Rancimat Practice Rancimat Practice

Principle of Rancimat methodPrinciple of Rancimat method

air inletmeasuring vessel

air inlet

conductivity cellreaction vessel

conductivity cell

sampleabsorption solution

heating block (e.g. 120°C)

(water)

Preparing a determination – reaction vessel

f l bl h f l• 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 immediatelyafter weighing the sample within a few minute.after weighing the sample within a few minute.

•When the sample is placed in the heating block in take approx. 10 -20 Secondbefore the gas flow in the measuring vessel.

S l i li id lSample size – liquid sample

• For liquid samples like q psunflower oil, FAME

• For solid samples that melt like margarine melt like margarine

Instrument cover

Insulating layerMaximumMaximum

A 12 LApprox. 12 mL

Heating blockMinimumMinimum

Approx. 2 mLHeating block Approx. 2 mL

S l i lid lSample size – solid sample

• For solid samples like nuts, PVC

Instrument cover

Insulating layer

Heating blockMaximumMaximum

Appro 0 5 gHeating block Approx. 0.5 g

Air inlet tubeAir inlet tube

With foam barrier Without foam barrierWith foam barrierok

Without foam barrierok not ok

F b i iti iFoam barrier – positioning• Glass fiber reinforced

polypropylene• Solvent resistant

Temperature resistantTemperature resistant120 – 130 °C

MaximumMaximum

Heating block

Preparing a determination – measuring vessel

b i l iAir supplyok

• Absorption solution• 50 – 60 mL deionized

water

Air supplynot ok

atelast for approx. 3 days

• Conductivity < 5 µS/cm

Preparing a determination – method settings

• Important parametersparameters

• Temperature• Temperature• Delta T• Gas flow• 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 Gas inlet tubes for oils (148 mm)• 6.2418.100 Gas inlet tubes for oils (148 mm)• 6.1428.100 Polycarbonate measuring vessels• 6.1816.010 Silicone tubingsg

• Method parameters• Temperature: 120°C• Sample amount: 3 g• Air flow: 20 L/h• Water amount: 60 mL• Water amount: 60 mL

• Evaluation• Automatic (2nd 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 ± 0 2 5 ± 0 2 g• Sample amount: 2.5 ± 0.2 … 5 ± 0.2 g• Air flow: 9 L/h• Water amount: 50 mL

• ISO 6886 «Animal and vegetable fats and oils –d t i ti f id ti t bilit ( l t d determination of oxidation stability (accelerated oxidation test)»

• Method parametersp• Temperature: 100°C• Sample amount: 3 ± 0.01 g• Air flow: 10 L/h• Water amount: 50 mL

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

Cleaning procedure – step 2Rinse with deionized Brush with acetone or wateracetone/ethanol or 2-

propanol

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 hoursHeat to 80 C for 2 hours

Oxidation stability of FAME (biodiesel)

• EN 14112 «Fatty acid methyl esters (FAME) – Determination of

• oxidation stability (accelerated oxidation test)»y ( )• Hardware

• 6.1429.040 Short reaction vessels (150 mm)• 6.2418.100 Gas inlet tubes for oils (148 mm)6.2418.100 Gas inlet tubes for oils (148 mm)• 6.1428.030 Glass measuring vessels• 6.1839.000 IsoVersinic tubings

• Method parameters• Method parameters• Temperature: 110°C• Sample amount: 3 ± 0.01 g

Air flow: 10 L/h• Air flow: 10 L/h• Water amount: 50 mL

• Evaluationi (2 d d i i )• Automatic (2nd derivative)

• 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

l t d id ti t t• accelerated oxidation test»• 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 gp g• Air flow: 10 L/h• Water amount: 60 mL

• EvaluationEvaluation• Automatic (2nd derivative), if possible• Manual (tangent method)

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

Cleaning procedure – step 2Rinse with deionized Brush with acetone or wateracetone/ethanol or 2-

propanol

Cleaning procedure – step 3

• Heat to 80°C for 2 hoursHeat to 80 C for 2 hours

Mi llMiscellaneous

•Dust filterDust filter

new still ok replace

•Molecular sieve

new still ok replace

Regenerate weekly in caseof continous use