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In the Laboratory

cost-effective teacher

edited by

Hal Harris
University of MissouriSt. Louis St. Louis, MO 63121

Low-Cost Constant-Temperature Heating Block

Charles G. Shevlin Department of Chemistry and Molecular Biology, The Scripps Research Institute, 10550 N. Torrey Pines Rd., La Jolla, CA 92037 Ward Coppersmith, Christopher Fish, and Stanley Block Instrument Laboratory, The Scripps Research Institute, 10550 N. Torrey Pines Rd., La Jolla, CA 92037 William Vellema Department of Chemistry, University of Missouri, 601 S. College Ave, Columbia, MO 65211 The need for a constant-temperature bath can be found in a variety of experiments ranging from microbiological assays to qualitative chemical analysis (13). In many undergraduate and secondary school laboratories, where cost is generally of paramount concern, the simplest solution is to place test tubes containing the reactants in a beaker of boiling water. Here, the samples are kept at approximately 100 C for the desired period of time. When temperature must be precisely governed somewhere between 25 and 100 C, the experimenter must manually regulate it (4). However, one should recognize several problems associated with the water-bath method. First, manual maintenance of temperature is inaccurate and time consuming unless a 100 C bath is needed. The risk of water entering the sample tube is high, and in some instances water can be a serious contaminant. Finally, it is somewhat difficult to use a water bath for temperatures greater than 100 C. A rather attractive, but expensive, alternative is to purchase one of the commercially available constant-temperature heating blocks where an aluminum block is drilled to accept a number of test tubes and the temperature is controlled with an electronic controller and heating element. These units are self-contained and can regulate a wide range of temperatures usually within one degree. Besides the high cost of commercial units, they are available in only a limited number of configurations, which may not meet the needed specifications. For example, work done in our laboratory involves combinatorial chemistry where 96 reaction tubes must be thermally controlled. In this case it is necessary to have a thermal block drilled in an 8 12 matrix. We also had a need for a small (48 test tubes, 10 75 mm) heat block, which is used for the Kaiser (ninhydrin) (5) test in peptide synthesis. In a crowded hood with limited space, a slim unit that can be placed out of the way is desirable. Design and Construction The principle behind the controlled temperature heat block is simple. An electric cartridge heater1 is fitted into an aluminum block with holes drilled into it to accommodate the desired number of test tubes. The temperature of the block is governed by an integrated circuit through a thermistor sensor. Construction of both the hardware and electronic temperature controller is straightforward and can be carried out in a few hours.

Figure 1. Photograph of the constant-temperature heating block. Although a bimetal thermometer is used here, a digital or other suitable thermometer could be used in its place.

length of the metal surface of the heater was in contact with the aluminum block. A small retaining washer was fitted so that when tightened it would prevent lateral movement of the heater. Before inserting the heater a small amount of heat-transfer silicon paste was applied to its surface to encourage even heat transfer. One 1/8-in. hole was drilled through the center back side of the heater block and 20 mm below its surface to accommodate the thermistor probe. This was treated in a fashion similar to that of the heater cartridge. Another hole was drilled somewhere into the top surface so that a temperature-measuring device could be accommodated. In our block we used a small bimetal thermometer with a 1/8-in. probe. The heat block was suspended from a piece of perforated aluminum formed around the perimeter of the blocks vertical surface (Fig. 2). This was done to minimize direct personal contact with the heater blocks surface and to support the circuit box.

The Heater Block The heater block was constructed out of a piece of scrap aluminum stock and drilled to conform to a diameter slightly larger than the test tubes (Fig. 1). A hole corresponding to the cartridge heater was drilled so that the full

The Thermistor Probe A 50-k thermistor was soldered to two 15-cm 18 gauge wires. One of the exposed leads was bent parallel to the other lead and insulated using the appropriate sized shrink tubing. Another piece of shrink tubing was placed around both leads to cover all exposed wire. The thermistor was placed into a 30-mm length of 1/8 in. metal tubing, which contained about 1/4 in. of heat-transfer paste and was sealed on one end. A small amount of heat-resistant epoxy was placed into the open end and the end was subsequently crimped. The two leads can be trimmed to the desired size afterwards.

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Journal of Chemical Education Vol. 74 No. 8 August 1997

In the Laboratory
Top View
3/8" dia 11/2"deep 1/8" dia

6.0"

5.0"

4.0"

3.0"

2.0"

1.0"

0.0"

Tap #10 screw 2.000"

5.250" deep 0.625" dia

the board. Figures 4 and 5 show both the solder side and component sides of the board that we used. The triac should be protected from overheating by using a heat sink. For this an 8 18 2-mm aluminum block (or other suitable size) is drilled and attached to the triac using a small machine screw and nut. It is also a good idea to apply a small amount of heat transfer silicone between the triac and the heat sink to enhance heat transfer.

0.625"

0.000" 0.000" 0.625"

1.500" 2.000"

Front View

Side View

Figure 2. Mechanical drawing of the heating block described in this article. These plans are only meant as a starting point for the experimenter, who may change the number and size of the tubes, as well as the overall dimension of the aluminum block, to meet the particular need.

