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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
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timely dissemination of this information in an accurate manner to the public.

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Mazdoor Kisan Shakti Sangathan Jawaharlal Nehru
“The Right to Information, The Right to Live” “Step Out From the Old to the New”

IS 9434 (1992): Guide for sampling and analysis of free and

dissolved gases and oil from oil-filled electrical
equipment [ETD 3: Fluids for Electrotechnical Applications]

“!ान $ एक न' भारत का +नम-ण”

Satyanarayan Gangaram Pitroda
“Invent a New India Using Knowledge”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह”

है”
ह
Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”
 ( Reaffirmed 2003 )

Indian Standard
GUIDE FOR SAMPLING AND ANALYSIS OF
FREE AND DISSoLVED GASES AND OIL
FROM OIL-FILLED ELECTRICAL EQUIPMENT
f First Revision /

UDC 621*315*615*2
: 543*27

0 BLS 1992

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

December 1992 Price Group 8

 - ,

Fluids for Electrotcchnical Applications Sectional Committee, ET 03

FOREWORD

This Indian Standard ( First Revision ) was adopted by the Bureau of Indian Standards, after the draft
finalized by the Fluids for Electrotechnical Applications Sectional Committee had been approved by the
Electrotechnical Division Council.
The growing importance of gas analysis of samples drawn from oil-filled electrical equipment has led to
the preparation of this guide which gives the procedures to be used for the sampling of gases and oils
containing gases and for their subsequent analysis.
This standard deals with the methods for sampling of free gases and oil from electrical equipment such as
power and instrument transformers and oil filled cables and for analysis of free gases and the gases dissolved
in the oil.
First revision of this standard has been taken up to align it with the latest procedure followed by the indus-
try and also to make it align with IEC methods as far as practicable.
The methods described in the main part of this guide are suitable for oil samples and take into account the
problems imposed by the transport of samples by unpressurized air freight, and where differences in
temperature exist between the plant and the examining laboratory.
Annexes give alternative methods of sampling and describe alternative methods applicable for the prepara-
tion of oil samples for the analysis of their dissolved gases, and for the analysis itself.
In preparing this standard, assistance has been derived from IEC Pub 567 ( 1977 ) ‘Guide for the sampling
of gases and oil from oil-filled electrical equipment and for the analysis of free and dissolved gases’ issued
by the International Electrotechnical Commission ( IEC ) and document IEC 10 ( CO ) 260 ‘Revision of
IEC Pub 567 ( 1977 )‘.
For the purpose of deciding whether a particular requirament of this standard is complied with, the final
value, observed or calculated, expressing the result of a test, shall be rounded off in accordance with
IS 2 : 1960 ‘Rules for rounding off numerical values m&d)‘. Tha number of significant places retained
in the rounded off value should be the same aa that o I the specified value in this srandard.
 IS9434:1992

Indian Standard
GUIDEFO SAMPLINGANDANALYSISOF
FREEANDDIS§OLVEDGASESANDOIL
FROM OIL-FILLEDELECTRICAL EQUIPMENT
/First Revision )
1 SCOPE 2 INTRODUCTION

2.1 Gases may be formed in oil-filled electrical

1.1 This guide deals with the methods for
equipment due to natural ageing, but also to a
sampling and analysis of free gases and ~for
much greater extent as a result of faults. The
sampling and analysis of gases dissolved in oil,
principal mechanisms of gas formation include
from oil-filled equipment such as power and
oxid ation, vapourization, insulation decomposition,
instrument transformers and oil-filled cables.
oil breakdown, and electrolytic action.
1.2 This guide assumes a measure of competence 2.2 Operation with a fault may seriously damage
in the technique of gas chromatography and the equipment and it is valuable to be able to
omits, for brevity, many details which may be detect the fault at an early stage of development.
found in practical manuals on these techniques.
2.3 In the case of a fault. its type and its severity
1.3 The methods described in this guide are may often be inferred from the composition of the
suitable for all samples and take into account the gases and the rate at which they are formed. In
problems imposed by the transport of samples by the case of an incipient fault the gases formed
unpressurized air freight, and where considerable remain partly dissolved in the liquid insulation;
difference in ambient temperature exists between free gases will be found only in special cases. The
the plant and the examining laboratory. dissolved gases will divide between the gaseous
and liquid phases by diffusion. Diffusion and
1.4 Alternative methods of sampling as given in achievement of saturation both take time, during
Annexes A and B may be used and Annexes G which serious damage to the equipment can
and D describe alternative methods applicable for occur undetected.
the preparation of oil samples for the analysis of
their dissolved gases and for the analysis itself. 2.4 Periodic analysis of oil samples for the amount
and composition of dissolved gases forms a means
1.4.1 Glass containers, when used, should be of of detecting faults.
amber colour or protected from sunlight. Glass
bottles should be capable of being sealed gas-tight 2.5 The growing importance of gas analysis of
either by a ground glass stopper or a screwed samples drawn from electrical equipment has led
plastic cap holding a conical polyethylene seal. to the preparation of this guide to the procedures
Any other containers, for example, plastic or glass to be used for the sampling from oil-filled electri-
with rubber or bark cork and the use of sealing cal equipment of gases and oil containing gases
material like tape, lac, plaster of paris shall be and for their subsequent analysis.
strictly avoided.
2.6 The provision of a guide for the evaluation
1.5 Experience so far shows that there is a wide of the results of gas analysis will be the aim of
scatter in results obtained by different laboratories future work.
on 011 samples from the same source. An agreed
standard of reproducibility of results among 3 SAMPLING
different laboratories can be arrived at only after
consistency is established by all concerned with 3.1 Sampling of Gases from Gas Cushions
respect to oil sampling, gas extraction and gas and Gas-Collecting ( Buchholz ) Relays
analysis procedures.
3.1.1 General Remarks

