions in this regard shall be followed.

A-5.1.4 Absorption Method

A-5.1.4.1 Apparatus

The apparatus consists of the following parts assembled as shown in Fig. 2.

A-5.1.4.1.1 Gas meter accurate to I percent

A-5.1.4.1.2 Absorption train

Three U-tubes containing phosphorus pentoxide connected in series to the gas meter. The one near to

3

IS 5760 : 1998

FIG. 2 ASSEMBLY OF APPARATUS FOR THE DETERMINATION OF MOISTURE

the gas meter will serve as a guard to prevent moisture from backing into the first two tubes.

A-5.1.4.2 Procedure

Connect the 3 tubes in series to the inlet of the gas meter and connect the free end of U-tubes to the gas sample. Allow the gas to flow through the train for a while to saturate the water in the gas meter with the gas as well as replacing the air in the first two U-tubes. Stop the gas flow, close the stopcocks of the U-tubes and weigh the first two U-tubes. Connect again, record the meter reading. Pass the gas through the train at the rate of 10 litres per hour for 4 to 5 h. Close the gas supply and record the meter reading. Remove the first two U-tubes and weigh.

A-5.1.4.3 Calculation

Convert the volume of gas taken for the test to normal temperature and pressure. From the increase in weight, calculate the volume of water vapour present on the basis that 1 g of water is equivalent to 1.244 litres of water vapour at normal temperature and pressure and express the result as percentage by volume.

A-6 DETERMINATION OF CARBON DIOXIDE

A-6.1 General

Three methods have been prescribed, namely, infra-red analyser, electrochemical method and gas chromatographic method.

A-6.1.1 Infra-Red Analyser

The infra-red analysers are used for determining impurities of hetro-atomic gases. The hetro-atomic

gases absorb energy at characteristic wavelengths when subjected to infra-red radiation. The procedure to be followed for determining the impurities shall depend on the type of apparatus to be used. The instrument manufacturer's instructions in this regard shall be followed.

A-6.1.2 Electrochemical Method

When a gas containing carbon dioxide passes through a reactive liquid, the electrical conductivity of the liquid changes depending on the carbon dioxide content. The measurement of the change in electrical conductivity gives a direct measurement of the carbon dioxide content. The procedure to be followed shall depend upon the type of apparatus to be used. The instrument manufacturer's instructions in this regard shall be followed.

A-6.1.3 Gas Chromatographic Method

The procedure for carrying out the determination shall be the same as prescribed under A-2.

A-7 DETERMINATION OF CARBON MONOXIDE

A-7.1 General

Two methods have been prescribed namely, gas chromatographic method and infra-red analyser method.

A-7.1.1 Gas Chromatographic Method

The procedure for carrying out the determination shall be the same as prescribed under A-2.

4

IS 5760 : 1998

A-7.1.2 Infra-Red Analyser Method

The procedure for carrying out the determination shall be the same as prescribed under A-6.1.1.

A-8 DETERMINATION OF HYDROCARBONS

A-8.1 General

Three methods have been prescribed, namely, gas chromatographic method, infra-red analyser method and total hydrocarbon analyser method.

A-8.1.1 Gas Chromatographic Method

The procedure for carrying out the determination shall be the same as prescribed under A-2.

A-8.1.2 Infra-Red Analyser Method

The procedure for carrying out the determination shall be the same as prescribed under A-6.1.1.

A-8.1.3 Total Hydrocarbon Analyser Method

A-8.1.3.1 Principle

The sample containing hydrocarbon impurities is burnt in a jet of hydrogen in the flame ionization detector and the organic component present in the sample gas provide the source of ions. Concentration of ions is proportional to the concentration of organic components. Electrodes having considerable potential differnce between them are used to measure the current produced due to ionization and the instrument is calibrated in the terms of concentration of hydrocarbons.

A-8.1.3.2 Procedure

Calibrate the instrument against calibration gas of known concentration of hydrocarbon following the instructions of the manufacturer. Then carry out the test according to the manufacturers instructions.

ANNEX B

(Clause 7) SAMPLING OF COMPRESSED ARGON

B-1 SCALE OF SAMPLING

B-1.1 Lot

In any consignment, all cylinders charged at a time from one charging manifold shall constitute a lot.

B-1.2 The number of cylinders (n) to be selected from a lot shall depend on the size of the lot (N) and shall be in accordance with col 1 and 2 of Table 2.

B-1.2.1 The cylinders shall be selected at random and in order to ensure the randomness of selection, a random number table (see IS 4905) shall be used. In case such a table is not available, the following procedure shall be followed:

Starting from any cylinder in the lot, count them in one order as 1, 2, 3 up to r and soon, where r is the integral part of N/n. Every rth cylinder thus counted shall be withdrawn to give the sample for test.

B-2 TEST SAMPLES

A sample of gas shall be drawn from each cylinder selected as in B-1.2 and shall be the individual test sample from each cylinder.

Table 2 Number of Cylinders to be Selected (Clause B-1.2)

Lot Size (N)

(1) Up to 50

51 to 100

101 to 150

151 to 300

301 and above

Number of Cylinders to be Selected

(n) (2)

5

8

15

20

25

B-3 NUMBER OF TESTS

All the individual test samples in B-2 shall be tested separately for the requirements given in Table 1.

B-4 CRITERIA FOR CONFORMITY

A lot shall be declared as conforming to the requirements of this specification if all individual samples tested, pass the requirements prescribed in 5.2.

