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“The Right to Information, The Right to Live” “Step Out From the Old to the New”

IS 7929 (1975): Methods of determination of electrical

resistivity of chemical coke [PCD 7: Solid Mineral Fuels]

“!ा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 2000 )
 IS : 7929 - 1975

Indian Standard
METHODS FOR DETERMINATION OF
ELECTRICAL RESISTIVITY OF
CHEMICAL COKE
Solid Mineral Fuels Sectional Committee, CDC 14

Chairman Rejwesenting
DR M. G. KRISHNA Central Fuel Research Institute ( CSIR ), Dhanbad

Vice-Chairman
SHRI A. K. MOITRA Central Fuel Research Institute ( CSIR ), Dhanbad

Members
SHRI A. BANERJEE Coal Controller, Calcutta
SHRI D. BASU Coal Mines Authority Ltd, Calcutta
SHRI S. K. BOSE National Test House, Calcutta
SHRI K. M. CHATTERJEE( Alternate )
SHRI D. R. CHATTERJEE Bharat Coking Coal Ltd, Dhanbad
CHIEF MININQ ADVISER, RAILWAY Ministry of Railways
BOARD, DHANBAD
JOINT DIRECTOR,MECHANICAL
EN~INEERINC (FUEL),
RAILWAY BOARD, NEW DELHI ( Alternate )
DRA.N. CHOWDHURY Geological Survev of India. Calcutta
DIRECTOR ( TMD ) Cent& Electric ’ Authority ( Thermal Power Divi-
sion ), New Delhi
DEPUTY DIRECTOR ( TMD ) ( Alternate )
SHRI J. K. JAIN Coal Consumers’ Association of India, Calcutta
SHRI S. K. MANDAL Steel Authoritv of India Ltd. Ranchi
S& S. N. WAZIR ( Alternate )
SHRI A. K. MITRA Coal Board, Calcutta
SHRI U. N. JHA ( Alternate )
SHRI S. K. MUKHERJEE National Coal Development Corporation Ltd, Ranchi
SHRI D. RAMAMOORTHY Bharat Heavy Electricals Ltd, New Delhi
SHRI S. SRINIVASAN( Alternate )
SHRI K. G. RAN~REZ Regional Research Laboratory ( CSIR ), Hyderabad
SHRI K. SESHACIRIRAO ( Alternate )
DR S. M. M. SAFVI Tata Iron & Steel Co Ltd, Jamshedpur
DR M. L. SAHA Cok; ycveteaManagers’ Association ( Indian Section ),
a
SECRETARY,COMA ( Alternate )
SHRI S. B. SARKAR Institute of Fuels ( Indian Section ), Calcutta
SHRI C. L. SESHADRI Neyveli Lignite Corporation Ltd, Neyveli
( Continued on page 2 )

@ Copyright 1976
INDIAN STANDARDS INSTITUTION
This publication is protected under the Indian Copyright Acf (XIV OP 1957) and
reproduction in whole or in part by any means except with written permission of the
publisher shall be deemed to be an infringement of copyright under the said Act.
IS : 7929 - 1975
( Continued from page 1)

Members Rejwwnting
SHRI S.S. SUBRAMANIAN Indian Iron & Steel Co Ltd, Calcutta
SHRI V. V. RAO ( Alternate)
DR G. M. SAXENA, Director General, IS1 ( Ex-oBcio Member )
Director ( Chem )
Secretary
SHRI G. P. SARMWAT
Deputy Director ( Chem), IS1

Methods of Test for Solid Mineral Fuels Subcommittee, CDC 14 : 2

Convener
SHRI B. K. MAZUMDAR Central Fuel Research Institute ( CSIR ), Dhanbad

Members
SHRI S. BAGCHI Central Mining Research Station ( CSIR ), Dhanbad
DR A. N. CHOWDHURY Geological Survey of India, Calcutta
SHRI B. K. DUTTA Fertilizer Corporation of India Ltd, New Delhi
I,.. _\
SHRI S. Cl. BISWAS( ALtLrnatC )
SHRI A. K. KARPHA National Test House, Calcutta
SHRI B. C. MATHUR Hindustan Steel Ltd, Ranchi
DR M. RANCA RAO Hindustan Steel Ltd (R&D ), Ranchi
SHRI S. B. SARKAR Coal Board, Calcutta

