Return from long vacation | laboratory instrument boot sequence
　　 Liquid chromatography
Boot sequence:
1. Check if the solvent on the solvent tray tray is sufficient, and the solvent level is more than 5 cm above the infusion tube filter head.
2. Check if there are any air bubbles inside the infusion tube. If there is, it should be discharged through the drain valve in time.
3. Treat the solvent (for the first item to see if it needs to be replenished) and sample, filter, and degas.
4. Turn on the power of the host, turn on the detector, pump A, pump B, and the power of the oven.
5. Turn on the computer and turn on the chromatographic workstation.
6. First turn on the piston pump in the workstation to balance the system with the required mobile phase (about 30min)
7. Turn on the xenon lamp and wait for the system baseline to stabilize.
8. Start injection test
Common malfunctions:
After the start-up, the pressure gradually changes (rises or decreases) over a period of time. This is often because the mobile phase is not well balanced in the column and the oven temperature is not constant. These are not instrumental problems, as long as they are balanced for a while, they will be stable. If a gradient program is used, the pressure will follow as the ratio of the mobile phase is changing.
The pressure changes momentarily after starting (>3MPa). The reasons are nothing more than the following four situations: (1) there are bubbles; (2) leakage; (3) the check valve is bad; (4) the pump working phase is incorrect, and can be eliminated one by one.
Gas Chromatograph
Boot up:
Before starting the gas chromatograph, the switch of the carrier gas, helium gas and air main valve should be opened first. The pressure of the secondary meter is generally 0.6 MPa (helium gas is 0.2 MPa). After the instrument power is turned on, you must first turn on the workstation through self-test, and confirm that each column has a flow rate before heating up.
The most important work to use before is the airtightness check. If the airway leaks, it will cause the instrument to work unstablely or the sensitivity may drop or even explode. Therefore, it is necessary to perform this work before the operation, that is, check the carrier airflow path. If the hydrogen and air flow paths have not been removed, they may not be inspected.
Detector:
For FID and TCD detection, the temperature should be controlled at room temperature from 10 ° C to 339 ° C, and the temperature control temperature is ± 0.1 ° C. The detection limit Mt of FID is less than or equal to 1×10-11g/s, the noise is less than or equal to 5×10-14A, and the drift is less than or equal to 5×10-13A/30min. The sensitivity S of TCD is greater than or equal to 3000 mV·mL/mg, the noise is less than or equal to 0.03 mV, and the drift is less than or equal to 0.1 mV/30 min.
Precautions:
When using the gas chromatograph, the temperature should not exceed the upper limit of the inlet temperature to avoid damage to the inlet; routine treatment of inlet contamination: replacement of the septum and deactivated glass wool, cleaning or replacement of the liner, Replace the gasket and the shunt plate; ensure that there is a clean carrier gas and a clean inlet to access the column. The most common problem is pollution. After making high-boiling substances, the column should be aged, and the temperature should be raised to drive out the residue to prevent long-term accumulation and damage to the column.
Mass spectrometer
Preparation before starting:
Check the oil level of the vacuum pump to ensure that the oil page in the pump is between the upper and lower lines of the calibration;
Check the cleanliness of the ion source. Check the ESI source for solids in the spout, whether the capillary port is intact, and whether the APCI spout has effusion;
Gas pressure, open the high-purity nitrogen cylinder total valve, adjust the outlet pressure to 0.65MPa, open the high-purity helium cylinder total valve, adjust the outlet pressure to 0.25Mpa;
Check the connection between the shell gas and the auxiliary gas interface, and loosen the interface between the liquid phase pipeline and the ion source;
Turn on the power supply, the voltage is stable and normal;
Make sure the room temperature is between 18 and 25 degrees.
Boot sequence:
Take the mass spectrometer as an example:
1. Turn on the UPS and nitrogen generator switch. After the pressure gauge of nitrogen is stabilized, turn on the power switch on the mechanical pump;
2. After the mechanical pump has been working for at least 15 minutes, turn on the main power switch of the mass spectrometer. After the system is vacuumed for more than 24 hours, the instrument can be scanned normally; the initial vacuum is 7~9.
