Article

RRIM TEST METHODS FOR STANDARD MALAYSIAN RUBBERS
SMR BULLETIN NO.7 REVISED EDITION 1992
RRIM TEST METHODS FOR STANDARD MALAYSIAN RUBBERS
Revised Edition 1992 by Ng Yu Tong
Published and Printed by the Rubber Research Institute of Malaysia (A Statutory Agency under the Ministry of Primary Industries)
COPYRIGHT MALAYSIAN RUBBER BOARD
Abbreviated title: SMR Bull. No. 7 Rubb. Res. Inst.
Malaysia
CONTENTS
PART A PART B
DEFINITIONS SAMPLING AND SMR CERTIFICATION TEST METHODS USED BY RRIM AND RECOMMENDED FOR ROUTINE USE BY PRODUCERS AND LABORATORIES B.l Routine Sampling for Testing and Certification Homogenisation of Piece Allocation of Homogenised Piece for Testing Determination of Dirt Determination of Volatile Matter Determination of Ash Determination of Nitrogen Determination of Rapid Plasticity and Plasticity Retention Index (PRI) Determination of Modhey Viscosity Determination of "Colour PRODUCTION CONTROL TEST METHODS USED BY RRIM AND RECOMMENDED FOR ROUTINE USE BY PRODUCERS AND LABORATORIES C.l Wallace Accelerated StorageHardening Test (WASHT) Mooney Accelerated StorageHardening Test (MASHT) Measurement of Curing Characteristics with the Oscillating Disc Rheometer
B.2 B.3
B.4 B.5 B.6 B.7 B.8
B.9 B.10 PART C
C.2
C.3
PART D
ADDITIONAL TEST METHODS FOR PRODUCTION CONTROL USED BY RRIM D. 1 Determination of Vulcanisation Characteristics Using the Relaxed Modulus Test (MOD Test) Test for Excessive Use of Castor Oil in Heveacrumb Determination of Acetone Extract
D.2
D.3
The RRIM Test Methods for Standard Malaysian Rubbers, which had been approved by the Technical Manager, SMR/TSR Control Testing Unit and endorsed by the Directorate of the Rubber Research Institute of Malaysia (RRIM) were published under the authority of RRIM, a statutory agency under the Ministry of Primary Industries. These test methods are subject to periodical review to keep abreast of progress in the industries concerned. All copyrights are reserved by the RRIM. No part of this publication may be reproduced in any form or by any means without permission in writing from the RRIM. These Test Methods thus supersede SMR Bulletin No. 7 (RRIM Test Methods for Standard Malaysian Rubbers) published in 1973.
PART A DEFINITIONS
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The following definitions shall apply Lot A quantity of bales of the same type and grade, from the same source, and forming one consignment not exceeding 50 tonnes. A collection of bales which represent the lot or consignment. Rubber taken from a bale to represent the bale. Rubber taken from the piece for testing.
Sample Piece Test portions (testpiece) Crumb rubber
Natural rubber (NR) processed, before final drying and baling, into a particulate structure of large surface area. Crumb rubber prepared by a method which includes the use of a crumbling agent as approved by the RRIM.
Heveacrumb
PART B SAMPLING AND SMR CERTIFICATION TEST METHODS USED BY RRIM AND RECOMMENDED FOR ROUTINE USE BY PRODUCERS AND LABORATORIES
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B.l 1.1
R O U T I N E SAMPLING FOR TESTING AND C E R T I F I C A T I O N Sampling is based on a production lot system wherein the size of a lot may vary from 1 tonne to 50 tonnes. The sampling frequency is set at 10% of the bales (or blocks) subject to a minimum sample size of six. For production lot exceeding 300 bales, at least one piece (bale sample) is taken from each pallet. Schematically, the sampling plan is represented as follows: SMR SAMPLING PLAN Lot Size 1 tonne 2 1 0 tonnes 10 30 pallets 31 - 50 pallets No. of Samples 6 10% of number of bales Minimum 30 with at least 1 piece from each pallet 1 piece from each pallet
The RRIM advises the producer on the exact method of sampling, particularly in special consignments upon consumer's request. The basis of SMR sampling shall be representative and non-selective in the sense that samples taken shall be genuinely reflective of the bales within the lot. 1.2 Method of Taking a Piece Pieces are taken from the bales selected as representative of the lot in the following manner. The pressed and unwrapped bale is placed on a clean, horizontal platform with the shortest edges in a vertical position. A clean, dry knife is used to cut a subpiece of triangular section (approximately 50 X 50 x 140 mm) down the entire length of one vertical edge so that a subpiece of minimum weight 180 g is obtained. Another similar subpiece is cut from the diagonally opposite vertical edge. The two subpieces which together constitute the piece representing the bale are placed in a polyethylene bag with appropriate markings complete with the necessary details inserted.
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B.2
HOMOGENISATION OF PIECE The piece is passed six times through the gap between the rolls of a 150 x 300 mm ( 6 x 1 2 in) laboratory mill having the rolls rotating at uneven speeds with friction ratio 1 : 1.4 + 0.1 the back roll rotating at 31 rev/min. The rolls are cooled with running water at room temperature and the gap is set at 1.65 + 0.16 mm. After each pass the rubber is rolled into a cylinder and introduced endwise for the next pass. A clean, stainless steel tray below the rolls should be available to catch any rubber or dirt from the piece; any such rubber or dirt is returned to the rubber at the next pass. The rubber is not rolled after the fifth pass but folded and passed lengthwise through the rolls. After this sixth pass, the rubber is folded before testpieces are cut out for the various tests.
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B.3
ALLOCATION OF HOMOGENISED PIECE FOR TESTING Portions of the following approximate weights (in grammes) are cut from the blended piece for the various tests. In case of repeat testing, the portions for tests will be cut from the remnant blended pieces from the rubber store. Test Dirt Volatile matter PRI Colour Mooney viscosity Ash Nitrogen Acetone extract Wallace accelerated storagehardening test Mooney accelerated storagehardening test Modulus Rheometric cure Approximate Weight (g) 20 - 30 20 - 30 15 - 25* 10-20 25 10 5-10 5 15 1 5 2 5* 25 100** 100
*Same piece for PRI and Wallace ASHT if both tests are required. **Same piece for Modulus and Rheometric cure if both tests are required.
Contamination on the surface of the rubber test portions should be avoided. Allocated test portions should be wrapped in clean polythene bags and kept in a clean, dry place.
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B. 4 4.1
DETERMINATION OF DIRT Explanatory Notes This is a very variable property of NR. Dirt is conveniently regarded as the foreign matter in raw NR which fails to pass a sieve of 44 /xm side-square aperture. Because the distribution of dirt in the rubber is not, as a rule, uniform, a recognised homogenisation procedure must be carefully followed.
4.2
Principle of Method This test is based on dissolution of the rubber in a high boiling solvent, passing the solution through a sieve of 44 /xm side-square aperture, thorough washing of the retained dirt, and weighing of the residue on the sieve.
4.3
Reagents (a) Rubber solvent, being mineral turpentine (high aromatic white spirit) of bp 155C to 196C or its equivalent. Normally filtered first through a filter paper.
(b) Rubber peptising agent, preferably xylyl mercaptan or its equivalent as recommended by RRIM from time to time depending on availability. 4.4 Apparatus (a) Conical flask, of 500 ml capacity
(b) Thermometer, reading 100C - 200C
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(c)
Sieve: This consists of a stainless steel cylinder of approximately of 30 mm external diameter, 2 mm to 3 mm wall thickness and 13 mm height, onto which a stainless steel or phosphor-bronze gauze of 44/xm side-square aperture is soldered. The sieve weighs about 15 g. The cylinder has a recess of about 1 mm around the inner edge of the top and around the outer edge of the lower end to allow for easy stacking of the sieves (Figure 1). Heating unit, preferably consisting of infra-red lamps (250 watts each) arranged in rows and columns with the base of the conical flask placed at about 20 cm above the top of the lamps. Each column of lamps can be switched off whenever there is risk of overheating of the samples placed directly above it. Analytical balance, weighing to 0.1 mg Drying oven, operating at 90C 100C
(d)
(e) (f) (g) (h) (i) (j) (k)
Ultrasonic bath, for cleaning the sieves Drying cabinet, for drying flasks, etc. Desiccator, for cooling the sieves Sieve holder, to facilitate filtration into a conical flask (Figure 2) Inspection holder, for sieves to fit a 50.8 X 50.8 mm ( 2 x 2 in) slide carrier (Figure 3)
4.5 4.5.1
Procedure Dissolution Take about 30 g of the homogenised rubber and pass twice through a cold mill with nip set at 0.33 + 0.05 mm. Accurately weigh a test portion of approximately 10 g of this rubber, cut into small strips (about twelve to fifteen) and place in a 500 ml conical flask containing about 250 ml of mineral turpentine and about 1 ml of rubber peptising agent (see 4.7.1). Place the
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flask and its content on the infra-red heating unit and heat with occasional agitation to assist dissolution which is usually completed in 1V2 h to 2 h (see 4.7.2). 4.5.2 Filtration When dissolution is complete, filter the hot solution through a previously weighed, clean and dry sieve (no suction should be applied) by decantation, leaving as much dirt as possible behind for further washings. Wash the dirt in the flask with 30 ml to 50 ml of hot mineral turpentine, and decant the washings into the sieve. Hold the flask mouth downwards at a convenient angle, blow a jet of cold mineral turpentine into it and allow to drain through the sieve. Repeat the process of washing again. Complete the washing with a rinse of hot mineral turpentine around the inside wall of the sieve. 4.5.3 Drying, etc. Dry the sieve with the retained dirt in an oven at 90 C to 100C for about 1 h, cool in a desiccator and reweigh to the nearest 0.1 mg. 4.6 Calculation The dirt content is expressed as a percentage of the test portion as follows: B A Percentage of dirt = ~ x 100
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where
A is the weight in grammes of the clean dry sieve; B is the weight in grammes of the sieve plus dirt; C is the weight in grammes of the test portion.
4.7 4.7.1
Notes The thinning out and cutting into strips of the homogenised test portion offer a larger surface area of the rubber and reduce the dissolution time. There is danger of fire if the rubber solution is overheated or if the mouth of the flask is pointed towards the heater. Over-heating may also result in gelling and therefore incomplete dissolution of rubber. Complete dissolution of the rubber in mineral turpentine should be attained. After dissolution, the flask should be shaken to observe that the dirt particles move freely and finally settled at the centre of the base of the flask. If this precaution is not taken, undissolved rubber particles sometimes stick to the sides of the flask and are subsequently washed into the sieve and dried, giving a spurious (high) result. Any rubber adhering to the sieve during and after filtration should be removed. This is indicated by the presence of gelatinuous substance which should be re-dissolved by immersing the sieve with its contents in a beaker of hot turpentine together with one drop to two drops of rubber peptising agent. The resulting solution should be re-filtered and the sieve dried and weighed. The dry dirt should be free-flowing and readily dislodged from the sieve by tapping gently.
4.7.2
4.7.3
4.7.4
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4.7.5
Flasks and sieves should be well cleaned and dried before use. Cleaning of sieves with an ultrasonic cleaner has proved to be most satisfactory. However, the ultrasonic cleaner should be loaded with a suitable number of sieves at a time, depending on its tank capacity and/or manufacturers' recommendation. The sieves are first soaked in mineral turpentine for about 25 min in the ultrasonic cleaning tank, followed by another 25 min in Teepol solution (a detergent of about 0.5% strength by volume) and finally soaked and rinsed in a basin of clean water. The sieves are then dried in an oven set at about 100C. Using this cleaning technique, the average life of the sieve is about fifty determinations. The use of jets of water for cleaning should be avoided as this operation damages the gauze which then lasts for only about twenty to twenty-five determinations. The sieves are checked prior to use for damage using a slide projector (to throw an image of the gauze on a screen). If noticeable distortion or damage of the gauze has occurred, it should be discarded and replaced by a new gauze.
4.7.6
Flasks after washing are dried in the drying cabinet until they are completely dried. Water and turpentine do not mix, so the presence of water in the flask renders filtration difficult. Sticky rubber particles (containing dirt) present in the water phase do not dissolve and may stick to the base of the flask. Flask must be carefully inspected after each drying. The use of a cracked or otherwise damaged flask is dangerous and may lead to explosion or fire. The mineral turpentine and rubber peptising agent should be free from dirt and water contamination and should be filtered through a filter paper.
4.7.7
4.7.8
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30-16mm < t > 952mm | _ t i 1428mm 4-76mm | - j 2778 mm < t > - 0 2 5 mm U-
-39 68 mm <t> -31 75 mm <)>