Study-Group for Electrical Conductivity and Reactivity of

Chemical Coke, CDC 14 : SG 1

Convener
SHRI S. K. MAZUMDAR Central Fuel Research Institute ( CSIR ), Dhanbad

Members
DR S. DUTTA Geological Survey of India, Calcutta
DR K. SWAMINATHAN Union Carbide of India Ltd, Calcutta
SHRI R. THYAGARAJAN Indian Aluminium Co Ltd, Calcutta
 IS : 7929 - 1975

Indian Standard
METHODS FOR DETERMINATION OF
ELECTRICAL RESISTJVITY OF
CHEMICAL COKE

0. FOREWORD
0.1 This Indian Standard was adopted by the Indian Standards Institution
on 28 August 1975, after the draft finalized by the Soild Mineral Fuels
Sectional Committee had been approved by the Chemical Division Council.
0.2 ’ Chemical coke ’ is a general term which is applied to various types of
coke other than that used in blast furnaces, cupolas, etc. Chief areas of
use of chemical coke are electro-thermal and electro-chemical industries
where this coke is used either as a carrier of current or as a source of
carbon. Chemical coke is generally used in the form of granules, green
moulded shapes or finished carbon blocks.
0.3 In this standard two methods of determination of electrical resistivity
have been prescribed. The first is the two-electrode method which is suitable
for chemical coke in granular form and the other is the four-probe method
which is suitable for green moulded shapes, finished carbon blocks and
lumps.
0.4 In the formulation of this standard valuable assistance has been
rendered by the Central Fuel Research Institute, Dhanbad, and Geological
Survey of India, Calcutta.
0.5 In reporting the result of a test made in accordance with this standard,
if the final value, observed or calculated, is to be rounded off, it shall be
done in accordance with IS : 2-1960*.

1. SCOPE
1.1 This standard prescribes methods for determination of electrical
resistivity of chemical coke at room temperature.

2. PRINCIPLES
2.1 Two-Electrode Method -This method is applicable to chemical
coke in the form of granules of definite size range, compressed to the shape
*Rules for rounding off numerical values ( revi.wf
).

3
IS : 7929 - 1975

of a cylinder between two metal electrodes in a tube made of a suitable

non-conducting material. A direct current is passed through this coke mass
and its resistance is measured by a double ohm Kelvin bridge or a poten-
tiometer or a dc vacuum-tube voltmeter. Electrical resistivity ( P) is
calculated from the following equation:

peEA=% ohmcm
IH H *

where
E = potential difference in volts across the electrodes,
Q, = cross-sectional area of the coke column in cm2,
I = current strength in amperes passing through the coke
column,
H = height of the coke column in cm, and
R = resistance of the coke column in ohms.
2.2 Four-Probe Method - This method is applicable to chemical coke
in the form of green moulded shapes, finished carbon blocks or lumps.
This method is independent of the shape or size of the specimen and
requires only a linear dimension of about 20 to 200 mm on a flat ground
face. By this method electrical resistivity can be measured in a part of the
whole bulk of the sample by placing four spring-loaded tungsten or harden-
ed steel probes in a line at equal intervals on the flat ground face of the
specimen. A low direct current is passed through the outer probes and
the potential difference between the remaining inner two probes is measured
by a vacuum tube voltmeter. To minimize the effect of anisotropy,
measurements should be made at different points and in different directions
on the specimen surface. Electrical resistivity ( P ) is calculated from the
following equation:

P =2x&S+ ohm.cm

where
S = distance in cm between the adjacent probes,
E = potential difference in volts between the two inner probes,
and
I = current strength in amperes passing through the two
outer probes.

3. APPARATUS

3.1 For Two-Electrode Method - The circuit diagram of the set-up is

given in Fig. 1. Details of accessories are given in 3.1.1 to 3.1.4.