1.6 The results and interpretation thereofcan be Gas samples from relavs should be taken from the
significant only if the approprtate apparatus and equipmertt with the mir~imum del,ry Changes in
techmques are used at all times. Otherwise, even composition caused bv the selective reabsorption
the assessment of gas formation rates between of components may occur if free gases are left in
different times can be erratic and misleading. contact with oil

1
IS 9434 : 1992

Certain precautions are necessary in the taking of :aken, cock (2) is closed and the apparatus is
gas samples. The connection between the sampl- disconnected.
ing device and the sampling vessel must avoid
the ingress of air. Temporary connection should 4ny oil in the syringe is expelled by inverting
be as short as possible Any rubber or plastic :he syringe and applying gentle pressure to the
tubing used should have been proved to be plunger.
impermeable to gases.
In the absence of a positive pressure within the
Gas samples should be properly labelled ( see 4 ) equipment, a supplementary air pump should
and analyzed without delay, and in any case be connected between the equipment sampling
within 7 days. valve and cock (2) and used to pump gas from the
equipment.
Oxygen, if present in the gas, may react with any
oil drawn out with the sample. Oxidation is
The equipment sampling valve (5) must be closed
delayed by excluding light from the sample, for
at the end of sampling.
example, by wrapping the syringe in aluminium
foil. The transport of samples is facilitated by the
use of special containers which hold the samples 3.2 Sampling Oil from Oil-Filled
firmly in place during transport. Equipment

The methods given in Annex A may be used as 3.2.11 General Remarks

alternative to the method given below.
The method of sampling with syringes ( given
Changes in the composition of gases generated by below ) is suitable irrespective of the mode of
a fault always occur during their movement to transportation of samples Other methods, given
the gas collecting relay. Information on the dura- in Annex B, may be used if there are no significant
tion of a fault may often be inferred by comparing changes of temperature and pressure during
the composition of free gases with those remaining transportation. For routine sampling on a large
dissolved in the oil and, since selective reabsorp- scale, the use of bottles or sampling tubes, rather
tion of components can also occur in the oil than syringes, may be the most economical
remaining within the relay, undue delay in sampl- method. The methods described are suitable for
ing may conceal valuable evidence. large oil-volume equipment such as power trans-
formers. With small oil-volume equipment, it is
3.1.2 Sampling Equipment
essential to ensure that the total volume of oil
The following sampling equipment is used: drawn off does not endanger the operation of the
equipment.
4 An impermeable oil resistant plastic or
rubber tube provided with a connector to The selection of points from which samples are
fit onto a suitable sampling connection of drawn should be made with care. The sample
the relay or gas cushion; should normally be taken from a point where it is
representative of the body of the 011 in the equip-
b) A gas-tight syringe of suitable size ( 25 cm3
ment and where changes in composition such as
to 250 ems ). Medical or veterinary quality
those due to pump cavitation do not exist. For
glass syringes with ground-in plungers may
forced-oil-cooled transformers, the oil pumps
be suitable; alternatively, syringes with oil-
should be run for at least ten minutes before
proof seals may be used ( see 3.2.2.2 ); and
samples are drawn from an area of moving oil
c) Tran {port containers - These should be such as inlet to a cooler.
designed to hold the syringe firmly in place
during transport. It will sometimes be necessary, however, delibera-
tely to draw samples where they are not expecter1
3.1.3 ,Yampling Procedure to be representative, for example, in trying to
The apparatus is connected as shown in Fig. 1. locate the site of a fault.
The connections should be possible and filled with
oil at the start of sampling. Samples should be taken with the equipment in
its normal working condition, so that the true
Sampling valve (5) is opened. If a positive pres- rate of gas production can be assessed. Oil samples
sure exists, the three-way cock (4) is carefully should be collected after free flushing of containers
opened and any oil present allowed to flow to to make sure any previous residual material is
waste When gas reaches the three-way cock (a), completely removed.
the latter is turned to disconnect the waste and
connect the syringe. Cock (2) is then opened and Two samples, instead of one, drawn at a time will
the syringe allowed to fill under the hydrostatic serve to check the consistency of results and help
pressure, taking care that its plunger is not improve reproducibility. Sample containers must
expelled. When a sufficient sample has been be full and completely sealed.

2
 IS 9434 I 1992

1 Svrioge 5 Equipment sampling valve

2 Cock 6 Gas-collecting relay and cushion valve
3 Connecting tubes I Waste vessel
4 Three-way cock

FIG. 1 SAMPLING BY SYRINGE

Some of the dissolved oxygen present in the oil the beginning and at the end of this period. An
sample may b$ consumed by .oxidation. The acceptable syringe will permit losses of hydrogen
reaction can be delayed by exdlusloa of light, for of less than 2.5 percent each week.
example, by wrapping the sampling vessel in
aluminium foil. 3.2.2.3 Transport container

Samples should be carefully labelled ( see 4 ). These should be designed to hold the syringe
Analysis of samples should be completed with the firmly in place during but allow the syringe
minimum possible delay, in any case not later plunger to be free.
than 7 days. !
3.2.3 Sampling Procedure
3.2.2 Sampling’ E&&ent
3.2.3.1 The blank flange or cover of the sampling
3.2.2.1 An impermeable oil-#roof plastic or rubber tube valve is removed and the outlet cleaned with a
to connect the equipment to the syrznge lint-free cloth to remove all visible dut. The
apparatus IS then connected as shown in Fig. 2,
This shall be as short as possible, A three-way
and the main sampling valve opened.
cock shall be inserted in the tube.

