ML OXIPRES INSTRUCTION MANUAL

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1 ML OXIPRES INSTRUCTION MNUL Version xel Kiers Vej Højbjerg - Denmark MIKROL RHUS /S Tlph: Fax: ml@mikrolab.dk

2 INDEX WRNING... page 2 DESCRIPTION... page 3 INSTLLTION... page 4 FUNCTIONS... page 5 PROCEDURE... page 6 EVLUTION OF RESULTS... page 8 CLENING... page 9 CONTROL... page 9 CLIRTION... page 10 LEKS... page 14 CCESSORIES and SPRE PRTS... page 15 Page 1

3 W R N I N G THE OXIPRES IS MODIFICTION OF THE OM METHOD USED FOR TESTING THE EFFICIENCY OF NTIOXIDNTS ON HETEROGENOUS PRODUCTS CONTINING OIL ND FTS. THE OXIPRES HS NOT EEN DEVELOPED FOR TESTING PRODUCTS POSING DIRECT RISK OF EXPLOSION DURING THE TEST. IT IS RECOMMENDED THT THE CYLINDER PRESSURE REGULTOR OR THE FILLING SYSTEM MUST HS SFETY VLVE WHICH OPENS T MX. 100 PSIG (7 R) SO THE PRESSURE VESSEL CNNOT E OVERFILLED. THE ML FILLING STTION HS SFETY VLVE WHICH OPENS T 10 R. THE MXIMUM WORKING TEMPERTURE FOR THE PRESSURE VESSEL IS 150 o C. THE PRESSURE VESSEL SHOULD NOT E OPENED EFORE IT HS RECHED MIENT TEMPERTURE. THE PRESSURE VESSEL MUST E CONTROLLED ON REGULR SIS. IF DMGE OR CORROSION PPERS THE PRESSURE VESSEL SHOULD E RETURNED TO MIKROL RHUS FOR REPIR. TOUCHING THE HETER LOCK DURING OPERTION COULD CUSE URN. LETHL VOLTGE EXISTS INSIDE THE INSTRUMENT. REMOVE THE POWER CORD FROM THE POWER SOURCE EFORE OPENING THE INSTRUMENT. Page 2

4 DESCRIPTION The ML OXIPRES is designed to monitor the oxidation of oil and fat in heterogenous products. It can also be used for samples of oil and fat. The measurement is based on the consumption of oxygen at elevated temperature and pressure. For safety the block-heater has a temperature cut-off acting at approx. 160 o C. If you have samples of oil and fat with no water content the ML OXIDOGRPH can also be used. Consumption of oxygen results in a pressure drop which is measured by means of pressure transducers. The samples are heated to accelerate the process and shorten the analysis time. 2 samples can be run at the same time in a unit and the pressure signal is sent to a PC. complete 2-positions OXIPRES consists of: 1 Control unit with temperature control and pressure measuring system with digital displays 1 2-position block heater (oven) 2 Pressure vessels with valve, stainless steel 1 Holder for pressure vessels for block heater 4 Glass reaction vessels 2 O-ring seals 1 Suction lifter 1 Rack for 6 glass reactions vessels 1 Cleaning rod for the pressure vessel 1 Coupling for charcoal filter 1 Charcoal filter, odour trap 1 Power cord 1 Manual Options: Paralog software (requires US-converter incl. cables) US-converter incl. cables Filling station with selector valve (FILL/VENT) Holding rack with wrench (for tightening the pressure vessel) Calibration kit Page 3