3175mm I
*|
7 1 4 mm
Side view
Side view
- 2 9 - 3 6 mm 0
-r -50-8mm
25-4mm - ->i
27-78mm <|>-025mm Section A - A
Figure 1. Sieve for dirt determination (325 mesh).
Figure 3.Details of inspection holder for sieves.
9525mm 14-28mnH 1-I9mm 9-5 2mm

476mm 1428mm -H 4-76mm! ,->i9-52mm
Braze on outside 27-78mm4>

3
27-78mm4> 2778mm<H -0 25mm . 0 2 5 m m
mm $ 0 2 5 mm
9-52 mm 0 / D brass tube

4 76mm
Mesh.-^ Sieve Sieve holder
Figure 2. Details of sieve and holder for dirt
determination.
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B.5 5.1
DETERMINATION OF VOLATILE MATTER Explanatory Notes This test is primarily intended for the determination of moisture in raw NR but the result includes the amount of any other material in the rubber which is volatile at 100C. The volatile matter limit is a safeguard against excessive moisture content and against possible contamination of the rubber by solvents. 5.2 Apparatus and Materials (a) Laboratory mill (150 x 300 mm or 6 X 12 in)
(b) Polythene bags (rectangular, approximately 200 x 100 x 0.06 mm) (c) Analytical balance weighing to 0.1 mg
(d) Aluminium trays each approximately 250 x 200 mm (10 X 8 in) with perforations and vertical projection for stacking (see Figure 4). (e) (f) Clips to seal bags Drying oven with temperature control to within 3 C at 100C
5.3
Procedure Cut about 30 g of the homogenised rubber piece and wrap it airtight in a polythene bag. This is then cooled for approximately half an hour in the airconditioned balance room. Remove the 30 g portion from the polythene bag, cut a test portion in one piece weighing approximately 10 g to 11 g. Weigh immediately to the nearest
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0.1 mg. Pass the test portion once through a cold laboratory mill with a nip setting at 0.5 + 0.05 mm at even roll speed. Ensure returning to the test portion any pieces which may fall off. Place six such test portions on one aluminium tray. Stack the trays one above the other and place them in the oven at 100C + 3C for 4 + 0 . 1 / - 0 . 0 h. At the end of the drying period, open the oven door, remove a tray and close the oven door immediately. Insert each test portion in a polythene bag, the open top end of which is folded lengthwise at least three times and breadthwise once after which it is clipped and hung on the rack. This procedure is repeated, the trays being taken out one at a time until all the test portions are individually bagged (time required is about 20 min for seventy test portions). Allow the test portions to cool for about half an hour in an airconditioned room. Thereafter, remove each test portion from the bag and weigh to the nearest 0.1 mg. 5.4 Calculation The volatile matter is calculated as follows:
Volatile matter (%) = ^r-
x 100
where A is the weight of test portion before drying; B is the weight of test portion after drying.
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5.5 5.5.1
Notes The RRIM homogenising method (using rolls at room temperature) gives rise to little loss of volatile matter during homogenisation of the piece. When the ISO/BSI/ASTM homogenisation procedure (involving blending the rubber on rolls heated to 70C) is used, the loss of blending is an important fraction of the total volatile matter and must be determined. In Malaysia, the blending loss is only important for volatile matter levels near 1 %. Only in the case requiring the determination of blending loss, the test portion is weighed before and after blending; the percentage volatile matter loss during blending is given as: Weight loss on blending Weight of piece ^
5.5.2
In this case, a top-pan balance of 1000 g capacity is used. 5.5.3 The total volatile matter is then obtained with sufficient accuracy as the sum of the two volatile matter percentages.
Flat head rivet
~c .
2
,
2
3175mm cj> ((*"<(
? J T ... ,
4 m m
127mm
aluminium perforated plate
1-587mm c t > holes C/ie" drill) 257-2,
L4
18SWG aluminium sheet
^ I h U 181mm ?064rrm Secfion X-X
>'' : \
Perforated aluminium plate 2 0 SWG 3-175mmcRS x 1-587 mm < J > hole (i/a'cRs x Vie"d> hole) 11 mm Exploded: Isometric view
Figure 4. Details of tray used for volatile matter
determination.
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B.6 6.1 Explanatory Notes
DETERMINATION OF ASH
The ash from NR contains in varying proportions the oxides, carbonates and phosphates of potassium, magnesium, calcium, sodium and other trace elements. The ash may also contain silica or silicates arising either from the rubber or from extraneous foreign matter to an extent depending on the history of the material. The specified ash content represents a minimal figure for the amount of mineral matter present in the rubber. The method of determination involves wrapping the test portion in filter paper and incinerating in a muffle furnace at about 550C. 6.2 Apparatus and Materials (a) (b) (c) (d) (e) 6.3 Crucible, of nominal capacity 50 ml Muffle furnace, with pyrometer and thermostatic control Ashless filter paper of 15 cm diameter Vacuum desiccator of 20 cm or 25 cm diameter Tong for handling crucibles
Procedure Weigh, to the nearest 0.1 mg, a 5 g to 10 g portion of the homogenised rubber. Wrap in ashless filter paper and place in a crucible which has been previously ignited and weighed. Introduce the crucible into a muffle furnace controlled at a temperature of 550C + 20C until free from carbon (approximately 2 h to 4 h). When ashing is complete, allow the crucible to cool in a desiccator and then weigh to the nearest 0.1 mg.
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6.4
Calculation Calculate as follows: Ash (%) =

