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IS 10823 (1994): Methods for Determination of Thermal

Degradation Index (TDI) and Reduction Degradation Index
(RDI) of Iron Oxides; Lump Ores, Sinter and Pellets [MTD
13: Ores and Raw Materials]

! $ ' +-
Satyanarayan Gangaram Pitroda
Invent a New India Using Knowledge

! > 0 B


BharthariNtiatakam
Knowledge is such a treasure which cannot be stolen
 IS 10823 : 1994
(Reaffirmed 2001)

( qeq;lT J;r?kJT )

Indian Standard
METHODS FOR DETERMINATION OF
THERMAL DEGRADATION INDEX ( TDI )
AND REDUCTION DEGRADATION INDEX
( RDI) OF IRON OXIDES; LUMP ORES,
SINTER AND PELLETS
(First Revision )

UDC 622.341.l*-12 : 620-186-4

@ BIS 1994

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MAR0
NEW DELHI 110002

December 1994 Price Groop 4

Ores and Raw Materials Sectional Committee, MTD 13

FOREWORD
This Indian Standard ( First Revision ) was adopted by the Bureau of Indian Standards, after the
draft finalized by the Ores and Raw Materials Sectional Committee had been approved by the
Metallurgical Engineering Division Council.
It is well known that iron ore and its agglomerates, namely, sinter and pellets, henceforth called
iron bearing materials, undergo size degradation as a result of thermal shock as well as phase
changes coupled with thermal stresses during reduction at elevated temperatures. The extent to
which a particular type of ore or its agglomerates undergo degradation, if known to the blast
furnace operator, helps to a great extent in the selection of the blast furnace burden. This
standard is one of a series of standards on the methods for determination of various characteris-
tics of iron ores and its agglomerates and it lays down the methods for determination of the
extent of degradation under thermal shock or under thermal shock combined with reduction
reaction.
Since the burden inside the blast furance is constantly moving downwards while the iron bearing
materials are simultaneously getting reduced, the extent of degradation may be measured in the
following two ways: (a) Thermal Degradation Index ( TDI ), that is the effect of thermal shock
on the degradation behaviour of iron bearing materials, and (b) Reduction Degradation
Index ( RDI ), that is degradation due to chemical changes which occur.
For determining these properties, tests may be done under static conditions and then the sample
may be tumbled in the cold condition after the test is over or else the sample itself may be placed
in a rotating bomb (dynamic ) while the heating and reduction is in progress.
Thus, there are four variants of the degradation tests as given below:
Degradation
_-- -_-------- h--d- ---
Thermal Degradation Index Reduction Degradation Index
(TDI) (RDI)
c---m h______~ ~--_--_*------_-~

(TDI) static (TDI) dynamic (RDI) static (RDI) dynamic

These four tests have been covered in the following two sections:
Section 1 - Static test, and
Section 2 - Dynamic test.
The (B) part ( Section 1 > titled Static Reduction Degradation ( RDI ) test of Section 1 of this
Indian Standard has been harmonized with the requirements given in IS0 4696. This test
method is now technically equivalent to that specified in IS0 4696 which would facilitate evalua-
tion of Indian Iron Ores as per the International Standards.
In the formulation of the standard, assistance has been derived from IS0 4696 : 1984 Iron ores -
Low temperature disintegration test - Method using cold tumbling after reduction issued by
the International Organisation for Standardization ( IS0 ).
In reporting the results of a test or analysis 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
Rules for rounding off numerical values ( revised).
 IS 10823: 1994