The connection between the tube and the equip- 3.2.3.2 The three-way cock is adjusted to allow
ment will depend upon the design If a sampling 1 litre to 2 litres of oil to flow to waste.
valve suitable fi)r fittmg to a tube has not been NOTE - In the case of small oil-volume equipment
provided, it may be necessary to improvise by the above procedure may be omitted and a small-
using stopper drilled flange, or a bored oil-proof volume syringe used.
rubber on a drain or fitted connection.
3.2.3.3 The three-way cock is then turned to
3.2.2.2 Gus-tight syringe allow oil to enter the syringe slowly The plunger
should not be withdrawn but allowed to move
This may be all glass or have plastic or oil-proof
back under the pressure of the oil.
rubber seals and a glass or plastic plunger. The
size may be 25 ems to 2.50 ems, largely depending
3.2.3.4 The three-way cock is then turned to allow
on the sensitivity of the analytical procedure and
the oil in the syringe to flow to waste and rhe
the volume of oil of the system to be sampled. The
plunger pushed to empty the s\,ringe (:o firm
syringe should be fitted with a cock enabling it to
that thr inner surfaces of the syringe and plunger
be sealed.
are complrtely oiled
The gas-tightness of a pattern of syringe may be
tested by storing an oil sample in a s\ringe for 3.2.3.5 The procedure described in 3.2.3.3 is then
two weeks and analyzing aliquots for hydrogen at repeated.

3
 a) FLushing connection.

b) Wetting and flushing of syringe.

c) Emptying of syringe.

d) Taking of sample.

e) Disconnecting of syringe.

FIQ. 2 SAMPLINQ WITH A SYRINGE

3.2.3.6 The cock on the syringe is then closed 3 Temperature of sample when drawn ( in
and the sampling valve closed. the case of oil );
3.2.3.7 The syringe is then disconnected. W Other pertinent data, for example, type of
tap changer if fitted, operation of pumps,
4 LABELLING OF SAMPLES oil preservation system, etc;
4.1 Oil and gas samples should be properly ml Date of commissioning of the transformer;
labellrd before despatch to the laboratory and the Date of last filtration of oil;
following information is desirable: n)
P) Details of repair ( if any ) carried out since
a>Customer or plant; the commissioning of transformer; and
b) Identification of equipment; 9) Previous result of DGA.
C) Object of sampling; 5 PREPARATION OF SAMPLES FOR
4 Date of sampling; ANALYSIS
e) Load at the time of sampling; 5.1 Gas Samples
f 1 Point where sample is taken; Gas samples require no special preparation and
g) Type of oil ( if known ); must be analyzed in the condition in wl~icll t!!fay
hl Volume of oil in equipment; are received at the la!)oratory,

4
 IS 9434 I 1992

5.2 Oil Samples 0.05 ems, or preferably O-01 ems or corres-

ponding pressure and to ensure that the
5.2.1 General Remarks gas extracted from different strokes is well
mixed before analysis.
These samples require preliminary treatment to
remove the dissolved gases for analysis. In the NOTE -Attention is drawn to the need for
method described in 5.2.3, the gases are extracted adequate precautions in the use of mercury to
from the oil by vacuum. The procedure described avoid danger to the health of operators.
in 5.2.3 can deal with any volume of oil and is
suitable for both low and high gas contents. With 5.2.3 Extraction Procedure ( see Fig. 3 )
a suitable apparatus, the volume of gases extracted
can be measured The extraction of gases will, 5.2.3.1 IYeigh the syringe (1) and connect it to
however, be incomplete, particularly that of the the degassing flask (10).
more soluble components but for the gases listed
in 6.1, it will normally be possible to extract 97 5.2.3.2 Evacuate the apparatus to O*l mbar using
to 99 percent of the total quantities present. either the Toepler pump (12) or an auxiliary
pump.
Oil samples may, on contraction, release bubbles
of gas which change the composition of the gases 5.2.3.3 Open the syringe cock and admit oil into
which remain dissolved, and this may cause an the degassing flask and switch on the magnetic
error in the analysis. The magnitude of the error stirrer.
will depend on the size of bubble in relation to
the volume of the oil sample and on the solubility
Degassing is improved by increasing the surface
of the gases.
of the oil such as by allowing the oil to enter
through a sintered filter or by impinging the jet
The bubble may sometimes be redissolved by care- of oil against the wall of the flask. The syringe
fully warming the sample and holding it for some stopcock should be closed while some oil still
time at the temperature at which it was taken. remains in the syringe, thus avoiding subjecting
Alternatively, the whole of the sample, including the syringe to vacuum,
the bubble, can be introduced into the laboratory
gas extraction apparatus.
5.2.3.4 Operate the Toepler pump and transfer
Some other methods are available which are the gas into the burette (13). Degassing will
specially suitable for routine use. These are des- be complete when no increase in the volume of
extracted gas is observed (see 5.2.2 ). For conveni-
cribed in Annex C.
ence, an automatic Toepler pump may be used in
place of the manual version.
5.2.2 Extraction ApParatus
A suitable design of apparatus is shown in Fig. 3. 5.2.3.5 Reweigh the syringe to obtain the mass
of 011 degassed. Measure the volume of extracted
The requirements of any apparatus used are as gas and record pressure and temperature.
follows:

a>Itvacuum
shall be capable of subjecting
of below 0.1 mhar;
theoil to a 5.2.3.6 Calculate the gas content of the oil sample
in microlitres per litre at 20°C and 1 013 mtar by
It shall be vacuum-tight. When subjected, the equation:
b)
when empty, to a vacuum of 0.1 mbar and
left for 3 hours, the vacuum should not P 243
x + x 10s
have changed; 1013 ’ 273 + t
It shall be tested for efficiency, and the
where
number of operations needed to extract at
least 97 percent of the dissolved gases
should be established by a preliminary P - pressure of the extracted gas in mbars;
test. t = temperature of the extracted gas in “Cl;
This may be done by extracting two identi-
cal samples, one for a. strokes and another V = volume of the extracted gas in cm3 at
fix 2n strokes, and establishing a value of tl pressure P;
such that no significant difference between
the two analyses can be found; and d = density of the oil in g/cm3 at 20°C;
and
It shall permit the measurement of the
extracted gas to be made to the nearest m = mass of the degassed oil in g.