A
f j
100
where ,4 B C D
is is is is
the the the the
weight weight weight weight
of of of of
crucible plus ash; empty crucible; ash from filter paper; sample taken.
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B.7 7.1
DETERMINATION O F N I T R O G E N Explanatory Notes Nitrogen occurs in raw rubber chiefly as protein and it can be used to provide an indication of the protein content. Although the proportion of nitrogen varies in different types of proteins, the formula, protein = 6.25 x nitrogen, is generally accepted, but should not be regarded as a precise indication of the protein content. Skim rubber contains notably high amounts of nitrogen. 7.2 Principles of Method Nitrogen is determined by a semi-Kjeldahl procedure. The rubber is oxidised by heating with a catalyst and concentrated sulphuric acid, thereby converting nitrogen compounds into ammonium hydrogen sulphate from which, after making the solution alkaline, the ammonia is removed by steam distillation. The liberated ammonia is absorbed in boric acid solution and titrated with standard acid. 7.3 Apparatus and Reagents Apparatus (a) Micro-Kjeldhal digestion and distillation unit (b) Kjeldahl digestion flask, 30 ml (c) Burette, graduated in 0.1 ml. A burette with a storage reservoir and automatic zero is preferable. (d) Stopwatch, accurate to 1/10 s (e) Racks for Kjeldahl flasks
7.3.1
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(f) Standard flask (g) Reagent dispensers, 10 ml (h) Reagent bottles (i) (j) 7.3.2 Spatula Bulb pipette and pipettes with safety control
Reagents All reagents shall be of recognised analytical reagent quality, and distilled water or water of equivalent purity shall be used wherever water is specified. (a) Catalyst. Prepare a finely divided, intimate mixture of anhydrous potassium sulphate, copper sulphate pentahydrate, and selenium powder in the ratio of 15:2:1, respectively, by weight. (b) Concentrated sulphuric acid, of specific gravity 1.84 (c) Sodium hydroxide solution, about 67% w/v (d) Boric acid solution, about 2% w/v. Dissolve 40 g of boric acid in distilled water, warming if necessary, and make up the volume to 2 litres. (e) Indicator solution, about 0.15% w/v. Dissolve about 0.1 g of methyl red and about 0.05 g of methylene blue in 100 ml of ethanol. (f) Standard sulphuric acid, N/100, standardised against sodium carbonate.
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7.4 7.4.1
Procedure Determination Weigh accurately about 0.1 g of the homogenised rubber into the micro Kjeldahl flask and add about 0.65 g of the catalyst and about 2.5 ml of concentrated sulphuric acid. Boil gently until the digest becomes clear green in colour or almost colourless with no yellow tint after cooling. Normally, the digestion requires about 1 h. Cool the digest and dilute with about 10 ml water. Pass steam to the distillation apparatus. Then pour in the digested solution. Transfer with two or three portions (approximately 2 ml or 3 ml) of water to the distillation apparatus which has been previously cleaned. Add about 10 ml of the NaOH solution to the distillation vessel, washing down with some water. Stopper the vessel with the glass peg. Add about 10 ml of boric acid solution and two or three drops of screened methyl red indicator to the 100 ml receiving conical flask. Place the receiver so that the end of the condenser dips below the surface of the acid solution. Clip the tubing connecting to the vessel. Start a 5 min timing when the boric acid turns green. Lower the receiver until the condenser tip is well above the solution and continue distilling for a further minute. Wash the end of the condenser with distilled water. Titrate the distillate with N/100 sulphuric acid. The colour changes from green to a light violet at the end-point.
7.4.2
Blank Conduct a blank determination, using all the reagents but omitting the sample.
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7.5 Calculation Calculate as follows: (V, Nitrogen (%) = V ) N x 0.0140 x 100

2 w
where V is the volume of H S 0 required for titration of the contents of the receiving flask; V is the volume of H S 0 required for titration of the blank; N is the normality of the H S 0 ; W is the weight of sample taken in grammes.
x 2 4 2 2 4 2 4
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B.8
DETERMINATION OF RAPID PLASTICITY AND PLASTICITY RETENTION INDEX 8.1 Explanatory Notes Rapid Plasticity A disc-shaped test pellet shall be rapidly compressed between small parallel platens to a fixed thickness of 1 mm and held thus for 15 s to reach approximate temperature equilibrium with the platens. It shall then be subjected to a constant compressive force of 10 0.1 kgf for 15 s; its thickness at the end of this period in 0.01 mm units shall be taken as the measure of plasticity.
8.1.1
8.1.2
Plasticity Retention Index The plasticity retention index (PRI) is a measure of the resistance of raw NR to oxidation. A high value of the index denotes high resistance to oxidation. The oxidation behaviour of raw NR may have an important bearing on processing behaviour and end product performance and the PRI test accordingly affords a convenient means of characterising rubber in certain of these respects. The test involves measurements of the plasticity of NR testpieces before and after heating in an air oven for 30 + 0.25 min at 140C 0.5C using the parallel plate plastimeter with a platen 10 mm in diameter. The PRI is the percentage ratio of the plasticities after and before heating. The time and temperature of heating are such as to give adequate discrimination between rubbers and a reasonable speed of testing at a temperature similar to that attained in factory internal mixers. The value of the index is, however, virtually independent of the initial plasticity of the rubber. It is not independent of the test method. A different value will be obtained if, for example, the time or temperature of heating is altered or if a different type of plastimeter is used.
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8.2
Equipment and Materials (a) Parallel plate plastimeter: This is a standard equipment with a 10 mm platen and a process timer giving 15 s of pre-heating time. (b) Punch, for the preparation of test pellets of approximately constant volume quickly and without difficulty. The punch shall compress a portion of the material to approximately 3 mm in thickness and shall cut out a disc approximately 13 mm in diameter. (c) Thickness gauge: The gauge shall have a scale graduated in unit divisions of 0.01 mm. (d) Lightweight aluminium tray, suitably marked for pellet identification. (e) Oven, operating at 140C 0.5C. The oven shall be such that: (i) (ii) (iii) The temperature fluctuation over a 30 min period is + 0.5C. The temperature variation within the ageing region is + 0.5C. It is an oven suitably designed for the testing of PRI.
8.3
(f) Approved cigarette paper, of about 0.03 mm thickness as authorised by RRIM. Calibration of Plastimeter The setting of the plastimeter shall be checked against the maker's instructions and calibration carried out according to manufacturer's
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recommendation. In SMR testing, plastimeters in all authorised laboratories are calibrated at approximately half-yearly intervals. 8.4 8.4.1 Procedure Preparation of Test Pellet Pass a test portion of 20 + 5 g twice through the rolls of a cool mill with nip setting adjusted such that the final sheet thickness is 1.6 mm to 1.8 mm. The sheeted rubber piece is doubled after the first and final passes (see Figure 5). If the sheet so obtained after two passes does not meet the thickness requirements, reject it and take a fresh test portion of the homogenised piece and repeat the operation by readjusting the nip setting. The final sheet which should be free from holes is immediately doubled and the two halves pressed lightly together by hand. Cut six test pellets from the doubled sheet with the punch as illustrated in Figure 5. The test pellets should be a disc of rubber of thickness between 3.2 mm to 3.6 mm and approximately 13 mm in diameter. The test pellets are divided into two sets of three, one set each for plasticity determination before and after oven ageing.
The gauge steam pressure shall indicate 1 / 2 - 1 psi with free-flowing steam at the discharge end. Compress a disc-shaped test pellet, sandwiched between two pieces of cigarette paper each of approximate dimensions 40 x 35 mm, between the two parallel platens to a fixed thickness of 1.00 + 0.01 mm and hold it in the compressed state for 15 + Is to reach approximate equilibrium. Then apply a constant compressive force of 10 + O.lkgf for 15 + 0.2s. The thickness at the end of this period (in 0.01 units) is taken as the measure of rapid plasticity.
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8.4.3
Determination of PRI Ensure that the oven is not overloaded, e.g. with an excessive number of dishes or a thick plate which has a large thermal capacity; this could cause a prolonged temperature drop and might upset temperature uniformity. Care should be taken that the test pellets are arranged within the temperature calibrated region of the oven. Before heating begins, check the oven temperature to ensure that it has been stable for at least 5 min. Quickly insert the tray with the dishes and test pellets, close the oven door, and start timing. It is necessary to ensure that the correct temperature is quickly regained and retained. After 30 + 0.25 min, remove the tray with the dishes and test pellets from the oven and allow to cool to room temperature. Measure the plasticity of the aged pellets, according to the procedure described in 8.4.2 at least 30 min and preferably 1 h after ageing of the test pellets. The procedures described in 8.4.2 and 8.4.3 shall preferably be made concurrently.
8.5 8.5.1
Calculation and Expression of Results Initial Rapid Plasticity Take as the rapid plasticity number, P , the median value of the thickness of the three test pellets, expressed in 0.01 mm and determined as in 8.4.2.
0
8.5.2
PRI Calculate the PRI using the median plasticity value of the three unaged test pellets (determined as in 8.4.2) and the median plasticity value of the three aged test pellets (determined as in 8.4.3), as follows:
PRI = p- x 100
"o
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where P is the plasticity number of the unaged test pellet; P is the rapid plasticity number of the test pellet after ageing at 140C for 30 min.
0 30
8.6 8.6.1
Notes Rapid checking with standard CV rubber should be carried out: (a) Immediately after loading spring calibration, to ensure that the job has been satisfactorily performed
(b) Once every morning, to ensure that the plastimeter is in good working condition. 8.6.2 The two pieces of cigarette paper used to sandwich the test pellets are obtained by cutting a piece into two equal parts. The paper should be cut and not used by folding on itself. The size, thickness and type of papers used as release medium have a noticeable effect on the test result.
Figure 5. Punched pellets for (1) initial plasticity determination, and (2) aged plasticity determination.
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B.9 9.1
DETERMINATION OF MOONEY VISCOSITY Explanatory Notes The test consists of determining the torque necessary to rotate a disc in a cylindrical chamber filled with rubber under specified conditions. A number proportional to this torque is taken as an index of the viscosity of the rubber. The Mooney viscometer (a shearing-disk viscometer) is used. 9.2 Apparatus (a) Mooney Viscometer The essential parts of the apparatus are a rotor, a hollow cylindrical die, a means for rotating the rotor, a means for indicating the torque required to rotate the rotor and controls for maintaining the die at a constant temperature (Figure 6). (b) Calibration gear and weights 9.3 Calibration and Maintenance The following system of checking and calibrating Mooney viscometer should be adopted:
9.3.1
Dead load calibration to check that zero reading for zero force and a reading of 100 for a pair of forces of 100 N should be regularly carried out following RRIM method. Dead load calibration by incremental loading to check the whole range of the meter's reading should be carried out at least once in about six months following RRIM method.
9.3.2
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9.3.3
The die cavity should be cleaned periodically according to the maker's instruction. If the viscometer is being used extensively, the frequency should be increased accordingly. Rapid checking with standard CV rubber should be carried out: (a) Immediately after dead-load calibration to ensure that the job has been satisfactorily performed
9.3.4
(b) Once every morning to ensure that the viscometer is in good working condition. Should it be found to be faulty, it must be rectified by procedures outlined in 9.3.1 followed by 9.3.4(a). 9.4 Procedure Determination of Mooney Viscosity The temperature of test should be 100C 1C. Check the die temperature for stability. Place the rotor in the die cavity to heat up to test temperature; 2 min are normally sufficient to heat the rotor from ambient temperature. Remove the hot rotor from the die cavity. Before this, divide about 25 g of the homogenised rubber into two equal portions. Place the preheated rotor stem through the centre of one portion. Put this whole combination in the lower die cavity and place the second portion on top of the rotor. Close the die immediately. Measure the time from the instant the die is closed, as indicated by the appropriate lamp on the control panel. Start the motor 1 min after closing the die cavity. Record the initial dial gauge reading immediately. Take as the viscosity of the rubber the dial reading at the end of the fourth minute from the instant when the motor is started.
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9.5
Expression of Results A typical test on NR with the normal rotor speed with viscosity number 60 should be reported as follows: 60 ML (1+4) 100C where 60 is the Mooney viscosity; M stands for Mooney viscosity; L indicates the use of a large rotor; 1 is the pre-heating time in min; 4 is the reading time in min; 100C is the test temperature.
9.6 9.6.1
Notes The test portions shall be allowed to rest at room temperature for at least 1 h before carrying out the Mooney viscosity test. To facilitate removal of the rubber after test when testing low viscosity or sticky materials it shall be permissible to use a pliable film (cellulose and rubber hydrochloride films are examples), approximately 0.025 mm thick, between the rubber and the metal surfaces of the die or a semi-permanent non stick polymeric coating (polytetrafluoroethylene is an example) of maximum thickness 0.013 mm applied to the surfaces of the rotor. The test temperature is defined as the steady-state temperature of the closed cavity, with rotor in place but without rubber. Since a temperature differential may exist between the platens and the die cavity, it may be necessary to adjust the platen temperatures to obtain the correct cavity temperature. In making such adjustments it is important that the temperatures of the two platens be within 0.5C of each other.
9.6.2
9.6.3
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Figure 6. Mooney
viscometer.
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B. 10 10.1
DETERMINATION OF COLOUR Explanatory Notes The colour of the raw rubber is compared and matched as closely as possible with that of standard colour slides. The raw rubber is tested in the form of a moulded disc of standard thickness. Colour matching is carried out under diffuse daylight illumination against a matt white background, preferably by use of a comparator which holds the test pellets and comparison slide in convenient juxtaposition. The standard coloured glasses used are calibrated in colour index units according to the intensity of their colour. The numerically higher index values have deeper colour. The basis of calibration is the 'Lovibond colour scale' in amber units.
10.2
Apparatus (a) Laboratory mill, as described in B.2 (b) Hydraulic press. The press should be capable of exerting a pressure of not less than 500 p.s.i. on the cavity areas of the mould during the entire period of moulding. The platen temperatures shall be capable of being maintained at 150C + 3C. (c) Mould. A stainless steel or aluminium mould 1.6 + 0.05 mm thick having holes approximately 14 mm diameter. A suitable example is illustrated in Figure 7. Two mould covers of similar material and at least 1.6 mm in thickness are required.
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(d) Lovibond comparison glasses. For this purpose Lovibond comparator disc (rubber latex colours - amber units) are used. The appropriate discs are: (i) (ii) No. 4/19A 1 to 5 units of 0.5 unit interval No. 4/19B 5 to 16 units of 1.0 unit interval
These have been calibrated by the makers as a combination of red and yellow colours. (e) Lovibond comparator or other similar comparator (Figure 8) (f) Transparent polyester or cellulose film. This should be about 0.025 mm in thickness. (g) Punch, as described in B.8.2 (b) 10.3 10.3.1 Procedure Test Pellet Preparation Take a test portion of 15 5 g from the homogenised sample and pass three times between the roll mills at room temperature with the nip adjusted so that the final sheet thickness is 1.6 mm to 1.8 mm. After the initial pass, the rubber is rolled and passed endwise through the rolls. Fold the rubber from the second pass and pass it lengthwise through the rolls for the last time. This final sheet, which should be uniform in texture and free from holes, shall immediately be doubled and the two halves pressed together lightly by hand. Cut two test pellets from the doubled sheet with the punch and measure their thickness until two test pellets are obtained with thickness between 3.2 mm and 3.6 mm. The two test pellets shall then be laminated together by lightly pressing with the fingers. Pre-heat the test pellets in the mould between two sheets of polyester or cellulose film using mould covers for 1 min. Then apply
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not less than 500 p.s.i. pressure on the cavity areas of the mould, for 4 + A min at 150C 3C. The moulded test pellet shall be 1.6 + 0.2 mm thick and free of colour contaminants.
l
10.3.2
Colour Determination Determine the colour of the test pellet by matching as closely as possible with the appropriate colour standard. Colour matching shall be carried out under diffuse daylight against a matt white background, preferably by using a comparator mounting which holds the test pellets and comparison colour at a convenient distance apart (Figure 8). The cover is put on and the colour matched for each sample in turn. (Alternatives to the comparator shown in Figure 8 are available commercially.)
10.4
Notes Very occasionally the rubber cannot be matched to any colour due to strong yellow, greenish or grey colours in it. Should this occur the rubber is regarded as not of normal raw NR colour, and a note to this effect is recorded on the test result sheet. Abnormal colours can arise from contamination of the rubber or from fractionation of the latex leading to concentration of naturally occurring pigments.
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1 5 2 mm
Section through A A ( n o t to s c a l e )
Figure 7. Mould for colour index test.
Base plate h 230 Section through AA 1