Indian Standard
METHODS FOR DETERMINATION OF
THERMAL DEGRADATION INDEX ( TDI )
AND REDUCTION -DEGRADATION INDEX
( RDI) OF IRON OXIDES; LUMP ORES,
SINTER AND PELLETS
( First Revision )
1 SCOPE 3.4 Reduction Degradation
1.1 This standard specifies the methods to be The degradation of the iron bearing materials
followed for the determination of the degrada- because of reduction and related stresses introd-
tion index of iron oxides; lump ores, sinter and uced in the matrix due to phase changes.
pellets. Section 1 of this standard prescribes
SECTION I STATIC DEGRADATION TEST
the method for the determination of degrada-
tion index under static bed followed by cold 4 PRINCIPLE OF TEST
tumbling whereas Section 2 of this standard
prescribes the method for the determination of 4.1 To evaluate the effect of rapid heating from
degradation index during tumbling. room temperature to 600C in 30 min on sized
test portion. This is done by measuring the
2 REFERENCES mass of material passing a 6.3 mm screen after
2.1 The following Indian Standards are necessary the heating cycle.
adjuncts to this standard: 4.2 The sample is placed in a sample holder
which is then covered. The holder with the
IS No. Title sample is then inserted into a furnace and heated
4F;$Part 1) : Wire cloth test sieves ( third either in normal or reducing atmosphere as the
revision ) case may be for a given period of time. After
that the sample is removed from the furnace
4:;8(5Part 2) : Perforated plate test sieves and cooled to room temperature. Then by a
( third revision ) mechanical treatment similar in principle to a
1405 : 1982 Methods for sampling iron tumbler test, the weak particles are disintegr-
ores ( second revision ) ated. The sample is then screened to determine
1607 : 1977 Methods for test sieving ( jirst the Degradation Index.
revision ) 5 APPARATUS
3 TERMINOLOGY 5.1 Furnace
3.1 For the purpose of this standard, the follow- An electrically heated furnace with heating
ing definitions shall apply. capacity and thermal response characteristics
3.2 Degradation sufficient to heat the sample from room temper-
ature to 700C in 30 minutes.
The tendency for the iron bearing materials to
undergo size degradation as a result of either The furnace is to be equipped with a control
thermal shock or reduction or both. The term device so that the heating rate of the sample
Decrepitation or Low temperature breakdown can be regulated.
( LTB ) are also used in place of Degradation 5.2 Sample Holder
in technical literature. However, Degradation
is used in this standard for clarity. The sample holder shall be made from heat
resisting steel or material ( like INCONEL 600 )
3.3 Thermal Degradation equipped with a thermocouple to measure the
The degradation of the iron bearing materials temperature of the sample. The cover shall be
under normal atmosphere because of thermal of the loose fitting type and shall not provide a
shock. gas-tight seal ( see Fig. 1 ).
IS 10823 : 1994

sample holder alongwith the sample into the

furnace. Wait for ihe charged bed to reach
6OOV. The test begin at this point and it
continues for 30 min. After 30 min remove
sample and container from furnace and cool to
room temperature. Discharge the sample care-
fully from the container and determine its mass
( mass ml ). The sample shall be tumbled for
30 minutes at 30 rpm. The size of the tumbler
vessel shall be 130 mm x 200 mm. Hand sieve
with care on 10, 6.3, 3.15 and 0.5 mm screen.
Mechanical sieving may be used provided that
preliminary tests give results similar to those
obtained by hand sieving, within the permissible
tolerance of 2 percent absolute.
NOTE - Jt is considered that the set of sieves used
for sieving shou Id include a sieve of suitable apcrt-
urc size between 10.0 mm and 6.3 mm ( for example
8.00 mm ) in order to improve the efficiency of the
6.3 mm sieve by decreasing the sample mass retained
ou it.

Determine and record the masses of the + 10,

-6.3, -3.15 and -0.5 fractions.
All dimensions in millimetres.
9 -EXPRESSION OF RESULTS
FIG. 1 TYPICALSAMPLEHOLDER
5.3 Sieves 9.1 Calculation of the TDI
Test sieves, having square mesh aperture of The thermal degradation index, TDI expressed
25 mm, 20 mm, 10.0 mm, 6-30 mm, 3.15 mm and as a percentage by mass, is calculated from the
500 pm following formula to one decimal place:
6 SAMPLING
TDI - 6.3==z >i 100
6.1 The test sample shall be prepared according 1
to IS 1405 from the sample for physical testing. Where l?zl is the mass of the test portion after
A quantity of sample sufficient to provide at the thermal treatment, m, is the mass of
least ten 500 g test portions shall be prepared. - 6.3 mm fraction obtained after screening.
Screen the sample on 12.5 and 10 mm sieves and The mass percent passing 3.15 mm and 0.5 mm
after sieving, this material shall be oven dried shall also be reported.
at 105 f 5C for at least 2 hours.
After drying, the test material shall be kept in 9.2 Number of Tests
a desiccator until testing and only particles
taken at random shall be used to constitute a Because of the heterogeneity of natural ores the
test portion. test shall be carried out five times and the
mean value of the individual results to be
7 TEST CONDITIONS reported as Ore Thermal Degradation Index.
The sample container shall be placed into the
furnace held at 600C. After the temperature of 10 TEST REPORT
the container reaches 600C it shall be held for The test report shall include the following
a further 30 minutes.
information:
8 PROCEDURE FOR STATIC THERMAL
DEGRADATION TEST ( TDI ) a) reference to this Indian Standard;
8.1 Mass b) details necessary for the identification of
Weigh approximately 500 g ( & 1 particle ) of the sample;
the predried test sample ( mass mo ).
c) the individual results of the five tests
8.2 Heating shall be reported;
Begin heating the furnace, when the furnace
temperature has reached 600C. Introduce the d) reference number of results; and