5 INSTLLTION Electric ssure that the mains voltage is equivalent to the voltage specified at the instrument. The voltage (230/115V C) can be changed on the control unit and oven unit. It is important that the instrument is connected to earth as a safety precaution and to give stable conditions. Connect the power cord from the block heater (oven) to the outlet at the rear of the control unit (Pt-100). Connect the block heater temperature sensor cable to the rear of the control unit. Connect the pressure transducer cables at the rear of the control unit to the corresponding pressure vessels which are marked with and. If you have more than one OXIPRES the control units can be marked 1, 2 and 3. (The small white square on the font is intended for this mark). In case of several units please be aware of the power consumption. More than 3 units should not be supplied from the same mains outlet. If you have electrical problems you can use a 3-phase outlet and use one phase per unit. Connect the control unit to the mains with the power cord. (LIVE = brown, NEUTRL = blue and ERTH = yellow/green). Signal Connect the signal output at the rear of the control unit to the US-converter. Connect the US-converter to a PC. Oxygen Mount the cylinder pressure regulator on the oxygen cylinder. Use a pressure regulator with 7 bar outlet pressure (100 psig). The filling station has a safety valve installed that opens at 10 bars. Filling station Connect the left valve port (FILL) to the pressure regulator. The right port of the valve is outlet to atmosphere (VENT). The quick connect couplings at the filling station have automatic shut-off when the filling tube is disconnected. Use the supplied tubing (or 1/8" SS-tubing) for filling the pressure vessels. DO NOT use rubber tubing or plastic tubing containing plasticizers. If the samples give off odour when the pressure vessel is vented connect the vent port to the odour trap (charcoal filter) or to a piece of tubing which leads into an exhaust system. Top holder Mount the supplied top holder on the oven with the nut supplied (see picture on front page). When not in use, the top of the pressure vessels can be placed in the holder. Page 4

6 FUNCTIONS POWER ON/OFF FUSES Situated at the back to the right. Situated at the back. TEMP MODE SWITCH OFF The heater in the block-heater is OFF. ON The heater in the block-heater is ON. The display shows the block temperature SET The temperature is set by means of the pot.meter. DISPLYS: TEMPERTURE Displays the block temperature. & Displays the pressure in the pressure vessels TEMPERTURE PRESSURE oxipres OFF RED 4.84 oxipres SET oxipres oxipres S/N Power IN S S Power Oven Power in US Oven 3 Power Pt S S Oven Power in US OFF S 1 Power in OUT Power ON S 6 US S Oven Power in S US PC (US) (Master Unit) US Convertor Pt-100 temperature sensor (block heater) Connection to pressure sensor on pressure vessel Connection to pressure sensor on pressure vessel In case of more units, the master unit is no.1 from which the output signal is taken. If stacked unit 2 is placed on top of unit 1, and unit 3 is placed on top of unit 2. Page 5

7 PROCEDURE Check If any of the samples are able to form an explosive mixture with oxygen at the test temperature, use eye and face protection while performing the experiment. Inspect the pressure vessel(s): 1. To see if it is clean. 2. Control that the O-ring seal is clean and undamaged. 3. Check that the sealing rim on the lid is free of scratches. N.: Never place the pressure vessel lid on a hard surface that could damage the sealing surface. lso be careful that the threads on the pressure vessel are not damaged. CYLINDER PRESSURE REGULTOR 1/8 " o.d. SS end VLVE TD PRESSURE TRNSDUCER 4 mm o.d. tubing QC REGULTOR OUTLET VLVE QUICK CONNECT STEM FILLER ROD OXYGEN TO OM TO OM CLOSURE RING O-RING QC QC SV OFF OXYGEN VENT FILL VENT Pressure Vessel VLVE FILLING STTION FILLING STTION Oxifill2a Page 6

8 Procedure 1. Choose a suitable oxidation temperature (e.g. 80 o C). Turn on the heater 20 minutes before the start of the experiment. 2. Weigh a suitable amount of sample in each glass vessel. (n amount containing 3-5 g fat will often give a reasonable result). Place the glass cover on top of the vessel. 3. Place the glass vessel in the pressure vessel. 4. Make sure that the O-ring and the groove are clean. Mount the top of the pressure vessel and tighten the closure by hand. The holding rack (optional) includes a wrench which makes tightening easier. Do not use excessive force. 5. Connect the pressure vessel(s) to the filling station. 6. a. Close the valve on the filling station (handle in vertical position). b. Close the regulator outlet valve. c. Open the main cylinder valve (slowly). d. djust the outlet pressure at the regulator to 5 bar (70 psig). e. Open the pressure vessel valve(s). 7. a. Open the regulator outlet valve. b. Turn the filling station valve to FILL c. To flush the pressure vessel for atmospheric air turn the valve to VENT. d. To repeat flushing repeat b and c. (Flushing 3 times will bring the nitrogen content below 1%). 8. Now fill the pressure vessel with oxygen (FILL). Using the cylinder pressure control try to hit 5 bar (70 psig) or lower if you want to use another pressure in your experiment. Read the pressure vessel pressure at the displays on the control unit. 9. Close the filling station valve (OFF) and then close the pressure vessel valves. 10. Watch the pressure for a few minutes to see if the pressure vessels have been tightened properly. 11. If tight turn the filling station valve to (VENT) and disconnect the filling tubes from the pressure vessels. 12. Place the pressure vessels in the block heater and start the test. 13. Remember to shut off the cylinder main valve. 14. fter the test the valve is opened. To reduce possible smell the venting can be done through a odour trap (charcoal filter) or in a fume cupboard. Page 7

