1975
year,
Small
The success of the continuous detection of column effluent by a conductivity detector indicates the birth of ion chromatography. After nearly three decades of development, ion chromatography (
IC
) has become a common method of analyzing ionic substances.
Ion chromatography has fast analysis speed, high detection sensitivity and good selectivity, and can detect multiple ions at the same time. However, the requirements for use are relatively high, and daily maintenance is prone to failure.
First, the basic structure and principle of ion chromatography
Basic structure: infusion system, injection system, separation system, detection system.
(1) Infusion pump: The function is to pass the mobile phase through the flow path system with a relatively stable flow or pressure.
(2) Sampler: The basic requirements are high pressure resistance, corrosion resistance, good repeatability and easy operation.
(3) Separation column: The separation mechanism is mainly ion exchange, based on the reversible exchange between the dissociable ions on the ion exchange resin and the solute ions having the same charge in the mobile phase, and the different ions have different affinity with the exchanger. Is separated.
(4) Detector: There are mainly conductivity detectors, ultraviolet visible light detectors, amperometric detectors, fluorescence detectors, etc.
(5) suppressor, conductivity detector
(6) Chromatography-mass spectrometry and other technologies
Second, ICS-1000
Diane ion chromatography systemDeionized water is tested in four parts in sequence:
(1) Infusion system: eluent bottle (1) - eluent valve (2) - pump (3) - pressure sensor (4) - damper (5)
(2) Injection system: injection valve (6) - sample ring (7) - heat exchanger (8)
(3) Separation system: separation column (9)
(4) Detection system: suppressor (10) - conductivity cell (11) - waste liquid
Third, failure analysis and elimination
The structure of the ion chromatogram is complex, and the analytical work after the failure needs to have a clear idea. Based on experience, it is recommended to start with the phenomenon to diagnose, find out the cause, and finally seek a solution.
Abnormal pressure
(1) No mobile phase flows out, and the pressure indication is zero or close to zero.
Possible cause 1: A large amount of gas in the high pressure constant current pump. The pressure relief valve needs to be opened to allow the pump to operate at a higher flow rate to drain the air bubbles. A syringe can also be used to assist in extracting gas at the outlet of the pump.
Possible cause 2: The system is leaking. Leakage is usually solved by tightening the fitting or replacing the tubing.
(2) The pressure indication is too high
Cause: Blockage. Need to analyze where it is blocked and then clean it. Column inlet membranes, pump valves, etc. are places that need to be focused.
(3) Pressure fluctuations
Cause 1: There is no solution in the eluent bottle, causing the pump to be evacuated. Need to refill the eluent and check if the eluent tube is inserted into the bottom of the container;
Cause 2: Check valve contamination. Need to clean or replace the check valve.
Cause 3: The pump was evacuated due to contamination or clogging of the filter head in the eluent container. It is generally necessary to replace the filter head.
2. Peak anomaly
(1) Peak height or retention time repeatability is poor
Cause 1: The column is contaminated or overloaded. It is necessary to change the sample concentration to the specified range.
Cause 2: The pipeline leaked. Need to be repaired or replaced.
(2) no peak
Reason 1: The analysis time is not reasonable. Need to extend the analysis time.
Cause 2: The conductivity cell is not installed correctly or the conductivity cell is damaged. The solution is to reinstall or replace the conductivity cell.
Cause 3: The pump has no output solution. At this time, the pressure reading should be checked to see if the pump is working. If the pump is not working, restart the pump to see if it is getting better.
3. Baseline anomaly
(1) Baseline regular jitter
Cause: There are air bubbles in the test cell or pump head. Need to exhaust bubbles.
(2) Irregular jitter
Cause 1: The system has a leak. Check the tubing and fittings, tighten or replace.
Cause 2: The suppressor is not working properly. You need to read the suppressor operation manual and reset it as needed.
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