Bohlin. Accessories manual. Malvern. Gemini & CVO

Transcription

1 Bohlin Gemini & CVO Accessories manual Malvern

2

3 Gemini & CVO Rheometers Accessories Guide MAN0432 Issue 1.0 November 2010

4 Copyright Malvern Instruments Ltd Malvern Instruments makes every effort to ensure that this document is correct. However, due to Malvern Instruments policy of continual product development we are unable to guarantee the accuracy of this, or any other document after the date of publication. We therefore disclaim all liability for any changes, errors or omissions after the date of publication. No reproduction or transmission of any part of this publication is allowed without the express written permission of Malvern Instruments Ltd. Head office: Malvern Instruments Ltd. Enigma Business Park, Grovewood Road, Malvern, Worcestershire WR14 1XZ United Kingdom. Tel + [44] (0) Fax + [44] (0) Windows 2000 and XP are registered trademarks of the Microsoft Corporation. Printed in England

5 Table of Contents Introduction to this manual Introduction Health and Safety Assumed information Where to get help Geometries Introduction Geometry selection Cone and plate measuring systems Parallel plate measuring systems Coaxial cylinders Double gap Other measuring systems Temperature control units Introduction Temperature controllers overview Switching between temperature control options Peltier Plate and Cylinders Introduction Connecting the Peltier plate system Peltier plate geometries Using Peltier cylinders Peltier geometries Peltier cylinder specifications Peltier plate specifications Making measurements at the temperature limits Peltier plate and cylinder problems Gemini & CVO Rheometers Page 1

6 Table of Contents Gemini & CVO Rheometers Extended Temperature Cell (ETC) Introduction Site requirements First-time installation Upper geometry holder Operational Considerations Troubleshooting Specification for ETC Extended Temperature Option (ETO) What is the ETO? The Melts Oven The Melts Oven Page 2 MAN 0432

7 1 Introduction to this manual Introduction This manual covers the operation and maintenance of the accessories designed for use with the Bohlin Gemini and CVO rheometers from Malvern Instruments. The aims of this manual are to: Provide an overview of the geometries available for use with the rheometer. Provide details on the differences between each of the temperature controllers. Explain the overall process of how to connect and disconnect temperature controllers to the instrument. Give troubleshooting advice. Explain Health and Safety issues relating to each accessory. Health and Safety Users must read the Health and Safety information in Appendix B of the User Manual before operating the instrument. Additionally, if using the Low Temperature Unit (LTU) option in conjunction with the Extended Temperature Cell (ETC), also read the Liquid Nitrogen Safety Guide. Assumed information Naming convention The Gemini or CVO rheometer is often referred to as the instrument. The combination of the rheometer, computer and software is referred to as the system. Gemini & CVO Rheometers Page 1-1

8 1 Chapter 1 Menu commands Introduction to this manual Menu commands in the software are always shown in bold text in this form: main menu-menu item-submenu item. For example, the command Tools-Options refers to selecting the Options command from the Tools menu. Where to get help Manuals and online help The primary source of information on the Gemini and CVO rheometer system is the Bohlin Gemini & CVO Rheometers User Manual. In addition the software has online help which gives detailed information. Each dialog within the software has a Help button giving information specific to that dialog. Help desk All queries regarding the system should initially be directed to the local Malvern Instruments representative. Please quote the following information: Model and serial number of the instrument located on its back panel. The software version. To find this choose, Help-About from within the software. Contact the United Kingdom help desk if the local Malvern Instruments representative is not available. Its direct line is +44 (0) Its address is helpdesk@malvern.com. Note This help line is primarily English speaking. Remote support Malvern Instruments offers a remote support service, delivered by an Internet connection which offers fast and efficient fault diagnosis, reduced downtime and costs. On-line user training is also available, plus software updates. A high speed Internet connection is recommended for making use of this facility. Page 1-2 MAN 0432

9 Introduction to this manual Chapter 1 Malvern Website - The Malvern website offers a comprehensive range of materials characterisation resources for use by customers 24 hours a day, seven days a week. Resources include software downloads, frequently asked questions, a knowledge base and application notes, plus information on other materials characterisation solutions that Malvern can provide. Gemini & CVO Rheometers Page 1-3

10 Chapter 1 Introduction to this manual Page 1-4 MAN 0432

11 2 Geometries Introduction The following chapter provides information about the more common geometries available for the Gemini and CVO rheometers: Cone and Plate Parallel Plate Coaxial Cylinders (DIN) Double Gap Tapered plugs Small Sample Cell Solids fixtures More details about the geometries designed for use with the peltier cylinders can be found in Chapter 4. Further information about geometries is also provided in the help system supplied with the Bohlin software. Additional specialist measuring systems are also available from Malvern Instruments - these are not documented in detail in this guide: Vane and paddle tool Serrated Plates Roughened Systems Solvent trap Rectangular torsion Fibre film fixture Gemini & CVO Rheometers Page 2-1

12 2 Chapter 2 Geometry selection Geometries The geometry used depends both on the intended application and the temperature controller. Refer to the table below for information about common pairings: Geometry Parallel plates Cone and plate Application Oscillation experiments, high shear rates with small gaps, samples with particles > 30μm Viscometry primarily (large cone for lower viscosity, smaller for higher viscosity samples) Temperature Controller Peltier plate and ETC Peltier plate and ETC Cup and bob Low viscosity samples Peltier cylinder Double gap Low viscosity fluids at Peltier cylinder low shear rates Solids fixtures (Rectangular torsion) Tapered plugs Measuring modulus of solid materials including polymers, glass and metals Characterisation at very high shear rates (e.g. pressure sensitive adhesives) ETC/LTU Peltier cylinder Small sample cell Low volume samples Peltier cylinder Vane and paddle Viscometry or oscillation on non-homogenous samples with large particles (e.g. slurries) and sensitive gel structures (e.g yoghurt) Peltier cylinder Roughened system/ serrated geometries Solvent trap Fibre film fixture measuring concentrated dispersions/emulsions where slippage can occur (e.g. tomato ketchup) Samples liable to evaporation Dynamic mechanical properties of fibres or films All systems All systems ETC/LTU Page 2-2 MAN 0432

