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IS 10016-6 (2000) : Methods of Test for Polybutadiene 
Rubbers, Part 6: Evaluation of Vulcanization 
Characteristics of Polybutadiene Rubbers (BR : 2) [PCD 13: 
Rubber and Rubber Products] 




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IS 10016 (Part 6) : 2000 

Indian Standard 
METHOD-SOFTESTFORPOLYBUTADIENERUBBERS 

PART 6 EVALUATION OF VULCANIZATION CHARACTERISTICS OF 
POLYBUTADIENE RUBBERS (BR : 2) 

ICS 83.060 



©BIS 2000 

BUREAU OF INDIAN STANDARDS 

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG 
NEW DELHI 110002 



May 2000 Price Group 2 



Rubber Sectional Committee, PCD 14 



FOREWORD 

This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the Rubber 
Sectional Committee had been approved by the Petroleum, Coal and Related Products Division Council. 

In this series methods of test for polybutadiene rubbers are given. Various other methods of test for 
polybutadiene rubbers are covered in following parts: 

Parti Method of taking out test portions from sample bales 

Part 2 Determination of ash 

Part 4 Determination of CIS, Trans and Vinyl structure 

Part5 Determination of gel content 

The committee has decided to prepare common methods of test for synthetic rubber under SR (synthetic tubber) 
series and will be applicable to all types of synthetic rubbers being produced indigenously. After preparation of 
common methods of test, Part 1 , Part 2 and Part 5 would be withdrawn. 

In preparation of this standard assistance has been drawn from ISO 2476 : 1996 'Rubber, butadiene (BR) — 
Solution-polymerized types — Evaluation procedure' published by International Organization for 
Standardization (ISO) and ASTM D 3189 Rubber-Evaluation Solution BR (Polybutadiene Rubber), 
published by American Standards for Testing and Materials. 

In reporting the result 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 10016 (Part 6): 2000 



Indian Standard 
METHODSOFTESTFORPOLYBUTADIENERUBBERS 

PART 6 EVALUATION OF VULCANIZATION CHARACTERISTICS OF 
POLYBUTADIENE RUBBERS (BR : 2) 



1 SCOPE 

This standard prescribes standard materials, 
equipment and processing methods for evaluating 
vulcanization characteristics of solution-polymerized 
butadiene rubbers (BR), including oil-extended types 
(OEBR). 

2 NORMATIVE REFERENCES 

The following standards contain provisions which 
through reference in this text, constitute provisions of 
this standard. At the time of publication the editions 
indicated were valid. All standards are subject to 
revision, and parties to agreements based on this 
standard are encouraged to investigate the possibility 
of applying the most recent editions of the standards 
indicated below: 



Title 
Stearic acid, technical (first 
revision) 

Methods of test for vulcanized 
rubbers: Part 1 Tensile stress-strain 
properties (second revision) 
Zinc oxide for rubber industry 
(second revision) 
Methods of test for natural rubber: 
Determination of ash (NR:3) 
(second revision) 

Determination of total copper 
(NR:4) (second revision) 
Determination of manganese 
(NR:5) (second revision) 
Determination of rubber hydro- 
carbon (NR:7) (second revision) 
Determination of Mooney viscosity 
(NR: 8) 

Mixing and vulcanizing of rubber 
in standard compound (second 
revision) 

Rubber — Raw, natural and 
synthetic — Methods for sampling 
and sample preparation (first 
revision) 

Benzothiazyi-2-cyclohexyl sulphe- 
namide (first revision) 
High abrasion furnace (HAP) 
carbon black (first revision) 
Sulphur for rubber industry (first 
revision) 



11720 



IS No. 
1675: 1971 


3400 (Part 1) : 

1987 


3399 : 1993 


3660 
(Part 3) : 


1988 


(Part 4) : 


1988 


(Part 5) : 


1988 


(Part 6) : 


1988 


(Part 7) : 


1988 


(Part 8) : 


1999 


5599 : 1999 



7069 : 1986 
7497 : 1985 
8851 : 1994 



(Part 2) 



(Part 3) 
(Part 4) 
13867 : 1993 



Methods of test for synthetic 

rubber: 
1989 Measurement of vulcanization 

characteristics with oscillating disc 

curemeter (SR:2) 
1993 Determination of Mooney viscosity 
1993 Determination of volatile matter 

Rubber standard temperature, 

humidities and times for the 

conditioning and testing of test 

pieces 

3 TEST RECIPE FOR EVALUATION OF 
VULCANIZATION CHARACTERISTICS 

3.1 Standard Test Formula 

The standard test formula is given below: 



SI Material 
No. 


