Autosystem Gc Manual

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  • Gas Chromatograph SPECIFICA TIONS G A S C H R O M A T O G R A P H Y www.perkinelmer.com The PerkinElmer ®Clarus 500 Gas Chromatograph (GC) is a fully automated gas chromatograph. The system offers the capabilities required for laborato-ries performing large numbers of routine analyses as well as those involved in research and develop-ment.

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Prevention

Autosystem gc manuals

Many GC problems can be prevented if the column is properly installed and GC is maintained routinely. For example, replacing septa or liner at regular intervals and keeping the injector and detector clean and well-maintained shoud solve many problems. Regular preventive maintenance depends on particular model of GC and you should consult required operations in the operator's and service manuals.

For the problem identification we recommend to use electronic flowmeter and leak detector.

Baseline problems

Baseline problems could be divided into 5 categories: drift, noise, offset, spiking and wander.

  • Drift means slow baseline movement in one direction
  • Noise is rapid and random movement of the baseline position
  • Offset is sudden unexplained change of the baseline position
  • Spiking is presented by peaks with no width, either positive or negative
  • Wander is low frequency noise
Downward drift
Possible causeSuggestions
Downward drift for a few minutes is normal after installing a new columnIncrease the oven temperature to close to the maximum continuous operating temperature for the column. Maintain the temperature until flat baseline is observed. If the detector signal does not drop in 10 minutes, immediately cool the column and check for leaks.
Unequilibrated detectorAllow sufficient time for temperature equilibration of the detector.
Downward drift is frequently due to the 'back-out' of contaminants from the detector or other parts of the GCClean out contamination.
Upward drift
Possible causeSuggestions
Damage to the stationary phase of the GC columnDetermine the cause of the damage. It may be due to impurities in the carrier gas or to excessive temperatures. Replace column.
Drift in gas flow ratesClean or replace flow or pressure regulator(s). Adjust pressure.
Noise
Manual
Possible causeSuggestions
The column may be inserted too far into the flame of an FID, NPD or FPD detectorReinstall the column. Be sure to insert the column into the detector exactly the correct distance specified in the instrument manual.
An air leak can result in noise in ECD and TCD detectorsEliminate the leak.
Incorrect combustion gases or flow rates can generate nois in FID, NPD or FPD detectors.Be sure yuor gases are the proper grade, as well as clean and dry. Reset the flow rates of the gases to their proper values.
Contaminated injectorClean injector. Replace inlet liner, septa and selas.
Contaminated columnBake out the column. Cut off first 10 cm of column. If it does not help, replace the column.
Defective detectorClean and/or replace parts as necessary.
Defective detector boardConsult GC manufacturer.
Offset
Possible causeSuggestions
Line voltage changesMonitor line voltage for correlation with offset. If correlation is found, install voltage regulator or ensure stable power supply.
Poor electrical changesCheck electrical connections. Tighten any loose connections. Clean any dirty or corroded connections.
Contaminated injectorClean injector. Replace inlet liner, septa and selas.
Contaminated columnBake out the column. Cut off first 10 cm of column. If it does not help, replace the column.
Column inserted too fat into the flame of FID, NPD or FPD detectorsReinstall the column. Be sure to insert the column into the detector exactly the correct distance specified in the instrument manual.
Contaminated detectorClean the detector if possible.
Spiking
Possible causeSuggestions
Electrical disturbances entering the chromatograph through power cables, even shielded cablesTry to correlate spikes with events in equipment near the chromatograph. Periodicity is often a clue. Turn off equipment or move it. If necessary, install a voltage regulator.
Wander
Possible causeSuggestions
Baseline wandering may be caused by changes in environmental conditions such as temperature or line voltageTry to correlate the wandering with environmental parameters. If a correlation is observed, you will know what to do.
Inadequate temperature control Check if variations can be correlated with changes in the baseline position.Measure detector temperature.
Wandering while using isothermal conditions may be due to contaminated carrier gasChange the carrier gas or the gas purification traps.
Contaminated injectorClean injector. Replace inlet liner, glass wool and seals.
Contaminated columnBake out the column. Cut off first 10 cm of column. If it does not help, replace the column.