5
IS 9434 : 1992

6 GAS ANALYSTS BY GAS-SOLID A precision gas-tight syringe may be used instead

CHROMATOGRAPHY of the injection valve.

6.1 General Remarks 6.2.2 Columns

Gas samples, whether obtained from gas cushions Several columns have been tried and found to be
or gas collection relays or removed from an oil suitable. Some suitable arrangements are described
sample, are analyzed by chromatography. The in Annex D, but many other arrangements are
gases to be determined are: possible.
a) hydrogen Hs 6.2.3 Carrier Gas
b) oxygen 0s
Helium, argon or nitrogen of grades suitable for
c) nitrogen Ns gas chromatography are normally used.
d) methane CHI
e) ethane 6.3 Calibration
t&H,
f ) ethylene ‘&HI The chromatograph is calibrated by the injection
g) acetylene of known amounts of pure gases to establish the
t&H, calibration curve and the retention time. For
h) carbon monoxide CO daily calibration checks, it is convenient to use
j) carbon dioxide COO a standard gas mixture containing a suitable
known amount of each of the gas components to
The determination of Cs hydrocarbons and argon be analyzed and diluted by nitrogen. Calibration
may be useful. may be in terms of molarity, partial pressure or
A number of methods may be used for the analy- volume.
sis. The method described in D-l is an example
of one which is acceptable. 6.4 Procedure for Gas Analysis

6.4.1 General Remarks

To obtain the sensitivity required in 7, both a
flame ionization detector for hydrocarbons and a Any convenient method may be used, provided
thermal conductivity unit for atmospheric gases that the sensitivity requirements are met. One
CO, CO, and Hs will be needed. example is given in detail in D-l and others in
outline in D-2.
A single stationary phase capable of resolving all
the gases under isothermal conditions is not 6.3 Calculations
available.
6.5.1 Measure the area of each peak and note its
Single column operation is possible but only with retention time.
temperature programming and sub-ambient start- 6.3.2 Identify the gas corresponding to each peak
ing temperature. Isothermal operation requires by comparison with the chromatogram obtained
two columns and these may be operated in paral- by calibration and apply the calibration data to
lel or switched. obtain the gas volume.
The carrier gas may be helium or argon or 6.5.3 Convert the gas volume to microhtres of
nitrogen. Helium gives improved sensitivity for gas per litre of oil.
carbon man-oxide with loss of sensitivity for
hydrogen. While with argon, improved sensitivity 7 SENSITIVITY AND PRECISION
for hydrogen is gained at the expense of loss of
sensitivity for carbon monoxide. 7.1 The detection limits for gases dissolved in oil
shall meet the following requirements:
A wide range of compositions can be expected
a) Hydrogen 5 pi/l oil ( 5 ppm )
and, to avoid constant alterations to the attenua-
tor settings, it will be convenient to use an b) Hydrocarbons 1 &l oil ( 1 ppm )
integrator. c) Carbon oxides 25 &l oil ( 25 ppm )
d) Atmospheric gases 50 pi/l oil ( 50 ppm )
6.2 Apparatus

6.2.1 Gas Ckromatograpky 7.2 For free gas samples, a sensitivity equivalent
to that obtained by the analysis of the gases
Any instrument, preferably fitted with both flame extracted from the oil is required.
ionization and thermal conductivity detectors, can
be used. Gas samples shall be injected preferably 7.3 Repeatability should be such that analysis of
by means of a properly deslgned injection valve two samples of the same oil, taken at the same
capable of injection of 0.5 ems to 5 cm3 gas time and tested consecutively, should agree to
volume ( see Fig. 4 ). within 5 percent of the higher value.

6
 IS 9434 : 1992

1 Sampling syringe 10 Degassing flask

2 Cock 11 Magnetic stnrer
3 Connecting tube 12 Tot pler pump
4 Three-way cock 13 Burette
FIG. 3 GAS EXTRACTIONAPPARATUS

016

016

14 Chromatograph gas sample valve 18 Recorder

Column selector valve I9 Integrator
:6” Columns 20 Connection to vacuum
17 Detectors 21 Switch
FIG. 4 ScHEa!ATIa ARRANGEMENT
FORGAS CHROMATOORAPHY

ANNEX A
( Clauses 1.4 and 3.1.1 )

SAMPLING OF GASES

A-l GENERAL REMARKS used, the different solubilities of the gas compo-
nents need to be taken into account. Brine as a
A-l.1 The methods described in this Annex may
sealant may be drawn into unflushed gas cushions
also be used instead of those described in 3.
if these are under a slight vacuum.
A-l.2 Sampling by liquid displacement using
either saturated brine or transformer oil as a A-1,3 The vacuum method requires skill to avoid
sealing fluid is simple but has drawbacks. If oil is contaminating the sample by leakage.

