LABORATORY MANUAL

(Student edition)

THERMODYNAMICS (II)

DEPARMENT Of CHEMICAL ENGINEERING

FA11-BEC-A

List of Experiments
Sr No. Experiment Name Date Signature

1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

Determination of Thermal Conductivity of Gases Determination of Molar Mass of a liquid ---------------------------------------------------------------------------------

Nov 18, 2013 Nov 18, 2013 ---------

EXPERIMENT No. 1
Thermal Conductivity of Different Gases

Objective:

1. Measure the Thermal Conductivity of different gases. 2. Prepare a calibration curve by making a semi-logarithmic plot of the tabulated thermal-conductivity values against the measurement signals.

Principal and Tasks:

The thermal conductivity of a gas is expressed by the coefficient of thermal conductivity which is a function of the average particle velocity and the free path distance. In the experimental set-up there is a functional correlation between the thermal conductivities of the gases at the measuring probe and the voltage signal at the control unit. If the logarithm of the respective coefficient of thermal conductivity is plotted against the measured voltages, a straight line is obtained which can be used as a calibration curve for the determination of the coefficients of additional gases.

Prerequisite & Related Concepts

Thermal conductivity:
Thermal conductivity (denoted by k) is the property of a material to conduct heat. Heat transfer occurs at a higher rate across materials of high thermal conductivity than across materials of low thermal conductivity. Correspondingly materials of high thermal conductivity are widely used in heat sink applications and materials of low thermal conductivity are used as thermal insulation. Thermal conductivity of materials is temperature dependent. The reciprocal of thermal conductivity is called thermal resistivity.

Coefficient of Thermal conductivity:

Thermal conductivity coefficient is denoted by . In SI units, thermal conductivity coefficient is measured in watts per meter Kelvin (W/(mK)). The thermal conductivity of a gas is expressed by the coefficient of thermal conductivity . The coefficient of thermal conductivity is a function of the average particle velocity and the gases free path distance. Furthermore, it is proportional to the thermal conductivity of the gas. So, = 1/2 Cv lf v Where, = Coefficient of thermal conductivity Cv = Heat capacity of the gas v = Average particle velocity

Thermal conductivity detector:

The thermal conductivity detector (TCD) , also known as a Katharometer, is a bulk property detector and a chemical specific detector commonly used in gas chromatography. This detector senses changes in the thermal conductivity of the

column effluent and compares it to a reference flow of carrier gas. Since most compounds have a thermal conductivity much less than that of the common carrier gases of helium or hydrogen, when an analyte elutes from the column the effluent thermal conductivity is reduced, and a detectable signal is produced. In the oil industry TCD have been used for a long time for hydrocarbon detection. Katharometers are used medically in lung function testing equipment and in gas chromatography.

GAS CHROMATOGRAPHY:
Gas chromatography - specifically gas-liquid chromatography - involves a sample being vaporized and injected onto the head of the chromatographic column. The sample is transported through the column by the flow of inert, gaseous mobile phase. The column itself contains a liquid stationary phase which is adsorbed onto the surface of an inert solid. Schematic diagram of a gas chromatograph:

Carrier gas:
The carrier gas must be chemically inert. Commonly used gases include nitrogen, helium, argon, and carbon dioxide. The choice of carrier gas is often dependent upon the type of detector which is used. The carrier gas system also contains a molecular sieve to remove water and other impurities.

Equipments:
Measuring probe for gas chromatograph Control unit for gas chromatograph Multirange meter with amplifier Connection cable, l = 250 mm, 32 A, blue Connection cable, l = 250 mm, 32 A, red Retort stand, h = 500 mm Right angle clamp Universal clamp Pasteur pipettes Graduated cylinder, 25 ml Gas syringe, 100 ml Rubber tubing, di = 6.0 mm Steel cylinder helium, 2 l, filled Reducing valve for helium Table stand for 2 l steel cylinders Wrench for steel cylinders Fine control valve Compressed gas, methane, 12 l Compressed gas, carbon dioxide, 21 g Silicone fluid for heating bath, 500 ml

Fig. Experimental set-up

Principle:
The thermal conductivity of different gases is measured with a gas-chromatographic thermal conductivity detector under stationary conditions. The electrical measurement parameter, which is obtained as a voltage signal in the experimental set-up, is proportional to the logarithm of the coefficient of thermal conductivity.

Set-up and procedure:

The experimental set-up is performed as shown in Fig. 1. Connect a Pasteur pipette to the lateral glass connection tube of the gas chromatographs measuring probe: it should project vertically into a 25 ml graduated cylinder. In the graduated cylinder there is approximately 4 ml of silicone fluid. The tip of the Pasteur pipette should be immersed in the silicone fluid to a depth of 1 to 2 mm. In this way the gas volume is isolated from its surroundings without a resulting internal pressure elevation of any significant size. The measuring probe is connected to the control unit for gas chromatograph, to which a multirange meter is connected. First, select a voltage measuring range of 20 V DC on the multirange meter and switch on the control unit of the gas chromatograph. By depressing the zero button, the voltage is adjusted to 0 V. Then the 2 V voltage range on the multirange meter is selected, and in the course of approximately 10 minutes the zero adjustment is repeated if necessary. The device is now calibrated for air. For the measurement of the thermal conductivity of a gas, the horizontal part of the measuring probe is connected with the outlet valve of the gas cylinder containing the gas to be investigated via a piece of rubber tubing. The apparatus is flushed for approximately 1 minute with a weak flow of test gas, whereby the gas escapes via the Pasteur pipette. Then the gas supply is turned off. In the course of about 1 minute, the voltage on the multirange meter becomes constant; this voltage is recorded. After the measurement, the apparatus is flushed with air using a 100 ml syringe, which is connected to the measuring probe in place of the gas supply. The measuring device should then again display 0 V. It may be necessary to perform another zero adjustment. Each gas should be measured several times to minimise errors.