Parts b) 


> Mass 




Non-oil 
Extended 


Oil 
Extended 


i) Butadiene rubber (BR) 


100.00 


100.00 


ii) Zinc oxide (see IS 3399) 


3.00 


3.00 


iii) Oil furnace black (HAP)" 

(No. 330) (see IS 7497) 


60.00 


60.00 


iv) Stearic acid (see IS 1675) 


2.00 


2.00 


v) Petroleum oil 
(naphthenic) 2 ' (see 
ASTM Type 103) 


15.00 




vi) Sulphur (see IS 885 1) 


1.50 


1.50 


vii) CBS (see IS 7069) or 
TBBS 3) (for method D) 
(min) 


0.90 


0.90 


viii) Calculated density, 
mg/m 3 


1.11 


1.14 to 
1.16 4) 



l> The current Industry Reference Black may be used in place 
of HAF carbon black but this may give slightly different 
results. 

2) ASTM Type 103 oil has the following characteristics: 

Kinematic viscosity at 100°C, 16.8 ± 1.2 mm 2 /s 

Viscosity gravity constant, 0.889 ± 0.002 

The Viscosity Gravity Constant (VGC) is calculated from 
the Say bolt Universal viscosity at 37.8°C and the relative 
density at 15.5/15.5°C. Use the following equation to 
calculate the VGC from the measured properties: 



IS 10016 (Part 6) : 2000 



VGC- 



10rf-1.07521og 10 (v-38) 



10»log l0 (v-38) 
where 

d = relative density at 15.5/15.5°C; 

v = Saybolt Universal Viscosity at 7.8°C. 

3) N-ter-butyl-2-benzothiaziIe sulphenamide as per Material 
Reference No. 384. 

4> Based on 37.5 percent oil-extended BR. 

3.2 Procedure 

3.2.1 Equipment and Procedure 

Equipment and procedure for the preparation, mixing 
and vulcanization shall be in accordance with 
different parts of IS 3660 (Part 8) wherever 
applicable. 

NOTE — Details of a suitable internal mixer are given in 
Annex A. 

3.2.2 Mixing Procedure 

The following four mixing procedures are specified: 

M ethod A Internal mixer for initial and final 
mixing; 

M ethod B Internal mixer for initial and mill 
for final mixing; 

M ethod C Mill mixing; and 

Method D Miniature internal mixing. 

NOTE — These procedures may give different results. 

The mill handling of solution butadiene rubbers is more 
difficult than for other rubbers and mixing is best accomplished 
by using an internal mixer. Because of the difficulty of mill 
mixing butadiene rubber, it is recommended that one of the 
internal mixer procedures (methods A, B or D) be used where 
such equipment is available. With some types of butadiene 
rubber it is not possible to get a satisfactory mix using the mill 
mixing procedure. 

3.2.2.1 Method A 

Internal Mixer for initial and final mixing 
Stage 1 — Initial mixing procedure 

Duration Cumu- 

(min) lative 
(min) 

a) Adjust the temperature, speed 
and ram pressure of the internal 

mixer to achieve the condition 
outlined in 3.2.2.1(e). Close the 
discharge gate, start the rotor 
and raise the ram. 

b) Charge one-half of the tubber, the 0.5 0.5 
zinc oxide, the carbon black, the oil 

(omit from Formula 2 for OEBR), 
the stearic acid and the balance of 
the rubber. Lower the ram. 



Duration Cumu- 

(min) lative 

(min) 

c) Allow the batch to mix. 3.0 3.5 

d) Raise the ram and clean the 0.5 4.0 
mixer throat and the top of the 

ram. Lower the ram. 

e) Discharge the batch at a 2.0 6.0 
temperature of 170°C or after a 

total time of 6 min, whichever 
occurs first. 

f) Immediately pass the batch three times through a 
laboratory mill with a mill opening of 5.0 mm 
and a temperature of 50 ± 5°C. Check, weigh the 
batch. If the batch weight differs from the 
theoretical value by more than 0.5 percent, 
discard the batch. 

g) Rest the batch for at least 30 minutes and up to 
24 h. 

