F-3004 Peltier Sample Cooler Operation Manual v. 1.0 http://jobinyvon.com In the USA: Jobin Yvon Inc. 3880 Park Avenue, Edison, NJ 08820 In France: Japan: +81 (0) 3 58230140 Tel:+1-732-494-8660 16-18, rue du Canal China: +86 (0) 10 6849 2216 Fax: +1-732-549-5157 91165 Longjumeau cedex Germany: +49 (0) 89 462317-0 E-Mail: info@jobinyvon.com Tel: +33 (0) 1 64 54 13 00 Italy: +39 0 2 57604762 1-800-533-5946 Fax: +33 (0) 1 69 09 93 19 U.K.: +44 (0) 8204 8142 I
Copyright 2001, 2004 by Jobin Yvon Inc. All rights reserved. No part of this work may be reproduced, stored in a retrieval system, or transmitted in any form by any means, including electronic or mechanical, photocopying and recording, without prior written permission from Jobin Yvon Inc. Requests for permission should be requested in writing. Information in this manual is subject to change without notice and does not represent a commitment on the part of the vendor. May 2004 Part Number 81049 II
Table of Contents 0: Introduction... 1 The Peltier effect... 1 Symbols used in this manual... 1 1: Requirements & Installation... 2 Requirements... 2 Installation... 3 2: System Operation... 9 Introduction... 9 To adjust the magnetic stirrer... 10 To purge the sample holder... 11 To adjust the basic Peltier-device parameters... 12 To run batch temperature-control experiments... 20 3: Troubleshooting...25 For further assistance... 26 4: Specifications...27 Computer requirements... 27 Software requirements... 27 Operating specifications... 27 Electrical and physical specifications... 27 5: Index...28 III
IV
0: Introduction Introduction The Peltier effect Jean Peltier discovered a thermoelectric effect in 1834, in which electricity flowing through certain materials causes a temperature gradient across those materials. Specifically, Peltier noticed that an electric current moving through two different conductors can cause emission or absorption of heat. That is, when electricity flows through a substance such as bismuth telluride (Bi 2 Te 3 ), heat is moved across the material, creating a warmer side and a colder side. Modern research on the Peltier effect shows that the charge carriers in doped semiconductors push hear in the direction of their motion. Therefore, reversing the current s direction changes the warm side to the cool side, so that the Peltier device may be used to heat a sample as well as cool it. Peltier devices are used to cool integrated circuitry, semiconductor photodetectors, and even food in picnic coolers. Their advantages over conventional cooling units are: no moving parts, small size, no refrigerant fluids, no vibration or mechanical noises, and high stability and long life. Their major disadvantage is their relative inefficiency. The Peltier Sample Cooler is an automated temperature controller for samples inside the SPEX series of spectrofluorometers. Thermoelectric heating and cooling controls the sample temperature faster than conventional water baths. A magnetic stirring system to keep your sample homogeneously mixed, and a port for nitrogen gas purging (to reduce condensation on a chilled sample) are included in the Peltier Sample Cooler. Symbols used in this manual Certain symbols are used throughout the text for special conditions when operating the instruments: Warning: A hazardous condition exists, or danger exists that could damage the equipment. Jobin Yvon Inc., is not responsible for damage arising out of improper use of the equipment. General information is given concerning operation of the equipment. Note: 1
Peltier Sample Cooler v. 1.0 (24 May 2004) Requirements & Installation 1: Requirements & Installation Requirements Computer requirements Dedicated serial COM port DataMax software Windows 95 or higher 973005 or equivalent PC computer Electrical requirements 115 VAC or 230 VAC ±15% (switch selectable), 60 or 50 Hz 25 W average with output off; 55 W average with output on Physical Requirements Controller must be within 36" (90 cm) of Peltier Sample Cooler (communications cable length) 2