4
 Z = Total bridge current from the battery Zs -Zs = Current along ‘ R ’ ( standard
11 r: Current along ‘ P’ and ‘ Q’ arms low resistance )
Zs - Current along ‘S ’ ( standard resistance ) X = y$;;y resistance (of the
and ‘ X’ unknown resistance of the
sample V = Vacuum tube volt meter
Za I Current along ‘ T’ and ‘ U’ arms B = Battery ( 12 volts)

FIG. 1 CIRCUIT DIAGRAM FOR TWO-ELECTRODE METHOD

3.1 .I Pressure Appliance - a hydraulic jack provided with a calibrated

gauge up to a pressure of 10 000 kN/ m2 ( 100 kgf/cm2 ) with one division
equivalent to 100 kN/m2 ( 1 kgf/cm2 ).
3.1.2 Specimen Cells ( or Conductivity Cells ) - made of stainless steel.
The inside of the cell is lined with ebonite or steatite or sillimanite.
A small cell can hold as small as 0.5 g and a big cell up to 20 g of sample.
A stainless steel electrode makes the contact. Details of the small and big
conductivity cells are shown in Fig. 2 and 3.
3.1.3 A Suitable Bridge - double ohm Kelvin bridge or potentiometer or
dc microvoltmeter ( vacuum tube microvoltmeter ) with necessary accessories
for measuring resistance of coke mass with an accuracy of about 0.5 percent.
These appliances are suitable for measuring resistance less than 10 ohms.
A Wheatstone bridge or a post office box may also be employed.

5
 NON-CONDUCTING
MATERIAL (EBONITE) ,STAINLESS STEEL

! b-2ic-4
LOWE’R
ELECTRODE
(STAINLESS STEEL)

CONDUCTIVITY CELL UPPER ELECTRODE

(SECTIONAL ELEVATION) (STAINLESS STEEL1
All dimensionsin millimetres.
FIG. 2 CONDUCTIVITY CELL (SMALL)

3.1.4 A Dial Gauge or a Scale- to measure in millimetres the height of

pressed coke column with an accuracy of 0.5 percent.
3.2 For F&m-Probe Method -The circuit diagram of the set-up and
arrangement of probes are given in Fig. 4 and 5. Details of the apparatus
and assembly are given below.
3.2.1 Probe Instrument - comprising of the probe head, specimen holder
and weight pan ( see Fig. 6A ), The probe head is made of polymerized
tetraflouroethylene base material and has four equidistant cylindrical
holes in a straight line. These holes lead to rectangular guide slots ( see
Fig. 6B ) ; each slot has a probe holder and a compression coil spring in
cylindrical form. The probes, four in number are made of tungsten or
steel, have diameter of 0.8 mm and terminate in a sharp tip to minimize
area of contact with the specimen. Each probe is brazed on the plate on
the probe holder. The probe holders are connected to the terminals.
Each probe is attached to its own spring loaded metallic holders.
With a view to ensuring proper contact between the probe tips and the
secimen surface, the probe holder is weighted by a load of 0.5 to 4 kg
placed on top of the vertical shaft of the probe holder. Details of specimen
holder are given in Fig. 6C.

6
 ls: 7929-1975

-=3n
-
NON-CONDUCTING
MATERIAL (EBONITE)

P
12' \ . --it--S
SCACE

1
IN mm-/
2

90

/
-32 +,- -I-
_I
116

UPPER ELECTRODE
(STAINLESS STEEL)

P-32 9---I
I

CONDUCTIVITY CELL
(SECTIONAL ELEVATION1

LOWER ELECTRODE
(STAINLESS STEEL 1
All dimensionsin millimetres.
FIG. 3 CONDUCTIVITY CELL (BIG )

3.2.2 V~~~acuu~
Tube Microvoltmeter -See 3.1.3.
3.2.3 Milliammeter - of range 0 to 250 I&L
3.2.4 Travelling Microscope-to measure distance between the probes
(with an accuracy of fO.01 mm).
3.2.5 Weights - 0.5 to 4 kg to be put on the weight pan of the
apparatus.

4. TEST SPECIMEN

4.1 For Two-Electrode Method - Carbon or coke particles lying in the

size range 0.21 and 0.42 mm are prepared from representative samples
[see IS : 436 ( Part II )-1965*]. Any coke dust adhering to the sized frac-
tion is removed by sieving on a sieve shaker for about 20 minutes.
The prepared specimen is then dried in a vacuum air-oven at a temperature

*Method for sampling of coal and coke: Part II Sampling of coke ( revised ).