2
 IS 10823 : 1994

e) any characteristics noticed during the 13 APPARATUS

test and any operations which may had The apparatus shall consist of the following
an influence on the results; for example, ( Fig. 2 ) :
sampling point, scalping sieves used;
method of sieving, loss of mass during a) a system to supply and regulate the gases;
the test. b) a reduction tube;
(B) STATIC REDUCTION DEGRADATION
( RDI ) TEST
11 PRINCIPLE
Static reduction of the test portion at a specified
size range of at a temperature of 500C using -0
8
reducing gas consisting of CO, and N,.
Cooling of the test portion, after 1 h reduction
time, to a temperature below lOOC, and tum-
bling by using a small tumbler drum for 300
revolutions in total. Sieving with test sieves
having square mesh apertures of 6.30 mm, 3.15
mm and 500 Pm.
Calculation of reduction degradation indices
o- 2
0 o-
0
as a ( RDI ), quantitative measure of the degree

-2
0 0
of degradation of iron ores that have been 0 0

reduced and then tumbled, the percentage mass 0

of material lesser than 6.30 mm, lesser than 3.15 3 0 0

o- 0
mm, and less than 500 rm respectively are related 0 0
to the total mass of test portion after reduction 0 0

and before tumbling. 0 0

0 0

12 TEST CONDITIONS 0 0
0 0
0 0
Gas volumes and flow rates are as measured at o-5
-73
0 0
a temperature of OoC and at atmospheric 0 0
pressure. 0
0 oc
12.1 Composition of Reducing Gas 0 0 01
0 -I-
The reducing gas shall consist of :
CO = 30 f o-5 %
6
o- -4 0
O
0
0
0 0
N, = 70 & 0 5% 0

0I-
0
Impurities in the reducing gas shall not exceed 0 0
0 0
H, 0.02% ( v/v ) 0 0
0
0, 0.1% ( v/v) 0 0
H,O 0.2% ( v/v ) 0 0
0 0
Significantly different reduction degradation 0 0
indices, however, can be obtained when the 3 o--
reducing gas contains 2 percent hydrogen rather c)-1
than less than 0.02% hydrogen.
12.2 I?low Rate of Reducing Gas
The reducing gas flow rate shall, during the test 1 Furnace ( 10 kVA ) 6 Layer of alumina balls
period, be maintained at 20 f 1 I l/min. 2 Reduction tube 7 Gas inlet
3 Heating element 8 Gas outlet
12.3 Temperature of Test 4 Perforated plate 9 Thermocouple
5 Test portion
The reducing gas shall be preheated before
entering the test portion to maintain the test FIG. 2 ExAhwLEOF TESTAPPARATUS :
portion at 500 f JOC during the entire test ARRANGEMENT OF REDUCTION TUBE ( 13.1 )
period. AND FURNACE( 13.2 )

3
1s 10823 : 1994

c) an electrically heated furnace to heat 13.2 Furance

the sample to the specified temperature; Having a heating capacity sufficient to maintain
d) a tumbler drum; the entire test portion and the gas entering the
e) test sieves; and bed at 500C f lo%!, and being equipped with
f) a weighing device. a heating element suitable for the specified
temperature.
13.1 Reduction Tube
13.3 Tumbler Drum
Made of non-scaling, heat-resisting metal to Consisting of a vessel having an internal dia-
withstand a temperature of greater than 600C. meter of 130 mm and an inside length of
The diameter of the sample bed shall be 75 f 200 mm.
1 mm. Two equally spaced steel lifters 200 mm long
The test portion may be placed on a perforated and 20 mm wide and 2 mm thick shall be
plate or, if desired, on alumina balls on the mounted longitudinally inside the drum. These
perforated plate, in order to ensure a uniform may be mounted on a frame that can be inserted
gas flow through the test portion ( Fig. 3 ). inside the vessel from one end.

FIG. 3 EXAMPLE OF REDUCTION TUBE ( 13.1 )

4
 IS 10823 : 1994

One end of the vessel shall be closed and the fractions and remove by sieving the plus 12.5
other open. A close fitting lid shall be held in mm and the minus 10.0 mm material from the
place on the opening to ensure a dust-tight sample.
seal ( see Fig. 4 ).
15 PROCEDURE
15.1 Number of Determinations
Carry out the test generally in duplicate.
15.2 Test Portion
Weigh to the nearest 0. Ig, approximately 500g
( & 1 particle ) of the test sample. The test
portion should be obtained from the test sample
either by means of riffle divider or by manual
increment division method.