Peltier Sample Cooler v. 1.0 (24 May 2004) Requirements & Installation Installation 1 Unpack and inspect all components. a The following Peltier Sample Cooler components should be included: Quantity Description Part Number 1 Peltier Sample Cooler 400313 1 Sample-cooler cover 1 Control unit with 50-Ω BNC terminator LFI-3751 1 Peltier Sample Cooler Operation manual 81049 1 Wavelength Electronics User s Guide with extra parts 1 9-pin-male-to-9-pin-female cable 400367 1 9-pin-to-25-pin RS-232 cable 35506 1 Power cord (115 V or 220 V) 98015 or 98020 4 #4-40 1¼" screw for FluoroMax installation 600105 4 #4-40 1½" screw for Fluorolog installation 600104 1 Magnetic stirring bar 53044 1 Certificate of Calibration for control unit 1 3.5" diskette (only if Peltier Sample Cooler was purchased separately form the spectrometer) b Inspect all the components for signs of damage that may have occurred during transit. If damage is evident, do not continue with the installation. Notify Jobin Yvon and the shipper at once. Note: Many public carriers do not recognize claims for concealed damage reported later than 15 days after delivery. For a shipping damage claim, inspection by the carrier agent normally is required. Therefore, the original packing material should be kept as evidence. While Jobin Yvon is not liable for damage occurring during transit, the company will extend every effort to aid and advise. 2 Read this instruction manual thoroughly before installing the Peltier Sample Cooler. 3 Install the Peltier Sample Cooler: 3
Peltier Sample Cooler v. 1.0 (24 May 2004) Requirements & Installation a Remove the existing sample holder from the sample compartment of the spectrofluorometer. b Install the control unit as directed in the Wavelength Electronics User s Guide (Chapter 1, Preparing the Temperature Controller for Use, steps A through F). c Make sure that the 50-Ω BNC terminator is attached to the ANALOG INPUT on the back of the controller. d Connect the 25-pin 9-pin adapter cable s 25-pin female end to the RS-232 OUTPUT on the back of the control unit. e Attach the 9-pin female end of the the 25-pin 9- pin adapter cable to the COM2 port on the host computer. 4
Peltier Sample Cooler v. 1.0 (24 May 2004) Requirements & Installation f Connect the 9-pin-female 9-pin-male s female end to the OUTPUT jack on the back of the control unit. g Attach the 9-pin-female 9-pin-male adapter cable s male end to the jack on the front of the Peltier Sample Cooler. h Insert the power cord into the jack on the control unit. Plug the other end of the power cord into a wall receptacle. i Place the Peltier Sample Cooler into the sample compartment. Note: Be sure that the communications jack inside the sample cooler is firmly seated in the connection within the sample compartment. 5
Peltier Sample Cooler v. 1.0 (24 May 2004) j Attach the Peltier Sample Cooler to the front panel of the sample compartment using four #4-40 screws. Requirements & Installation Note: For installation in a Fluoro- Max, use the shorter screws; for installation in a Fluorolog, use the longer screws. k (optional) If condensation may be a problem for the chilled sample, attach a dry-nitrogen gas line to the small metal purging inlet on the front of the sample cooler. 4 Install the software on the host computer. (only if the Peltier Sample Cooler was purchased separately from the spectrofluorometer) 5 Confirm that the upper and lower temperature limits are set correctly. a Start the instrument and computer, according to the instrument s instruction manual. b Start DataMax. c Choose a layout that includes a Peltier device. 6
Peltier Sample Cooler v. 1.0 (24 May 2004) Requirements & Installation d Open Visual Instrument Setup. e Click on the sampleholder icon. The Sample Compartment Accessories dialog box opens. f Choose the Temperature control option. g Click on the thermometer icon. The Peltier Setup dialog box opens. h Click Advanced. The Dialog window appears. 7
Peltier Sample Cooler v. 1.0 (24 May 2004) Requirements & Installation i Switch on the controller s POWER button. j Turn knob to SET T. This setting adjusts the temperature limits. k Push the TEMP LIMIT button once. Starting with the upper temperature limit, the upper and lower temperature limits are displayed alternately. l Push the TEMP LIMIT button once to release this display. If the green LED display shows the limits that match the values in the Safety Limits area of the Dialog window, no further action is needed. If the green LED display does not match these values, change the values in the Safety Limits area of the Dialog window. 8
