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Indian Standard
ACTIVATED ALUMINA - SPECIFICATION
( First Revision)
UDC -661’183’8
0 BIS 1991
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General Inorganic chemicals sectional committee, CHD 003
FOREWORD
This Indian Sl:andard ( First Revision ) was adopted by the Bureau of Indian Standards, after the
draft finalized by the General Inorganic Chemicals Sectional Committee had been approved by
the Chemical -Division Council.
The thermal treatment is given so that eta, gamma and chi alumina phases are formed which are
the major constituents of adsorbent alumina.
Activated alumina is used in the industry at a desiccant/adsorbent, primarily intended for applica-
tion in industrial air drying, gas and liquid drying, packing and in chromatographic analysis.
This standard, however, does not cover the material intended for chromatographic use.
This standard was originally published in 1981. In this revision, new requirements on alumina
content, pore volume and surface area have been incorporated along with the relevant methods of
test. Also, requirements on pH, loss on ignition, adsorption capacity, loss on attrition, bulk
density and bed crushing strength have been modified.
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.
IS 9700:1991
Indian Standard
ACTIVATED ALUMINA - SPECIFICATION
( First Revision )
1 SCOPE Table 1 Requirements for Activated Alumina
( Clause 4.2 )
This standard prescribes the requirements and
methods of sampling and test for activated Characteristic Requirement Method
r?z. r-,_Jc-_,__ of Test
alumina used as a desiccant/adsorbent. Grade 1 Grade 2 ( Ref to
Annex of
2 REFERENCES this
Standard )
The following Indian Standards are necessary (1) (2) (3) (4) (5)
adjuncts to this standard: i) Moisture, percent by 2.0 2.0 A-2
mass, Max
IS No. Title ii) pH value 4.6 to 6.0 to A-3
264 : 1976 Nitric acid ( second revision ) 8.0 10.0
iii) Aluminium oxide ( as 91’0 90.0 A-4
460 Test sieves : Part 1 Wire cloth ( Al,Os ), percent
( Part 1 ) : 1985 test sieves ( third revision ) by mass, Min,
iv) Water soluble chlo- 0.7 A-5
1070 : 1977 Water for general laboratory
use ( second revision ) rides ( as Cl ),
percent by mass,
4905 : 1968 Methods for random Max
sampling v) Water soluble sulphates 0.7 A-6
(as SO*), percent by
3 GRADES mass, Max
vi) Sodium and its corn- 0.8 - A-7
There shall be following two grades of the pounds (as NasO),
material: percent by mass, Max
vii) Loss on ignition, per- 8.0 8.5 A-8
Grade I For high pressure air drying, and cent by mass, Max
viii) Adsorption capacity, 20-O 14’0 A-9
Grade 2 For general purposes. percent, Min
ix) Pore volume, ml/g, 0.40 0.30 A-10
4 REQUIREMENTS Min
x) Surface area, m*/g, 350 250 A-11
4.1 Description Min
xi) Bulk density, g/ml, 0.75 0.85 A-12
The material shall consist of activated alumina Min
in spherical or pellet form as agreed to between xii) Attrition, Loss, per- - - A-13
the purchaser and the supplier. cent by mass, Max
a) By tumbing 0.50 1.0
4.2 The material shall comply with the b) By rotation 1.50 2.50
requirements given in Table 1 when tested xiii) Bed crushing strength, 90 80 A-14
according to the methods prescribed in Annex percent, Min,
A. Reference to the relevant clauses of Annex
A is given in co1 5 of the table. NOTE - Requirements for moisture, adsorption
capacity, pore volume, surface area, loss on
attrition and bed crushing strength are critical
5 PACKING AND MARKING for adsor~bent application.
1
IS 9700 : 1991
ANNEX A
( Clause 4.2 )
F
IS 9700 : 1991
A-6.3 Calculation
A-5.2.1 Preparation of Solution
Water solubles, sulphate,
Weigh accurately_2g of the material in a platinum percent by mass = MX343’34
crucible of 40 ml capacity previously washed where
with nitric acid. Heat the crucible and its
contents in a furnace at 350°C for 45 minutes. M=mass, in g, of ignited residue.
