IS 13913: Molybdenum Disulphide, Paste

12 Pages·1994·1.3 MB·English

by  Bureau of Indian Standards

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IS 13913 (1994): Molybdenum Disulphide, Paste [PCD 3:
Petroleum, Lubricants and their Related Products]
“!ान $ एक न’ भारत का +नम-ण”
Satyanarayan Gangaram Pitroda
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“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता हहहहै””ै”
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“Knowledge is such a treasure which cannot be stolen”

Indian Standard
.
MOLYBDENUM DISULPHIDE, PASTE -
SPECIFICATION
UDC 621.892

Q SIB 1994
BUREAU OF INDIAN STANDARDS
KANAM ,NAVAHB 9 RUDAHAB HAHS RAFAZ MARG
WEN IHLED 110002
February 1994 Price Group 3
Lubricants and Related Products Sectional Committee, PCD 4
FOREWORD
This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the
Lubricants and Related Products Sectional Committee had been approved by the Petroleum Coal and
Related Products Division Council.
Molybdenum disulphide in concentrated paste form is an important solid lubricant. It can be easily
applied in paste form. It has found wide application for reducing friction and metal to metal contact
under extreme pressure conditions, for example, in press fittings, power screws, running-in-lubricant for
new parts and gears. It is applied where there are chances of gelling and welding.
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 13913 : 1994
Indian Standcvd
MOLYBDENUMDISULPHIDE,PASTE-
SPECIFICATION
1 SCOPE Table 1 Requirements of Molybdenum
Disulphide, Paste
This standard prescribes the requirements and the
( Clause 3.2 )
methods of sampling and test for Molybdenum
Disulphide, Paste.
Sl Characteristic Requirt- Ann tx Method
NO. ment of Test
2 NORMATIVE REFERENCES ( l’s :1&f
The following Indian Standards contain provi- (‘1 (2)
(3) (4) (5)
sions which through reference in this text consti- i) Consistency at P : 60
tute the provisions of the standard. At the time 25 & 0.5%
of publication, the editions indicated were valid.
a) Unworked To report
All standards are subject to revision and parties
b) Worked ( 60 dou- 310 - 340
to agreements based on this standard are ble strokes )
encouraged to investigate the possibility of
ii) Drop point “C, Min 320 A
applying the most recent editions of the standards
iii) Molybdenum di- 60 B
indicated below: )
sulpbide ( MoS,
i) IS 1447 : 1966 Methods of sampling of cmoanstse,n tM, inp ercent by
petroleum and its products;
iv) Particle size, per- 60 C
cent by mass ( less
ii) IS 1448 Methods of test for petroleum and
than 10 microns ),
its products; and MCI
iii) IS 13797 : 1993 Molybdenum disulphide
4.2 Marking
dispersion in oil.
The containers shall be marked with the
following:
3 REQUIREMENTS
i) Name of the material;
3.1 Composition ii) Net mass in the container;