2: System Operation System Operation Introduction Aside from the magnetic stirrer and nitrogen purge port, operation of the Peltier Sample Cooler is entirely user-controlled from the computer. There are two ways to alter the operation of the Peltier Sample Cooler: To adjust the basic Peltier-device parameters: maximum and minimum allowable temperatures, maximum and minimum allowable electric current to the Peltier device, and PID settings for rate of temperature change and sensitivity of the control unit to the thermal inertia of the sample holder, Use the Peltier Setup dialog box from the Visual Instrument Setup within DataMax. To modify temperature-based experiments: how many temperature points at which to set, what temperatures they ought to be, and batch experiments, Use the Peltier Batch Scan dialog box. Enter this dialog box from the Collect... command of the DataMax toolbar. 9
System Operation To adjust the magnetic stirrer 1 Place the magnetic stirring bar in the sample cuvette. 2 Place the cover on the Peltier Sample Cooler. 3 Close the lid of the spectrofluorometer s sample compartment. 4 Turn the knob on the front of the Peltier Sample Cooler from OFF to the desired stirring speed. 0 is the slowest speed, and 10 is the fastest speed. 10
To purge the sample holder System Operation Purging the sample holder with dry nitrogen gas is usually done when the sample temperature is below the ambient dew point, i.e., in a cold, humid environment. Purging with dry nitrogen prevents water condensation on the cuvette, improving spectroscopic scan quality. 1 Attach the dry-nitrogen gas line to the purging port. 2 Start the gas. 11
System Operation To adjust the basic Peltier Sample Cooler parameters 1 In Visual Instrument Setup, click on the sample-holder icon. Note: The Visual Instrument Setup may differ from that shown here, based on the accessories and model of instrument. The Sample Compartment Accessories dialog box appears. 2 Choose the Temperature control option. Other options, such as a sample changer, might be present. 3 Click on the thermometer icon. The Peltier Setup dialog box appears. Basic operations are displayed in this window. 12
4 Adjust the parameters. The Temperatures area displays current and desired temperatures. System Operation Note: Values are updated approximately every 5 seconds. The Output area displays the electrical status of the Peltier Sample Cooler. Use the Advanced button to adjust heating and cooling parameters, and electrical and thermal limits of the Peltier device. 5 Click Apply. The parameters are updated. 6 Click OK. The Peltier Setup dialog box closes. 13
System Operation To adjust the set-point of the sample The Temperatures area displays the current Sample Block, Immersion, and Setpoint temperatures. 1 Enter the desired sample temperature here. 2 Click Apply. Note: If the temperature entered is beyond the user-selectable, allowable range of the Peltier Sample Cooler, a warning message appears. 14
To set electrical and thermal limits 1 Click Advanced. The Dialog window appears. System Operation Note: For safety reasons, the maximum allowable current is factory-set to ±5.0 A. The software refuses to accept any value greater than a magnitude of 5.0 A. The temperature limits of the Peltier device are 10 to +110 C. 2 Enter the maximum and minimum allowable temperatures in these two fields. 3 Enter the maximum positive and negative allowable currents in these two fields. 4 Click OK. 5 Click Apply in the Peltier Setup dialog box. 6 Adjust the controller to match: 15
System Operation a Turn knob to SET T. This setting adjusts the temperature limits. b Push the TEMP LIMIT button once. Starting with the upper temperature limit, the upper and lower temperature limits are displayed alternately. c When the upper temperature limit is displayed, turn the knob immediately to the desired value matching that in the Dialog window. d Push the TEMP LIMIT button once to confirm. e Push the TEMP LIMIT button once. Starting with the upper temperature limit, the upper and lower temperature limits are displayed alternately. f When the lower temperature limit is displayed, turn the knob immediately to the desired value matching that in the Dialog window. g Push the TEMP LIMIT button once to confirm. 16
System Operation To start or stop the heating or cooling cycles The electrical output of the controller is displayed in this area. 1 Choose Enable to start the Peltier Sample Cooler, OR 2 Choose Disable to stop the Peltier device. 3 Click Apply. Note: If the Enable button does not engage and start operation of the Peltier, check connections and settings to the Peltier device. 17
To change PID parameters System Operation Instructions 1 Click Advanced. The Dialog window appears. 2 Enter the new settings in the Peltier Device Control area. 3 Click Restore Defaults to return the PID values back to Jobin Yvon s default settings. 4 Click OK. The Dialog window closes. 5 Click Apply in the Peltier Setup window. 18