T
All dimensions in millimetres Top lid
Scale:
60mm
1 1
X' 1
-Ink-
Section through BB :
C O
(
I CO
o 3
I <
00,
\
1
T
L
182
njr
M
6 0
H . p^i
6mm radius -jIOf
b , 1
J
15
4=3
Section through YY Section through Z Z
Figure 8. Comparator mounting (for use with Lovibond comparator discs).
commercial
PART C PRODUCTION CONTROL TEST METHODS USED BY RRIM AND RECOMMENDED FOR ROUTINE USE BY PRODUCERS AND LABORATORIES
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C. 1 1.1
WALLACE ACCELERATED STORAGE-HARDENING TEST (WASHT) Explanatory Notes The Wallace accelerated storage-hardening test provides an indication of the propensity of solid NR to increase its viscosity during storage as a result of the formation of crosslinks between the rubber molecules. These crosslink formations are contributed largely from some condensation reactions involving aldehyde groups naturally present in the rubber molecule and presumably, to a very smaller extent, from peroxidic groups in the rubber. This test provides a means of characterising viscosity-stabilised rubbers. 1.2 Principle of Method Wallace ASHT involves the measurement of the rapid plasticity of standard test pellets before and after a short period of storage under conditions which accelerate the storage-hardening reaction. Accelerated storage-hardening is achieved by storing standard test pellets over phosphorus pentoxide at atmospheric pressure at 60 C for 24 + 0.1 h. The resultant increase in plasticity (AP) represents the accelerated storage-hardening. 1.3 Equipment and Materials (a) Wallace rapid plastimeter. This should be equipped with a 10 mm platen [see B.8.2(a)]. (b) Punch [see B.8.2(b)] (c) Two-roll laboratory mill. The mill should have rolls nominally 150 mm diameter x 300 mm length (see B.2).
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(d) Laboratory oven. This should be such that temperature fluctuation is + 1 throughout the working space, and recovery of oven is + 1 C of the set temperature in a time not exceeding 10 min after inserting a full load of weighing bottles. (e) Thickness gauge. The gauge shall have a scale graduated in unit divisions of 0.01 mm and fitted with a flat contact of about 9 mm diameter. (f) Weighing bottles. These should preferably conform to dimensions shown in Figure 9.
(g) Test pellet platform. This should be fabricated from stainless steel wire mesh (mesh size 40) as shown in Figure 10. It is used with the weighing bottle as shown in Figure 11. (h) Tongs. Any suitable laboratory tongs may be used to handle the test pellet platforms. (i) Small spatula, resistant to phosphoric acid corrosion, for handling phosphorus pentoxide Phosphorus pentoxide P 0 . Care should be exercised in the handling and storage of this corrosive chemical. The chemical should be kept in air tight containers (avoiding plastic container) and stored in a cool dry place. Goggles and rubber gloves should be worn when handling the material.
2 5
(j)
(k) Sealant (1) Approved cigarette paper of about 0.03 mm thickness
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1.4 1.4.1
Procedure Preparation of Test Pellets A test portion of 20 + 5 g of the homogenised piece is prepared as for the PRI test (see B.8.4.1) by passing it twice through the rolls of a cool mill running with the nip setting adjusted so that the final sheet thickness is 1.6 mm to 1.8 mm. If the sheet so obtained after two passes does not meet the thickness requirements, reject it, take a fresh test portion of the homogenised bale piece and repeat the operation by readjusting the nip setting. Immediately double the sheet, which should be free from holes, and press the two halves lightly together by hand. Cut six test pellets from the doubled sheet with the punch. The thickness of the test pellets should be 3.2 mm to 3.6 mm. These are then divided into two sets of three, one set each for plasticity tests before and after accelerated storage-hardening. Test pellets numbered (1) and (2) are taken for plasticity tests before and after storage-hardening respectively.
1.4.2
Storage of Test Pellets The weighing bottle and test pellets shall be clean and dry. The weighing bottle with test pellets ready for storage shall be as shown in Figure 11. It is important that the conditions specified, e.g. height of test pellet platform, quantity of P 0 (6 g to 8 g) are strictly adhered to if good test reproducibility is to be obtained. The test pellets shall be equally spaced on the platform with no two test pellets in contact with one another.
2 5
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1.4.3
Temperature and Duration of Storage Test pellets shall be storage-hardened at 60C 1C for 24 0.1 h. After about 30 min in the oven the bottles shall be checked for airtightness of the lids and the timing of the test started.
1.4.4
Measurement of Plasticity Non-storage-hardened test pellets shall be kept apart and the plasticities of these tested concurrently with the storage-hardened test pellets. The rapid plasticity measurements shall be carried out as in B.8.4.2
1.5
Expression of Results The accelerated storage hardening in terms of plasticity shall be expressed as: where AP = P P P is the median plasticity value of three storage-hardened test pellets; P is the median plasticity value of three non-storaged hardened test pellets; AP is the difference in plasticity units between P and P .
H 0 H 0 H 0
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5 4 mm
H Grease sealant Test pieces
49mm'
Platform Phosphorus pentoxide (weight 6 - 8 g )
46mm -
Figure 9. Weighing bottle (Quickfit WB 50L/50B).
Figure 11. Weighing bottle with test-pieces ready for storagehardening.
Figure 10. Testpiece platform (stainless steel gauze, 40 mesh).
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C .2 2.1
MOONEY ACCELERATED STORAGE-HARDENING TEST (MASHT) Explanatory Notes Mooney ASHT provides an indicator of the propensity of solid NR to increase its viscosity during storage as a result of the formation of crosslinks between the rubber molecules. These crosslink formations are contributed largely from some condensation reactions involving aldehyde groups naturally present in the rubber molecule and presumably, to a very smaller extent, from peroxidic groups in the rubber. This test provides a means of characterising viscosity-stabilised rubbers. 2.2 Principle of Method Mooney ASHT involves the measurement of the Mooney viscosity of rubber test portions before and after a certain period of storage under conditions which accelerate the storage-hardening reaction. In this test, accelerated storage-hardening is achieved by storing rubber test portions over phosphorus pentoxide in a vacuum at 60 C + 1C for 48 + 0.1 h. The resultant increase in viscosity (AV) represents the accelerated storagehardening. 2.3 Equipment and Materials (a) Mooney viscometer {see B.9.2) (b) Laboratory oven. A general purpose type with fan large enough to accommodate one or more vacuum desiccator of BLWA pattern. It should be such that temperature fluctuation is 1 C throughout the working space.
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(c) High vacuum pump (d) Desiccator BLWA pattern, designed for vacuum use with cover, collar stopcock, plate and glass container (e) Thermometer 0C (f) Thermostatted flask 110C
(g) All glass water trap unit as shown in Figure 12 (h) Spirit, industrial methylated (i) Phosphorus pentoxide (phosphoric oxide), laboratory reagent grade. This chemical should be stored in a cool dry place. (j) High vacuum grease
(k) Dry ice or ice saturated with common salt (sodium chloride) (1) 2.4 Spatula, resistant to phosphorus pentoxide corrosion
Procedure A test portion weighing about 25 g of the homogenised piece is prepared as for the Mooney viscosity test (see B.9.4.1). The test portion should not be folded. Ensure that the desiccator is clean and dry. Transfer approximately 180 g of P 0 into the glass container. Place the test portions (twelve to fifteen pieces per desiccator) on the porcelain plate. Apply grease to the cover and stopcock. Check to ensure that grease does not block the entry of air into the desiccator. Pour methylated spirit into the thermos flask and add dry ice which has been split into small bits (see Figure 12). Stop the addition of dry ice after the spirit is saturated with it. This mixture will sufficiently cool the air which is drawn through the glass tubing so that no moisture will enter the vacuum pump to render it ineffective.
2 5
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Attach one end of a vacuum-type rubber tube to the stopcock of the desiccator and fit the other end with a glass rod which fits a 14/23 joint of the vacuum apparatus. Start the pump and leave it to run for about 1 h. Then close the stopcock. Remove the rubber tube. Place the desiccator in an oven at 60C 1C for 48 0.1 h. Remove the desiccator from the oven. Slowly open the stopcock of the desiccator to allow the entry of air. Take out the hardened test portions from the desiccator and leave them to cool in the open on a plate. Test the hardened rubber portions for Mooney viscosity as in B.9.4.1 after at least 4 h but not exceeding 24 h of cooling. 2.5 Expression of Results The accelerated storage hardening in terms of Mooney viscosity shall be expressed as: AV = V H H
where V is the Mooney viscosity of the hardened test portion; V is the Mooney viscosity of the non-storage-hardened test portion; AV is the difference in Mooney units between V and V .
0 H 0
2.6 2.6.1
Notes In the event of a power failure for less than half an hour in the course of ageing the test portions in the oven for 48 0.1 h and such failure not occurring within the first 10 h of ageing, the test shall proceed and the test results shall be accepted and used as such. In any other cases, the test shall be repeated. In the event of a failure to obtain dry ice, a good substitute for dry ice is ice saturated with common salt.
2.6.2
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B 19/26 stopper 4 120mm 300mm Socket for B 19/26 stopper B 29/32 socket (to supply 2 pieces) 20mm glass tubing Stopcock 14/23 socket 14/23 cone 14/23 socket
8mnri0 8mm0
Vacuum pump
glass tubing
glass tubing
8mm<2>
Dry ice/spirit mixture glass 40mm a/330mm Inner vessel Thermos tatted flask tubing
1
Desiccator Figure 12. All-glass water trap unit for MASHT.
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C .3
MEASUREMENT OF CURING CHARACTERISTICS WITH THE OSCILLATING DISC RHEOMETER 3.1 Explanatory Notes This method is used for determining the curing characteristics of vulcanisable compounds of NR. The advantages of this method are: (a) A continuous measurement of the cure behaviour of the rubber is possible. (b) The separate stage of curing the test mix is eliminated; thus the procedure is to mix on day one and test on day two. (c) There is no need for a Mooney viscometer to determine the compound viscosity of the rubber as required in the relaxed modulus method. (d) End-users of NR are generally more familiar with this method of cure measurement.
3.1.1
3.1.2
This test method is essentially that of ISO 1658 (gum recipe) and ISO 3417 (oscillating disc curemeter), but differs in detail in that the test procedure prescribed herein is based exclusively on a masterbatch technique, and a specific instrument is recommended for cure measurement. Principle of Method In this test, a specimen of rubber prepared on a formulation according to 3.3 is contained in a sealed die cavity under a positive pressure and maintained at an elevated temperature. A biconical disc is embedded in the test specimen and is oscillated through a small arc. This action exerts a shear strain on the test specimen and the force (torque) required to oscillate the disc is proportional to the stiffness modulus of the rubber. The torque is recorded autographically as a function of time.
3.2 3.2.1
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3.2.2
The stiffness of the rubber specimen increases as vulcanisation proceeds (see Figure 13). A complete curve (rheometric trace) is obtained when the recorder torque either rises to an equilibrium value or to a maximum value (see Figure 14). The time required to obtain a vulcanisation curve is a function of the test temperature and the cure behaviour of the rubber compound. The following measurements may be taken from the rheometric trace (see also Figure 14): (a) Minimum torque (Tj) (b) Maximum, equilibrium or highest torque Delta torque = (b) - (a) (c) Scorch time or time of incipient cure t ; this is taken as period from close of die cavity to time when torque has risen by 2 in.lb. above minimum torque.
2
3.2.3
(T^T^/T^
(d) Optimum cure time ? ; this is taken as period from close of die cavity to
90
time when torque has risen to: T +^