13 Geometries Chapter 2 Cone and plate measuring systems The Cone and plate measuring system consists of a rotating upper Cone and a fixed lower plate with a sample contained between them. Since the shear stress is constant (within 0.3%) with radial position for Cones with a small Cone angle, the viscosity can be calculated directly from the experimental torque / speed relation (see A Basic Introduction to Rheology for more information). All Cones supplied by Malvern Instruments are truncated. Application materials include mobile liquids, suspensions, emulsions, dough and pastes. Notes Easy to clean. Easy to set the gap. Convenient for sample placement. Small sample volume required. Shear rate constant across the sample. High shear rates possible with small angle Cone. It is possible that particulate materials may jam in the gap at the cone truncation, leading to noisy data. To alleviate this, ensure that the fixed gap is around 10 times larger than the average particle size. CP 4º/40 CP 4º/20 CP 1º/40 CP 1º/20 Cone angle, a (º) C1 (Pa/Nm) C2 (1/rad) Gemini & CVO Rheometers Page 2-3

14 Chapter 2 Geometries CP 4º/40 CP 4º/20 CP 1º/40 CP 1º/20 C3 (mm) C4 (kgm 2 ) 2.6e e e e-07 C5 (mm) Truncation (mm) D1 (mm) D2 (mm) Material S. S. S. S. S. S. S. S. For other sizes of geometry, refer to the certificate supplied with the geometry. (S.S. = Stainless steel) Parallel plate measuring systems The parallel plate measuring system consists of a rotating upper plate and a fixed lower plate with a sample contained between them. The gap between the plates can be adjusted to meet the user s needs. Unlike the Cone and plate measuring systems, the shear rate is not constant with radial position, but varies from zero at the centre to a maximum at the edge. The induced shear rate is inversely proportional to the gap size. Application materials include mobile liquids, suspensions, emulsions, dough and pastes. Page 2-4 MAN 0432

15 Geometries Chapter 2 Notes Easy to clean. Easy to set the gap. Convenient sample placement. Small sample volume required. Particulate materials tolerable. High shear rates possible with small gap. Shear rate changes across the radius. PP 40 PP 20 C1 (Pa/Nm) C2 (1/rad) C3 (mm) 1 1 C4 (kgm 2 ) 4.1e e-07 C5 (mm) D1 (mm) D2 (mm) Material Stainless steel Stainless steel Note The C1 and C2 constants quoted above assume that the shear rate is taken at the ¾ plate diameter. Gemini & CVO Rheometers Page 2-5

16 Chapter 2 Geometries Coaxial cylinders The concentric cylinder measuring systems consist of a rotating bob (inner cylinder) located in a fixed cup (outer cylinder) with the sample contained in the annular gap between them. The concentric cylinder system has many applications in routine laboratory measurements. Application materials include mobile liquids and emulsions. Notes Particulate materials tolerable. Good repeatability. Not so critical on misalignment. Good temperature control. Longer cleaning process. Shear rate / stress vary slightly over the gap. C 8 C 14 C25 C1 (Pa/Nm) C2 (1/rad) C3 (mm) C4 (kgm 2 ) 5.4e e e-06 C5 (mm) D1 (mm) D2 (mm) H1 (mm) Page 2-6 MAN 0432

17 Geometries Chapter 2 C 8 C 14 C25 H2 (mm) a (º) Sample volume (ml) Bob Material Titanium Titanium Titanium Cup Material Stainless steel Stainless steel Stainless steel Note The figures given here relate to standard setups only, i.e. where the supplied cup and bob pair are used together. The shear rate and shear stress vary slightly over the gap. The C1 and C2 values listed refer to the average radius position. Double gap Double gap geometries are used to measure low viscosity fluids at low shear rates. At high shear rates a secondary flow is induced. The onset of this secondary flow depends on the viscosity of the sample and the gap (Taylor Vortex flow). The double gap measuring system consists of a hollow cylinder that is lowered into a cylindrical groove in the outer cylinder. The sample is contained in the double annular gap between them. Application materials include mobile liquids, suspensions and emulsions. Notes Particulate materials tolerable. Relatively large sample volume required. Gemini & CVO Rheometers Page 2-7

18 Chapter 2 Geometries Good repeatability. Shear rate / stress vary slightly over the gap. Not so easy to clean. DG 40/50 DG 24/27 C1 (Pa/Nm) C2 (1/rad) C3 (mm) 0 0 C4 (kgm 2 ) 2.6e e-06 C5 (mm) D1 (mm) D2 (mm) D3 (mm) D4 (mm) H (mm) Sample volume (ml) Bob Material Titanium Stainless steel Cup Material Stainless steel Stainless steel Note The shear rate and shear stress vary slightly over the gap. The C1 and C2 values given here refer to the average radius position. Page 2-8 MAN 0432

19 Geometries Chapter 2 Other measuring systems Tapered plugs The Tapered Plug set is a set of three tapered plugs and lower sample cup and is used to make very high shear rate measurements, above 10 5 s -1 to be achieved with a gap size of 10μm. Notes Easy to clean. Small sample volume. Very high shear rates possible. Maximum particle size less than gap / 10 Gap setting for tapered plugs 1. Place the lower cylinder into the rheometer. 2. Insert one of the tapered plugs (with the universal joint attached) into the chuck. 3. Set the gap to read 7000 (7mm) on the instrument and then press the Down button. Guide the plug into the cup. 4. Press and hold the GAP button until the Gap indicator starts to flash - gap capture mode. Using the Down arrow button, slowly lower the tapered plug into the cup. When it is at the bottom make sure the links are straight. 5. Press the Zero button. You have now set the zero position. 6. Set the required gap, either in the software or on the instrument panel. Gemini & CVO Rheometers Page 2-9