3. Open the liquid pump, autosampler and column thermostat power switch;
4. Start the computer and open the Analysis software software on the desktop of the computer;
Precautions for use:
The mass spectrometer is operated under high vacuum conditions with an ion source between 10-3 and 10-5 Pa and a mass analyzer at 10-6 Pa. Change the filament early, clean the ion source or adjust the mass spectrometer after the instrument is overhauled. Pay attention to the inspection of the seal of the mouth gasket during the preparation. A monthly inspection of the He carrier gas system leak is required. If necessary, overhaul the aged column. The desiccant should be replaced every six months. The oil level of the mechanical pump is checked every month. Pay attention to the molecular pump filling lubricant every year. Clean the molecular pump and ion pump if necessary. In addition, the inspection of the inlet septum seal and the leakage of the carrier gas system is required. Only good maintenance can increase the service life of the instrument.
remind:
The sample should be treated with the filtering function of the processing system. The sample entering the mass spectrometer should have a particle size of no more than 1 μm, and reduce the lag time of the sample during the transfer process because of the extremely fast analysis speed of the mass spectrometer. If the sample transfer time is too long, the meaning of mass spectrometry will be lost.
problem:
When the mass spectrum is turned on, the pump speed can only rise to half. When the tone is heard, the control panel prompts: system vented; at the same time, the pump speed drops slowly. Judging that it may be caused by air leakage, the molecular turbo pump cannot be turned on, and the mass spectrometer is turned back on after the leak detection. The fault is not eliminated. What is the cause?
User tips:
After analysis, it is believed that only a very serious air leak will lead to this situation, and a full inspection is required:
1. Whether the inlet and the seal are installed in the inlet.
2. Whether the two ends of the column are in place.
3. Is the vent valve tightened?
4. The MS seal is clean or damaged.
5. Is the pump oil too little or too much?
6. The cylinder is out of gas or the carrier gas partial pressure is insufficient.
7. The position of the cylinder interface is leaking.
8. None of the above problems, it is recommended to check if the vacuum pump is broken.
ICP-MS
Preparations before starting up:
1. Check whether ultra-pure water (2), 5% nitric acid, tuning solution, and internal standard solution are sufficient. Note: Add in time. The waste liquid tank should be emptied in time.
2. Turn on the air conditioner, cooling water device, exhaust system, card peristaltic pump tube, ultrapure water, 5% nitric acid, and the lid of the tuning solution before starting the machine.
3. Regularly check the oil level and color of the mechanical pump, and periodically open the vibrating valve of the mechanical pump to return the pump oil in the oil filter to the pump.
After the ICP-MS is turned on, the vacuum does not go up, the vacuum is displayed as ERROR, and the molecular pump and the vacuum pump are checked. There is no problem. I don't know why?
1. The display is error, it must be a problem with control and communication.
2. Check if the circulating water is open, whether the flow rate and water pressure are correct. The general molecular pump has a water flow interlock protection function. If our instrument does not open the water circulation, the vacuum cannot be pumped up because the molecular pump does not start.
3. If there is a problem with the X7 series communication of the thermoelectric power, you can click the gear icon under the Windows taskbar to find the connection, disconnect and reconnect, or restart the machine.
4. Is the temperature difference set, and the temperature of the environment is also related.
5. It is also possible that the pump is a problem.
atom absorption
Troubleshoot boot usage:
1. After the power is turned on, the slit motor is locked by self-test. The cause of the fault is that the mechanical drive of the motor drive part or the motor is faulty or the photo of the slit is weak, or the interface board is faulty, and the correct judgment is made and replaced.
2. The power-on self-test shows that the wavelength motor is locked. The reason is the same as above, that is, the motor drive or mechanical fault wavelength zero and low-end limit switch fault, or the interface board fault, the elimination method is as above.
3. No light zero can be found. The element light or semi-transparent mirror and the burning head are not installed to block the optical path when starting up, and the photomultiplier tube, high voltage and interface board are faulty.
4. After starting the software, there is no light zero curve, and it crashes, which belongs to the interface board failure.
5. When the ignition is checked, the air pressure is low. Check the working condition of the air compressor and the outlet pressure. Also, whether the air knob is fully open or the pipeline is leaking.
6. The acetylene pressure is low, check the acetylene cylinder and the pipeline for leaks.
7. When the peak is automatically found, the signal is too weak, less than 100%. Check whether there is light blocking or elemental light. If the above reasons are eliminated, the wavelength can be adjusted to the theoretical wavelength to find the maximum value. If it still cannot be solved, it belongs to the interface board or the preamplifier part is faulty.
8. The power-on indicator does not light, check the external power supply system and the host fuse.
9. When the background is deducted, the xenon lamp is not lit, the xenon switch is turned on, and the xenon control button on the software is selected to be in the "on" state.
10. It takes a certain warm-up time to ignite the xenon lamp. If it cannot be lit or unstable for a long time, check whether the power supply system is in the normal range.
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