9 EVLUTION OF RESULTS s a result of the consumption of oxygen the pressure in the bombs will drop. (t the beginning the pressure will rise due to the heating). The signals from the pressure transducers are shown on the displays. The signals are recorded as a function of time. trace could look like this: The samples are characterized by the induction period. The induction period (IP) can be found as follows: Draw the tangents T1 and T2 to the curve. The time from STRT to the intersection is the IP. The STRT is when the pressure vessel is placed in the block heater. The induction period will then be the time elapsed between placing the pressure vessel in the block heater and the break-point at a given temperature (e.g. 80 o C). Page 8

10 CLENING Cleaning of glassware: Pour out the sample and wipe the glassware clean with tissue. Remove residuals with water and alkaline soap (harmful to the eyes and to the mucous membranes). Rinse with water and finally with demineralized water. Dry at max. 80 o C. The pressure vessel can be cleaned in the same way. If the heater block should require cleaning wait until it is cold and clean it with paper tissue and demineralized water. (Do not use organic solvents, tap water or soaps). The stem of the pressure vessel can be cleaned with the supplied cleaning rod after the filler rod is removed. Use a coin to loosen the filler rod. felt disc is placed at the end of the cleaning rod. The felt disc is a caliber 0.45 rifle cleaner disc and extras can possibly be bought locally. Use a detergent and flush with demineralized water. The stem can be blown dry with air. CONTROL The experimental variation from sample hole to sample hole can be tested by running the same sample in both pressure vessels in one experiment. To check if the system is tight fill the pressure vessel with oxygen or air to 5 bar (70 psig). The pressure should not drop more than 0,2 bar (3 psig) during 24 hours after equilibration. If the test fails check (and replace) the O-ring. Page 9

11 OXIPRES CLIRTION using Calibration kit ML The calibration kit consist of a: air hose pressure gauge screwdriver test connector voltmeter test leads 3 test plugs,100.0, and Ohms CLIRTION PROCEDURE Pressure on circuit bord Page 10

12 To calibrate the control unit you need a pressure gauge, male test connector, red and black test leads, a voltmeter, and a screwdriver (trimmer). ll parts are included in the calibration kit, ML Preparation of the control unit. 1. Connect the pressure vessels to the control unit. 2. Remove the cover of the housing. CUTION: MINS VOLTGE IS PRESENT. 3. Turn on the Oxipres. Wait 20 minutes to stabilize. Zero Calibration (without pressure, 0 bar): 4. Connect the test connector to the socket marked OUT. Set the voltmeter to measure 2000 mv DC. 5. On the test connector, set the switch to. 6. djust the potentiometer P2 until voltmeter reads 0 mv. 7. On the test connector, set the switch to. 8. djust the potentiometer P1 until voltmeter reads 0 mv. Span Calibration (with pressure, 5 bar): Install the pressure gauge in series with one of the pressure vessels (as shown). Fill the pressure vessels to 5 bar. Make sure there are no leaks in the pressure vessels. 9. On the test connector, set the switch to. 10. djust the potentiometer P4 until voltmeter reads 1250 mv. 11. On the test connector, set the switch to. 12. djust the potentiometer P3 until voltmeter reads 1250 mv. Calibration of the pressure read circuit: 13. djust the potentiometer P9 on the temperature board until the pressure display shows 5.00 bar. Find the potentiometer on the picture on next page. 14. djust the potentiometer P8 on the temperature board until the pressure display shows 5.00 bar. Find the potentiometer on the picture on next page. Page 11