L
(T /T /T
m HF
T)
L
TH
T?\ (T /T /T
HR HF
Tj)
The minimum torque is proportional to the stiffness or low shear rate viscosity of the uncured compound. The time of incipient cure is a measure of processing safety. The time to optimum cure is measured as
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some percentage [see 3.2.3(d)] of the highest torque. The highest torque is a measure of shear modulus or stiffness of the fully vulcanised specimen at the test temperature. Note 1. All torque values are expressed in in.lb and cure times in minutes. 1 in.lb is approximately equal to 0.113 mN.
3.3 3.3.1
Test Formulation The test mix used shall consist of the following compound ingredients in the proportions, by weight: NR Zinc oxide (370) Stearic acid (372) Sulphur (371) MBT* (383) Mercaptobenzthiazole Note 2, This test formulation is commonly known as the ACS 1 recipe. All compounding ingredients are of National Bureau of Standards (NBS) quality or its equivalent. The codes within brackets indicate NBS standard sample number. 100.0 6.0 0.5 3.5 0.5 + + + + 1 0.1 0.1 0.1 0.1
3.3.2
Storage of Compounding Ingredients It is essential that only standard compounding ingredients or recognised alternatives be used if reliable and reproducible results are to be obtained. Compounding ingredients are stored in the dark (in bins) under cool, dry conditions. This is important because test results are dependent on the moisture content of the unvulcanised stock.
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3.3.3
Use of Masterbatches For convenience and greater accuracy, the compounding ingredients are incorporated into the rubber as (a) MBT and (b) sulphur masterbatches. The rubber for the masterbatches shall preferably be of similar quality to that being tested, and of average characteristics i.e. medium cure characteristic. The proportions, by weight, of the compounding ingredients used are as follows: Ingredient (Parts bv weight) Masterbatch MBT Sulphur
Rubber* Zinc oxide Stearic acid MBT Sulphur Total
100 120 10 20
1 1 0.1 0.1
100 120 10
+ + + +
1 1 0.1 1
140 370
250
*Note 3.
SMR L, SMR CV or SMR GP respectively may be used as far as possible for the three groups of rubber (SMR L, SMR CV and SMR CV 50 or SMR GP, SMR 10CV and SMR 20CV).
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The test mix is then made up as follows: Test rubber** MBT masterbatch Sulphur masterbatch Total Note 4. 95.00 g 1 g 6.25 g 0.05 g 9.25 g + 0.05 g 110.50 g A composite testpiece obtained by TC blending of six approximate equiportions taken from six respective testpieces of a lot sample. Laboratories are advised to crosscheck their masterbatches with RRIM from time to time.
Note 5.
3.4 3.4.1
C ompounding Compounding of masterbatches and test mixes is done on a 150 x 300 mm laboratory mill with friction ratio between the rolls of approximately 1:1.4 + 0 . 1 , with the back roll rotating at 31 rev/min. The mill shall be equipped with adjustable stock retaining guides. Means shall be provided for controlling the mill rolls temperature to 70C + 5C. The roll surface temperature may be checked with a suitable pyrometer. Masterbatches Masterbatches shall be prepared in the proportions as shown in 3.3.3. Keep the rolls of the laboratory mill cool with running water. Set the guide plates about 150 mm apart and pass the rubber through zero nip once. Set the nip at 0.6 + 0.06 mm and put in the rubber until a smooth band is obtained, the powders are to be added slowly and the nip gradually widened so as to maintain a rolling band. When about 80% of the powders have been incorporated (roll nip approximately 1.0 mm), cut the band once on each side. Incorporate the rest of the powders. When no free powder is evident on the band or on the milling surface, cut the band once on each side till dispersion
3.4.2
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appears fully uniform. Whenever cuts are made, the band shall be cut 3/4 of the distance across the roll and the knife held in this position until the band just disappears. Successive 3/4 cuts shall be made from alternate directions. Cut off the stock, set the nip tight (zero) and grind the stock three times through the rolls, rolling the rubber into a sphere between each pass. Sheet out the masterbatch at a nip setting of 1.42 + 0.14 mm. 3.4.3 The test mix based on 95 g of the rubber under test (which shall be composed of equal amounts taken from six remnant blended pieces representing bale samples taken from a production lot) shall be prepared in the proportions shown in 3.3.1. The full width of the rolls shall be used and the roll temperature shall be 70C + / - 5C. The treatments, in sequence, are:
Treatment Rubber in to form a band MBT and S masterbatches in Six cuts on each side Cut off and roll up once presenting end-wise Sheet out
Gap (mm) 0.76 -
Time O'OO" 0'20" l'OO" - 2'35"
2'35" - 3'00" 1.42 3'00"
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3.5 3.5.1
Storage of Masterbatches and Test Mixes Masterbatches prepared as in 3.4.2 shall be stored in air-tight containers in a dry atmosphere at ambient temperature or preferably a t 2 3 C + / - 2C. The storage period shall preferably not exceed three months. Storage in airconditioned room would be considered adequate. The compounded stock shall be stored overnight in the dark in a dry atmosphere at room temperature or preferably at 23C + / - 2C for a period not less than 16 h and not exceeding 96 h. Storage in air-conditioned room would be considered adequate. Apparatus The rheometer has a biconical disc oscillating in a temperature-controlled die cavity. The shaft of the disc is secured in a drive shaft and oscillated through a small arc. The torque applied to the disc represents the resistance of the rubber specimen to deformation and is recorded autographically to yield a curve of torque versus time. The die assembly of the rheometer is shown in Figure 15. Note 6. The Monsanto Rheometer R100 Model complies with the instrument characteristics described in this test method. Equivalent equipment may be recommended by RRIM from time to time.
3.5.2
3.6 3.6.1
3.6.2
Temperature Measurement (a) The temperature-measuring system shall enable the temperature of the dies to be determined within + / - 0.1 C. Calibrated thermocouples, or other suitable temperature sensors inserted in the dies, shall be used for periodically checking the die temperature. (b) The dies shall be mounted in electrically-heated (aluminium) platens. Temperature controllers shall be used for controlling the temperature of each platen within + / - 0.3C at steady state.
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3.6.3
Die Cavity (a) The dies shall be fabricated from a non-deforming tool steel having a minimum Rockwell hardness of HRC 50. The geometry of the standard dies is shown in Figures 16 and 17. The dimensions of the dies are given in Tables 1 and 2. Holes shall be drilled in both the upper and lower die members to enable temperature sensors to be inserted. Surfaces of the die cavity shall contain rectangular-shaped grooves located at 20C intervals to minimise slippage. The lower die dimensions are given in Table I. The upper die member shall contain identically-shaped grooves. The dimensions of the upper die are given in Table 2. (b) The lower die shall have a hole in the centre to allow for insertion of the disc stem. A suitable seal shall be provided in this hole to prevent materials from leaking from the cavity.
3.6.4
Disc The biconical disc shall be fabricated from a non-deforming tool steel having a minimum Rockwell hardness of HRC 50. The disc is shown in Figure 18 and the critical dimensions given in Table 3.
3.6.5
Rotor Oscillation The frequency of the rotary oscillation of the disc shall be constant at 100 cycles/min. The arc of the rotor oscillation shall be adjusted at 3.00 + 0.02C about its centre position.
3.6.6
Die Closure The dies shall be closed and held closed during the test by a pneumatic cylinder with a force of 11.0 + 0.5 kN. (An air pressure supply which can deliver approximately 60 p.s.i. to the rheometer would be suitable. Where a long air-line is necessary, a suitable water-trap would be required.)
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3.6.7
Torque Measurements A transducer which produces a signal that is directly proportional to the torque required to turn the disc shall be used to measure the torque on the disc.
3.6.8
A recorder shall be used to record the signal from the torque transducer. The recorder shall have a speed of response for full-scale deflection on the torque scale of 1 s or less. The torque shall be recorded with an accuracy of + / - 0.5% of the torque range. Three torque ranges from 0 - 25, 50 and 100 in.lb. (or 0 2.5, 5 and 10 mN) shall be provided. It is found that a torque range of 50 in.lb. is usually adequate. Calibration of Torque Transducer and Recorder Provisions shall be made for a mechanical torque standard for calibrating the sensitivity of the recorder, the proper functioning of the recorder, stress transducer and entire oscillating system. The rheometer shall be calibrated in accordance with the manufacturer's instructions.
3.6.9
3.7
Test Specimen Preparation of Test Specimen (a) The ACS 1 mix is sheeted out at a roll nip of 1.4 + 0.14 mm and folded onto itself. The folded piece shall give a thickness of approximately 10 mm. (b) The test specimen shall be cut from the sheeted sample, which shall be as free from air as far as practicable. The dimensions of the test specimen shall measure approximately 35 X 35 X 10 mm (depth) and weigh 6 + 0 . 2 / - 0 . 0 g. This size and weight are considered suitable for use with a micro-die system (Figures 16 and 17).
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(c)
Proper specimen size is assured if a small amount of material is extruded between all edges of the dies. Oversized specimens cool the cavity excessively during the early part of the test cycle.
3.8 3.8.1
Test Temperature Recommended test temperature is 160C. Tolerance at this temperature shall be + / - 0.3C. Procedure Preparation of Test Bring the temperature of both die members to the test temperature with the disc in place and the die cavity in the closed position. With the disc in place and the dies closed, adjust the recorder pen to zero torque line on the chart. Position the pen to the zero time if needed (see 3.6.9) and select the correct torque range (see 3.6.8).
3.9 3.9.1
3.9.2
Loading the Curemeter (a) Open the dies, place the specimen on top of the disc, clamp the disc and close the dies immediately. Note 7. When testing tacky rubbers or rubber without curing agents, insert some suitable thin film material (e.g. Melinex polyester film Type S Gauge 100) below and above the specimen to keep the rubber from sticking to the dies.