Distorted peak shapes

All peaks redused in size
Possible causeSuggestions
Sample validityCheck the concentration and stability of the sample.
Flattened top peaks
Possible causeSuggestions
Detector overload. The broad peaks may have a rounded top or even valleys in the top.Reduce sample volume, dilute with solvent or use higher split ratio.
Overload of the signal processing electronics. The peaks are clipped with flat tops.Attenuate detector output or reduce sample amount (see above).
Fronting peaks

Autosystem Gc Manual User

Fronting peaks are usually the result of column overloading. In this case, the effect should be a function of injection volume. Solutions include reducing the injection volume or using a column with greatr capacity. Columns with larger diameter or thicker stationary phase coatings generally have larger sample capacities, however, resolution may be reduced.

Ghost peaks
Possible causeSuggestions
Remmants of previous samples in the inlet or column. Ghost peaks due to remmants are most likely to occur when increasing inlet or column temperatures.Increase the final temperature and lengthen the run time to allow for complete elution of previous samples. If ghost peaks continue to occur, clean the inlet. Condition the column at temperature higher than has been used but lower than the maximum continuous operation temperature for the column. Cut 10 cm off the inlet end of the column and/orreverese it before reconditioning it. If it does not help, replace the column.
Backflash may cause remmants. Backflash refers to vapours from the sample which expand to exceed the volume of the injector liner. These vapours may come in contact with colder spots, such as the septum and gas inlets of the injector. Less volatile components may condense. These condensates may vaporize later and interfere with subsequent analyses, sometimes producing 'ghost peaks'.
  • Use septum purge
  • Lower injection volume
  • Enlarge injector liner
  • Optimize injector temperature
  • Use pressure pulsed program
Bleed from the septum or fragments of the septum lodged in the inlet or liner.Clean the inlet. Replace the inlet liner, glass wool and seals.
Irreproducible peak heights or areas
Possible causeSuggestions
Inconsistent injectionDevelop a reproducible injection technique. Use autosampler.
Distorted peak shapes can adversely affect quantitative determinationsCorrect any problems that result in the distortion of peak shape. See Peak shape problems.
Baseline disturbancesSee Baseline problems.
Variations in GC operating parametersStandardize operating parameters.
Negative peaks
Possible causeSuggestions
Incorrect polarity of the recorderReverse polarity of recorder connections.
Incorrect setup in the softwareSet-up right parameters in your chromatography software.
Sample compound has greater thermal conductivity than the carrier gas and you are using a TCD or µTCD detectorIf possible, change carrier gas. Otherwise there is not a solution.
Detector overload in element-specific detectors such as ECD, NPD, FPD, etc., can produce both positive and negative peaksHave the compound of interest arrive at the detector at a different time from the solvent or other compounds in high concentration. H2 produces negative peaks with TCD (µTCD) and helium carrier gas.
Dirty ECD detector can give negative peak after a positive oneClean or replace the ECD detector.
No peaks at all
Possible causeSuggestions
Defective syringeTry a new or proven syringe.
'Blown' septum or massive leaks at the inletFind and fix leaks.
Problems with carrier gas flowAdjust gas flow. Check the column flow ath the column outlet by immersion to methanol.
Broken column or column installed in the wrong wayReplace or reinstall the column.
The detector is not functioning or not connected to the recorder or integrator.Ensure that detector is working properly. E.g.: Is the flame in a FID on? Check connection to the output device.
Selective sensitivity loss
Possible causeSuggestions
Contamination of column and/or liner can lead to loss of sensitivity for active compoundsClean liner. Bake out the column or replace it.
Injector leaks reduce the peak height of the most volatile components of a sample more than less volatileFind and fix any leaks.
Initial column temperature too high for splitless injection which can prevent refocusing of sample. This affects the more volatile components most.Initial column temperature should be below the boiling point of the solvent. Decrease the initial column temperature or use less volatile solvent.
Inlet descrimination. Injector temperature is too low. Later eluting and less volatile compounds have low response.Increase injection temperature.
Split peaks
Possible peaksSuggestions
Fluctuations in column temperatureRepair temperature control system
Mixed sample solvent for splitless or on-column injectionsUse single solvent
When using injection techniques that require 'solvent effect' refocusing such as splitless injectiion, the solvent must form a compact, continuous flooded zone in the column. If the solvent does not wet the stationary phase sufficiently as might be the case for methanol used with a nonpolarstationary phase, the solvent flooded zone may be several meters long and not of uniform thickness. This will result in broad and distorted peaks because the solutes will not be refocused into a narrow band near the beginning of the column.Installing a retention gap (5 meters of uncoated but deactivated column) ahead of the crhomatographic column may reduce or eliminate this problem.
Tailing peaks
Autosystem
Possible causeSuggestions
Contaminated or active injector liner, seal or columnClean or replace injector liner. Do not use glass wool in the liner. If necessary, replace the column.
Dead volume due to poorly installed liner or column.Confirm by injecting inert peak (methane). If it tails, column is not properly installed. Reinstall liner and column as necessary.
Ragged column endScore the tubing lightly with a ceramic scoring wafer or sapphire scriber before breaking it. Examine the end using magnifying glass. If the break is not clean and the end square, cut the column again. Point the end down while breaking it and while installing a nut and ferrule to prevent fragments from entering the column. Reinstall the column.
A bad match between the polarities of the stationary phase and the solventChange the stationaryphase. Usually polar analytes tail on no-polar columns, or dirty columns.
A cold region in the sample flow pathRemove any cold zones in the flow path
Debris in the liner or columnClean or replace the liner. Cut 10 cm off the end of the column and reinstall it.
Injection takes too long.Improve injection technique.
Split ration is too lowIncrease split ratio to at least 20:1
Overloading the inletDecrease the sample volume or dilute sample
Some types of compounds such as alcoholic amines, primary and secondary amines and carboxylic acids tend to tail.Try a more polar column. Make a derivative of the dsample.
Retention time shifts
Possible causeSuggestions
Change in column temperatureCheck GC oven temperature
Change in gas flow rate (linear velocity)Inject a detectable unretained sample such as methane to determine the linear gas velocity. Adjust gas pressure or flow to obtain proper values for your analytical method.
Leak in the injectorCheck the septum first. Change, if necessary. Find the leak and fix it.
Change of solventUse the same solvent for standards and samples.
Contaminated columnBake out the column. Cut 10 cm off the end of the column. If necessary, replace the column.
Loss of resolution

