PURPOSE:

To determine the amount of Xylene Soluble component (Non-crystalline, or Atactic polymer)

in polypropylene.

SAFETY:

1. Xylene is a flammable liquid and may cause skin irritation. Use solvent resistant
gloves, keep clear of open flames and use an explosion proof hot plate for the
evaporation step.

2. Avoid restricting the flow of purge nitrogen or cooling water to the condenser since
dangerous over pressure could result.

3. Used Xylene is collected in a safety container for further recycle.

4. Refluxing, filtering and evaporating is done in the fume hood having proper exhaust
system.

5. Avoid eye contact and inhalation of Xylene.

6. Nitrogen is an Asphyxiation hazard. Take care while working with Fume hood &
Vacuum oven.

SUMMARY:

The sample is completely dissolved in distillated xylene (500ml) by stirring at reflux. The
solution is cooled to 25°C in a water bath, during this time the insoluble portion precipitates.
The solution is filtered, and then a 100-ml aliquot of the filtrate is taken into an aluminum pan
and evaporated to dryness on a vacuum oven. The solubles present are determined by
weighing the residual polymer.

PRINCIPLE:

Extraction and Evaporation.

Dr Ajay K Nema, Sr Technical Officer (Testing), CIPET, Bhopal

INSTRUMENTS AND CHEMICALS:

1. Hot plate with stirrer and stirring bar.

2. Fluted paper filter, 10 – 15 µm average pore diameter, Ø 385 mm.

3. Vacuum oven.

4. Analytical balance.

5. Desiccator with desiccant.

6. Constant temperature bath, 25 ± 0.5°C.

7. Erlenmeyer flask: 1 liter – 3- necked flsak with stirrer.

8. Reflux condenser (with flow guard)

9. Thermometer.

10. Xylene.

11. Aluminum pan.

12. Funnel.

13. Pipette 100 ml

14. Water supply tubing with indicator.

15. Gloves, solvent resistant.

16. Flask support and tripod stand.

CALIBRATION CHECK:

1. Calibration is to be done after each new stabilized xylene is prepared.

2. The procedure for the calibration check is to be same as the procedure for
determination of Xylene soluble.

3. Log the results on the zone control chart.

4. If the zone CONTROL CHART rating is 8 or more than 8, rerun the test. If the blank is
suspected, use a new drum of Xylene with a new blank and rerun the test.

5. If the quality standard still fails, notify the Lab Staff as soon as possible.

6. The Lab Staff will review and make the appropriate decision.

7. If this problem occurs on shift, notify the Shift Supervisor.

8. Save samples so that they may be analyzed after the problem has been resolved.

Dr Ajay K Nema, Sr Technical Officer (Testing), CIPET, Bhopal

PROCEDURE:

1. Add 5 ± 0.1g of sample to a clean and dried 1000 ml 3-necked flask which is equipped
with stirer and add 500 ml of stabilized Xylene. Record the sample weight.

2. Connect flask to the condenser, stir vigorously and reflux till it dissolves completely for
circa 60 minutes. Be sure nitrogen is flowing through the bubbler.

3. Turn off the heater & stirrer, lift the flask and condenser assembly and support it on a
wire tripod if necessary. Allow the flask to cool for about 10 minutes.

4. Remove the flask from the condenser, close with a glass stopper and transfer to the 25
°±0.5°C water bath using a clamp to hold the flask. Hold the flask at this temperature
for approximately 35 minutes.

5. Remove the flask from the bath and filter its contents through a funnel containing
Whatman 2V filter paper. For impact co-polymer resin the filter paper and contents
may be squeezed to remove enough filtrate for an aliquot to be taken. Shake or stir
the contents before filtering to break up the gel.

6. Transfer 100 ml of filtrate into a pre-weighed aluminum pan (W1).

7. Using an explosion proof hot plate, evaporate the filtrate to dryness under a gentle
stream of nitrogen in fume hood.

8. Complete the drying by placing the aluminum pan in nitrogen purged vacuum oven
around 100°C for one hour. Adequate nitrogen flow can be obtained by using the
purge control valve on the oven.

9. Remove the pan, cool in desiccator and weigh to the nearest 0.0001g (W2). Allow
about 5 minutes for the pan to equilibrate with the lab atmosphere before weighing.

CALCULATION:

Xylene soluble is determined by:

2 (W2 - W1) - 2 (Blank)

% XS = x 100
Sample Weight

NOTE: The following can be major sources of error:

1. Too rapid or too slow cooling times.

2. Final equilibrium temperature. Water bath temperature other than 25 ± 0.5°C can
affect results.
3. After evaporation if the residue turns to yellow or brown, which is the sign of oxidation
or degradation, repeat the analysis.

REPORT:

1. Report the result as % Xylene soluble in the appropriate format in LIMS up to two
decimals.

Dr Ajay K Nema, Sr Technical Officer (Testing), CIPET, Bhopal

REFERENCE:

1. ASTM D5492-94, Standard Test Method for Determination of Xylene Solubles in

Propylene Plastics.

2. ISO 6247.

Dr Ajay K Nema, Sr Technical Officer (Testing), CIPET, Bhopal