iii) Indication of the source of manufacture;
The product shall be a homogeneo u s paste con- iv) Date of manufacture;
taining high percentage of molybdenum
v) Recognized trade-mark, if any; and
disulphide powder in refined mineral lubricating
vi) Batch number, or code number.
base oil having a viscosity index, 80 A& and
kinematic viscosity at 40°C as 90 - 100 cSt with 4.2.1 The containers may also be marked suitably
or without additives. with the Standard Mark.
3.2 I he material shall also comply with the 4.2.2 The use of the Standard Mark is governed
requirements given in Table 1 when tested by the provisions of Burean of Indian Standards
according to the methods prescribed in co1 4 Act, 1986 and the Rules and Regulations made
and 5 of the table. thereunder. The details of conditions under
which the licence for the use of Standard Mark
may be granted to manuf.acturers or producers
4 PACKING AND MARKING
may be obtained f’rom the Bureau of Indian
4.1 Packing Standards.
5 SAMPLING
The material shall be packed in suitable
containers as agreed to between the purchaser Representative samples Gf the material shall be
and the supplier. drawn as prescribed in IS 1447 : 1966.
SI 31931 : 4991
ANNEX A
r Table 1, Sl hro. (ii) ]
DETERMINATION OF DROPPING POINT
A-l GENERAL The test method is useful to assist in identifying
the grease as to type and for establishing and
This test method covers the determination of the maintaining bench marks for quality control. The
dropping point of lubricating grease, this point results are to be considered to have only limited
being the temperature at which the first drop of significance with respect to service performance
material falls from the cup. as dropping point is a static test.
NOTE - evitarepooC gnitset setacidni ,taht in
A-2 SIGNIFICANCE AND USE
general, dropping point by this method and test
method IS 1418 [ P : 52 ] : 1971 are ni agreement. In
Dropping Point - In general, the dropping case where results differ, there is no known signifi-
point is the temperature at which the grease cance. However, agreement between the manufacturer
and the purchaser as to the test method used is
passes from a semisolid to a liquid state under
advisable.
the conditions of test. This change in sta.te is
typical of greases containing as thickeners soaps A-3 APPARATUS
of conventional types. Greases containing as
thickeners materials other than conventional A-3.1 Dropping Point Assembly ( Fig. 1 ) -
soaps may, without change in state, separate oil. consisting of the following.
n
k-
D- THERMOMETER
76 IMMERSION
* 06.73-7.11 n
t-l 5.87 4-J .794
E-7 CUP PLUG GAUGE
MAiL:- AISI.01 HARDEN
E-l TO SO-52 ROCKWELL ‘C’
WI
*5=d---k-~12.7 iI I
E-l THERMOtiETER
CLAMP
d $-R 4.54
-615,87 w B- THIN WALL
1 ,f+KNtJRL TEST TUBE
2.4 LENGTH 1 OOf 1
i W=lS*l
ID=1 2fl
66.!
E-2 AL OR TRANSITE
BUSHING
6
12.7 0
! 34
E-3 AL OR ~~012.~ A- GREASE CUP
BUSHING
MATL:- AL OR TRANSITE A-GREASE CUC-
U
4.7 F- THERMOMETER
*ASSEMBLY
E-4 BUSHING
iI;LpORT RING (0 l?B6 1 E-5 THERMOMETER C-CUP SUPPORT G-TUBE
:- 0 1 .O SS WIRE DEPTH GAUGE LENGTH 16+1 ASSEMBLY
MATL:- CHROMIUM OD 11+0.4
PLATED BRASS ID 9+0.5
llA snoisnemid ni .sertemillim
FIG. 1 APPARATUSF ORD ROPPINOP OINTT EST OF LUBRICATINGG REASE
2
s1 31931 : 1994
1.1.3-A esaerG puC
A-4 PROCEDURE
A chromium-plated brass cup conforming to the
A-4.1 Insert empty test tubes in every test tube
dimensions shown in A, Fig. 1.
well and a thermometer having a range from
-5 to 400°C in the thermometer well of the
A-3.1.2 Test Tube
oven.
A thin walled, soft glass test tube with rim,
A-4.2 Select the lowest oven temperature from
having dimensions shown in B, Fig. 1.
the four listed below that will permit a dropping
point determination.
A-3.1.3 Cup Support
Oven Temperature Dropping Point
Glass tubing as shown in C, Fig. 1.
“C “C
A-3.1.4 Thermometer 12L f 3 116
232 f 3 221
Immersion thermometer ( 76-mm immersion ),
288 f 3 277
graduated in Celcius degrees, having a range
343 f 3 330
from - 5 to 400°C and contorming to the require-
ments for thermometer 3C as prescribed in A-4.3 Select and use test tubes and accessories
ASTM Specification E 1 and shown in D, Fig. 1 E-l, E-2, and E-3 to minimize wobble of the
or its equivalent. thermometer. All components E-l through E 4
on the thermometer in the order shown by the
A-3.1.5 Accessories thermometer assembly (F) Fig. 1. Adjust the
bushing E-3 and the bushing support ring E-4 so
Thermometer clamp as shown in E-l, bushings
that E-4 is about 25 mm from the tip of the
as shown in E-2 and E-3, bushing support ring as
thermometer. Place the cup support C in tube B.
shown in E-4, thermometer depth gauge as shown
Insert the thermometer depth gauge E-5 and the
in E-5, and a metal rod as shown in E-6, and CUP thermometer assembly in the tube. Position the
gauge as shown in E-7, ail of Fig. 1.
thermometer so that the tip bottoms in the gauge.
Adjust the bushing E-2 and the thermometer
A-3.2 Ahminium Block Oven
clamp E-l so that the bushing shoulders on the
An aluminium block oven of the design and di- top edge of the tube. By use of the cup gauge E-7
mensions shown in Fig. 2. The block shall be select for test a cup conforming to the dimen-
equipped with an integral cartridge-type heater. sions of the gauge. Check the diameter of the
Control of the current to the heater shall be used bottom opening of the cup using as gauges a
to obtain and maintain the desired oven 2*78-mm rod as the GO gauge and a 2.83 mm rod
temperature. as the No-GO gauge. If the orifice is undersize it