Perkin Elmer Autosystem Gc Manual

Possible causeSuggestions
Damage to stationary phase of columnReplace the column. This is usually indicated by excessive column bleeding or peak tailing.
Injector problemsCheck for leaks, inapropriate temperature, split ration, purge time, dirty liner, glass wool in liner.
Large increase in sample concentration
  • Dilute sample
  • Inject less
  • Use higher split ratio
Broad solvent front
Possible causeSuggestions
Bad column installationReinstall column
Injector leakFind and fix leak
Injection volume too largeDecrease sample size or dilute it
Injection temperature too lowIncrease injection temperature so the entire sample is vaporized 'instantly'. An injection temperature higher than the temperature limit of the column will not damage the column.
Split ratio is too lowIncrease split ratio.
Column temperature too lowIncrease column temperature (ba careful on maximum column temperature limit). Use a lower boiling solvent.
Initial column temperature too high for splitless injectionDecrease the initial column temperature. Use a less volatile solvent so the initial column temperature is below the solvent boiling point.
Purge time too long (splitless injection)Use a shorter purge valve close time.
Rapid column performance degradation
Possible causeSuggestions
Broken columnReplace column. Avoid damaging the polyimide coating on the column. Avoide temperatures above maximu column temperature limit. Avoid abrasion of the column. Remember, even if the column does not break immediately, when protective coating is damaged the column may possibly break spontaneously later.
Column too hot for too longReplace the column. Stay below limits specified for the column.
Exposure to oxygen, particularly at elevated temperaturesFind and fix any lieaks. Be sure carrier gas is sufficiently pure.
Chemical damage due to inorganic acids or basesKeep inorganic acids or bases out of column. Neutralize samples.
Contamination of the column with nonvolatile materialsPrevent nonvolatile materials from getting into column. For expample, use a guard column.

Column installation

Detailed information about GC column installation is available here.

Preventive maintenance

Autosystem Gc Manual Pdf

Injector cleaning

Autosystem Gc Manuals

Detector cleaning




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