(b) Time shall be counted from the instant the dies are closed.
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3.9.3
To ensure reproducibility, the following schedule should be closely maintained: Step 1 (a) Allow time for temperature in die cavity to stabilise at test temperature (160C + / - 0.3C) Recorder pen in OFF position Open die cavity Insert rotor disc; clamp rotor disc Close die cavity to preheat die cavity and rotor disc while changing graph paper Step 3 (a) (b) Open die cavity MOTOR switch on and wait for recorder pen to register zero torque (c) (d) (e) Step 4 (a) Recorder pen in REMOTE position Place the compound testportion on top of the rotor Close dies After completion of recording run, recorder pen in OFF position, switch off MOTOR Unclamp rotor disc Open die cavity
(b) Step 2 (a) (b) (c)
(b) (c) (d)
Remove rotor disc together with testportion (cleanse rotor disc if necessary) Repeat cycle from STEP 2 for next test. Note 8. In the more recent version of the Rheometer, clamping and unclamping of rotor disc is done automatically.
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3.10
Reporting of Test Results (a) A rheograph together with information on test conditions (temperature, arc, torque range and recipe) shall be attached to the SMR certificate. (b) The following cure data are reported besides the rheograph (see 3.2.3): Delta torque (maximum minimum torque) (in. lb) Scorch time t (min)
2
Optimum cure time t^, (min)
3.10.1
Conditions of testing shall also be as follows: (a) Arc used; reported as half of total arc i.e. 3 for a total arc swing of 6 . (b) Temperature of test 160C + 0.3C (c) Range selected (preferably 50 in. lb)
(d) Frequency of oscillation, 100 cycles/min (e) Chart time shall normally be about 12 min (longer if necessary to ensure that T /T /T
HF HR H
is attained).
(f)
Nature of compound recipe, ACS 1 formulation
(g) Die cavity with rotor disc between successive testing to be closed.
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3.11
Precision and Repeatibility The precision and repeatibility of the rheometric test is a function of the rubber under test, preparation of the mix, test temperature, cure parameters and overall care in carrying out the test. An indication is given below in terms of the percentage uncertainty of variation of each of the cure parameters for SMR, compounded to and ACS 1 formulation and tested at 160C + 0.3C, 3 arc and 100 cycles/min: Within lab (%) Delta Torque 2.9 U 8.1 tgo 5.0 Between lab (%) Delta Torque 6.0 t
2
90
19.8
10.7
Note:Values at 95% confidence level
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TABLE 1. LOWER DIE DIMENSIONS
Code
Dimension (mm)
Tolerance (mm)
Dimension (in)
Tolerance (in)
A B C D E F
55.88 10.64 7.94 18.26 1.57 0.79
0.13 0.25 0.13 0.13 0.13 0.13
2.200 0.419 0.314 0.719 0.062 0.31
0.005 0.008 0.005 0.005 0.005 0.005
TABLE 2. UPPER DIE DIMENSIONS
Code
Dimension (mm)
Tolerance (mm)
Dimension (in)
Tolerance (in)
G H I J K L M N 0 P
Q
R
4.76 24.07 12.70 2.38 54.61 41.91 5.35 1.65 4.57 15.37 5.08 41.91
0.13 0.06 0.40 0.40 0.05 0.03 0.01 0.03 0.13 0.03 0.05 0.03
0.187 0.948 0.500 0.094 2.150 1.650 0.2106 0.065 0.180 0.605 0.200 1.650
0.005 0.002 0.015 0.015 0.002 0.001 0.0004 0.001 0.005 0.001 0.002 0.001
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TABLE 3. DISC DIMENSIONS
Code
Dimension (mm)
Tolerance (mm)
s
T V
a
Diameter Radius Groove width Groove depth Groove lengths
35.55 0.80 0.80 0.8 7.5 min. 12.5 min. 0.80 0.8 7.5 min. 9.5 min. 9.51
0.01 0.03 0.05 0.1
Groove width Groove depth Groove lengths
0.05 0.1
Diameter Length of the circular part of the disc shaft Length of the square part of the disc shaft
0.01
20.0
0.5
35.0
0.5
Grooves on top and bottom surfaces should be displaced 5 .
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Figure 13. Cure curve.
Figure 14. Type of cure curves.
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Figure 17. Upper die.
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Figure 18. Biconical disk.
PART D ADDITIONAL TEST METHODS FOR PRODUCTION CONTROL USED BY RRIM
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D. 1
DETERMINATION OF VULCANISATION CHARACTERISTICS THROUGH THE RELAXED MODULUS TEST (MOD TEST) Explanatory Notes The vulcanisation characteristics are assessed by measurement of the relaxed modulus (tension stress at 100% extension) in the ACS 1 mix vulcanised at 140C + 2C for 40 + 0.1 min. The ACS 1 compound is prepared to a standard schedule using vulcanising masterbatches for the incorporation of compounding ingredients. The normal procedure is to mix on day one, cure on day two and test on day three. In a rapid procedure, results are obtained in one day and these are equated to normal by applying a correction. Results in both the normal and rapid procedures are corrected to a compound Mooney viscosity of 40. 1.2 Test Formulation (see C.3.3) 1.3 Compounding (see C.3.4) 1.4 Storage of Masterbatches and Test Mixes (see C.3.5) 1.5 Vulcanisation
1.1 1.1.1
1.1.2
1.1.3
1.5.1
Vulcanisation shall be for a period of 40 + 0.1 min at 140C 2C. For the determination of 100% relaxed modulus (MOD), cut testpieces from the vulcanised sheet of about but not more than 3 mm in thickness.
1.5.2
Alternatively, individual testpieces may be moulded.
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1.5.3
Load the unvulcanised compound into hot moulds in not more than 2 min. After vulcanisation rapidly remove the sheets or testpieces from the hot mould and immediately chill them in cold water. Preparation of Testpiece The testpiece shall be of the dumbbell shape as shown in Figure 19. Cut the dumbbells from a sheet by punching with an appropriate die using a single blow of a mallet or preferably a single stroke of a press. The rubber should be wetted with water or soap solution and supported on a sheet of slightly yielding material {e.g. cardboard) on a flat rigid surface.
1.6 1.6.1
1.6.2
All dumbbells shall be cut with the grain running along their length. Any dumbbells showing irregularities or imperfections along their length shall not be used. Thickness of Testpieces In any one dumbbell, the thickness of the narrow part shall nowhere deviate by more than 2% from the mean. Thickness shall be measured by means of a gauge reading in 1/100 mm in which the foot has a diameter of about 4 mm and exerts a pressure of 0.200 + 0.030 kfg/cm .
2
1.6.3
1.6.4
Number of Testpieces Duplicate testpieces shall be prepared from each mixing at each vulcanisation time.
1.6.5
Conditioning of Testpieces Testpieces shall be conditioned for a period not exceeding 24 h at 20C + 2C before testing.
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1.6.6
In the rapid procedure, no conditioning is given and the testpieces are tested within 2 h after vulcanisation. Equipment and Procedure MOD Measurement The equipment (see Figure 20) shall be of the triple beam balance type with sliding weight giving a maximum load of not less than 2 kg and capable of being read to 0.5 g or less. An upper grip in the form of jaws capable of gripping the testpiece at one end of its narrow length shall be attached to the underside of the normal balance pan support by means of an extension rod projecting downwards through a clearance gap in the base casting. The base casting shall carry a fixed and vertically aligned rod. A lower grip, similar in construction to the upper grip, shall be provided with a fixed projecting cylindrical peg which slides into one of two drilled and bushed holes in the vertical rod. In either position the lower and upper grips shall be vertically opposed. When the lower grip is supported in the higher position its distance from the upper grip shall be such that a testpiece contained in the grips is straight and unstretched. When the lower grip is in the lower position its distance from the upper grip shall be such that the testpiece is elongated 100%. The balance shall be fitted with means for counterpoising the weight of the assembly attached to the balance pan support, and with stops to restrict the swing of the beam so that the corresponding change in extension of the testpiece is within 1 % . The testpiece shall be placed in the grips with the lower grip in the upper position. The lower grip shall then be moved down to the lower position, giving 100% elongation to the testpiece and a time device to be started. The movement of the lower grip shall be completed within 5 s. The tension in the rubber shall be balanced by sliding the weights, adjustment being made to allow for any stress relaxation during 1 min. The balancing load shall be read at this time and recorded.
1.7 1.7.1
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1.7.2
Mooney Viscosity Measurement The compound Mooney viscosity is required to be known in order to apply the correction to MOD values. About 25 g of compound is used, of thickness about 6 mm in two portions. The rotor stem shall be placed through a hole in the centre of one portion backed with polyester or cellophane film; the rotor and compound shall be placed in the die cavity. The second portion shall be covered with polyester or cellophane film and placed on top, and the dies closed. Measure the compound viscosity as ML (1+4) 100C, according to the method described in B.9.
1.8 1.8.1
Calculation and Adjustment of Results Thickness of Testpiece The 100% relaxed modulus (MOD) shall be calculated as the stress in kg/cm of the original cross-section for 100% elongation.
2
1.8.2
Compound Viscosity The relaxed modulus shall be further adjusted to the value corresponding to Mooney viscosity 40 of the unvulcanised compound as follows: Compound viscositv 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 Adjustment (kg/cm )
2
+0.23 +0.20 +0.18 +0.15 +0.13 +0.10 +0.08 +0.06 +0.04 +0.02 0 -0.02 -0.04 -0.05 -0.07 -0.09
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1.8.3
Rapid Procedure MOD values adjusted for cross-sectional area and compound Mooney viscosity are further adjusted if the rapid procedure has been used, as follows: MOD (normal) = 0.45 + 0.97 MOD (rapid)
1.8.4
Expression of Results The average value of the adjusted MOD value of the duplicate testpieces is reported.
1.8.5
Tolerances Mixing and testing tolerances are as follows:
Detail Maximum allowable range of replicate tests Maximum allowable range of two batch averages
Percentage of mean 5 5
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Thickness not greater than 3 mm
3-61 0 - 0 8 mm
!2-7mm
100 + 0 5 m m
Figure 19. Modulus