7
Is 9434 t 1992

A.2 SAMPLING BY VACUUM A-3 SAMPLING BY LIQUID

DISPLACEMENT
A-2.1 The apparatus is connected as shown in A-3.1 Degassed transformer oil or saturated brine
Fig 5. With the equipment sampling valve (5) may be used as sealing liquid in the alternative
closed and both cocks (21 open, and the three-way designs of apparatus shown in Fig 6 and 7. The
cock (4) turned as shown in the figure, the principles of both designs are similar.
vacuum pump is allowed to evacuate the connect-
A-3.2 The connecting tube is filled with oil either
ing tubing, the trap and the sampling vessel.
from a separate vessel, or if the connection
A-2.2 A satisfactory between the relay and the sampling valve is filled
vacuum will be below
I mbar. The system should be checked for leaks with oil, by allowing this oil to fill the connecting
by closing the pump suction cock and observing tube.
that no appreciable change in vacuum occurs A-3.3 The open end of the tube is connected to
within a time equal to that which will be taken for the gas sampling valve. The sampling valve and
sampling. inlet cock of the sampling vessel are carefully
opened. If the apparatus in Fig. 6 is used, the
A-2.3 If the connecting tube between the equip- sampling vessel is then inclined so that its closed
ment sampling valve (5) and the gas collecting end becomes its lowest point. Outlet cock (2) on
relay has been filled with oil, the three-way cock the sampling vessel is then opened, allowing the
is turned to position (A). The equipment sampling sealing liquid to run to waste, thus drawing the
valve (5) is carefully opened and oil allowed to gas into the sampling vessel.
flow into the trap. When the end of the oil stream A-3.4 If the apparatus in Fig. 7 is used, the lower
is observed to reach the three-way cock, it is turn- cock on the sampling vessel is opened and the
ed to position (El). When sampling is complete levelling bulb lowered, drawing sample gas into
cock (2) is closed first, then the equipment sampl- the sampling vessel,
ing valve (5) and the apparatus disconnected. A-3.5 In both cases, sampling is complete when
the gas-collecting relay is completely filled with
A-2.4 If the connecting tube between the equip- oil or when nearly all the sealing liquid in the
ment and the sampling valve is empty, the sampling vessel has been displaced.
procedure for draining oil is omitted and the A-3.6 Both the cocks on the sampling vessel and
three-way cock used in position (B) after testing the equipment sampling valve are closed and then
tha’t the apparatus is leak-proof. the connections removed.

POSITION @

COCK @
POSITION @ IL
=dv-

1 Sampling vessel 5 Equipment sampling valve

2 Cock 6 Gas collecting relay and cushion valve
3 Connecting tubes 0 Vacuum gauge
4 Three-way cock 9 Trap
FIO. 5 SAMPLING BY VACUUM
8
 JS 9434 : 1992
I

Fro. 6 SAMPLINQ BY LIQUID DISPLACEMENT( U’SINODECASSEDTRANSFORMER

01~ )

Cock 7 Waste vessel

Connectingtubes 28 Sampling vessel
Equipment sampling valve 29 Levelling bulb
Gas collecting relay and cushion valve
FIN. 7 SAMPLINGBY LIQUID DISPLACEMENT

ANNEX B
( Clauses 1.4 and 3.2.1. )

SAMPLING OF OIL

-B-l GENERAL REMARKS volume are involved. This method may be used
in conjunction with the ‘partial degassing method’
B-l.1 The general principles are outlined
( see C-3.2 ).
in 3.2.1.
B-l.2 The method using sampling vessels or B-1.3 The method using bottles is simple, requires
‘bombs’ is convenient especially when oils with little skill and will be adequate for many pur-
low dissolved gas contents requiring a large sample poses.
IS 9434 t 1992

B-2 SAMPLING BY SAMPLING TUBE have screwed plastic caps holding a conical poly-
ethylene seal.
B-2.1 The sampling tube ( see Fig. 8 ), may be of
glass or metal and of volume 250 cm3 to 1 litre. B-3.2 Before accepting a design of bottle, its gas-
Itmay be closed either by cocks or pinch cocks tightness should be proved by taking identical
on impermeable oil-resistant rubber tubing, or by samples in two bottles, and making an analysis
valves. for dissolved hydrogen content using one bottle at
the beginnmg and one at the end of a P-week
B-2.2 The sampling tube is connected to the storage period.
sample point by tubing. The cocks on the sampling
tube are opened and the sampling valve on the B-3.3 A bottle and seal design is acceptable if it
equipment carefully opened, so that oil flows permits losses of hydrogen of less than 5 percent
through the sampling tube to waste. each week.
B.2.3 After the sampling tube has been comple- B-3.4 A design of seal cap found satisfactory is
tely filled with oil, about 1 litre to 2 litres are shown in Fig. 9.
allowed to flow to waste.
B-3.5 The connection to the sample point may
B-2.4 The oil flow is then closed by shutting off
be made by oil-proof plastic or rubber tubing
firstly the outer cock, then the inner one and
about 5 mm diameter.
finally the sampling valve.
B-2.5 The sampling tube is then disconnected. B-3.6 If the connection is to be made to a drain
valve for sampling, use should be made of suitable
B-3 SAMPLING BY BOTTLES oil-proof bung drilled to take a 5 mm diameter
B-3.1 This method requires the use of bottles brass tube. A set of bungs 12 mm to 100 mm will
capable of being sealed gas-tight. Suitable bottles fit almost every unit.

028

2 Cock 7 Waste vessel

3 Cconnecting tubes 28 Sampling vessel ( sampling tube )
5 Equipment sampling valve
Fm. 8 EQUIPMENTFOR SAMPLINGOILSFROM TRANFPORMRRS: BY SAMPLINGTUBE

10
 IS 9434 : 1992

HARD PLASTIC SCREW

CAP

CONICAL SOFT POLYETHYL ,ENE

SEAL

BOTTLE

FIQ.9 SEAL CAP FOR SAMPLING BOTTLE

B-3.7 The sampling valve is opened and about tube is gently withdrawn with the oil flow
1 litre of oil allowed to flow to waste through the continuing. The bottle is then tilted, allowing the
tube. The end of the tube is then placed, with the oil level to fall to 1 mm to 2 mm from the rim
oil still flowing, at the bottom of the sampling and the bottle cap is placed in position. The
bottle and the bottle allowed to fill. After allowing sampling valve is then closed.
about one bottle volume to overflow, the sample

ANNEX C
( Clauses1.4 and 5.2.1 )