13 ssembly of the control unit: 15. Mount the cover on the control unit. CLIRTION PROCEDURE -Temperature on circuit board To calibrate the control unit you need 3 test plugs/resistors, a voltmeter and a screwdriver (trimmer). The value on the resistors must be 100.0, and Ohms. ll parts are included in the calibration kit, ML Preparation of the control unit: 1. Disconnect the wires from the oven to the control unit. 2. Remove the cover on the control unit. CUTION: MINS VOLTGE IS PRESENT. 3. Turn on the Oxipres. Wait 20 minutes to stabilize the electronic. Calibrate measuring circuit: 4. Connect the test connector to the socket marked OUT. Set the voltmeter to measure 20 V DC. 5. On the test connector, set the switch to Temp. 6. Place the Ohm test plug in the Pt-100 connector. 7. djust potentiometer P2 until voltmeter reads 0.00 V. 8. Place the Ohm test plug in the Pt-100 connector. 9. djust potentiometer P4 until voltmeter reads 1.40 V. 10. Place the Ohm test plug in the Pt-100 connector. 11. djust potentiometer P3 until voltmeter reads 4.00 V. 12. Repeat step 6 to 11 until no further adjustment is required. Page 12

14 Calibrate the temperature read circuit and the setting circuit: 13. Place the Ohm test plug in the Pt-100 connector. 14. djust potentiometer P10 until display reads is C. 15. Press and hold the SET-switch and turn the SET-knob CW until LED D3 (yellow) lights continually. 16. Press and hold the SET-switch and turn the SET-knob CCW until LED D3 goes from blinking to off. 17. Press and hold the SET-switch and adjust potmeter P7, until display reads C. 18. Turn the SET-knob to max (CW). 19. Press and hold the SET-switch and adjust potmeter P6, until display reads C. 20. Turn the SET-knob to min (CCW). 21. Press and hold the SET-switch and adjust potmeter P5, until display reads 25.0 C. ssembly of the control unit: 22. Mount the cover on the control unit. 23. Connect the wires from the oven to the control unit. 24. Check temperature on the oven to match with the control unit. djust compliance between Read and Set temperature readings on the display Let the oven heat up to the most often used temperature and give it time to stabilize. Toggle the switch on the front of the Oxidograph between Read and Set, while adjusting the potentiometer P7, until the values on the display are the same. Page 13

15 LEKS When you have a leak the pressure will drop unexpectedly (red graph): Fig. 1 Fig. 2 Fig. 3 The O-ring, groove and sealing rim must be clean and free of scratches (fig. 1). The gasket for the pressure transducer is a possibility (almost never) (fig. 2). The soft seal at the valve stem may be damaged (fig. 3). Unscrew the valve handle for inspection. The main cause for leak is the O-ring or small particles in the sealing area. Some leaks can be detected before you start the run: When you have filled the pressure vessel to the starting pressure (5 bar) leave it on the table for some time and watch the pressure. You can do that while you fill in your group and sample data. You can also just fill the pressure vessel to 5 bar - create a test sample in Paralog -and collect the data over a certain time. Then you get a documentation. Page 14

16 CCESSORIES ND SPRE PRTS ML ML ML ML ML ML ML ML ML ML ML ML ML ML ML ML ML ML ML ML ML Control unit for 2 samples Calibration kit for pressure and temperature Power and signal cable links (for 6 positions 2 sets are required) lock heater for 2 samples Pressure vessel with pressure transducer Cleaning rod for pressure vessel incl. 20 cleaning discs Coupling for charcoal filter Charcoal filter, odour trap TD-tupe adaptor O-ring Filling station, 2-pos. incl. tubing Filling station, 6-pos. incl. tubing Filling tube station to vessel Filling tube supply to station Holding rack, 2 pos. + wrench Reaction vessel (D525), glass, with 125 ml with cover Cover for reaction vessel Reaction vessel U-shaped Lid for reaction vessel U-shaped Suction lifter for lid Rack for 6 reaction vessels ML PRLOG TM software ver. 3 ML US-converter incl. cables (ML /ML ) ML Signal cable (1-3 units to one US-converter) ML Signal cable (US-converter to PC) Page 15

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