Balance pan
testpiece.
-J Beam type balance
Incremental weight
' ( h i
A
T-R
Sliding weight
Sir
/TV
Table support (or balance
Upper g r i p ' ,Test piece
Cylindrical peg Lower grip test piece unstrained

i-ii
- m
Lower grip test piece 1 0 0 % elongation
Figure 20. Modulus test apparatus.
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D.2 2.1
TEST FOR EXCESSIVE USE OF CASTOR OIL IN HEVEACRUMB Explanatory Notes In the production of Heveacrumb rubber, crumbling agent (usually castor oil) is used. If excess castor oil is used in production, it can be detected and approximately estimated by this castor oil bloom (COB) test.
2.2
Principle of Method The rubber is compounded in a conventional gum formulation and vulcanised in the usual manner. The vulcanisate is then examined for castor oil bloom, both after curing and after conditioning at a fixed temperature for certain periods, by pressing the vulcanisate under a heavy roller against a matt black surface and observing the intensity of stain produced.
2.3
Equipment The equipment required consists of the following: (a) A 150 x 300 mm (6 x 12 in) laboratory mill with adjustable guides; vulcanising mould, e.g. with circular cavity of 60 mm (2.4 in) nominal diameter and 4 mm (0.15 in) nominal depth; slab moulds of 4 mm nominal depth are also suitable.
(b) Vulcanising press (c) Black matt-surfaced formica sheet of nominal dimensions 150 x 300 mm (6 x 12 in). The sheet is cleaned before use with petrol or similar grease solvent. It should present a completely matt appearance. (d) Hard metal roller weighing about 2.5 - 3 kg ( 5 - 6 lb).
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2.4
Compound Formula Rubber Zinc oxide Stearic acid Cyclohexylbenzthiazyl sulphenamide (CBS) Sulphur Total 100.0 5.0 1.5 0.5 2.5 109.5 + + 1 0.1 0.1 0.1 0.1
2.5
Mixing Procedure Mixing is carried out with the temperature of the rolls at 70C 5C, and nip setting 0.5 0.05 mm (0.020 in) Normally mixing is based on 50 g rubber, and the guides are set about 150 mm (6 in) apart; if 100 g rubber is used, the guides are kept at full distance apart. Compounding ingredients are added as powders. The mixing cycle is: Time (min) Rubber in, banded on front roll Ingredients added: 3/4 cut made six times on alternate sides: material parting from rolls swept up and returned to rubber 0.00 0.25
0.25 - 2.5
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Nip closed: compound passed twice through closed rolls and rolled up: nip setting adjusted to about 0.13 mm (0.050 in) compound passed endwise through rolls, rolled up, passed through end wise again and sheeted off 2.6 Vulcanisation
2.5-3.0
About 11 g of compound are placed in a mould cavity (nominal diameter 60 mm): nominally several compounds are prepared from different rubbers and single test portions from each compound are vulcanised together in a multicavity mould; alternatively, test vulcanisate may conveniently be about 50 mm (2 in) square shape, moulded or cut from a vulcanised slab. The vulcanisation is to be performed at 150C 2C for 30 min. The test vulcanisates are placed in an air-conditioned room before testing, side by side and not piled up, in order to avoid possible contamination of the surface. 2.7 Testing The test vulcanisate is placed on the clean black matt formica surface and the metal roller passed over it without applying pressure. The testpiece is removed and the formica surface examined visually, if castor oil bloom exists the formica surface is stained: if there is no bloom, the surface remains unchanged.
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Blooming is assessed as nil, slight, moderate or heavy by reference to a comparison standard print (see Figure 21). After the test, the formica sheet is cleaned of oil stains with petrol or other solvent and is ready for reuse. Testing is carried out after storing in the conditioned atmosphere for 1 + 0.1 h, 24 + 0.1 h and 48 0.1 h. A test vulcanisate which shows no staining after 48 h is considered satisfactory.
Nil
Slight
Moderate
Heavy
Figure 21. Assessment of castor oil bloom. Score from left shows: (a) nil (control); (b) slight; (c) moderate; and (d) heavy.
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D.3 3.1
DETERMINATION OF ACETONE EXTRACT Explanatory Notes The acetone extract contains naturally occurring non-rubber constituents rubber (such as fatty acids, sterols, quebrachitol, etc.). Additionally, acetone will extract degraded rubber {i.e. rubber of low molecular weight) if the rubber has been exposed to oxidative influences such as strong sunlight. Two methods are used: (a) Direct Method
This involves the individual extraction of a sample, and then direct weighing of the extract. It is particularly used when the extract is required for examination. (b) Difference Method In this method fifty samples are extracted together, and the weight of the extract is obtained by the difference in weight of the sample before and after extraction. This method requires slightly less time, and is particularly suitable for application to quality control of rubbers. However, it is not applicable to rubbers which flake, disintegrate or become tacky after extraction. 3.2 3.2.1 Direct Method Principle of Method The method involves the individual extraction of a sample, and then direct weighing of the extract.
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3.2.2
Equipment and Materials (a) Extraction apparatus is of the reflux type with the condenser placed immediately above the cup which holds the rubber. The cup (40 ml capacity) is situated in the vapour of boiling solvent and is emptied by a siphon. The apparatus is wholly of glass and fits together so that loss of vapour during extraction does not exceed 20% of the extraction liquid (see Figure 22),
(b) Soxhlet extraction thimble (optional) (c) Filter paper or organdy cloth
(d) Water-bath, to provide heat for extraction with acetone (e) Solvent recovery apparatus, consisting of a recovery bend, a Liebig condenser and a receiver adaptor, to collect the solvent from the extract Redistillation apparatus, consisting of a round-bottom flask (of 3 litres capacity), a fractionating Dufton column, a stillhead with thermometer, a Liebig condenser and a receiver adaptor
(f)
(g) Suitable isothermal heating mantles (h) Redistilled acetone, substantially pure and free from water and polymers of acetone
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3.2.3
Procedure Take a test portion of about 5 g rubber from the piece blended as in B.2 and pass it twice between the cold, tightly closed rolls of a laboratory mill. Allow the test portion to equilibrate at room temperature for about half an hour and weigh accurately to the nearest 0.1 mg. Wrap it in filter paper or organdy cloth (previously extracted) so that no two portions of the rubber surface are in contact with each other, and place it in a previously extracted Soxhlet thimble (the thimble is optional). Place the sample in the extraction apparatus. Pour sufficient acetone (about 100 ml) into the weighed 150 ml extraction flask, and subject the sample to at least eighty hot extractions during a continuous period of 16 Vi h in a water-bath maintained at 70C 5C. Distill the acetone from the extracted material taking care not to scorch the extract by local overheating. (The recovered acetone is collected and redistilled by fractionation before reuse.) Dry the residue at 70C 5C for about 1 h, cool in a desiccator, and weigh.
3.2.4
Calculation Calculate as follows: Acetone extract (%) = x 100
where A is the weight in grammes of test portion; B is the weight in grammes of extraction flask plus extracted residue; C is the weight in grammes of empty flask.
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3.3 3.3.1
Difference Method Principle of Method In this method about 1.5 g of each sample is individually placed in an organdy cloth envelope. Fifty such envelopes are bulk extracted together in a larger soxhlet-type apparatus (600 ml capacity) for 16 Vi h. When extraction is complete, the extracted rubber is oven-dried and then weighed after 2 - 3 h equilibrium at room temperature. The difference in weights before and after extraction gives the weight of the extract.
3.3.2
Apparatus The extraction apparatus is of the soxhlet-type similar to that described for the previous method, except that this has a much larger extractor, the capacity of extraction cup being 600 ml; with a 2-litre round-bottom flask and a suitable isothermal heating mantle. Organdy cloth 'envelopes' of size approximately 70 x 70 mm are also required. The solvent recovery and redistillation apparatus used is the same as for the Direct Method. Redistilled acetone, substantially pure and free from water and polymers of acetone, is the reagent used.
3.3.3
Procedure A test portion of about 1.5 g rubber is taken from the piece blended as in B.2 and passed twice between the cold, tightly closed rolls of a laboratory mill.
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The sample is allowed to equilibrate at room atmosphere for about half an hour, and then weighed accurately and placed in the prepared organdy envelope previously acetone extracted. Sixteen (or seventeen) such envelopes are arranged upright in the soxhlet cup so that no two envelopes overlap each other completely (petalwise). This forms the first tier. The soxhlet cup accommodates three such tiers, the total number of samples therein being about fifty. About 1.5 litres of acetone is poured into the round-bottom flask, and the samples subjected to at least forty hot extractions during a continuous period of 16 + V2 h (overnight). At the end of the extraction period the samples are removed from the extraction cup and dried at 70C 5C in an oven for about 1 h. The dry samples are taken from the oven, then the extracted test portions are removed from their envelopes and placed on labelled aluminium trays to equilibrate at room atmosphere for 2 - 3 h. The extracted test portions are then weighed. The acetone is removed from the extract and factionally redistilled for further use.
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3.3.4
Calculation The acetone extract is determined as follows: A B Acetone extract (% wt) = x 100
7
where A is the weight in grammes of rubber test portion before extraction; B is the weight in grammes of rubber test portion after extraction.
Figure 22. Acetone extraction
apparatus.