20 Chapter 2 Geometries 7. Lift the tapered plug a small distance. 8. Start the cylinder rotating and insert the sample. 9. Lower the tapered plug to the chosen gap. Small sample cell (Mooney Cell) The Mooney Cell is intended for use with low viscosity samples, where only a small amount of sample is available. A trapped air bubble at the base of the bob reduces end drag. Application materials include pharmaceutical and biomedical products. SSC 25 C1 (Pa/Nm) C2 (1/rad) C3 (mm) 0 C4 (kgm 2 ) 4.9e-06 C5 (mm) D1 (mm) 26.5 D2 (mm) 25 H (mm) 29 Sample volume (cc) 2.0 Bob Material Stainless steel Cup Material Stainless steel Page 2-10 MAN 0432

21 Geometries Chapter 2 Solids Fixtures The solids fixtures are ideal for measuring the torsional modulus properties of polymers, composites, glass and steel, etc. Properties such as glass transitions and rubbery transitions can be investigated for most materials. Results can be closely compared with those from a traditional DMA (DMTA) instrument. The measuring system consists of clamps to hold the top and bottom of the sample together with a bellows system to allow gentle sample tensioning. See Chapter 5 for more information on using this measuring system with the ETC or LTU. Notes Can measure a range of solids, from rubber to glass. Can measure thermal expansion of solids. Samples of very high modulus can be measured. Good repeatability. Flexible sample sizes. Good temperature control (-150 to 550ºC with the ETC/LTU). Gemini & CVO Rheometers Page 2-11

22 Chapter 2 Geometries Mooney Ewart Cell The Mooney Ewart Cell is intended for use with very low viscosity samples, and small sample volumes where high shear rates are required. The conical lower face of the bob creates a shearing surface. Vane tools Vane tools act as serrations, and help overcome slippage problems. Page 2-12 MAN 0432

23 Geometries Chapter 2 Roughened bobs A common problem when measuring concentrated suspensions is that instead of shearing in the normal laminar way, the sample starts to slip. The surface texture of roughened bobs helps to overcome this problem. See references to slippage in the application notes available from your Malvern Instruments representative. Solvent Trap The Solvent Trap provides a means of reducing the effect of solvent evaporation from the sample. A trap, which fits over the upper geometry, holds the solvent. This is then contained in the measuring system along with the sample, underneath the thermal enclosure, and so reduces the propensity of the solvent to evaporation. This image also shows a standard upper geometry and standard thermal enclosure. Gemini & CVO Rheometers Page 2-13

24 Chapter 2 Geometries Page 2-14 MAN 0432

25 3 Temperature control units Introduction Malvern Instruments produce a range of temperature controllers that are compatible with the Gemini and CVO instruments. This chapter provides an overview of these devices: Peltier Plate Peltier Cylinders Melts Oven Extended Temperature Cell (ETC) Extended Temperature Option (ETO) Each of the units is discussed in operational detail within its own chapter. Gemini & CVO Rheometers Page 3-1

26 3 Chapter 3 Temperature control units Temperature controllers overview The relative merits of each temperature controller are shown in the table below. Controller name Extended Temperature Option (ETO) -15ºC to 300ºC 30ºC / min heating and cooling (max) Melts Oven Ambient to 450ºC 60ºC / min max heating Extended Temperature Cell (ETC) and optional Low Temperature Unit (LTU) Ambient to 550 C (ETC) -150 C to 550 C (ETC and LTU) Peltier System -30ºC to 200ºC 60ºC heating & cooling (max) -30 C needs refrigerated coolant Advantages Provides extremely rapid temperature changes. Large temperature range. Can work with thermosets and other materials that cure. (Disposable option) High top end temperature, designed to minimise thermal gradients across the sample. Can work with thermosets and other materials that cure. (Option) Rapid temperature changes with excellent conductivity. Wide temperature range from -150 C (with LTU) to 550 C. Minimal thermal gradients within the sample. Provides extremely rapid temperature changes. Only requires a small flow of liquid to assist heat pump. Page 3-2 MAN 0432

27 Temperature control units Chapter 3 Installing temperature control units All temperature control units lock into the instrument s clamp in the same manner. The following process describes the installation of a temperature controller (the peltier plate). Removal is the reversal of this process. See the individual chapters concerning the temperature controllers for more specific information. Warning! Ensure that any previously installed temperature controller is at a safe temperature to handle before removal. 1. Press the UP arrow on the control panel to raise the measuring head to its upper stop. 2. Lift off the protective metal trim plate. 3. Press down on the metal clip at the front of the white cover and then slide the cover forward and upwards (at an angle of approximately 30º) to remove it ill 8562 Gemini & CVO Rheometers Page 3-3

28 Chapter 3 Temperature control units 4. Swing open the clamp arm and insert the device - be sure to locate the unit in the grooves: 5. Close the clamp around the temperature control unit and then tighten up the locking screw : 1 6. If installing a peltier plate or cylinder on the Gemini, connect the comms cable to the front 16 pin D-connector. 7. Depending on the temperature controller, a temperature probe and/or thermocouple may be integrated - these connect to the PT100 or TC-1/2 input on the back of the instrument respectively. 8. Refit the plastic cover and the metal trim plate. Page 3-4 MAN 0432

