measuring vessel air inlet conductivity cell reaction vessel sample absorption solution (water) heating block (e.g. 120 C)

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Transcription:

Rancimat Practice

Principle of Rancimat method air inlet measuring vessel reaction vessel conductivity cell sample heating block (e.g. 120 C) absorption solution (water)

Preparing a determination reaction vessel Before use vessel was blown out a sharp steam of nitrogen to remove particles The reaction vessel cover with the gas inlet tube to be placed immediately after weighing the sample within a few minute. When the sample is placed in the heating block in take approx. 10-20 Second before the gas flow in the measuring vessel.

S Sample l size i liquid li id sample l For liquid q samples p like sunflower oil, FAME For solid samples that melt like margarine Instrument cover Insulating layer Maximum A Approx. 12 ml L Minimum Heating block Approx. 2 ml

Sample size solid sample For solid samples like nuts, PVC Instrument cover Insulating layer Heating block Maximum Approx. 05g 0.5

Air inlet tube With foam barrier ok Without foam barrier ok not ok

Foam barrier positioning i Glass fiber reinforced polypropylene Solvent resistant Temperature resistant 120 130 C Maximum Heating block

Preparing a determination measuring vessel Air supply ok Air supply not ok Absorption solution 50 60 ml deionized water last for approx. 3 days Conductivity < 5 µs/cm

Preparing a determination method settings Important parameters Temperature Delta T Gas flow Stop criteria

Oxidation stability of natural fats and oils Standard Rancimat settings Hardware 6.1429.040 Short reaction vessels (150 mm) 6.2418.100 100 Gas inlet tubes for oils (148 mm) 6.1428.100 Polycarbonate measuring vessels 6.1816.010 Silicone tubings Method parameters Temperature: 120 C Sample amount: 3 g Air flow: 20 L/h Water amount: 60 ml Evaluation Automatic (2 nd derivative) Optional: Manual (tangent method)

Oxidation stability of natural fats and oils AOCS Method Cd 12b-92 «Oil Stability Index (OSI)» Method parameters Temperature: 100, 110, 120, 130 and 140 C Sample amount: 2.5 ± 02 0.2 5 ± 02 0.2 g Air flow: 9 L/h Water amount: 50 ml ISO 6886 «Animal and vegetable fats and oils determination ti of oxidation stability (accelerated oxidation test)» Method parameters Temperature: 100 C Sample amount: 3 ± 0.01 g Air flow: 10 L/h Water amount: 50 ml

Cleaning procedure step 1 Brush with hot water and dish washing detergent Rinse with deionized water

Cleaning procedure step 2 Brush with acetone or acetone/ethanol or 2- propanol Rinse with deionized water

Cleaning procedure step 2 for polycarbonate measuring vessel Brush with ethanol or 2-propanol Do not use acetone!

Cleaning procedure step 3 Heat to 80 C for 2 hours

Oxidation stability of FAME (biodiesel) EN 14112 «Fatty acid methyl esters (FAME) Determination of oxidation stability y( (accelerated oxidation test)» Hardware 6.1429.040 Short reaction vessels (150 mm) 6.2418.100 Gas inlet tubes for oils (148 mm) 6.1428.030 Glass measuring vessels 6.1839.000 IsoVersinic tubings Method parameters Temperature: 110 C Sample amount: 3 ± 0.01 g Air flow: 10 L/h Water amount: 50 ml Evaluation Automatic (2 nd derivative) i Manual (tangent method)

Oxidation stability of FAME (biodiesel) EN 15751 «Fatty acid methyl esters (FAME) fuel and blends with diesel fuel Determination of oxidation stability by accelerated oxidation test» t Hardware 6.1429.050 Long reaction vessels (250 mm) 6.2418.130 Gas inlet tubes for diesel (248 mm) 6.1428.030 Glass measuring vessels 6.1839.000 IsoVersinic tubings Method parameters Temperature: 110 C Sample amount: 7.5 ± 0.1 g Air flow: 10 L/h Water amount: 60 ml Evaluation Automatic (2 nd derivative), if possible Manual (tangent method)

Cleaning procedure step 1 Brush with hot water and dish washing detergent Rinse with deionized water

Cleaning procedure step 2 Brush with acetone or acetone/ethanol or 2- propanol Rinse with deionized water

Cleaning procedure step 3 Heat to 80 C for 2 hours

Miscellaneous Dust filter Molecular sieve new still ok replace Regenerate weekly in case of continous use