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RRIM TEST METHODS FOR STANDARD MALAYSIAN RUBBERS

SMR BULLETIN NO.7 REVISED EDITION 1992

RRIM TEST METHODS FOR STANDARD MALAYSIAN RUBBERS

Revised Edition 1992 by Ng Yu Tong

COPYRIGHT MALAYSIAN RUBBER BOARD

Abbreviated title: SMR Bull. No. 7 Rubb. Res. Inst.

B.4 B.5 B.6 B.7 B.8

B.9 B.10 PART C

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Sample Piece Test portions (testpiece) Crumb rubber

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(b) Thermometer, reading 100C - 200C

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(e) (f) (g) (h) (i) (j) (k)

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30-16mm < t > 952mm | _ t i 1428mm 4-76mm | - j 2778 mm < t > - 0 2 5 mm U-

-39 68 mm <t> -31 75 mm <)>

27-78mm <|>-025mm Section A - A

Figure 1. Sieve for dirt determination (325 mesh).

Figure 3.Details of inspection holder for sieves.

9525mm 14-28mnH 1-I9mm 9-5 2mm

Braze on outside 27-78mm4>

27-78mm4> 2778mm<H -0 25mm . 0 2 5 m m

9-52 mm 0 / D brass tube

Mesh.-^ Sieve Sieve holder

Figure 2. Details of sieve and holder for dirt

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Volatile matter (%) = ^r-

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Flat head rivet

3175mm cj> ((*"<(