29 4 Peltier Plate and Cylinders Introduction The Plate and Cylinder Peltier systems allow rapid temperature control of samples. Using the principle of the Peltier heat pump, the sample can be heated or cooled rapidly to any temperature within the operating range of the unit. With the Gemini, the system consists of the Peltier unit, water circulator and interconnecting cables. The CVO adds an additional electronic drive unit (or peltier control box). A chilled water supply is also required if the Peltier is to be used at low temperatures (< -5 C). The flow of water provided by the circulator is used to allow the heat energy in the Peltier system to be dissipated. Connecting the Peltier plate system Connection process Use the following procedure to connect the peltier cylinder or plate to your instrument. 1. Ensure that the power supply to the instrument (and power to any existing temperature control box, if using a CVO) is turned off. 2. Disconnect all cables connecting currently installed temperature controllers from the instrument. On a Gemini this is likely to be just a single connection to the front of the unit from the temperature controller. 3. Refer to the process in Chapter 3 for details on how to remove a previously installed temperature control unit. 4. Fill the water bottle with distilled water / ethylene glycol solution (approx 0.5%). Gemini & CVO Rheometers Page 4-1

30 4 Chapter 4 Peltier Plate and Cylinders 5. Connect the water pipes to the push fit connectors on the water bottle and on the underside of the peltier unit. 6. Insert the peltier into the clamping ring and tighten it - see Chapter 3 for more information. The cables should lead out between the clamping ring and the base plate. The inlet pipe should lead out behind the front leg and the outlet pipe should lead out between the bib and the trim plate (there is a hole in the trim plate for this). 7. Now refer to the relevant cable connection for your instrument (below). After this, replace the plastic cover and trim plate - refer to Chapter 3 for more information on this process. CVO cable connection: Use the following procedure to make all cable connections to a CVO instrument. 1. Connect the cable terminating in a round plug to the PT-100 input on the rear of the instrument. 2. Connect the D plug from the Peltier unit to the Peltier Drive input on the back of the Peltier control box Connect the TCU cable from the control box to the TCU input on the back of the instrument. 4. Connect the power cables to the control box and water bottle. Page 4-2 MAN 0432

31 Peltier Plate and Cylinders Chapter 4 Gemini cable connection Use the following process to connect the cables to a Gemini instrument. 1. Connect the single communications cable from the bottom of the peltier unit to the D-connector on the front of the instrument. 2. Slide the connector lock to the right to lock the cable in place. Cooling fluid connection A flow of cooling fluid is required for the correct operation of the Peltier. The supply should have a minimum flow rate of 1 litre/min. The inlet connection to the Peltier system is the one at the underside of the unit. The outlet (return) is at the side. CVO connection Gemini connection Gemini & CVO Rheometers Page 4-3

32 Chapter 4 Peltier Plate and Cylinders Operating the Peltier system Having installed the Peltier system, switch on the instrument (and the Peltier electronics box if using a CVO). Ensure that water is flowing through the Peltier unit by removing the lid of the circulator bottle and visually checking the water flow. CVO only - Visual indicators on peltier control box The front of the Peltier electronics box is fitted with two LED indicators: 1 2 ill 8580 Illuminated to show power applied and unit functional. If the Peltier is operated without cooling, it may overheat and a trip will cause the unit to shut down. At this point, the red light will switch off. Indicates heating when active. Peltier plate geometries The Peltier plate system works in the same way as other Bohlin plate systems, the main advantage being the ability for rapid heating and cooling. A wide range of compatible cones and parallel plates are available. Choosing geometries Generally, the larger the plate/cone size, the lower the viscosity being measured. Very small diameter geometries such as an 8mm parallel plate are used for measuring solids and semi solids (up to G* of 10E6). Medium sized geometries such as 40mm cones and plates are used for measuring thick suspensions such as tomato Ketchup etc. Large geometries 50 to 60 mm in diameter are used to test low viscosity samples - to as low a viscosity as water. Page 4-4 MAN 0432

33 Peltier Plate and Cylinders Chapter 4 Using Peltier cylinders The following section provides more information on how to use Peltier cylinders with the rheometer. Peltier cylinders follow the same general principles as the Peltier plates described previously. It is assumed that the user has already connected the base unit to the instrument as previously described in the Peltier plate section. Fitting the Cup To fit the cup into the system, position it vertically and carefully push it down into the base unit. Note: Do not force the cup. If not aligned properly it will jam. Also, do not use excessive force. After the cup is inserted fully, rotate the cup until you feel a click. This will stop the cup from rotating during the test. A groove is marked on the upper flange of the cup. 1 Gemini & CVO Rheometers Page 4-5

34 Chapter 4 Peltier Plate and Cylinders Operating the Peltier cylinders To operate the system, the lower cup is inserted into the Peltier module and rotated in a horizontal plane until the locator ball locks it into place. After Zeroing the gap, the cylinders may be used in the same way as a standard C25 system. Gap Setting A tool is provided to set the gap for the C14, C25 and Double Gap systems. C14 and C25 1. Lift up the cup and position the gap set tool as shown in the image below Zero the instrument, the bob will zero on the base of the cup. 3. Remove the gap set tool and drop the cup into the system, making sure it is correctly seated. The gap is now set. A different tool is required for each system. Page 4-6 MAN 0432

35 Peltier Plate and Cylinders Chapter 4 Double Gap Geometry 1. Position the spacer coin on the top of the double gap insert as shown below. 2. Press Zero on the rheometer. 1 Making measurements at the temperature limits Testing at 180 C The peltier will reach 180 C more quickly if the water bottle is filled with hot water. Testing at sub ambient temperatures Using mains cold water will help when measuring at low temperatures. Make sure the water pipes are insulated to prevent heat loss. Use distilled water as hard water could cause limescale, which will block the heat exchanger. Testing below 0 C The peltier may require the circulating water to be cooled using a chiller unit. Contact your Malvern Instruments representative for details. Gemini & CVO Rheometers Page 4-7

36 Chapter 4 Peltier Plate and Cylinders Peltier cylinder geometries There are a wide range of measuring systems that can be used with the Peltier Cylinders. In general Cup and bob systems are typically used for viscometry testing, rather than oscillatory testing. The inertia of the bob is significant (in comparison with a plate or a cone), and will effect the oscillatory data at high frequencies. Din cup and bob geometries conform to DIN standard 53019, which describes a standard flow field for viscometry measurements. Use larger bobs for lower viscosity fluids. See the Accessories Guide for more information about geometries. Peltier plate and cylinder problems This section provides information to help users solve common problems with either the Peltier plate or cylinder. Refer to the Troubleshooting section in the User Manual for information on how to solve other common peltier problems. Error codes and solutions The Error Log is displayed automatically by the software whenever user intervention is required. Page 4-8 MAN 0432