Boil for 2 to 3 minutes and then digest for half
an hour. Allow to settle for 10 minutes A-7 SODIUM AND ITS COMPOUNDS
.gnd filter through Whatman No. 40 filter
paper or equivalent into 200 ml standard A-7.1 Apparatus
flask; wash 3 times with hot distilled water.
,Cool the solution and make up to the mark. A-7.1.1 Flame Photometer
3
IS 9700:1991
Flame the diluted solution using a flame photo- NOTE - Saturated solution of sodium nitrite at
30°C gives a relative humidity of 60 percent.
meter. The instrument shall be calibrated in Evacuation of the desiccator will help in the
the range of 0 to 5 mg/l of sodium. attainment of faster and reproducible equilibrium
conditions. It will be ‘more appropriate to place
A-7.4 Calculation the desiccator at a constant temperature.
F
1 Manome:ets 5 Dilution Chamber
2 Stirrer 6 Sample Cell
3 Heating Coil 7 Adsorption Chamber
4 Benzene Saturator 8 Thermometer
-purge. Cool the sample in an empty The specific surface area is given by:
desiccator. Adjust the two nitrogen flow inlets NxB
to get a partial pressure of 0’05 to 0’075 *mm S, m”/g = gl”m M
of Hg. Weigh the cooled sample and place it m
the adsorption chamber. Carry out the where
adsorption for two hours till equilibrium is N = Avogadros No. ( = 6’023 X 1O23)
reached. Weigh the cell. Change the partial pres-
sure of benzene to a higher value, ray 0’125 to B = molecular area of the adsorbate
0’150 and continue the adsorptionby replacing (benzene),
the cell in the chamber for 1 hour. Note four = 41 A2 = 41 x 1O-2oma ,
readings in the partial pressure range of 0’05
m = mass of the sample, and
to 0’35 mm of Hg.
M= molecular mass of benzene ( 78 ).
A-11.3 Calculation -On substitution, we get,
grtl x 3 166
BET equation is s= m ’
PIP0
g(l--p/PO) A-12 BULK DENSITY
where
g = amount of benzene adsorbed at any A-12.1 Procedure
PIP,, Take the material as received and fill it in a
gm = amount of absorbate ( benzene ) re- 250-ml measuring cylinder up to 50-ml mark
quired to from monolayer on the surface, and without knocking. Shake the sample down by
C = constant. gently lifting the cylinder as far as 5 cm from the
base pad and releasing it on the table. Repeat
PIP0 this knocking for 4 more times. Add further
is plotted against PIP,, a
If g ( l-P/P, > 50 ml of the sample and knock five times, as
straight line ( BET ) plot is obtained in above, after every 50 ml addition up to 250 ml.
which Level the cylinder with the material without
any further knocking. Empty out the material
c- 1
and Intercept = -
1 from the cylinder and weigh to the nearest 0’5 g.
Slope = ~
gm C gm C Then heat the sample in an unventilated oven
C-l at 250 f 5°C for 3 h. Place the cylinder in a
Slope + intercept = s + ---& = 2 desiccator, cool and weigh to constant mass.
From the plot, the value of gm can be A-12.2 Calculation
obtained.
Slope + 1 Bulk density, g/ml = 0’004 M
The constant C = , is a measure
Intercept where
of the difference in heats of adsorption of the M = mass, in g, of the material in the
first layer and the succeeding layers. cylinder.
