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How to increase sensitivity on GCMS?
Discussions about GC-MS, LC-MS, LC-FTIR, and other "coupled" analytical techniques.
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I am running 6890/5973 with PT (524.2 Method). I am only able to see down to 5ppb, but need to see lower (0.5ppb). I am only purging 5mL of sample. I also do not know the last time the source was cleaned (new to this instrument), but just about everything else in GC and MSD has been cleaned or replaced. Do you have any suggestions on how to increase sensitivity?
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The tune report gives an indication of the condition of the mass spectrometer. It is independant of the GC as long as the column flow is the same each time the tune report is made. The condition of GC and MS together can be checked with injection of a liquid sample (like OFN or HCB). And a reference sample run through the P&T will give you an indication of the whole system. If you check the MS first and find no problem, then a problem in the GC and MS combined has to be the GC. Likewise if the GC and MX combined are OK, but the problem occurs when you bring in the sampler, the problem is with the sampler.
And do not neglect to tune (or optimize) the instrument on a regular basis. Some like daily, others weekly. But I've seen an instrument go for three months without being tuned. Sensitivity returned dramatically after the instrument was tuned... (It apparently was a surprise to the operator. Story for a different day...)
First make sure all the PM stuff is up to date (inlet liners, septa, leak check the column, etc.) Then, look to see what is not running to spec. With the instrument known to be in good shape, look at things like peak shape in the chromatography. Narrower peaks give better signal to noise values than short, fat peaks -- even if they have the same area. Look at injection conditions. Again, the narrower the sample band on the column, the narrower the peak and the better the signal to noise. Adjustments of the chromatography are low cost or no cost. Look at sampling rate to be sure that you are properly sampling the chromatographic peak - undersampling or oversampling will affect peak RSD's - and detection limits. After you have looked at all of those parameters, look at detector voltage. Increase it to obtain the detection limits you need. Just understand that this is not a no-cost adjustment. Higher detector voltages shorten the life of the detector - so use the "no cost" changes first.
And do not neglect to tune (or optimize) the instrument on a regular basis. Some like daily, others weekly. But I've seen an instrument go for three months without being tuned. Sensitivity returned dramatically after the instrument was tuned... (It apparently was a surprise to the operator. Story for a different day...)
First make sure all the PM stuff is up to date (inlet liners, septa, leak check the column, etc.) Then, look to see what is not running to spec. With the instrument known to be in good shape, look at things like peak shape in the chromatography. Narrower peaks give better signal to noise values than short, fat peaks -- even if they have the same area. Look at injection conditions. Again, the narrower the sample band on the column, the narrower the peak and the better the signal to noise. Adjustments of the chromatography are low cost or no cost. Look at sampling rate to be sure that you are properly sampling the chromatographic peak - undersampling or oversampling will affect peak RSD's - and detection limits. After you have looked at all of those parameters, look at detector voltage. Increase it to obtain the detection limits you need. Just understand that this is not a no-cost adjustment. Higher detector voltages shorten the life of the detector - so use the "no cost" changes first.
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More information would be useful. What size column, split ratio , and tune that you use?
Do you have agilent support? If yes call the 800 number and explain your problem. There are two guys there that have been working with me for 18 months on this same problem. They can explain it to you better than I can.
Do you have agilent support? If yes call the 800 number and explain your problem. There are two guys there that have been working with me for 18 months on this same problem. They can explain it to you better than I can.
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Hi eachem,
Try using 25 mL sparger on PT and i think more suitable to have PTV inlet or VI inlet than S/SL when connected to PT.
Try using 25 mL sparger on PT and i think more suitable to have PTV inlet or VI inlet than S/SL when connected to PT.
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You should easily see 0.5ppb in a 5ml purge on a 5973 system. As mentioned earlier, general maintenance and split ratio info would be helpful. What column are you using?
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