The Housing A 90 60 30-mm hobby box is used to house the circuit board, on/off switch, potentiometer, fuse, and indicating lamp. The circuit board should be attached to the box with standoffs so that none of the components are mobile and no parts of the circuit board touch the housing. The housing is then screwed to the rear side of the perforated guard. A standard 3-lead outlet cord is used. Make certain that the ground lead is electrically connected to the outside perforated metal housing so that the potential of the exposed unit is neutral, thereby minimizing the risk of electric shock.
Circuit Description The theory behind the operation of this device is quite simple (6). Referring to Figure 3 it is easy to see that Rx and R2 along with R1 and R4 comprise a Wheatstone bridge circuit (7). The output of the circuit is applied to pin 13 of the IC. When the potential at pin 13 is greater than that of pin 2 (using Kirchoff s rules; when the resistance of Rx is greater than that of R2) pin 4 sends a gate signal to the triac causing it to apply current to the heater and the indicator lamp. Likewise, when the potential of pin 13 is lower than that of pin 2 the heater is shut off. R3 is a trimmer pot and is used to control the maximum temperature of the device. Increasing its resistance will lower the Tmax.

R1

C1 100 F/15 VDC R1 3.3 k R2 50 k 10 turn R3 5k trimmer R4 1.2 k R5 10 kW 2W RX thermistor 50k/25 C Keystone RL0504-2776K-120g1 Q1 traic 400VAC, 12 A 2N6347A U1 CA3059 or CA3079 RL cartridge heater2 F1 2A, 120 V fuse L1 120 VAC indicator lamp

R2

RX U1
1

13 2

11 10 9 8 4 5 7

MT1 Q1 g MT2

R3

R4

RL

L1

Operation To use the constant temperature heating block, one needs to turn on the switch and balance the desired temperature with the potentiometer. For example, if one needs to regulate the temperature at, say at 110 C, the unit is switched on and the pot turned in a direction that allows the indicating lamp to go on. When the temperature reaches 110 C, the pot is turned in the opposite direction until the light just goes out. If you fit the pot with a vernier knob it is possible to calibrate the heater by taking a number of temperature readings throughout the range and recording the vernier setting at that temperature. Another Application The same circuit used here, along with an extended (10 cm) thermistor probe, can be utilized to control the temperature of an oil bath, sand bath, or the temperature in the reaction vessel itself. With this type of temperature controller, the unit is housed in a plastic outlet box with the temperature probe on a 40-cm lead and the output of the triac wired to a normal 3-prong outlet. A laboratory footplate is epoxied to the box so that the unit can the be conveniently connected to standard lattice support bars. A variety of heaters, including those used in conjunction with a Variac, can be controlled with this unit. The probe is placed in the heating medium (oil or sand) or directly into the reaction solvent (in this case the probe should be enclosed in a glass tube) for precise temperature control.2

+
C1 R5 F1 120 VAC

Figure 3. Schematic and component values of temperature control circuit.

The Circuit Board The control circuit (Fig. 3) consists of a linear integrated circuit (CA3079) (6) which controls the triac (2N6347a). A 10turn, 50-k potentiometer (R2) was used to establish fine control over the temperature range. Lamp 1 is used to indicate when current is being supplied to the heater. A 14-pin standard IC socket is recommended so that the IC is not exposed to the high temperatures experienced during soldering. For the more adventurous, a neater looking printed circuit board can be custom made. The procedure for making one of these boards is quite simple. It first involves drawing out the circuit using a laboratory marker on a copper foil backed board. The board is then immersed into a solution of ferric chloride for 20 minutes or until all of the exposed copper has been etched off. Simply wiping off the marker ink with isopropanol leaves behind the required copper tracks, which are drilled in the appropriate places with a 3/64 bit. The components are then soldered directly to the foil side of

Vol. 74 No. 8 August 1997 Journal of Chemical Education

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In the Laboratory
R3 Rx R4

+ C1

U1 4

R2 R1 Gate MT2

+
R5

MT1 and lamp

lamp

RL 120 VAC

RL

Figure 4. Solder side (bottom) of the heater control board. This figure has been drawn to scale and can be traced directly on to the copper side of the board using carbon paper with a ball point pen. Then go over the tracings with a laboratory marker. All of the circles should have a 3/64 inch hole drilled through them to accept the component leads.

Figure 5. Component side (top) of the heater control board. Note the wire from terminal 4 of U1 and the gate of Q1.

Conclusion The temperature block described here provides a lowcost improvement over the water bath where fairly precise temperature control of test-tube reactions is important. The unit is fairly easy to build and, with a well-equipped shop, can be fabricated in several hours. In addition to its low cost, building this unit allows both the student and professor to review several electronic principles, including Ohms law and Kirchoff s rules, and demonstrates how these principles are put to practice in every-day laboratory situations. Notes
1. The cartridge heater used here was purchased from C&H Sales Co. (HE8551), Pasadena, CA 91107. Tel 1-800/325-9465. 2. We have been using this temperature controller in our laboratories for more than five trouble-free years.

Literature Cited
1. 2. 3. 4. Badger, R. C. J. Chem. Educ. 1978, 55, 747. Alzabet, H. R.; Barbero, J. A. J. Chem. Educ. 1987, 64, 380. Ogle, C. A.; Barnes, C. E. J. Chem. Educ. 1990, 67, 240. One can also build a device for water bath temperature control (see Mercer, G. D. J. Chem. Educ. 1992, 69, 568 and Salvador, F.; Gonzalez, J. L.; Tel, L. M. J. Chem. Educ. 1985, 62, 613). 5. Atherton, E.; Sheppard, R. C. Solid Phase Peptide Synthesis; IRL: Oxford, 1989; p 83. 6. A more complete description of this IC can be found in Motorolas Linear and Interface Integrated Circuits, publication series D. 7. Horowitz, P.; Hill, W. The Art of Electronics; Cambridge University: Cambridge, 1980.

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Journal of Chemical Education Vol. 74 No. 8 August 1997