7
ls : 7929 - 1975

+ VOLTAGE
I-DIVIDER

PROBES

COKE OR CARBON BLOCK

J
FIG. 4 CIRCUIT DIAGRAM FOR FOUR-PROBE METHOD

+I

I
I COKE OR CARBON BLOCK
I

I = Current passing through probes 1 and 4

E = Potential difference between probes 2 and 3
S = Distance between adjacent probes

NOTE - 1, 2, 3 and 4 are probes.

FIG. 5 ARRANGEMENT OF PROBES

8
 IS : 7929 - 1975

WEIGHT

-PROBE HEAD
-SAMPLE

-.N;~

6A Assembly of Four-Probe Instrument

FIG. 6 FOUR-PROBEINSTRUMENT
- Contd

of 150 to 200°C for a period of 2 hours to remove moisture and then cooled
in a desiccator to room temperature and stored in it until required for
testing.

4.2 For Four-Probe Method -Specimens of green moulded shapes,

finished carbon blocks, coke lumps or blocks having linear dimensions
ranging from 20 to 200 mm independent of shape or size (including oval
shaped briquettes ) are ground on a grinding machine or a glass plate
to provide a flat surface to accommodate the four probes. The prepared
specimen is then dried in a vacuum air-oven at a temperature of 150 to
200°C and cooled and stored as mentioned in 4.1.

9
 SECTION AA

1. Transparent plastic material 8. Setting nut

2. Cylindrical holes for the probe 9. Endplate on the probe holder
3. Guide slots 10. Attaching rod between probe head
4. Probe holder and terminal plate

5. Probe 11. Terminal plate

6. Compression coil spring 12. Terminal
7. Cylindrical shank 13. Leads

6B Probe Head

FIG. 6 FOUR-PROBEINSTRUMENT
- Contd

5. PROCEDURE

5.1 For Two-Electrode Method

5.1.1 Calibration of the Afiparatus - Calibrate the measuring bridge or

potentiometer using standard resistance; 0.001 ohm for low and 10 ohms
for high resistance. Check the contact resistance of the stainless steel
electrodes of the conductivity cell as described below after cleaning the
contact (flat ) surfaces with alcohol or acetone.

10
 Probe head
Shaped rubber faced clamping jaws
Specimen of carbon or coke
Clamping jaw axis
Spring
6C Briquette Holder

FIG. 6 FOUR-PROBEINSTRUMENT

5.1.2 Determination of Contact Resistance and Electrical Resistivity -

Carefully charge a specific quantity of the test sample ( see 4.1) into the
cell, using a funnel to avoid adhering of particles to the insulating sides of
the cell. Place the charged cell on a rotary or syntron vibrator for half a
minute to consolidate the charge. Then put the cell on the flat surface of
the spindle of a hydraulic jack, place the upper electrode on the coke mass
and compress it by applying a pressure of 4.25 MPa ( 42’5 kgf/cm”) for
10 to 15 minutes till the dial gauge shows no further change in the height
of the coke column in the cell. Note the height ( H) in cm of the coke
column from the dial gauge. Then pass a definite current through the
coke column, from a storage battery or cell and a rheostat and note the
resistance. Then reverse the direction of the flow of current and again

11
IS I 7929 - 1975

note the resistance and take the mean of the two values. Carry out dup-
licate determinations as above using increasing quantities of the test sample
and plot a curve of resistance values for increasing column heights of the
test sample. Extrapolate the curve which is a straight line, to meet the
resistance axis as shown below and obtain contact resistance:

HEIGHT OF COKE COLUMN IN cm

5.1.2.1 Calculate the electrical resistivity Pas follows:

P= (RI- ohm.cm

where
RI = resistance in ohms of the coke column of height HI cm;
R, = contact resistance in ohms, obtained from the graph
in 5.1.2; and
Q =: cross-sectional area of the coke column in ems.

