ISO 247-2-2018 pdf free.Rubber- Determination of ash – Part 2: Thermogravimetric analysis (TGA).
6.1 Thermogravlmetric analyser. comprising the following elements:
a) Therino-balance;
b) Heating furnace;
c) Temperature programmer;
d) Gas flow controller, for controlling the purge gas to the balance and furnace, and keeping a constant flow rate.
6.2 Sample pan. platinum pan or alumina ceramic pan.
6.3 Analytical balance, capable of weighing to the nearest 0,1 mg.
7 Preparation of the test sample
7.1 For raw natural rubber, test samples shall be cut from the homogenized piece prepared in accordance with ISO 1795. For raw synthetic rubber, test samples shall be cut from the dried rubber obtained after carrying out the determination of volatile-matter content in accordance with the hot-mill method of ISO 248-1.
Take a test portion of about 2 g to 5 g from the homogenized sample and cut into pieces by hand.
7.2 Test samples of rubber compounds shall be sheeted on a mill and cut into pieces by hand.
7.3 Test samples of vulcanizates shall be sheeted or crumbed on a mill or comminuted by hand.
7.4 Care shall be taken to ensure that test samples of rubber compounds and vulcanizates are representative of the sample.
8 Calibration
Calibrate the thermogravimetric analyser (see &1) according to the manufacturers instructions.
Temperature and mass calibration should be performed.
To ensure consistent results, the thermogravimetric analyser shall be calibrated periodically. It is recommended to perform mass calibration once a month.
9.1.1 Switch on and stabilize the instrument, set the temperature of furnace to 30 °C.
9.1.2 Place an empty sample pan on the platform and tare the sample pan.
9.1.3 Take about 10 mg to 20 mg from the test portion of raw rubber (see LI) and weigh to the nearest
0,1 mg. Place it in the sample pan. Position the sample pan on the sample platform and load the sample pan onto the thermo-balance.
9.1.4 Set the flow rate according to the manufacturer’s instructions. Raise the temperature to 500 °C at a rate of 20 °C/min or 30 °C/min under an atmosphere of nitrogen. Maintain at this temperature for 1 mm.
9.1.5 Switch from the stream of nitrogen toa stream of oxygen or air. Raise the temperature to 550 °C. Maintain the temperature at 550 °C for 5 mm or until the mass is constant.
9.1.6 Calculate the ash using the apparatus microprocessor.
9.2 Method B
9.2.1 Switch on and stabilize the instrument, set the temperature of furnace to 30°C.
9.2.2 Place an empty sample pan on the platform and tare the sample pan.
9.2.3 Take a test portion of about 10mg to 20mg from the test sample of compounded or vulcanized rubbers (see Z2 or L3) and weigh to the nearest 0,1 mg. Place it in the sample pan. Position the sample pan on the sample platform and load the sample pan onto the thermobalance.
9.2.4 Set the flow rate according to the manufacturer’s instructions. Raise the temperature to 550 °C at a rate of 20 °C/min or 30 °C/min under an atmosphere of nitrogen. Maintain at this temperature for 1 mm.
9.2.5 Switch from the stream of nitrogen to a stream of oxygen or air. Raise the temperature to 650 °C. Maintain the temperature at 650 °C for 5 mm or until the mass is constant.
For compounded or vulcanized rubbers containing inorganic fillers such as calcium carbonate, a temperature of 850 °C should be used.
9.2.6 Calculate the ash using the apparatus micro-processor.ISO 247-2 pdf download.
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