15.3 Reduction
Place the test portion ( 15.2 ) in the reduction
tube ( 13.1) so that the surface is even. Close
the top of the reduction tube. Then insert the
reduction tube into the furnace ( 13.2 ) and, if
desired, attach it to the weighing device of
FIG. 4 EXAMPLEOF TUMBLERDRUM appropriate capacity and accuracy ( 13.5 ),
ensuring that here is no contact with the furnace
13.4 Test Sieves or heating elements.
Having square mesh apertures of the following NOTE - The use of weighing device for continuous
nominal sizes: monitoring is optional.
16-O mm, 125 mm, 10.0 mm, 6.30 mm, 3.15 Replace the air in the tube with inert gas.
mm and 500 pm. Heat the test portion and while heating pass
a flow of inert gas through the test portion at
13.5 Weighing Device a flow rate of approximately 10 I/min the begin-
Adequate load capacity and accurate to 0.1 g. ning and 20 l/min approximately for the last 10
minutes. Continue the heating, while passing
14 PREPARATION OF TEST SAMPLE inert gas until the test portion reaches the test
In the case of commercial test, the test sample temperature of 500 f 10C.
shall be prepared according to IS 1405 from the NOTE - Unless the characteristics of the furnace
sample for physical testing. The test sample shall and thermocouple~are very well known a period of
be oven-dried at 105 f 5C for at least 2 h and about 15 min should be allowed for temperature at
cooled to room temperature before testing. 500C.
CAUTION - Carbon monoxide and the
The total mass of the test sample shall be 2 kg. reducing gas which contains carbon mono-
approximately on a dry basis prepared as xide are toxic and therefore hazardous. The
follows: reduction shall be carried out in a well
a) Pellets ventilated area or under a hood. Precautions,
shall be taken for the safety of the operator.
The test sample in the size range of 10.0 mm
to 12.5 mm or other sizes as agreed to between Introduce the reducing gas ( 12.1 ) at a flow
the supplier and the purchaser, shall be obtained rate of 20 f 1 l/min to replace the inert gas
by sieving. After sieving pellets taken at to reduce the test portion. Continue the redu-
random only, for example by riffling shall be ction with the reducing gas for lh.
used for the test.
After 1 h reduction time, stop the flow of the
b) Ore or sinter reducing gas and cool the test portion, to
a ~temperature below 100C in the reduction
The test sample in the size range of 10.0 mm to tube under a flow of inert gas.
12.5 mm shall be prepared as follows:
15.4 Tumbling
Screen the sample on a 12.5 mm sieve and care-
fully crush the plus 12.5 mm material until it Remove the test portion carefully from the
all passes the 16.0 mm sieve. Combine all reduction tube, determine the mass ( mass mo
1
IS 10823 : 1994

and place it in ahe tumbler drum ( 13.3 ). g) any operation and any test conditions
Fasten the lid tightly and rotate the drum for not specified in this standard or regarded
a total of 300 revolutions at a rate of 30 f 1 as optional which may have had an infl-
rev/min. uence on the results.
Remove all material from the drum, determine
SECTION 2 DYNAMIC DEGRADATION
the mass, hand sieve with care on 6.30 mm,
TEST
3.15 mm and 500 ium sieves. Determine and
record the mass of each fraction retained on
6.30 mm ( mass ml ), 3.15 mm ( mass m, ) and 18 PRINCIPLE OF TEST
500 pm ( mass m3 ). Material lost during The sample is placed in a sample holder
tumbling and sieving shall be corisidered to be ( barrel ) which can rotate and give a mechani-
minus 500 tLm. cal treatment similar in principle to a tumbler
NOTE - Mechanical sieving may be used provided test. The holder ( barrel ) with the sample is
that prelirninaly test results give similar results to then inserted into a furnace and heated either
hand sieving within the permissible tolerance of 2 in normal or reducing atmosphere as the case
percent absolute. may be for a given period of time. After the
16 EXPRESSION OF RESULTS test, the sample is removed from the furnace
and cooled to room temperature. The sample
The reduction disintegration index, RDI as is then sized to determine the Degradation
a percentage by mass, is calculated from the Index.
following formulae:
19 SAMPLE
RDI _ 6.3 = %&% x 100 A sample in the size range of + 10 - 12.5 mm
and a quantity of 500 f 1 g drawn as per the
RDI - 3.15 zzz mti - (m, -t m2)
x 100 method given in IS 1405 : 1982, dried at
nlo 105 f 5C for 2 hours shall be selected for the
purpose of this test.
RDI
20 APPARATUS
where
??lO= is the mass, in grams, of test portion 20.1 Furnace
after reduction and before tumbling; An electrically heated furnace with heating
capacity and thermal response characteristics
m, = is the mass, in grams, of oversize
fraction retained on the 6.30 mm sufficient to heat the sample and holder to
sieve; 600C in 60 minutes.

