BS ISO 17257:2013 pdf download

BS ISO 17257:2013 pdf download.Rubber —ldentification of polymers-Pyrolytic gas-chromatographic method using mass-spectrometric detection.
3.2 Group 0
3.2.1 Homopolymer of epichiorhydrin (CO), copolymer of epichiorhydrin-ethylene oxide (ECO), terpolymer of epichioi-hydrin-ethylene oxide-allyl glycidyl ether (GECO)
The method cannot distinguish between them.
3.3 GroupQ
3.3.1 Polysiloxanes (MQ, VMQ, PVMQ)
The method Cannot distinguish MQ and VMQ, but can distinguish PVMQ from the two other polymers.
3.4 GroupR
3.4.1 Butadlenc rubber (BR)
3.4.2 Chloroprene rubber (CR)
3.4.3 Isobutene-Isoprenc rubber (IIR), chlorinated hR (CuR) and broininated IIR (Bilk) The method cannot distinguish between them.
3.4.4 Natural rubber (NR) and synthetic isoprene rubber (1k) The method cannot distinguish between them.
3.4.5 Acrylonitriie-butadiene rubber (NBR), hydrogenated NBR (HNBR) and carboxylated NBR (XNBR)
The method can only distinguish HN HR from the two other polymers (N HR and XNBR).
3.4.6 Styrene-butadiene rubber (SBR)
The method allows butadiene-a-methylstyrene rubber to be distinguished from butadiene-styrene rubber.
3.S Rubber blends
In copolymer-homopolymer blends having one common monomer (e.g SBR/ BR. NBR/BR), the technique does not allow the homopolymer to he distinguished.
This is also valid for blends with terpotymers.
4 Principle
4.1 Raw rubbers, or vulcanized or unvulcanized compounds which previously have been solvent extracted, are pyrolysed and the pyrolysate analysed by gas chromatography with mass spectrometric detection.
4.2 The interpretation of the results is made by examining the mass spectra of the specific chromatographic peaks.
6.2.2.2 Examples of useful capillary columns
a) Capillary column in fused silica of 0,32 mm diameter and 30 m ,of apolar type. Stationary phase. film of dimethyl polysiloxane, 1 pm thick:
b) Capillary column in fused silica of 0.32 mm diameter and 30 m • of polar type. Stationary phase – film of polyethylene glycol. 0,5 jim thick.
7 Operating conditions
7.1 General
The reproducibility is guaranteed by checking the conformity of the device and by respecting the procedure.
7.2 Gas chromatograph adjustment
Adjust the various controls of the gas chromatograph according to the retained operating conditions.
For Information, typical operating conditions are given In AnnexB.
7.3 ExtractIon
Carry out the extraction according to ISO 1407. The rubber residue is dried until constant mass.
NOTE This preliminary extraction Is not mandatory but allows (he elimination of compound constituents which could interfere with the pyrolysis product.
7.4 Test portion
Take a test portion of mass appropriate to the apparatus used, usually about 0,1 mg.
7.5 Pyrolysis
Place the test portion In the pyrolysis device and purge for the necessary time.
Pyrolyse at a temperature between 400°C and 800 °C; usually the pyrolysis temperature is about 600 °C.
Record the experimental data.
8 Interpretation of results
8.1 General
The identification of rubbers is achieved by noting the presence of certain characteristic decomposition products and by consulting the mass spectra database.
Two examples of chromatograms are presented in Annex C.
The following clauses summarize all the characteristic products by Family of polymer. For the
interpretation of the results, refer to Annex D according to the type of column used.
8.2 GroupM
8.2.1 Chloropolyethylene (CM) and chlorosulfonyl polyethylene (CSM)
– Hydrochloric acid (CAS 7647.01.0)
— 1-Chloro-4-(1-chloroethenyl)-cyclohexene (CAS 13547-06-3)
8.5.3 Isobutene-Isoprene rubber (IIR), chlorinated Ilk (CUR) and broininated hR (Bilk)
— hsobutylene (CAS 115-11-7)
— t)iisobutylene or 2,4,4-tnmethyl-1-pentene (CAS 107-39-1)
— Triisobutylene or 2-methylpropane (CAS 7756-94-7)
8.5.4 Natural rubber (NR) or synthetic isoprene rubber (1k)
— Isoprene (CAS 78.79-5)
Isomers of the limonene:
— 1-Methyl-5-(1-methylethenyl)-cyclohexene (CAS 13898-73-2)
— 1-Methyl.4-(1-methylethenyl)-cyciohexenc (CAS 138.86-3)
8.5.5 Acrylonltrlle-butadlene rubber (NI3R), hydrogenated NIIR (HNHR) and carboxylatcd NI1R (XNBR)
8.5.5.1 NBR and XNBR
— 1,3-Butadiene (CAS 106-99.0)
— 4-Ethenylcyclohexene or 4-Vinyl-1-cyclohexene (CAS 100-40-3)
— 2-Propenenitrile or Acryionitrile (CAS 107-13-1)
8.5.5.2 HNBR
— 2-Propenenitrile or Acrylonitrile (CAS 107-13-1)
— Hexanenitrile or Capronitrile (CAS 628-73-9)
8.5.6 Styrene-hutadiene rubber (SBR)
— 1,3-Butadiene (CAS 106-99-0)
— 4-Ethenylcyclohexene or 4-Vinyl-1-cyclohexene (CAS 100-40-3)
— Ethenylbenzene or Styrene (CAS 100-42-5)
in case of butadiene-alpha-methyistyrene copolymers, there is a strong peak of aipha-methyistyrene or
isupropcnylbi’nzene (CAS 98-83 -9).
9 Test report
The test report shall Include the following particulars:
a) sample details: a lull description of the sample;
b) test method:
— a relerence to this international Standard. (i.e. ISO 17257:2013);
— characteristics olthe column, if necessary thermal program and spectral condition:
— identification of the pyrolyser GC-MS equipment used.