37 Peltier Plate and Cylinders Chapter 4 Error codes are shown in the Error column and numbered between 0 and 999. Refer to the table below for more information on common errors. Error code Meaning 16 TC-1 failure 17 TC-2 failure This error is caused by a very high PT-100 resistance. Occurs if no PT-100 is connected. As above, but too low PT-100 resistence. The temperature card ADC converter input voltage is out of range. Could be caused by a bad sensor reading, incorrectly calibrated temperature board or malfunctioning system. Controller mode not implemented. The temperature you have requested is too low for the current temperature controller set-up. The temperature you have requested is too high for the current temperature controller set-up. A/D converter on the temperature board is over range. Possibly caused by a high PT-100 resistance or excessively high measured temperature. 30 Temperature board not calibrated 128 Illegal instrument type 129 Illegal TCU type Solution Check that PT-100 is connected. Try restarting the instrument. Check that PT-100 is connected. Try restarting the instrument. Switch off the instrument and peltier control box, leaving the water cooling switched on and allow the peltier to return to ambient before restarting. Change the test conditions to inside the correct range. Check the PT-100 and TC2 jumpers are in place, restart the instrument. Change the test conditions to inside the correct range. Check the PT-100 and TC2 jumpers are in place, restart the instrument. Switch off the instrument and peltier control box, leaving the water cooling switched on and allow the peltier to return to ambient before restarting. Check that the thermocouple jumper plug is in TC2, not TC1. Gemini & CVO Rheometers Page 4-9

38 Chapter 4 Peltier Plate and Cylinders Error code 130 Illegal HTC type Illegal instrument/tcu combination Illegal instrument/tcu combination 133 TCU not installed 134 HTC not installed Other error codes Meaning Various meanings Solution Check that the thermocouple jumper plug is in TC2, not TC1, and that the PT-100 is connected. Check that the thermocouple jumper plug is in TC2, not TC1, and that the PT-100 is connected. Try restarting the system, check that all the plugs are connected. If in doubt, contact your Malvern representative. These error messages relate to the temperature board and Peltier unit only. Details about error messages shown on the instrument s display panel and also advice notes given by the software can be found in the Troubleshooting section of the User Manual, or in the software help system. Page 4-10 MAN 0432

39 Peltier Plate and Cylinders Chapter 4 Common peltier plate/cylinder problems The unit will not heat or cool The unit will not heat or cool Gemini CVO Is the Peltier power box switched on? Yes No Is the red power indicator lit? No Switch on the power Yes Are all cables connected as described and properly triggered? No Check the mains fuse Yes Power down and restart the system Connect and tighten the cables Does the Peltier work now? No Contact your Malvern Bohlin representative Gemini & CVO Rheometers Page 4-11

40 Chapter 4 Peltier Plate and Cylinders The unit heats, but will not cool The Peltier heats, but will not cool Is the software communicating? Yes No Restart communications from Options -Instrument Serial Port Is water flowing through the Peltier? No Check the water level in the cooling bottle, refill if necessary. Raise the water bottle to lessen the head of water being pumped against Yes Is the water in the bottle warm? No Connect the Peltier unit to a cold tap (if available) to increase water flow Yes Refill the bottle with cold water and 0.5% Ethylene Glycol Is the Peltier cooling now? No Is the Peltier cooling now? No Contact your Malvern Bohlin representative Page 4-12 MAN 0432

41 Peltier Plate and Cylinders Chapter 4 Peltier plate specifications Temperature Operating range Stability Maximum Heating Rate Maximum Cooling rate Electrical power Mains supply Maximum power consumption Fuse -30 C to 200 C ± 0.1 C 60 C/min (range dependent) 30 C/min (range dependent) 110 / 220 volts AC ± 10% 120 Watts volts, 110 volts Peltier cylinder specifications Temperature Operating range Stability Maximum Heating Rate Maximum Cooling rate Electrical power Mains supply Maximum power consumption Fuse Ampage requirement -20 C to 180 C ± 0.1 C 30 C/min (range dependent) 20 C/min (range dependent) 110/220V switched (±10%) 120 Watts volts 110 volts Gemini & CVO Rheometers Page 4-13

42 Chapter 4 Peltier Plate and Cylinders Page 4-14 MAN 0432

43 5 Extended Temperature Cell (ETC) Introduction The Malvern Bohlin ETC is a forced gas oven that ensures rapid temperature changes with excellent conductivity and therefore minimal thermal gradients within the sample. The use of inert gas avoids sample degradation. A wide temperature range to 550 C is suitable for testing a variety of materials, including polymer melts and composites as well as solid samples, giving DMTA capability. To cool below ambient temperature, the ETC must also be fitted with the optional liquid nitrogen Low Temperature Unit (LTU). Warning! The ETC and LTU can become very HOT and very COLD in operation. Malvern Instruments recommend the use of suitable thermally insulated gloves for handling of this equipment at all times. Note If purchasing an ETC unit, contact Malvern Instruments initally for compatibility advice. Gemini & CVO Rheometers Page 5-1

44 5 Chapter 5 Site requirements Extended Temperature Cell (ETC) The ETC is initially installed and tested by a Malvern Instruments service engineer. The following information is provided for reference only, should the rheometer require re-location. The following services need to be present at the installation site: A supply of compressed, dry air. The compressor should be capable of delivering air pressure in the range of 5.0 to 10.0 bar (gauge) at a rate of 30 litres/ minute. A V AC mains outlet for the control box. Note Further items may be required when the unit is used with the Low Temperature Unit Option see Chapter 6. Page 5-2 MAN 0432