PREPARATION OF OIL SAMPLES FOR ANALYSIS

C-1 GENERAL REMARKS C-2.1 Torricelli Vacuum Method

C-l.1 This Annex describes optional methods. C-2.1.1 The apparatus shall conform to the
C-l.2 The Torricelli vacuum method is basically general principles described in 5.2.2.
a field version of the Toepler pump method. C-2.1.2 Assemble the apparatus as shown in
C-1.3 The partial degassing methads allow the Fig. 10, with cocks (2) and (3) closed. A tempo-
oil sample to come into equilibrium with vacuum rary connection to a vacuum pump, if available,
in a known volume, and correction for gases is made at the upper cock (4). Lower the mercury
remaining dissolved is made with the solubility level to empty flask (11).
data.
C-l.4 One variant of this method, which uses a C-2.1.3 With both cocks (4) open, evacuate the
whole apparatus using the vacuum pump If a
large vacuum-to-oil ratio, approaches the Toepler
vacuum pump is not available, the evacuation is
method.
done by using the apparatus as a Toepler pump.
C-l.5 The second variant uses an almost equal
vacuum-to-oil ratio and is useful for rapid screen- C-2.1.4 Close upper cock (4) and lower mercury
ing. Since equilibrium can be achieved immedia- reservoir (30) to bring the mercury level to the
tely after extraction, this method avoids many of bottom of flask (1 I).
the difficulties associated with sample transport. It
Check the tightness of the apparatus.
is also useful for dealing with those gas samples
taken by the oil displacement method, where the C-2.1.5 Slowly open Cock (2) on the sample
gas volume is insufficrent to displace the whole of syringe ancl cock (3) on the degassing flask. Allow
the oil used as a sealant. about 30 cm3 of oil to flow into the dcgassing flask.
( If a sampling tube is used in place ot a syrir:ge,
C-2 EXTRACTION OF DISSOLVED GASES
open the outer cock, and then slowly, the inrler
C-2.0 Two different methods fcr the extraction of cock ). Finally close cock (3) on the degassing
dissolved gases are described below. flask.

11
IS 9434 : 1992

C-2.1.6 Transfer the evolved gas to gas burette C-2.2.5 Heat, if required, degassing flask using a
(13). water bath and allow the temperature to come up
to 70°C.
C-2.1.7 Close lower three-way cock (4), lower the
reservoir until the oil has flowed into the lower C-2.2.6 Quickly transfer 50 ml of oil from sample
vessel and again compress the liberated gases into bottle to oil funnel. Care is taken that air bubble
the gas burette. is not trapped between oil and stopcock (1).

C-2.1.8 Repeat the operation, described in point C-2.2.7 Open the stopcock (1) slowly and transfer
(6), about four to six times until no further extrac- oil into the degassing flask. Care is taken so that
tion is observed. degassing flask is not open to atmosphere. This
can be avoided by leaving some oil in the limb
G-2.1.9 After the oil in the degassing flask has before closing the stopcock. Switch on the magne-
been degassed, turn lower three-way cock (4) and tic stirrer.
discharge the degassed oil through the oil outlet.
Collect all the discharged oil since after the C-2.2.8 Isolate the vacuum pump by turning the
degassing procedure the total volume of degassed stopcock (3).
oil has to be determined.
C-2.2.9 Open the stopcock (1) in such a way as
C-2.1.10 Repeat these operations until a sufficient to connect degassing flask to gas collecting bulb.
amount of gas has been collected in the burette.
C-2.2.18 Allow 20 minutes for degassing to com-
C-2.1.11 Open lower three-way cock (4) and raise plete.
the mercury reservoir until the gas pressure inside
C-2.2.11 Transfer the evolved gas from gas
the gas burette has reached atmospheric pressure
collecting bulb into the burette by operating the
and read the gas volume from the graduations on
stopcocks ( 1 and 2 ) and raising the mercury
the burette.
reservoir.
Record the ambient temperature and barometric C-2.2.12 This operation is repeated at least 5 times
pressure. by alternatively connecting the gas collecting bulb
C-2.1.12 Determine the total volume of oil which (5) to degassing flask and then to mercury reser-
has been degassed. voir so that all the evolved gas is transferred in
the gas measuring burette. Stop the stirrer.
C-2.1.13 Calculate the gas content of the oil
sample in microlitres per litre at 20°C, and C-2.2.13 The gas volume at atmospheric pressure
1 013 mbar by the equation: is measured by keeping the mercury in the
P 293 burette as well as in the mercury reservoir at the
---
1013 ’ 273 +t
x$ x 106 same level.
C-2.2.14 After measuring the volume, the gas is
where transferred into the gas withdrawal port by turn-
ing the stopcock (3) such as to connect it to gas
P = pressure of the extracted gas in mbars,
measuring burette.
t = temperature of the extracted gas in “C,
lJr- volume of the extracted gas in cm3 at C-2.2.15 The sample is pressurized by raising the
pressure P, and mercury reservoir and measured amount of gas is
taken from the port with the help of gas-tight
u = volume of the degassed oil in cubic syringe and injected to GC for analysis. The gas
centimetres. sample should be kept at pressure above atmos-
~-2.2 Operating Procedure for Gas phere for sampling with gas-tight syringe.
Extraction Apparatus c-3 PARTIAL DEGASSING METHOD
G-2.2.1 Fix the mercury reservoir position at the C-3.1 Partial Degassing Method
lower end of the stand before evacuating the ( Laboratory Version )
system. ( Arrangement shown in Fig, 10A and
10B ). The apparatus is shown in Fig. 11.
Samples are introduced through a narrow bore
G-2.2.2 Attach the degassing flask containing
polytetrafluoroethylene tube which terminates in
strurer into the system.
a connector matching that on the sample syringe.
G-2.2.3 Evacuate the system by opening appro- The degassing flask has sufficient volume to con-
priate stopcocks. tain 50 cm3 of oil below the end of the inlet tube.
The flask contains a magnetic stirrer.
C-2.2.4 Check whether system is maintaining
vacuum; the apparatus must be free of leaks. The The volume of the vacuum expansion flask is
system blank for l/2 hour must be less than large compared with that of the oil sample 500
0.1 ml. cm3 being suitable. The burette is calibrated in

