HP 5890A Gas Chromatograph Operation Manual

Figure 1. HP 5890A Gas Chromatograph This machine has both a Thermo-Conductivity Detector (TCD) and a Flame Ionization Detector (FID). For the alcohol mixture analysis, you will be utilizing the TCD. Procedure 1. Before you turn on the machine, you must turn on the helium gas by opening all the way of the large knob directly attached to the tank (Figure 2). Allowing helium gas flow through the column can prevent damage to the TCD. The tank pressure should be at least 500 psig, and the low pressure gauge should read at least 40 psig.

Figure 2. Helium Gas Tank

2. The column head pressure gauge on the GC (Figure 3.) should be set to ~60kPa (NOT PSI!!). Use the valve marked CARRIER FLOW (located underneath the pressure gauge) to adjust the column pressure if necessary.

Figure 3. Column Head Pressure Gauge 3. Connect the soap-bubble flow meter to the TCD exhaust (Figure 5.) by using the provided adapter (Figure 6.), and verify that there is gas exiting the column. The soap solution level should be filled just above its reservoir.

Figure 4. GC with the Flip-up Cover Open

Figure 5. TCD Exhaust

Figure 6. Bubble-flow Meter Adapter Attached to the TCD Exhaust

Figure 7. Appropriate Level of Soap Solution

Figure 8. Correct Setup for the Soap Bubble Flow Meter 4. If there is gas flowing through the column, you can now turn on the HP 3392A integrator (The power switch is located at the back of the integrator), and then the GC (The power switch located at the bottom right of the GC). Both the integrator and the GC will run a self-test every time when they are on.

Figure 9. HP 3392A Integrator 5. Once the GC passed its self-test, several working conditions need to be entered. - Set the oven temperature to 100 oC by pressing OVEN TEMP, followed by 1 0 0, and then ENTER. - By employing the same manner, set the INT TIME and FINAL TIME to 7 minutes. - Make sure the RATE is set at 0 oC/min. - Set the INJ A TEMP to 90 oC. - Set the DET A TEMP to 120 oC. - Set the RANGE to 5. - Set the ATTN 2 to 1. - Check if ZERO is set at 0.

Figure 10. HP 5890A Control Panel 6. Once the working conditions have been reached, you can now turn on the TCD by pressing DET, then A, followed by ON, and then ENTER. The TCD is now on, and it is necessary to warm-up the detector for 20-25 minutes before starting any test. At this point, the flow rate of gas should be about 10 mL/min. If the flow rate is much higher than 10 mL/min, you might need to turn off the reference gas by fully closing the valve marked REF (Figure 11.)

Figure 11. Gas Flow Control on GC 7. While waiting for the TCD to be stabilized, several parameters of the integrator need to be entered. a. First, make sure the READY light on the integrator is on. If the READY light is not on, press ESC key. b. Press ATTN 2 key on the integrator, followed by 4, and then ENTER.

c. Press CHT SPD key, followed by 0 . 8 and then ENTER to set the chart speed to 0.8 cm/min. d. Press PK WD, followed by 0 . 0 4, and then ENTER. e. Once you are finished, press LIST twice, and you should see the following: LIST: LIST PEAK CAPACITY: 996 ZERO = 0, 0.05 ATT 2 = 4 CHT SP = 0.8 PK WD = 0.04 THRSH = 0 AR REJ = 0 f. Note that the peak capacity and the second value of ZERO are just the detected values. You can disregard these two numbers, even they do not match with the above values. 8. While the TCD is warming-up, turn on the reference gas by adjusting the REF gas valve (Figure 11.). The total flow rate should be set at 20-22 mL/min. 9. If the desired flow rate has reached and the TCD is already warmed-up, you are now ready to inject a sample to the GC. You need to use a Hamilton 701RN micro-syringe (Figure 12.) to inject a 1 -1.5 L sample to the injector septum (Figure 13.). After placing the needle through the injector septum, you should press the START button on the GC and quickly inject the sample. (You must handle the syringe with extreme care, since it is very fragile.). The integrator should start automatically.

Figure 12. Hamilton 701RN Micro-Syringe

Figure 13. Injector Septum 10. When all of your peaks have eluted, press the stop button on the control panel. However, you must make sure all of the components have eluted before you begin another run. 11. To turn the instrument off, you must first turn off the TCD by pressing DET A OFF, followed by ENTER. Then, you must set all temperatures to zero (Employ the same command logic as described in step 5). Let the GC cool with helium flow until the detector temperature drops below 100oC. 12. Once the detector temperature has cooled below 100oC, you can turn off the GC and the integrator. Dont forget to close the main valve on the helium tank before you leave.