45 Extended Temperature Cell (ETC) Chapter 5 Hardware setup Note The ETC is set up initally by a Malvern Instruments service engineer. The following information is provided for reference. The following illustration is referred to throughout this section: ETC control box controlled by the software to provide air supply to the oven and give oven temperature feedback. ill 8565 Gemini & CVO Rheometers Page 5-3

46 Chapter 5 Extended Temperature Cell (ETC) Fan exhaust port ensure that enough air is allowed to freely circulate aroung this opening. TCU Cable communications cable connected to instrument. Air supply in provides an air supply from the double air regulator. Air hose supplies warm air from the control box to the oven. Oven thermally insulated unit that completely surrounds the sample measurement area. Oven cap release switch press down to remove the oven cap. When removed this provides access to the sample area. Replace the cap prior to measurement. Oven clamping ring provides a means of securing the oven into the Easy Swap clamping ring on the instrument. Blanking plug when removed, provides an input for the Low Temperature Unit option. Installing the oven onto the instrument 1. Find a suitable place to locate the ETC control box. The hose that connects the oven to the control box will limit the distance from the instrument to the control box. The oven mounts on and to the left of the instrument. This means that the control box must be placed to the left of or behind the instrument. 2. Check that the fan exhaust at the back of the control box is allowed enough space for the air to flow through, and that the hose to the oven has not been bent too sharply. 3. Remove the front closure from the oven by pressing the white switch to release the catch. 4. On the instrument, remove the bib and trim plate and then open the clamp. (See Chapter 3 for more information on this process.) 5. Insert the oven into the rheometer s clamp using one of the following methods: Partially open the clamp and locate the oven into the moving part of the clamp. Then swing the entire assembly (i.e. clamp arm and oven) into place or... Insert the unit into the main part of the open clamp first, and then close the clamp arm. Tighten the clamp lock once the oven is in position. Page 5-4 MAN 0432

47 Extended Temperature Cell (ETC) Chapter 5 6. Ensure that the oven is perpendicular to the front of the instrument, as shown in the photograph. 7. Fit the the specially shaped plastic cover (bib) supplied with the ETC to the rheometer, and then replace the trim plate on top of this. 8. Press and hold the up arrow key on the gap setting panel of the rheometer while powering it up to select the POS HI gap system mode, suitable for the longer ETC measuring systems. (Press and hold the down arrow key while powering up to reset to normal mode). Gemini & CVO Rheometers Page 5-5

48 Chapter 5 Extended Temperature Cell (ETC) Making connections 1. Connect the air supply to an air regulator as configured below - so that both the ETC and rheometer have an independently adjustable air flow. Other configurations are possible, including the use of a nitrogen supply to the ETC, which could be appropriate if testing samples prone to degredation in air. 2. Connect the mains cable from the control box to a wall outlet that is capable of supplying the required voltage and current. 3. Connect the ETC control cable from the rear of the instrument to the 9 pin D- sub connector at the back of the ETC control box (labelled TCU). Tighten the connector retaining screws. 4. Connect the thermocouple extension cable (a cable with a male 2-pin connector at each end) between TC1 on the instrument and the thermocouple connector at the back of the ETC control box (TC1). 5. If using a measuring system with an integral thermocouple, connect this to the TC2 input on the instrument. 6. Switch on the ETC control box. 7. Turn on the air to the air regulator and open the ETC air regulator. Set the ETC supply to 5.0 bar (gauge), using the valve on top of the regulator. 8. Turn on the power to the rheometer and computer, and then start the Bohlin software. 9. Check that the unit heats correctly when a manual temperature is set the meter on the front of the ETC control box indicates when power is being applied to the oven heater. Page 5-6 MAN 0432

49 Extended Temperature Cell (ETC) Chapter 5 Upper geometry holder The ETC requires the use of a special upper geometry holder. This section provides information on how to fit and remove this holder. The parts of the holder are shown in the illustration below: A 1 C B Shaft - pushes up into the rheometer chuck. Hex bolt - holds the upper geometry in place. Upper geometry - shorter stemmed than a regular geometry. To fit the upper geometry holder It is preferable to insert the upper geometry into the geometry holder when the holder is not yet installed in the Rheometer. 1. Use a 2.5mm hex key to loosen the bolt. 2. Insert a geometry into the holder and, whilst maintaining the pressure on the geometry, tighten the bolt. 3. Insert the geometry holder (with the geometry installed) into the chuck as with any standard geomery. 4. Load and trim the sample. 5. Slide the oven fully to the right -it will encase half of the geometry holder. 6. Fit the oven cap by pressing the white catch, then locating the cap in place on the oven and finally releasing the catch. ill 8064 Gemini & CVO Rheometers Page 5-7

50 Chapter 5 Extended Temperature Cell (ETC) To remove the upper geometry holder Warning! Take care when handling the measuring system - it may be hot. 1. Remove the oven cap by pressing the white release catch first. 2. Remove the complete upper measuring system assembly by removing the shaft from the rheometer chuck. Caution! Do not try to loosen the hex bolt while the assembly is in the rheometer chuck - it may damage the measuring system or even the rheometer itself. 3. Use a 2.5mm hex key to loosen the bolt. 4. This releases the upper geometry plate itself. Cured samples When disposable plates are used and the sample is cured after the test, use the following procedure. In this situation error message 8 (Normal Force overload) may be seen when driving the measuring system up. 1. Loosen the chuck as much as possible. 2. Press the Up button and undo the chuck as the bearing moves upwards. 3. Once the bearing is at the top stop and no longer connected to the upper geometry, undo the hex nut. 4. Remove the geometry stem. 5. Undo the hex nut for the lower geometry. 6. Remove the two plates together. Page 5-8 MAN 0432