12
 IS 9434 : 1992

RUBBER
/ SEPTUM
GAS I
WITHDRAWAlf
PORT

WRETTE

FUNNEL
FOR OIL

“A::“M
PiJMP

TO EXTRACT10
DFGASQNC ii
APPARAT

FLASK
t
HOT PLATE CUM
MAGNETIC STIRRER MAGNETIC STtRRER
SAMPLING USING
HYPODERMIC SYRtNGE

Fm. 10A GAS EXTRACTIONSYSTEM

“3.01 cm3 divisions and has a total volume of and burette is designated VC, the total volume I/T.
3.5 cm3. It terminates in a septum holder shown The ratio Vo/VT is defined as the volumetric
inFig. 11. collection ratro.
C-3.1.1 Preliminary The total volume T:r is calculated by:
C-3.1.1.1 The apparatus shall be free of leaks and
should be capable of evacuation to 10-6 mbar,
v, = 6k - VOll

preferably 10-s mbar. where Li;, is the empty volume of the SJ stem cm-
C-3.1.1.2 The volume of the apparatus shall be sisting of burette (13), expansion flask (21) and
established. The volume of the expansion flask degassing flask (I 1).

13
18 9434 : 1992

SAMPLING

WITH VALVES

:. :

i, ; ,,’

?
- ST&ND
: .
‘. ,

.:

TO DEGASSING ,ll,: I
FLASK THROUGH
: : STOP COCK

Fra. 1OB: ‘ARRAN&.MENT FORTRANSFERRING OIL SAMPI E FROM SAMPLINCJCYLINDER TO GAS

EXTRACTION SWTEM
C-3.1.2 Procedure ; C-3.1.2.5 Close cock (2) to the vacuum pump and
then SIUWIVopen three-way cock (4) to ahow oil
C-3.1.2.1 Lower the mercury level of the expan- and any gas bubbles that may be present in the
sion flask. sample syringe to enter the degassing flask.
C-3.1.2.2 Evacuate the system of expansion and C-3.1.2.6 Allow the desired amount of oil to enter
degassing flasks to a pressure of 1 x lo-3 mbar the degassing flask and operate the magnetic
or less. stirrer vigorously for approximately 10 minutes.

C-3.1.2.3 Connect the oil sample syringe by PTFE C-3.1.7.7 Close cock (5) isolating the expansion
tubing to three-way cock (4) leading to the flask and allow mercury to flow into it.
drgassing flask.
C-3.1.2.8 Open cock (6) to the reference column
C-3.1.2.4 Flush to waste a small quantity of oil and by means of mercury reservoir (30), bring the
from the syringe through the tubing and cock level of the mrrcury in the reference column to
making sure that all the air in the connecting that in the burette.
tubing is displaced by oil. C-3.1.2.9 Measure the volume of extracted gas in
the burette and correct by dividing it by the
Any gas bubbles present in the syringe should be
volumetr.ic collection ratio defined in C-3.1.1.2.
retained during the flushing operation and inclu-
ded in the measurement of total gas content and Correct to 2VC: and 1 013 mbar. Determine the
subsequent analysis. volume of ~1 degassed.

14
 IS 9434 : 1992

C-3.1.2.10 Increase the pressure of the extracted C-3.2.3.8 Analyze the gas in the upper vessel
gas contained in the burette slightly above atmos- following the procedure described in C-3.2.4.
pheric pressure by rising the level of the mercury
C-3.2.3.9 Displace the oil sample, clean and dry
in the reference column.
both sample vessels and re-weigh them in order
C-3.1.2.11 Insert the needle of the gas-tight in- to determine the total weight of oil sample. Deter-
jection syringe through the septum of the burette mine the volume of the pair of glass vessels by any
and withdraw a suitable volume of gas into the convenient method.
syringe.
C-3.2.4 Analysis
Adjust the gas pressure, as indicated by the refe-
rence column, precisely to atmospheric pressure The sample vessel containing the gas sample is
before closing the syringe or withdrawing the connected to the gas sample valve of the chroma-
needle from the septum. tograph. The latter is evacuated and after
disconnection from the vacuum is allowed to fill
C-3.1.2.12 When the conditions in the chromato- with the gas sample. The pressure is measured
graph are equivalent to those established during and the sample introduced into the chromato-
the calibration procedure, quickly inject the graph,
known volume of gas through the injection port.
C-3.3 Calculation
C-3.2 Partial Degassing Method
( Screening Version ) C-3.3.1 The degassing efficiencies for gases are
calculated using the formula:
C-3.2.1 Scope
1
This method is suitable for rapid screening since E-
K&
no further gas extraction is required. 1+7
T
The principle is to allow the oil sample to expand
into a vacuum of known volume and to analyze where
the resultant free gas mixture. The calculation of
the results requires a knowledge of the gas solu- E = degassing efficiency for a given gas,
bilities. V0 = volume of oil sample,
C-3.2.2 Sampling V, - volume of expansion space, and
K = Ostwald solubility coefficient of the gas.
Sampling is done according to B-2.
C-3.3.2 Determine the amount of each gas pre-
C-3.2.3 Treatment of Samples
sent by the calibration graph.
C-3.2.3.1 Connect the sample vessel to a similar
C-3.3.3 Calculate the volume concentration of
glass vessel, previously evacuated, by suitable
each gas component as a’ percentage of the total
tubing.
volume in the gas sample. Also the oil volume
C-3.2.3.2 Open the cocks separating the vessels concentration of each gas component be corrected
and all cw the oil to distribute itself over the entire by dividing it by the degassing efficiency xivrrl
volume. in C-3.3.1.