m2 = is the mass in grams of oversize 20.2 Sample Holder

fraction retained on the 3.15 mm
A sketch of the sample holder barrel is given
sieve; and
in Fig. 5. This barrel is 200 mm in length and
m, = is the mass, in grams, of oversize 130 mm internal diameter in its central portion
fraction retained on the 500 pm which holds the sample. This portion has four
sieve. equally spaced 200 mm x 20 mm lifters moun-
17 TEST REPORT ted on its inside face. The barrel tapers on
its both ends to 50 mm internal diameter in
The test report shall include the following 75 mm length. The ends of the barrel are
information: provided with arrangements for rotating it at
a>reference to this standard; 10 rpm and for gas flow through this.

b) results of the test, reduction-disintegra-

20.3 Sieves
tion indices expressed to one decimal
place; Sieves shall be 01 the square mesh type and
shall conform to the requirements given in
C>identification of the sample;
is97i60 ( Part 1 ) : 1978 or IS 460 ( Part 2 ) ;
d) reducing gas composition used;
e> sieving conditions
and sieving time;
: method of sieving,
21 PROCEDURE

f) total mass of material inserted into the 21.1 Dry the sample till a constant mass is
tumbler drum and taken from the tumbler reached. Then place the sample in the sample
drum; and holder barrel at room temperature.

6
 IS 10823: 1994

All dimensians in millimetres.

FIG. 5 BARRELFOR DYNAMIC DEGRADATIONTEST
21.2 For Dynamic Thermal Degradation Test according to IS 1607 : 1977. Determine the
( TDI )dynamic mass of each of the fractions to the nearest
0.1 g.
Place the barrel with the furnace which has
been preheated 550 f 10C and start the rota- 21.5 The Dynamic Thermal Degradation lndex
tion the barrel at 10 f 0.5 rev/min. After the ( TDI ) dynamic or Dynamic Reduction Degra-
sample has attained 550C soak it for 60 dation Index ( RDI ) dynamic is expressed as
minutes at this temperature. the percentage of - 3.15 mm fraction genera-
ted after tumbling.
21.3 For Dynamic Reduction Degradation Test
( RDI )dynamic 21.6 Indices for other screen sizes ( -6.3 mm,
Place the barrel containing the sample in the -5 mm, -1 mm or -0.5 mm ) may also be
furnace at room temperature and start rotating reported since this data shall be collected in
it at 10 f 0.5 rpm and put on the furance and any case.
raise the temperature of sample at the rate of
10C per minute to 553 & iOC and soak it 21.7 Number of Tests
for 10 minutes under neutral atmosphere ( by At least two tests shall be carried out and the
passing nitrogen gas at a rate of about 3 litres individual as well as the average values reported.
per minute through the barrel from the time the
barrel starts rotating ). Then pass gas mixture 22 TEST REPORT
of 30 percent carbon monoxide and 70 percent
nitrogen at the rate of 15 litres per minute for The test report shall contain the following
one hour maintaining the sample temperature at information:
550 f 10C. Then cool the sample to 350C
under neutral atmosphere ( by passing nitrogen a) Identification of the sample;
gas at the rate of about 3 litres per minute in b) Initial and final mass of the sample be-
the barrel ) by putting off the furnace. Then fore and after the test;
take out the barrel and cool it to room
temperature. c) Degradation Index for each test and the
mean; and
21.4 Take out the sample and weigh the sample
to~an accuracy of 0.1 g. Sieve the sample d) Reference to this Indian Standard.
Bureau of Indian Standards
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promote harmoious development of the activities of standardization, marking and quality
certification of goods and attending to connected matters in the country.

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or grade designations. Enquiries relating to copyright b:: addressed to the Director
( Publications ), IBIS.

Revision 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 Handbook and Standards
Monthly Addition.

This Indian Standard has been developed from Dot : No. MTD 13 ( 3927 ).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

-

___- _____

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