Post on 24-Jan-2020
SEMINAR: UPDATES ON SMR AND SMR LABORATORY INTEGRATION SYSTEM (SLIS)
REVISED TEST METHOD :DETERMINATION OF ASH
Scope
Principle
Apparatus
Procedure
Expression of Result
Outline
Differences between previous & revised test method
PREVIOUS TEST METHOD REVISED TEST METHOD
• Explanatory notes• Apparatus and
Materials• Procedure• Calculation
• Scope• Principle• Apparatus • Procedure• Expression of result• Precision• Test report
Scope
This part of SMR Bulletin No.7 specifies a method for the determination of ash from raw natural rubbers.
Principle
Explanatory notes
A weighed test piece is wrapped in ashless filter paper, followed by incineration in a muffle furnace at about 550 °C ± 25 °C for two to four hours until all the carbonaceous matter has been burnt off and constant mass is attained.
Apparatus
CrucibleMuffle furnace
Ashlessfilter paper
Desiccator Tong
Procedure
Weigh 5 g to 10 g test piece of the homogenisedrubber
Wrap in ashlessfilter paper and place in a crucible
Introduce the crucible into a muffle furnace
(550 °C ± 25 °C ,
2 h to 4 h)
Cool the crucible in a desiccator and then weigh
Expression of Result
Where
A is the mass, in grams, of the crucible and ash;
B is the mass, in grams, of the empty crucible; and
C is the mass, in grams, of the test piece.
100(%)
C
BAAsh
Expression of Result
TEST METHODS CALCULATION
SMR BULLETIN NO.7
ISO 247 (METHOD A & B)
(NEWLY PROPOSED METHOD C BY MALAYSIA)100(%)
C
BAAsh
100(%)
C
DBAAsh
Where A is the mass, in grams, of the crucible and ash;B is the mass, in grams, of the empty crucible; C is the mass, in grams, of the test piece; andD is the mass, in grams, of the ash from filter paper.
ISO 247
TEST METHODS SCOPES
AShall not be used for the determination of ash from raw, compounded or vulcanized rubbers containing chlorine, bromine or iodine
BShall be used for compounded or vulcanized rubbers containing chlorine, bromine or iodine. It shall not be used for uncompounded rubbers
C
Intended to be used for the determination of ash from raw, compounded or vulcanized rubber not containing chlorine, bromine or iodine by wrapping the test portion in ashlessfilter paper
Proposed Lab Works to resolve the comments on calculation
• 1st Lab Work
• 2nd Lab Work
Lab Work 1
Ashing all raw rubber samples, including control (w/o filter paper) and wrapped samples (by using 3 different brands of filter paper) together in one furnace to eliminate uncertainties due to temperature, human and variation in days and time if any that could have affected the results.
Filter papers employed in the studies
• DR
• NICE
• W
CALCULATION OF ASH BY USING FEW FORMULAS
Aim: To observe the closest value of ash to the control value
Control (Without Fi l ter
Paper) From Worksheet
Control to be done
SMR BULLETIN NO.7 ISO 247
DR 0.3224 0.3319
NICE 0.3340 0.3450
W 0.3244 0.3354
0.3269 0.3374
DR 0.3303 0.3395
NICE 0.3123 0.3230
W 0.3264 0.3374
0.3230 0.3333
DR 0.3601 0.3689
NICE 0.3549 0.3658
W 0.3636 0.3744
0.3596 0.3697
DR 0.3562 0.3652
NICE 0.3513 0.3617
W 0.3535 0.3640
0.3537 0.3637AVERAGE
270916 (am) 0.36240.0087 0.0013
AVERAGE
270916 (pm) 0.36780.0082 0.0019
AVERAGE
041016 (am) 0.33920.0162 0.0059
041016 (pm) 0.33620.0092 0.0013
AVERAGE
Date Brands Diff. Di ff.
Lab Work 2
Ashing all the raw rubber samples, including control (w/o filter paper) and wrapped samples together in one furnace but using different amount of filter papers to wrap the samples. This is to confirm that regardless of the numbers of filter paper used; the percent ratio of ash from filter paper to the weight of filter paper will remain the same.
CALCULATION OF ASH BY USING FEW FORMULAS
Aim: To observe the closest value of ash to the control value
Control (Without Fi l ter
Paper) From Worksheet
Control to be done
SMR BULLETIN NO.7 ISO 247
W (1) 0.3396 0.3503
W (2) 0.3411 0.3517
W (3) 0.3351 0.3473
0.3386 0.3498
W (1) 0.3453 0.3562
W (2) 0.3521 0.3631
W (3) 0.3478 0.3605
0.3484 0.3599
NICE (1) 0.3551 0.3657
NICE (2) 0.3596 0.3705
NICE (3) 0.3554 0.3699
0.3567 0.3687
NICE (1) 0.3425 0.3530
NICE (2) 0.3398 0.3504
NICE (3) 0.3421 0.3568
0.3415 0.3534
DR (1) 0.3464 0.3535
DR (2) 0.3430 0.3520
DR (3) 0.3428 0.3535
0.3441 0.3530
DR (1) 0.3535 0.3606
DR (2) 0.3482 0.3570
DR (3) 0.3454 0.3560
0.3490 0.3579
0.0083
0.0130
0.0005
0.0041
0.0007
0.0041
0.0006
0.0115
0.0161
Diff.
0.0072 0.00400.3458
0.3593
0.3682
0.3575
Diff.
0.0109
Sample IDDate
061016
280916
051016
AVERAGE
0.3523
0.3620
AVERAGE
AVERAGE
AVERAGE
AVERAGE
AVERAGE
290916
051016
280916
OBSERVATION
1) From Lab work 1, results for ISO 247 formula are closer tothe control values. The filter paper was not affectingsignificantly the ash content of the rubber samples.
2) Lab Work 2 is supporting the earlier observation whereresults of Ash following ISO 247 formula are closer to thecontrol values.
Based on the observation, it is proposed for ash test method in SMR Bulletin No. 7 to use the same
formula as ISO 247.
CONCLUSION
THANK YOU
for your
ATTENTION