51 Extended Temperature Cell (ETC) Chapter 5 Operational Considerations Safety The ETC contains two safety features: An inlet air pressure switch checks that the air pressure is above 4.0 bar (gauge). If the pressure drops below this limit the heater will be switched off to prevent it burning out. In this instance a warning message is displayed in the Bohlin software. If the door of the oven is removed the heater is switched off to reduce the risk of burns from hot air. Warning! Many parts inside the oven, including the measurement system, can become very hot after use - wear protective gloves and exercise caution when handling. Warning! Ensure that the ventilation around the unit and the fan exhaust is sufficient to remove any harmful vapours emerging from the sample. A carbon filter in the ETC will filter out some of these, but should not be seen as a substitute to proper ventilation. If necessary a vent hose can be connected to the fan outlet duct. Miscellaneous Always use a measuring system with a thermocouple to obtain the most accurate results. Non-thermocouple measuring systems will only measure and control temperatures based on the air stream reaching the sample - thus the actual sample temperature is likely to deviate from the set temperature. The rheometer determines its operating mode by examining which thermocouples are connected when powered up. Ensure that any thermocouple connections to the instrument are in place before switching it on. The TC1 input connection must be in place if the ETC is to be used. For accurate gap setting at high or low temperatures, pre-heat (or cool if using the LTU) the geometry before zeroing the gap. Use the Bohlin software to manually set the ETC s temperature to do this. Gemini & CVO Rheometers Page 5-9

52 Chapter 5 Extended Temperature Cell (ETC) If the ETC is to be regularly swapped with another temperature controller, the instrument should be switched into high mode before use, and back in to low mode after use. High mode is for use with long stemmed geometries, with the gap zeroing procedure starting at a higher position than in low mode. To switch into high mode switch the rheometer on whilst pressing the UP arrow on the control panel. The display should show, POS HI and then To switch into low mode, press the DOWN arrow on the gap panel whilst switching the instrument on - the display should show Use of Solids Strip Fixtures with the ETC To use the Solids Fixture with the ETC follow this procedure. 1. Fit the upper and lower fixtures and the ETC system onto the rheometer. 2. Switch on the instrument. Press and hold the UP arrow to initialise the instrument and place it into HI mode. 3. Fit the 32mm aluminium spacer into the lower fixture and press ZERO on the instrument control panel. 4. Cut the solid sample to approximately 10mm wide (up to 12mm) by 50mm long and fit into the appropriate thickness sample clamps (ie 0.3, 0.5, 1mm). Other sizes are available from Malvern Instruments if required. Additionally, it is possible to fit cylindrical samples into the solids fixture using the clamps or seated into the clamp holders, should the cylinder diameter be compatible. 5. In the software, choose Solids Fixture (S Fix) from the Measuring System selector and click Edit. 6. In the Edit Measuring System window, click the following button to display the Solid Fixture Calculation window: 7. Enter the dimensions of the sample between the clamps and then click the Calculate button. If standard sample clamps are used with a 50mm sample, this length will be 35mm. (It may be necessary to add a Solids Fixture measuring system to the list if none is present - refer to the software Help system for more information on this.) 8. The constants are now shown in a further window for information purposes. Click Close on this window, and then OK on the Solid Fixture Calculation window. The constants are now updated in the Edit Measuring System win- Page 5-10 MAN 0432

53 Extended Temperature Cell (ETC) Chapter 5 dow automatically. The C4 constant value should be entered manually and depends on the fixture size: Solids fixture size (mm) C4 inertia value (MI Kgm^2) E E Click OK on the Edit Measuring System window and then set the gap at 3mm. 10. Place the sample into the fixtures, gripping it in place tightly by means of the ring clamps. 11. In the Oscillation Parameters it is typical to use a very small strain (eg. 1e-5) and a large stress (eg. 1e3 Pa) initially. A small negative normal force, (eg. 5%) is set in Auto-tension. These factors may need to be optimised depending on the nature of the sample. 12. The default speed and number of iterations for gap setting are sufficient for a wide range of samples, but can be adjusted in Options - Auto-Gap Control - Auto-tension. 13. Set a temperature equilibrium time of at least 2 minutes in the test method, to allow the sample to tension before the oscillation test starts. Gemini & CVO Rheometers Page 5-11

54 Chapter 5 Extended Temperature Cell (ETC) Troubleshooting The unit will not heat. Check that the power switch to the ETC is on. If the red lamp on the front panel does not illuminate, check the mains fuse, which is accessible in the mains voltage connector at the back of the control box. Warning! Remove the mains cable before examining this fuse. Make sure that all cables have been connected as described. Check that the air supply to the ETC is turned on. Check that the oven s front casing has been fitted properly. The lights on the front casing should activate when the electrical connections to the casing have been connected correctly. Ensure that the air regulator has been set to the correct pressure (5.0 bar). Check the action of the pressure switch by bending the air hose so that the air is blocked off. The pressure switch in the control box will give an audible click when it goes on and off. Poor temperature stability. Check that the air supply to the air regulators is constant and free of large pressure fluctuations the pressure gauge of the ETC regulator should be perfectly stable. The air pressure to the regulators should be at least 6 bar to allow the regulators to work correctly. Sample oxidises. Supply the ETC with dry nitrogen gas instaed of compressed air. The gas supply should be capable of 30l/minute at 6 bar. Page 5-12 MAN 0432

55 Extended Temperature Cell (ETC) Chapter 5 Specification for ETC Temperature Programming / Calibration Via Bohlin Windows Software Temperature Range Ambient temperature to 550 C Heating Rate (single loop mode) >50 50 C Cooling Rate (single loop mode) > C, > C Temperature Accuracy (single loop mode) Heating Rate (dual loop mode) Cooling Rate (dual loop mode) Temperature Accuracy (dual loop mode) Power Supply Heating Method Air Supply Cooling Method Available Geometries Better than ±0.5 C within 2 minutes, 50 C step change >50 50 C, 25mm parallel plate geometries > C, > C, 25mm parallel plate geometries Better than ±0.2 C within 2 minutes, 50 C step change, 25mm parallel plate geometries 220V AC ±10%@ 4.5A max. Forced hot air gun with PID controlled electrical heating 6 to 10 bar, regulated down to 5 bar Flow rate approx. 30 litres/minute Natural (no heating) with forced air gun Parallel plate and cones up to 40mm diameter Fibre / film. Solid sample, max sample dims. 38 x 10 x 0.8mm Single loop mode = single thermocouple in air stream providing input for measurement and control. Dual loop mode = two thermocouples, one in air stream and one in lower geometry. Thermocouple in geometry providing input for measurement, both thermocouples providing input for control. Gemini & CVO Rheometers Page 5-13

