DATE :- 2020.01.

07

EXPERIMENT NO :- 09

EXPERIMENT NAME :- DETERMINATION OF ASH CONTENT NATURAL

RUBBER.

THEORY

Methods used in ashing Natural rubber and other similar organic compounds call for

distillation of the dry sample by gradually raising the temperature of the specimen from room

temperature to a point somewhat below the ignition temperature of the gases formed. The

carbonaceous residue is then ashed to constant weight at temperatures varying from 400 to

550° C, depending on the substance tested. Along with this, setting accurate time and the

temperature is also mandatory to treat the rubbers and to measure the actual % of ash in the

materials.

Determine the ash content of the rubber sample by the following equation.

Ash content = WRf + c - Wc

X 100%
WR
WC = Weight of the crucible

WR = Weight of the rubber specimen

WRf + c = weight after heating of the rubber specimen and the crucible
PROCEDURE

Firstly the weight of the empty crucible was weighed and recorded the value as the WC. Then

the to the nearest 2g of rubber specimen (are prevulcanized CaCO3 filled, prevulcanized

Carbon Black filled , uncompounded HANR and prevulcanized unfilled HANR film rubber

was weighed and it was recorded as the WR . After that the crucible with rubber pieces was

placed in the furnace which the temperature was set to the 550 o c. then the furnace was

closed and then the furnace was not opened for about 45 minutes. After that the crucible was

taken out from the furnace and then the crucible was kept to cooled to the room temperature.

After that the weight of the crucible was weighed and finally the values was recorded as WRf

+c. after that the crucible was cleaned.

READINGS

Sample name Weight / g

Crucible rubber pieces After heating

( crucible+ rubber)
ETP / CaCO3 / 01 61.55 2.016 62.473

ETP/ CarbonB/ 02 59.515 1.968 60.966

ETP / HANR / 03 62.840 2.06 62.842

ETP / NONF / 04 55.8 1.843 55.925

TABLE OF WEIGHT OF DETERMINE THE ASH CONTENT OF NATURAL RUBBER

CALCULATION
Ash content = WRf + c - Wc X 100%
WR

Calculation of ash content for the CaCO3 sample ,

Ash content = 62.473 – 61.55

X 100%
2.016

= 45.783%

Calculation of ash content for the non filler sample ,

Ash content = 55.925 – 55.842

X 100%
1.843

= 4.503%

Calculation of ash content for the carbon black sample ,

Ash content = 60.966 – 59.515

X 100%
1.968

= 73.72%

Calculation of ash content for the HANR sample ,

Ash content = 62.842 – 62.840 X 100%

2.06

= 0.097%

DISCUSSION
The ash content is mainly used for the Quality Assurance test for raw materials (rubber based

raw materials). Ash content test cannot be done for the latex because the latex contains water.

There is no product are at latex stage so that the test is done for the dry sheet which was the

ingredients are added to the latex then make a dry sheet to compare the properties after the

product made. Testing the sample at initial stage would help in correcting the whole

manufacturing line in the early stage thus helps in reducing errors and cost of rectification.

The volatile materials or the things that are not decomposable of the rubber at the temperature

around 5000c or 9500c if they are not decomposing called as “Ash”. Below 5000c mostly all

the organic compounds decomposed into Carbon, Oxygen containing gases. That is CO2 or

CO3. When heat up to very high temperature all the organic compounds are decomposed.

The process of ash content determination of natural rubber can be done using high quality of

Muffle Furnaces. This method is known as the gravimetric method of determining ash test.

A muffle furnace burns down the sample completely until it turns into ash. The ash content is

weighed and compared with weight or original sample, to determine the percentage of ash.

After burning down the sample, the organic contents will get changed into fumes and taken

out.

In this ash content test it only determine the filler content but it cannot identify individual

percentage of multi filled materials without performed additional test procedures.

The ash content of natural rubber is varying due to the reasons such as when the filler is

inside the rubber, the ash content has to be higher than the unfilled compound. And also it

contains ZnO, accelerators and everything inside the latex. So all these will come into the

generation of ash. In this practical, the ash content test was done for the four samples which

are prevulcanized CaCO3 filled, prevulcanized Carbon Black filled , uncompounded HANR

and prevulcanized unfilled HANR film rubber. It can be see that the higher ash content is in
the prevulcanized carbon black filled rubber and in the prevulcanized CaCO3 filled rubber

than the prevulcanized Unfilled HANR and uncompounded HANR.

For the determination of ash content in the smaller size sample the thermo gravimetric

method can be used as an alternative method.

The standard operating procedure of muffle furnace sound very easy, actually it is. But this

is a very complicated machine. The temperature range of muffle furnace is very high,

approximately 900°C or 1200°C or 1400°C. In the practical, the sample with crucible was

placed inside the furnace at the temperature of 550cc for 45 minutes. Optimum temperature is

about 550oc for 2 hours.

Ash (Fillers) Content Testing

Standard Test Methods for Rubber Products-Chemical Analysis

ASTM D 297

Ash Content in Carbon Black

Standard Test Methods for Carbon Black—Ash Content

ASTM D 1506

CONCLUSION
Comparison of the experimental results with the prevulcanized filled compound with unfilled

and uncompounded samples showed a high difference of ash content % . It can be concluded

that for the ash content will vary when fillers and other ingredients are inside the rubber will

caused for the higher ash content. And also the results showed that the uncompounded

HANR sample having a very low ash content that less than 0.1% value.

REFERENCES

 .L.Babitskii and L.E Vintskii, Soviet rubber tehnology, 1961 ,20,28

 Joseph, R. 2013. Practical guide to latex technology. UK: smithers Rapra Technology

LTD.