System Operation About PID parameters P = Proportional Gain The Error Voltage is the difference between set-point voltage (the desired temperature) and measured thermocouple voltage (actual temperature). The proportional gain, P, supplies a current proportional to the Error Voltage. If P is large, the Peltier device approaches the desired temperature rapidly. This, however, may overshoot the desired temperature. As the Error Voltage drops to 0 when the actual temperature reaches the set-point, so does P, cutting off heating or cooling. Thus over- and undershoots of the set-point may happen without adjusting the next two parameters listed below. I = Integrator The integrator charges up based on how close the Error Voltage is to 0. Rapid charging (small integrator time-constant, or Integrator Time Const.) occurs if the Error Voltage is large; slow charging (large time-constant) occurs if the Error Voltage is small. At Error Voltage = 0, no charging occurs, and the output current is run via the integrator. Try to keep the time-constant large enough to compensate for the thermal inertia of the sample holder and Peltier device, otherwise the temperature may oscillate. D = Differentiator The Differentiator (or Differentiator Time Const.) uses the change in Error Voltage with time, dv/dt (the derivative). The faster the Error Voltage changes (the larger the slope of dv/dt), the larger the opposing current. Thus, the Differentiator opposes radical changes in the sample s temperature. Note: Jobin Yvon has set the PID values for an optimum response from the Peltier device. We do not recommend changing these default values. 19
To run batch temperature-control experiments 1 In the DataMax toolbar, choose Collect. A drop-down menu appears. System Operation 2 Choose Temperature Scan. This opens the Temperature Scan dialog box. 3 Choose a predetermined experimental setup or existing file with these buttons. 4 Adjust parameters related to the temperature during a scan. 5 Get help. 20
System Operation To choose a single experimental setup Enter the full pathname for an experimental setup here, OR Click on Exp. Browse to browse through a folder of experimental-setup files: Choose the drive and directory in this area. Click on Info to preview a file. From the list, click on a file to use. It is highlighted in the space. List all files of types *.exp or *.* 21
To search for specific output files Output files from the spectrometer are of the form.spc System Operation Enter a unique file name with the file path, OR Click on File Browse. This opens the Select File Name dialog box, and selects a file for overwriting all previous data in that file will be lost: Choose the drive and directory in this area. Click on Info to preview a file. From the list, click on a file to use. It is highlighted in the space. List all files of types *.spc or *.* 22
To adjust temperaturecontrol parameters 1 Click Temp Control. The Temperature Control dialog box opens. 2 Enter the experiment s starting temperature in Start Temp. 3 Enter the experiment s final temperature in End Temp. System Operation 4 Enter how many different temperatures the Peltier should reach in Number of Temps. 23
5 Enter the Tolerance (how close, in C, the heater must be to the desired temperatures). 6 Enter the Equilibration Time. Equilibration Time is how long, in min, the heater waits before moving to the next temperature. System Operation 7 Choose to Insert, Replace, or Add to End a new temperature into the list, then type the value into the field. 8 Choose Probe 9 Check this to measure an box to shut external thermocouple s tem- Peltier de- off the perature, or vice after Bath for the the experiment. Peltier device s temperature. 11 Click OK. The Temperature Control dialog box closes. 10 Enter the Standby Temperature (at which the Peltier holds after the experiment ends). 24
3: Troubleshooting Troubleshooting Consult the Wavelength Electronics User s Guide for any problems that may occur with the control unit. Below are listed some problems that might occur: Problem Possible Cause Suggested Remedies Control unit does not turn on. Peltier Sample Cooler will not operate Disconnected power cord Faulty wall receptacle Fuse is blown No Peltier layout available Communications cables have bad connection Connect power cord.. Check wall receptacle. Check and replace fuse. Select layout with Peltier in Visual Instrument Setup. Check communications cables. Check connection between spectrofluorometer and Peltier Sample Cooler inside sample compartment. Check all software settings. 25