Stage 2 — Final mixing procedure 

Duration Cumu- 

(min) lative 

(min) 

a) Cool the internal mixer to a 
temperature of 40 ± 5°C with 

full cooling water on the rotors. 
Start the motor and raise the 
ram. 

b) Leave the cooling water on and 0.5 0.5 
the steam off. Roll all the 

sulphur and the CBS into one- 
half of the masterbatch and 
charge into the mixer. Add the 
remaining portion of the 
masterbatch. Lower the ram: 

c) Allow the batch to mix until a 2.5 3.0 
temperature of 110°C or a total 

time of 3 min is reached, 
whichever occurs first. 

d) Immediately pass the batch through a laboratory 
mill with a mill opening set at 0.3 mm and at a 
temperature of 50 ± 5°C. 

e) Pass the rolled batch endwise through the rolls 
six times. 

f) Sheet the batch to approximately 6 mm and 
check, weigh. Remove sufficient sample for 
curemeter testing, if required. 

g) Sheet the batch to approximately 2.2 mm for 
preparing test slabs or to the appropriate 
thickness for preparing ring specimen. 

3.2.2.2 Method B 

Internal mixer for initial and mill for final mixing 
Stage 1 — Initial mixing procedure 



IS 10016 (Part 6) : 2000 



Prepare the initial mix in accordance with procedure 
outlined in3.2.2X (Stage 1) 

Stage 2 — Final mill mixing procedure 

Adjust the mass of all material (that is masterbatch, 
sulphur and CBS) to give a final batch mass of four 
times the formula mass, 

NOTE — AU null openings should be adjusted to maintain a 
good rolling bank at the nip of the rolls mixing. If this is not 
obtained with the settings specified hereunder, small 
adjustments to mill openings may be necessary: 

Dura- Cumu- 
tion lative 

(min) (min) 

a) Set and maintain the mill roll 1.0 1.0 
temperature at 40 ± 5°C and the mill 

opening at 1.5 mm. Band the 
masterbatch and band round the front 
roll. 

b) Add the sulphur and the CBS slowly to 1.0 2.0 
the batch. 

c) Make six 3/4 cuts from each side. 1.5 3.5 

d) Cut the batch from the mill. Set tbe mill \J5 5.0 
opening to 0.8 mm and .pass the rolled 

batch end-wise through the rolls six 
times. 

e) Sheet the batch to approximately 6 mm and check, weigh. 
Remove sufficient sample for curemeter testing, if required. If 
the weight differs more than 0.5 percent from the theoretical 
value, discard the batch. 

Sheet the batch to approximately 2.2 mm for preparing test 
slabs or to the appropriate thickness for preparing specimens. 
Cool the compound on a flat dry metal surface at 23 ± 3°C for 
1 6 h and RH £ 55 percent. 

3.2.23 MethedC — Mill mixing procedure 

The standard laboratory batch mass, in grams, shah 
be based on four times the formula mass. Adjust the 
mill roll cooling conditions to maintain a temperature 
of 35 ± 5°C throughout the mixing operations. 

NOTES 

1 Methods A and B, which give better diipension of the 
ingredients, are to be preferred if an internal mixer is available. 

2 All mill openings should be adjusted to maintain a good 
rolling bank at the nip of the rolls during mixing. If this is not 
obtained with the settings specified hereunder, small 
adjustments to mill openings may be necessary: 



a) 



b) Add the zinc oxide and the stearic acid 2 3 
evenly across the rolls. Make two -3/4 

cuts from each side. 

c) Add the carbon black evenly across the 15 to 18 18 to 21 

rolls at a uniform rate. When about half 
the black has been incorporated, open the 
rolls to 1.8 mm and then add the 
remainder of the black. Make hvo 3/4 cuts 
from each side, allowing 30 s between 
each cut. Be certain to add the black that 
has dropped into the mill pan. 



Duration 


Cumu- 


(min) 


lative 




(min) 


Band the rubber with the mill opening 1 


1 


set at 1.3 mm. 





Dumtion Cumu- 

(min) latjve 

(min) 

d) Add the oil (omit from Formula 2 for 8 to 10 26 to 31 
OEBR) very slowly drop by drop. 

e) Add the sulphur and the CBS. 2 28 to 33 

f) Make six successive 3/4 cuts from each 2 30 to 35 
side. 

g) Cut the batch from the mill, set the mill 2 32 to 37 
opening to 0.8 mm and pass the rolled 

batch end-wise through the rolls six 
times. 

h) Sheet the batch to approximately 6 mm and check, weigh the 
batch. Remove sufficient sample for curemeter testing if re- 
quired. The weight should not differ more than 0.5 percent 
from the theoretical value, if more discard the batch. 

j) Sheet the batch to approximately 2.2 mm for preparing teat 
slabs or to the appropriate thickness for preparing ring speci- 
mens. Cool the compound on a flat dry metal surface at 23 * 
3°C for 1-24 h and RH < 55 percent. 