56 Chapter 5 Extended Temperature Cell (ETC) Page 5-14 MAN 0432

57 6 Extended Temperature Option (ETO) What is the ETO? The ETO offers higher temperatures than usually available with Peltier and fluid circulation systems, but is also a compact alternative to a fluids circulator where parallel plate or cone and plate measurements are required. Rapid heating and cooling rates are available for applications requiring temperature cycles. Accurate temperature control is achieved using a thermocouple sensor embedded in the lower measuring plate. A thermal enclosure ensures uniform sample temperature. Gemini & CVO Rheometers Page 6-1

58 6 Chapter 6 Connecting the ETO Extended Temperature Option (ETO) Connect the ETO to the instrument using the following procedure: 1. Ensure that the power supplies to the rheometer and the ETO electronics box are turned off. 2. Remove any currently installed temperature controller (see Chapter 3). 3. Insert the ETO into the mounting bracket. 4. Feed the metal trim plate over the ETO, then replace the rheometer s plastic cover. 5. Use the following schematic as reference for making the ETO connections: Heater Plate 2 Page 6-2 MAN 0432

59 Extended Temperature Option (ETO) Chapter 6 Air from supply to ETO control box. Air from ETO control box to ETO collar. Air from supply to rheometer. Communications link from ETO control box to rheometer. Thermocouple to ETO collar from ETO control box PT-100 cable from ETO collar to rheometer. Operating the ETO It is important that the thermal enclosure is used at all times to ensure that the heat from the upper fixture is kept at the same temperature as the bottom surface. Important Safety Points A constant supply of air must be provided for the ETO at all times during operation, even if the cooling capacity of the vortex chiller is not required. (If for some reason it is not possible to supply the unit with air, you should not operate the ETO above 150 C). The red 8mm exhaust hose has a maximum temperature rating of 80ºC for prolonged use, or 150ºC for short periods. Remove the red 8mm exhaust hose from the ETO when operating above this temperature. The rheometer determines its operating mode by examining which thermocouples are connected when it is first powered up. Make sure that the thermocouple is connected before you switch on the rheometer. (If it is not connected, the rheometer assumes a fluid circulator is connected even if it is not.) If you have a fluid circulator as well as the ETO connected to the instrument, switch off the power to the circulator when you are using the ETO and vice versa. The vortex cooler s efficiency depends on the pressure at the hot and cold air exhaust outlets. Thus, any objects obstructing the air s passage from the exhaust outlets will degrade the cooling capacity of the unit. Noise Whilst not a fault, if the unit is excessively noisy in operation, this can be reduced by attaching a longer pipe to the cold air exhaust outlet and ensuring that this is located away from the immediate area of the operator. Gemini & CVO Rheometers Page 6-3

60 Chapter 6 Extended Temperature Option (ETO) Warning A workplace noise risk assessment should be carried out and ear protection may be required by operators. Fault finding The unit will not heat Check that the ETO power box is switched on. Ensure that the red power indicator is lit; if not, check the mains fuse and the front panel fuse. Check that all cables have been connected as described. Finally, power off the rheometer system and then re-start. The unit will not cool Check that the ETO power box is switched on. Check that air is connected and switched on. Ensure that the inlets and outlets are clear from obstructions. If the unit has iced up, which may happen if the supplied air is too damp, heat the unit and then try again. If the problem re-occurs, consider installing an air dryer unit. Page 6-4 MAN 0432

61 Extended Temperature Option (ETO) Chapter 6 Operational specifications for the ETO Air Pressure Air Flow Temperature Operating range Stability Max. Heating rate Max. Cooling rate Electrical power Mains supply Max. power consumption Heater power 5.0 to 7.0 bar (the lower pressure will lower the minimum operating temperature) 120 litres / minute at 7.0 bar or 10 litres / minute at 5.0 bar 5 C to 300 C at 7.0 bar ± 0.2 C 45 C /min (range dependent) 15 C /min (range dependent) 110 / 220 volts AC ± 10% 1.0 Amps 100 Watts Gemini & CVO Rheometers Page 6-5

62 Chapter 6 Extended Temperature Option (ETO) Page 6-6 MAN 0432

63 7 The Melts Oven The Melts Oven The Melts Oven is an enclosed high temperature system intended for both polymer melts and thermoset applications. The Bohlin Melts Oven offers precise temperature control with minimal thermal gradients, using both conductive and radiative heating of the sample. Connecting the Melts Oven To connect the melts oven to the rheometer, use the following procedure: 1. Ensure that the power supplies to the rheometer and the Melts oven control box are turned off. 2. Remove the currently installed temperature control option as described in Chapter Attach the upper oven assembly to the measuring head. Gemini & CVO Rheometers Page 7-1

64 7 Chapter 7 4. Insert the lower melts assembly into the mounting bracket. The Melts Oven 5. Place the circular metal cover (shown in the above image) onto the lower assembly. (Feed the cable from the upper oven through the plate.) 6. Connect the cable from the upper oven to the lower plate connection. 7. Replace the white cover onto the rheometer. 8. Connect the cable from the oven s lower plate to the Oven input on the control box. 9. Connect the Control Cable input from the control box to the rheometer s TCU input. 10. Connect the thermocouple from the oven to the rheometer s TC-1 input. 11. Finally, make all electrical connections. Page 7-2 MAN 0432