Capillary column installation method

Capillary column installation method

The capillary column consists of a column tube, a pressure cap, a ferrule (seal ring), a sieve plate (filter), a joint, a screw, etc., and a sieve plate is arranged in the column joint at both ends.

The steps to properly install a capillary column are as follows:

Step 1: Check the gas filter, carrier gas, sample pad and liner to check the sample pad and gas filter to ensure that the auxiliary gas and detector gas are smooth and effective. If you have previously made a compound with a higher boiling point, you need to clean or replace the inlet liner.

Step 2: Put the nut and the card on the column, and carefully cut the two ports of the column with the corresponding nut and ferrule at one end of the column. At this time, the column port has no front and rear points, and the column support is supported. The part should always face the oven door. After installing the nut and ferrule, cut the column port and check with a magnifying glass to verify that the slit is at right angles to the tube wall and that there are no residual debris, no burrs or uneven cutting surfaces.

Step 3: Connect the column to the inlet. Generally, the top of the column should be kept in the middle and lower part of the inlet liner. If the needle is inserted through the septum completely into the inlet, if the needle tip and liner The top of the column in the tube differs by 1-2 cm, which is the ideal state. Remove enough length from the column holder to connect and cut the column in step 2 to connect to the inlet. Avoid bending the capillary column with force and be careful not to let the sharp-edged items such as the label contact the column to prevent the column from breaking or being damaged. After the column is properly inserted into the inlet, screw the coupling nut by hand, tighten by hand, and then tighten 1/4-1/2 turn with a wrench.

Step 4: The carrier gas carrier must be high-purity nitrogen (or helium) with a purity of 99.999%. When using a polar column (such as FFAP, PEG-20M, etc.), the carrier gas plus deoxidizer can be further deoxidized. Extend the life of the column. When the column is connected to the inlet, the carrier gas is turned on. The pre-column pressure is adjusted to obtain a suitable carrier gas flow rate. Insert the other end of the column (empty end) into a vial containing hexane. Under normal conditions, we can see the steady and continuous bubbles in the bottle. If there are no air bubbles, it is necessary to check whether the downloading device and the flow controller are installed completely or correctly, and check whether the entire gas path is leaking. After all the problems have been solved, remove the column port from the bottle and wipe it clean to ensure that there is no solvent residue in the column port before proceeding to the next step. Capillary column front pressure reference setting (Mpa) column length m column inner diameter (mm) 0.25 0.32 0.53 15 0.05 0.04 0.02 30 0.1 0.08 0.03 50 0.18 0.14 0.05

Step 5: Attach the column to the detector. The installation and precautions are similar to those described in the section Connecting the Column to the Inlet (Step 3) above. When installing, pay attention to the end of the column is higher than the end point, or install according to the chromatograph instructions.

Step 6: Perform Gas Leak Detection Before the column is heated, the GC system should be leak tested. It is recommended to use a 1:1 mixture of isopropyl alcohol/water for inspection.

Step 7: Column aging After the column installation and system leak detection are completed, the column can be aged. The column was programmed to warm to below 30 ° C of the use temperature and kept at a constant temperature for 30 minutes. The components adsorbed in the column will be blown out so as not to affect your analysis. Finally, the actual sample analysis can be performed by lowering the temperature of the column to the desired temperature.

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