190.5 -
t---w 25.4 p,,,,,Eu
-i
INSULATION
All dimensions in millimetres.
FIG. 2 ALUMINNJMB LOCK OVEN
3
IS 13913 : 1994
must be reamed to the correct size or if too A-6 PRECXSION AND BIAS
large, discarded.
A-6.1 Repeatability
A-4.4 Fill the grease cup by pressing the larger The difference between two test results obtained
opening into the grease to be tested until the cup by the same operator with the same apparatus
is filled. Remove excess grease flush with the under constant operating conditions on identical
top edge of the cup with a spatula. Gently press test material would, in the long run, in the nor-
the cup, held in a vertical position with the mal and correct operation of the test method,
smaller opening at the bottom, down over the exceed the following values in only one case on
metal rod E-6, Fig. 1, until the latter protrudes twenty:
about ‘25 mm. Press the rod against the cup in
Grease Dropping “C
such a manner that the rod makes contact at
both the upper and lower peripheries of the cup. “C
Maintain this contact, rotating the cup in the Up to 116 5.5
rod along the index finger to give it a spiral-like
117 to 221 7.7
motion down the rod to remove a conical section
of the grease which adheres along the rod. As 222 to 277 4.4
the cup approaches the end of the rod, carefully 258 to 330 5.5
slip the rod out of the cup so that a smooth film
of reproducible thickness remains inside the A-6.2 Reproducibility
cup.
The difference between two single and indepen-
dent results obtained by different operators
A-4.5 Remove the thermometer assembly and
working in different laboratories on identical test
depth gauge from the tube. Place the grease cup
material would, in the long run, in the normal
on the cup support in the test tube and carefully
and correct operation of the test method, exceed
reinsert the thermometer assembly. Make no
the following values in only one case in twenty:
further adjustment as the thermometer bulb is
now positioned to provide adequate clearance Grease Dr@ping “C
between the tip of the bulb and cup orifice.
“C
A-4.6 Remove an empty tube from the oven and Up to 116 8.9
gently insert the tube assembly, G Fig. 1, making 117 to 221 11.7
certain that the cup remains upright in the cup
222 to 277 13.9
support. If the cup is tilted, the thermometer
bulb may come in contact with the film of grease 278 to 330 23-9
and result in an erroneous value. A-6.3 Bias
A-4.7 Multiple determinations may be made There is no bias for this test method because the
simultaneously. value of the dropping point can be defined only