5.2 For Four-Probe Method - Fix the specimen ( see 4.2 ) into the
specimen holder with the ground face upwards to accommodate the four
probes. If necessary, rubber faced recessed plates may be employed for
holding the specimen firmly in the case of non-uniform shapes. Set the
four probes on the flat surface of the specimen firmly to ensure proper
contact.

5.2.1 Depending on the resistivity of the specimen, pass a current up to

250 mA through probes 1 and 4 and measure the potential difference
between the probes 2 and 3 using the potentiometer or the vacuum tube
microvoltmeter and calculate resistivity as prescribed in 2.2.

12
 IS : 7929 - 1975

6. RESULTS

6.1 The results shall be computed from the arithmetic mean of duplicate
determinations, and shall be expressed in terms of ohm.centimetres.

7. REPORT

7 .l The report shall include the following information:

a) Identification and previous history of the sample,
b) Ambient temperature in degrees Celsius at the time of the test,
and
c) Method used for determining electrical resistivity.

8. PRECISION OF THE METHOD

8.1 Repeatability - The results of duplicate determinations, carried out

at different times in the same laboratory, by the same operator, with the
same apparatus, on representative samples drawn from the same lot, shall
not differ by more than 2 percent.
8.2 Reproducibility - The means of the results of determinations carried
out in different laboratories on representative portions drawn from the
same lot, shall not differ by more than 4 percent.

13
INDEAN STANDARDS

ON
COAL AND COKE

IS: ,
436 ( Part I )-1964 Methods for sampling of coal and coke: Part I Sampling of coal
( rev&d )
436 ( Part II )-1965 Methods for sampling of coal and coke: Part II Sampling of coke
( revised )
437-l! 365 Size grading of curd and coke for-marketing ( second revidon )
439-1965 Hard coke for marketing ( revised )
770-1964 General class&cation of coal (revised)
135Q (Part I )-I969 Methods of test for coal and coke: Part I Proximate analysis (first
revision )
1350 ( Part II )-1970 Methods of test for coal and coke: Part II Determination of calorific
value
1350 (Part III )-1969 Methods of test for coal and coke: Part III Determination of
sulphur
1350 (Part IV/Section 1 )-1974 Methods of test for coal and coke: Part IV Ultimate
analysis, Section 1 Determination of carbon and hydrogen
1350 (Part IV/Sectron 2 )-1975 Methods of test for coal and coke: Part IV Ultimate
analysis, Section 2 Determination of nitrogen
1352-1959 Methods of test for coal and coke- special impurities
1353;1959 Methods of test for coal carbonization -caking index, swelling properties and
Gray-King assay ( L.T. ) coke types
1354-1964 Methods of test for coke -special tests ( revised)
1355-1959 Methods of test for ash of coal and coke
3746-1966 Graphical symbols for coal preparation plant
3810-1966 Glossary of terms used in coal preparation practice
4023-1966 Methods for the determination of reactivity of cake
4286-1967 Processed solid smokeless domestic fuel
43 1 1- 1967 Methods for the determination of mineral matter in coal
4433-1967 Methods for the determination of the hardgrove grindability index of coal
4836-1968 Foundry coke
5018-1968 Classification of hard coals by type
5062 ( Part I )-1969 Methods of test for brown coals and lignites: Part I Determination
of moisture by the direct volumetric method
5062 (Part II )-1969 Methods of test for brown coals and lignites: Part II Determination
ash
5062 (Part III )-I969 Methods of test for brown coals and lignites: Part III Determina-
tion of the yields of tar, water, gas and coke by low temperature distillation
5062 ( Part IV )-1969 Methods oftest for brown coals and lignites: Part IV Determination
of the yield of benzene-soluble extract
5062 ( Part V )-1973 Methods of test for brown coals and lignites: Part V Determination
of acetone-soluble material resinous substances in the benzene extract from
brown coals and lignites
5209-1968 Principles and conventions for flowsheets for coal preparation plant
5615-1970 Gas coke
6345-1971 Methods of sampling of coal for float and sink analysis
6372- 197 1 Specification for coke for ferro-alloys industry
7 189-l 974 Blast furnace coke
7190-1974 Methods of determination of bulk density of coke
7221-1974 Method of determining the moisture holding capacity of hard coals