5

IS 5760 : 1998

ANNEX C

(Foreword) COMMITTEE COMPOSITION

Industrial Gases Sectional Committee, CHD 006

Chairman SHRI I MOOKHERJEE

Praxair India Private Limited, Raheja Towers, 6th Floor, East Wing, 26-27, M G Road, Bangalore 560001

Members SHRI A K AGARWALA

SHRI I B PRASAD ( Alternate ) SHRI A K ANEJA

SHRI M P DHANUKA ( Alternate )

SHRI D BANDHYOPADHYAY

SHRI S G K MURTHY ( Alternate ) SHRI SHAISH KUMAR

SHRI B B SHARMA (Alternate)

SHRI H P DUBEY

DR B B PAI ( Alternate ) SHRI T GARG

SHRI N K RAI ( Alternate I )

SHRI L R GARG ( Alternate II )

SHRI D R GHOSAI

SHRI M KALYANARAMAN( Alternate )

REPRESENTATIVF

SHRI P R NARASIMHAN

SHRI R P KATHOR

DR K N NINAN

SHRI A K MUKHOPADHYAY ( Alternate )

DR U C PANDEY

SHRI S S N PRASAD

DR BADRI PRASAD

DEPUTY CHIEF CHEMIST ( Alternate )

SHRI H N SINHA

SHRI N V S RAMANI

SHRI K P JAFFAR ALI ( Alternate ) SHRI M I ALAM

SHRI A S GHOSHAL

SHRI S K BHARDWAJ ( Alternate ) SHRI P K JAIN

SHRI R S SAIGAI

DR P L BHATIA ( Alternate ) SHRI B D REHANI

SHRI R N CHOKHSI ( Alternate ) SHRI S K KAPOOR

SHRI N SIKKA ( Alternate ) SHRI S K SRIVASTAVA

SHRI S P SINGH ( Alternate ) DR V N SINGH

DR R S RAJAGOPALAN,

Director (Chem)

Representing Hindustan Gas and Industries Ltd, 24 Parganas (WB)

Asiatic Oxygen Ltd, Calcutta

Steel Authority of India Ltd, New Delhi

Department of Industrial Policy and Promotion, New Delhi

National Test House, Calcutta

Industnal Gases Ltd, Calcutta

Rashtnya Chemicals and Fertilizers Ltd, Mumbai

IOL Ltd, Calcutta Bharal Electronics Ltd, Bangalore Bombay Oxygen Ltd, Mumbai Vikram Sarabhai Space Centre, Thiruvanathapuram

Department of Electronics, New Delhi Semi Conductor Complex Ltd, Punjab Central Revenues Control Laboratory, New Delhi

Asiatic Oxygen and Acetate Co Ltd, Calcutta Bharat Heavy Electncals Ltd, Hyderabad

Central Electronics Ltd, Ghaziabad Chief Controller of Explosives, Nagpur

Industrial Oxygen Co Ltd, Mumbai All India Industnal Gas Manufacturers Association, New Delhi

Gujarat State Fertilizer Corporation, Vadodara

Laxman Sylvanu Ltd, New Delhi

Ministry of Defence (DGQA), New Delhi

Ordinance Factory, Bhandara Director General, BIS (Ex officio Member)

Member Secretary SIIRI S MAJUMDER

JOINT DIRECTOR (Chem), BIS

6

( Continued on page 7 )

IS 5760 : 1998

( Continued from page 6 )

Representing Asiatic Oxygen Ltd, Calcutta

Electric Lamp Mfrs (I) Ltd, Calcutta

South India Carbonic Gas Industries Ltd, Chennai

National Test House, Calcutta

Industrial Gases Ltd, Calcutta

Rashtriya Chemicals Fertilizers Ltd, Calcutta Mohan Meakins Ltd, Mohan Nagar Gujarat State Fertilizer Corporation, Vadodara

Laxman Sylvania Ltd, New Delhi RDSO, Lucknow Kamrup Industnal Gases Ltd, Calcutta

All India Industrial Gas Manufacturers Association, New Delhi

Hindustan Lever Ltd, Mumbai

National Thermal Power Corporation, New Delhi

7

Oxygen, Argon, Acetylene, Hydrogen, Nitrogen, Carbon Dioxide, Helium Subcommittee, CHD 006 01

Convener

SHRI 1 MOOKHERJEE

Praxair India Private Limited, Raheja Towers, 6th Floor, East Wing, 26-27, M G Road, Bangalore 560001

Members SHRI R C AGGARWAL

SHRI M P DHANUKA (Alternate)

SHRI M M BANDOPADHYAY

SHRI S B BHATTACHARYA (Alternate)

SHRI F L DADABHOY

SHRI T JAGDEESAN ( Alternate )

SHRI H P DUBEY

DR S RAHUT ( Alternate ) SHRI T GARG

SHRI N K PAI ( Alternate I ) SHRI RAM SINGH ( Alternate II )

SHRI D R GHOSAL

DR E R JAYNARAYANA

SHRI M A PATEL

SHRI JASALPURA ( Alternate )

REPRESENTATIVE

REPRESENTATIVE

SHRI S L ROY

SHRI D K GARG ( Alternate )

SHRI R S SAIGAL

DR P L BHATIA( Alternate ) SHRI V K SHARMA

SHRI R J A PAI ( Alternate ) SHRI P K VERMA

SHRI P K BANERJEE ( Alternate )

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Amendments Issued Since Publication

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