5
IS 9700 : 1991
ANNEX B
( Clause 6 )
SAMPLING AND CRITERIA FOR CONFORMITY OF ACTIVATED ALUMINA
6
IS 9700 : 1991
B-2.3 The number of containers to be chosen with the help of a suitable sampling implement.
from the lot shall depend on the size of the lot The material drawn from different containers
iV shall be as given in Table 2. shall be mixed thoroughly to give a composite
sample which shall be sufficient to make
Table 2 Scale of Sampling triplicate determination for all the characteristics
( Clause B-2.3 ) given in the specification.
Lot Size Number of Containers B-3.2 The composite sample shall then be
to be Selected divided into three parts, one for the purchaser,
another for the supplier and the third for the
t”;‘, $1
up to 15 3
referee. These parts shall be transferred to
16 to 50 5
separate containers which shall be suitably
51 to 100 8
closed and marked with all the details of
IOlandabove 13
sampling.
B-2.4 The containers to be selected for sampling B-3.3 The referee sample bearing the seals of
shall be chosen at random -from the lot. - For both the purchaser and the supplier shall be
this purpose a random number table shall be kept at a place agreed to between the two.
used ( see 1s 4905 : 1968 ). In case such~a table It shall be used in case of a dispute between the
is not available, the following procedure shall two.
be adopted:
B-4 NUMBER OF TESTS AND CRITERIA
‘Starting from any container, count them as
FOR CONFORMITY
, ) , . . . . . . . . . . . . , r, and so on in a systematic
123
manner, where r is the integral part of N/n.
Every rth container thus counted shall be B-4.1 Tests for all the characteristics given in 4
withdrawn to constitute the required sample.’ shall be conducted on the composite sample.
The use of the Standard Mark is governed by the provisions of the Bureau ofIndian
Srandards Act, 2986 and the Rules and Regulations made thereunder. The Standard Mark on
products covered by an Indian Standard conveys the assurance that they have been produced
to comply with the requirements of that standard under a well defined system of inspection,
testing and quality control which is devised and supervised by BIS and operated by the pro-
ducer. Standard marked products are also continuously checked by BIS for conformity to
that standard as a further safeguard. Details of conditions under which a licence for the use
of the Standard Mark may be granted to manufacturers or producers may be obtained from
the Bureau of Indian Standards.
Boreao of Indian Standards
BIS is a statutory institution established under the Bureau of Indian Siandatdr Act, I986 to promoto
ha,rmonious development of the activities of standardization, marking and quality certification of
goods and attending to connected matters in the country.
Copyright
BIS has the copyright of all its publications. No part of these publications may be reproduced in
any form without the prior permission in writing of BIS. This does not preclude the free use, in
the course of implementing the standard, of necessary details, such as symbols and siaes, type or ’
grade designations. Enquiries relating to copyright be addressed to the Director ( Publication ), BIS.
Indian Standards are reviewed periodically and revised, when necessary and amendments, lf anyI
are issued from time to time. Users of Indian Standards should ascertain that they are in
possession of the latest amendments or edition. Comments on this Indian Standard may be sent
to BIS giving the following reference : .A:’
;: 4
BUREAU;OF;INDIAN STANDARDS
Headquarters :
(Page 2, clause A-2.1.1 ) - Insert the following new clauses after A-2.1.1:
‘A-2.1.2 Desiccator
Vacuum desiccator of 15 to 20 cm diameter.
A-2.1.3 Weighing Bottle
Diameter - 6.5 to 70 mm
Height - 30 to 35 mm’
(Page 4, clause A-9.1.1 ) - Insert the following new clause after A-9.1.1:
A -9.1.2 Desiccator
( Page 4, clause A-9.3, line 1) - Substitute ‘5 g’ for ‘10 g’
( Page 4, clause A-9.3, line 8) - Substitute ‘Place the sample with lid
removed alongwith a dial hygrometer in a desiccator, which is partly filled at its
bottom with saturated aqueous solution of sodium nitrite’for ‘Place a dish filled
with saturated solution of sodium nitrite and then the sample with the lid
removed in a desiccator, preferably a dial hygometer.’
(CHD3)