in terms of the test method.
A-5 CALCULATION NOTES
1 Values for greases dropping below 221°C based on
A-5.1 Calculate the dropping point as follows: the use of the older heavy wall temperature resistance
tubes. Values for greases dropping above 221“C are
DP = ODP + [ ( BT - ODP )/3 ] based on the use of the thin wall test tube ( A-3.1.2 ).
2 Certain greases for example, some aluminium-base
greases, may form a drop with a tailing thread upon
where melting, which may break off or which may hold
until the drop reaches the bottom of the test tube; in
DP = dropping point; any case, the dropping point shall be taken as the
temperature when the drop reaches the bottom of the
ODP = thermometer reading when first drop test tube.
falls from the cup; and 3 The dropping points of some grease, particularly
those containing simple aluminium soaps, are known
BT = block temperature when the drop to decrease upon aging, the change being much
falls. greater than the deviation permitted in results obtain-
ed by different laboratories. Therefore, comparative
tests between laboratories should be made within a
A-5.2 It is recommended that both the calculated
period of six days.
dropping point value and the oven temperature
4 The cooperative data given in NLGT Spokesman,
at which the dropping point was determined be
Vol 31., 1957, p 76 indicate that precision varies with
reported. droppmg point range.
4
IS 13913 : 1994
ANNEX B
)iii( ]
[ Table 1, Sl JVo.
DETERMINATION OF MOLYBDENUM DISULPHIDE CONTENT
B-l REAGENTS distilled water. The final volume of the filtrate
should be approximately 400 ml.
B-I .I Concentrated Nitric Acid - Sp.
Gravity, 1.42 A-R, Grade. B-2.4 Add 2-3 drops of Methyl Orange Indicator
and neutralise by the dropwise addition of con-
B-1.2 Perchloric Acid - 60 percent, A.R.
centrate hydrochloric acid with constant stirring.
Grade.
B-Z.5 Add 30 ml of ammonium acetate solution
B-l.3 Concentrated Ammonia Solution -
and 10 ml glacial acetic acid and bring almost to
Sp. Gravity 0.880.
boil.
B-l.4 Methyl Orange Indicator - 0.5 percent
B-2.6 Add lead acetate solution slowly with
( v/u ) in industrial methylated spirit.
constant stirring until an excess of 30 ml has
B-l.5 Concentrated Hydrochloric Acid - been added. The bulk of the reagent should be
Sp. Gravity 1.18, A.R. Grade. added at a fixed rate of 30 ml in 2 minutes with
mechanical stirring. Tannic acid solution is used
B-l.6 Ammonium Acetate Solution ( Aque-
as an external indicator, the endpoint being
ous ) - 30 percent ( W/V ).
reached when a drop of filtrate added to a small
B-l.7 Lead Acetate Solution - 2 percent volume of the tannic acid solution on a spot plate
( W/V ) in 2 percent ( v/v ) Acetic acid. fails to develop a brown colouration.
B-1.8 Tannic Acid Indicator - O-1 percent B-2.7 Bring the solution to almost boiling condi-
( W/V ) in 4 percent ( v/v ) Acetic acid. tion and allow to remain at this temperature for
one hour.
B-l.9 Acetic Acid, Glacial
B-2.8 Filter the precipitate on to a 15 cm No. 42
B-2 PROCEDURE
Whatman Filter Paper and wash thoroughly with
B-2.1 Weigh approximately 0 25 g ( to the hot water.
nearest of 0.001 g ) (W 1) of the sample into a
B-2.9 Ignite the precipitate in a tared porcelain
400 ml beaker. Add 15 ml concentrate nitric
crucible at 700°C - 800X, cool and weigh (W,).
acid and 25 ml of perchloric acid. Place on hot
plate and allow to fume vigorously ( do not cover
the beaker ), Continue heating un til the sample B-2.16 Calculation
is white and the volume of the acid is about
Calculate the percentage molybdenum disulphide
5 ml.
content from the following:
B-2.2 Cool and dilute to about 50 ml with dis-
tilled water. Add 40 ml of concentrate ammonia Molybdenum disulphide, W, x 43.60
slowly with constant stirring and bring to boil. percent by mass =
WI
B-2.3 Filter while hot through a 12.5 cm NO 41 where
Whatman Filter Paper, Collect the filtrate in a
WI = mass of the ignited residue, and
600-ml beaker and wash the residue on filter
paper at least 8 times with hot. WI = mass of the sample taken.