NOTE — It is sometimes easier and mote practical to combine 
steps 3.2.23(c) and 3.2.2.3(d) above, either by premixing the 
oil and black together-and then adding the oiled black directly 
to the rubber on the mill as described in 4JL23(c) and 
thus omitting 4.2.23(d) or by adding carbon black and oil 
alternately. 

3.2.2.4 Method D — Miniature Internal Mixer (MM) 
procedure 

a) For general mixing procedure. 

b) Mix with the head temperature of the 

miniature internal mixer maintained at 
60 ± 3°C and the rotor speed set at 6.3 to 
63 rpm. 

c) Prepare the rubber by passing it through a 

mill one time with the temperature set at 
40 ±3°C and an opening that would give 
approximately 5 mm thick sheet. Cut the 
sheet into strips that are approximately 
2 5 mm wide. 

Dura- Cumu- 
tion lative 

(min) (min) 

a) Charge the mixing chamber with 0.0 0.0 
the rubber strips lower the ram, 

and start timer. 

b) Masticate the rubber. 0.5 0.5 
c) Raise the ram, add zinc oxide, 1.0 7.5 

sulphur, stearic acid and TBBS 
that have previously been blended 
taking cam to avoid any loss. 

d) Add portions of carbon black 1 2.5 
and oil alternately sweep the 

orifice and lower the ram. 

e) Allow the batch to mix, raising 6.5 9.0 
the ram momentarily to sweep 

down if necessary. 

f) Turn off the motor, raise the ram, remove the mixing 
chamber, and discharge the batch. Record the 
maximum batch temperature indicated if desired. 



IS 10016 (Part 6) : 2000 



g) Pass the batch through a mill at 40 ± 5°C and 

0.5 mm opening once then twice at 3 mm 

opening, 
h) Check the batch mass and record. If it differs from 

the theoretical value by more than 0.5 percent, 

discard the batch. 

4 CONDITIONING OF COMPOUNDS 

Conditioning all batches produced by methods A, B, 
C or D at a standard laboratory temperature for 1 to 
24 h after mixing and prior to vulcanizing as per 
IS 13867. 

5 EVALUATION OF WLCANIZATION 
CHARACTERISTICS 

5.1 Evaluation According to. Stress-Strain 
Properties 

5.1.1 Vulcanize sheets at r45°C for 25, 35 and 50 
min. 

Alternatively, vulcanize sheet at 150°C for 20, 30 and 
50 min. The recommended cure time for the 
miniature internal mixture compound if 35 min at 
M5°C. 



5.1.2 Condition the vulcanized sheets for 16 to 96 h 
at a standard laboratory temperature and humidity 
defined in IS 13867. 

5.13 Measure the stress-strain properties in 
accordance with IS 3400 (Part 1). 

5.2 Evaluation According to Oscillating Disc 
Curemeter Test 

Measure the following standard test parameters: 

M u A/ H , ts\, f c (50) and f c = (90) 

in accordance with IS 11720 (Part 2) t using the 
following test conditions: 

Oscillation frequency : 1.7 Hz (100 cycles/ 

min) 
Amplitude of oscillation : 1°C arc 



Selectivity. 


: To be selected to give 
at least 75 percent full 
scale deflection 




NOTE — With some 
rubber, 75 percent may not 
be attainable. 


Die temperature 


:160±1°C 


Pre-heat time 


:None 



ANNEX A 

. (Clause 3.2.1) 

INTERNAL MIXER 



A-l The internal mixer should have a nominal 

capacity of approximately 1000 CC. 

A-2 The rotor speed(s), ram pressure and coolant 
<- flow of the internal mixer should be such that the 
conditions specified in 3.2.2.1(e), 3.2.2.2(c) and 
3.233(e) will be accomplished. 



A-3 The batch size should be the nominal capacity of 
the internal mixer measured in cubic centimetres, 
multiplied by the density (+ 0, - 10 percent). 

NOTE — If an old or worn internal mixer is used, the batch 
muss should be increased accordingly. 



Bureau of Indian Standards 

BIS is a statutory institution established under the Bureau of Indian Standards Act, 1986 to promote 
harmonious development of the activities of stardardization, 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 sizes, type or grade designations. 
Enquiries relating to copyright be addressed to the Director (Publication), BIS 

Review 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 Additions'. 

This Indian Standard has been developed from Doc: No. PCD 14 (1058). 

Amendments Issued Since Publication 



Amend No. 



Date of Issue 



Text Affected 



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