For further assistance... Troubleshooting Before contacting the service department, complete the following steps: 1 Reboot the system if this the first time the problem has occurred. a Turn off the system and accessories. b After a cool-down period, turn the system back on and see if the failure persists. 2 Make sure all accessories are properly configured and switched on as appropriate. 3 Check the Troubleshooting chart to see if the problem is duscussed. 4 Try to duplicate the problem. Write down the steps required to repeat the error. Our service engineers will attempt to do the same with a test system. 5 If a DataMax software error or Windows error is displayed, write down the exact error shown. 6 Determine the serial numbers. a Open DataMax. b In the Instrument Control Center, under Help, find the version of the software. c Make a note of the instrument s serial number and instrument configuration, including all the accessories. 7 If you require further assistance in the United States, call us at (732) 494-8660, fax us at (732) 549-5157, or send an e-mail to service. Outside the United States, contact your local distributor. 26
4: Specifications Appendix Computer requirements 973005 or equivalent PC computer with RS-232 port Software requirements Windows 9x or NT4 (SP3 or higher) DataMax 2.2.10 Operating specifications Ambient environment for controller: 0 55 C Minimum Peltier temperature for samples = 10 C Maximum Peltier temperature for samples = +110 C Display update to software ~ 0.2 Hz (every 5 s) Electrical and physical specifications 115 VAC or 230 VAC ±15% (switch selectable), 60 or 50 Hz 25 W average with output off; 55 W average with output on 3 32 " (2.4 mm) O.D. inlet for dry-nitrogen purging Controller dimensions are 4¼" (10.8 cm) W 7" (17.8 cm) H 12 11 16 " (32.2 cm) D (allow 2¾" [7 cm] extra clearance depth for cables) Peltier Sample Cooler dimensions are 6¼" (15.9 cm) W 7½" (19.1 cm) H 9" (22.9 cm) D 27
5: Index Index Key to the entries: Times New Roman font...subject or keyword Arial font...command, menu choice, or data-entry field Arial Condensed Bold font...dialog box danger... 1 2 DataMax... 2, 6, 9, 20, 26, 27 derivative...19 25-pin 9-pin adapter cable... 4 Dialog...7, 8, 15, 16, 18 differentiator...19 dimensions...27 9 directory...21, 22 Disable...17 9-pin-female 9-pin-male adapter cable... 5 diskette... 3 drive...21, 22 A dv/dt...19 Add to End...24 Advanced...7, 13, 15, 18 Analog Input... 4 Apply...14, 15, 17, 18 B batch...9, 20 Bath...24 bismuth telluride... 1 BNC terminator... 4 C cable...2, 3, 25, 27 Certificate of Calibration... 3 Collect...9, 20 COM port... 2 COM2... 4 computer...2, 6, 9, 27 condensation...1, 6, 11 controller...3, 4, 5, 8, 9, 15, 25 cover...3, 10 current temperature...13 D damage...1, 3 E Enable...17 Equilibration Time...24 Error Voltage...19 exp...21 Exp. Browse...21 external thermocouple...24 F File Browse...22 final temperature...23 fuse...25 H hazardous condition... 1 Help...26 host computer... 6 I Immersion...14 Info...21, 22 Insert...5, 24 Instrument Control Center...26 28
integrator...19 J Jean Peltier...1 L layout...25 M magnetic stirrer...1, 9, 10 N nitrogen...1, 6, 9, 11, 27 O OK...15, 18 P pathname...21 Peltier Batch Scan...9 Peltier device... 1, 9, 13, 17, 19, 24 Peltier effect...1 Peltier Setup... 7, 9, 12, 13, 15, 18 PID...9, 18 power cord...5, 25 preview...21, 22 Probe...24 proportional gain...19 purge...1, 6, 9, 11, 27 R reboot...26 Replace...24 Restore Defaults...18 RS-232...3, 4, 27 S Index Sample Block...14 sample compartment...4, 5, 10, 25 Sample Compartment Accessories...7, 12 sample temperature...1, 11, 14 sample-holder icon...7 Select File Name...22 serial number...26 SET T...8, 16 set-point...14, 19 Setpoint...14 setup...20, 21 software... 2, 6, 25, 26, 27 spc...22 Standby Temperature...24 starting temperature...23 stirring speed...10 symbols...1 T TEMP LIMIT...8, 16 Temperature control...7, 12, 20 temperature limits...6, 8, 16 Temperature Scan...20 thermal inertia...9, 19 thermal limits...13, 15 thermoelectric effect... See Peltier effect thermometer icon...7, 12 time constant...19 Tolerance...24 Troubleshooting...25, 26 U update...27 V Visual Instrument Setup...7, 9, 12, 25 W Wavelength Electronics User s Guide3, 4, 25 Windows...2, 26, 27 Safety Limits...8 29
Index 30