C-3.2.3.3 If the oil sample has been shipped as C-3.3.4 Correct the total volume of extracted gas
described above, store the connected pair of to 20°C and 1013 mbar and express as a ratio
sample vessels until room temperature is reached. to the oil volume.
If only one sample vessel has been shipped,
C-3.3.5 Calculate the gas-in-oil concentration in
connect the oil sample vessel before storage to a
microlitres per litre for each gas component and
similar, previously evacuated glass vessel.
correct it for degassing efhciency by dividing by
C-3.2.3.4 Shake the oil in both sample vessels the degassing efficiency defined in C-3.3.1.
axis horizontal.
Typical Ostwald solubility coefhcients at 20°C and
C-3.2.3.5 Wait another 10 minutes and repeat 1 013 mbar are given below;
shaking.
Gas
C-3.2.3.6 About 10 minutes after the second Hydrogen 0.05
shaking, weigh the connected vessels and arrange
them one above the other in order to return the Nitrogen 0.09
entire oil volume into the original oil sample Carbon monoxide 0.12
vessel. Oxygen 0.17

C-3.2.3.7 Close the cocks separating the two Methane 0.43

vessels and disconnect the upper vessel. Carbon dioxide I.06

15
IS 9434 : 1992

Gas Gas
1.20 Propane 10.0
Acetylene
I.70 NOTE - Use of manual Toepler pump ( 5.2.3 and
Ethylene Fig. 3 ) or an automatic Toepler pump obviates the need
Ethane 2.4 for correction suggested above.

1 Syringe 21 Expansion flask

2,3, 5,6 Cocks 22 Reference column
4 Three-way cock 24 Septum holder
8 Vacuum gauge 25 Septum
11 Degassing flask 26 Cemented collar
13 Burette 27 Septum retaining ring
18 Magnetic stirrer 30 Mercury reservoir
20 Connection to vacuum

Fro. 11 APPARATUS FOR LABORATORY PARTIAL DEGASSING METHOD

ANNEX D
( Clauses 1.4 and 6.2.2 )
GAS ANALYSIS

D-l EXAMPLE OF PROCEDURE the Porapak N column and the other with the
molecular sieve 5A column.
D-l .1 Scope
Each column is 2 m long with an outer diameter
In this example of an acceptable method ( see of 6 mm.
Fig. 4 ), two parallel columns are used, being The above should be considered only as giving
selected by a valve=. The outlets of both columrrs the broad scope of the procedure and details can
are connected to flame ionization and thermal vary from one model of gas chromatograph to
conductivity drtrctllrs in parallel. The detector another based on the features built-in by the
output is fed into a recorder and integrator, either manufacturer.
output being srlected by a switch.
The users should satisfy themselves that all rele-
Samples are injrrtcd by a calibrated valve, which vant fault gases can be analyzed on a particular
is evacuated before being filled with the gas instrument with reasonable ease and at the
sample. Two separate ruus are mad:*, one with detection limit laid down in 7.1.

16
 IS 9434 : 1992

Quite often, the detection and measurement of molecular sieve 5A column into use. Obtain a
CO is given the go-bye. This is a crucial gas stable base line.
indicative of insulated conductor overheating and
of which the concentration is influenced by the D-1.3.5 Refill the gas sample loop according
presence of oxygen and moisture in oil. Accurate to D-1.2.
detection of CO and its ratio with COP requires D-1.3.6 Turn the sample valve to introduce the
catalytic conversion to CH4 and detection as CHa gas sample.
on F. I. D. These features should, if not factory-
incorporated, be added to the existing units for a D-1.3.7 Select the thermal conductivity detector.
complete analysis for condition-monitoring. The peaks will emerge in the order hydrogen
( H, ), oxygen ( 0s ), nitrogen ( N% ), methane
D-1.2 Preparation of Apparatus ( CH4 ) and carbon monoxide ( CO ).
D-1.2.1 Set up the chromatograph and allow the D-1.3.8 Purge any retained gases from both the
flow of carrier gas and the temperature to stabi- columns.
lize as shown by the production of a steady base
1)
.~ NOTE - A dual channel recorder eliminates the need
Ime. for switching from one detector to another.
D-1.2.2 Evacuate the gas sample loop to a pres- D-l.4 Calculations
sure below O-1 mbar. Disconnect the vacuum
line. D-1.4.1 Measure the area of each peak and note
its retention time.
D-1.2.3 Introduce the gas sample into the loop.
Adjust the pressure to atmospheric or some other D-1.4.2 Identify the gases corresponding to each
known pressure. peak by comparison with the charomatograph
obtained by calibration and apply the calibra-
D-l.3 Analysis tion data to obtain the gas volume.
D-1.3.1 Adjust the sector valve to bring the Pora- D-1.4.3 Gns Analysis-Interpretation Techniques
pak N column into use.
D-1.4.3.1 The methods of interpretation of result
D-1.3.2 Turn the sample valve to introduce the shall be based on the well-known following tech-
gas sample. niques:
~-1.3.3 Select the flame ionization detector; the a) Roger’s Ratio Methods,
first peak to emerge will be that of methane
(CH4).
b) Gas-Liquid Equilibrium Methods, and
When the recorder returns to the base line, select c) Regression Methods.
the thermal conductivity detector to record the
carbon dioxide ( COs ) peak. Finally, re-select D-2 EXAMPLES OF SUITABLE COLUMN
the flame ionization deteetor for ethane ( CsHs ), ASSEMBLY
ethylene ( C&H4 ) and acetylene ( C,Hs ) . D-2.1 The examples are given in tabular form on
D-1.3.4 Adjust the selector valve to bring the next page.

17
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