Advertisement

Agilent GC-MS: Issue With Internal Standard Recovery

Discussions about GC-MS, LC-MS, LC-FTIR, and other "coupled" analytical techniques.

5 posts Page 1 of 1
Hello all! I have browsed the boards before and found it to be a great resource with help in diagnosing and resolving issues with an instrument in our laboratory that is quite difficult to work with, as it never seems to want to stay up and running for more than a few days before having issues! I am curious to see if anyone out here has had similar issues with a similar system and, if so, what they were able to do to diagnose/resolve the issues. Any input or widsom learned from past experience is greatly welcomed. Thanks so much!

System: Teledyne Tekmar Aquatek 70 Vial AutoSampler, Teledyne Tekmar Stratum Purge and Trap, Agilent 5975C VL MSD with Triple-Axis Detector, Agilent 7890A GC System

Method: EPA Method 8260B used for detection of Benzene (ppb level) in Wastewater samples

Standards/Trap: Pentafluorobenzene (internal standard), Bromofluorobenzene (surrogate), Vocarb 3000 Trap

Description of Issues:
Over the last 2 years, the laboratory I now work for have had numerous issues related to sudden spikes or losses in internal standard recoveries which result from random, sudden decreases in the bromofluorobenzene responses (typically, the internal standard we now use - pentafluorobenzene - does not decrease). These drops are essentially "hit or miss." That is, if you run 10 samples, you may have one or two that the bromofluorobenzene response drops just enough on to move the percent recovery out of the acceptable method limits of 86-115%. Any thoughts?

Tuning has also been an issue. I have found several good resources regarding some ways to do a modified autotune to suit the particular needs (i.e. I have learned how to change the Ion Focus, Voltages, Lens, Offset, etc. to increase/decrease abundance for different m/z that may fall out of range over time as the source gets dirty). However, it seems as though I am in a constant battle of either re-tune the instrument (typically followed by the need to re-calibrate), or take it down, clean the source, and have to waste nearly 2 days re-tuning and calibrating. I have tried many suggestions (including, time and again, the modified autotune suggested in an Agilent technical document that I have see many state works for them... but it doesn't hardly ever for us). Any suggestions?
What are your auto sampler/purge and trap settings? It would also help if you could post your tune.
Water in the source is a constant problem for VOA analysis with the 5975. Anything you can do to limit it will help, inlcuding dry purge, >50:1 split with a 0.18mm column, 1 minute or less desorb, etc.

There have been several threads related to this especially related to method 524.2
Is the instrument having problems tuning even after cleaning? If so, I would definitely try to resolve this before concerning anything with the GC or P&T. Have you inspected the filament or tried switching to the 2nd and tuning?

The rapid dirtying of the source (causing issues with tune) could be tied to hardware configuration and GC/MS/P&T parameters. A 6mm drawout plate in the source can help alleviate some of the issues with water. The same can be said for higher split ratios or shorter desorption times. Anything that can keep water out of the source will be beneficial.

Agilent does have a newer application note out on optimized conditions to run a 7890/5975 TAD for VOAs that might be worth taking a look at.
Nathan Valentine
Purge and Trap Product Line Manager
Teledyne Tekmar
http://www.teledynetekmar.com
http://www.teledynetekmarblog.com/
Bet you are dealing with the water issue. Agilent has a fix . It's a kit for about $1000 that works well. Includes inlet liner, inert column, and 6mm drawout plate. It also has a bfb autotune that adjusts the ion focus and repeller.
I had it installed early last month ( new drawout plate without cleaning) and so far the system is still stable.
Call the 800 number.
5 posts Page 1 of 1

Who is online

In total there are 174 users online :: 1 registered, 0 hidden and 173 guests (based on users active over the past 5 minutes)
Most users ever online was 5108 on Wed Nov 05, 2025 8:51 pm

Users browsing this forum: Google [Bot] and 173 guests

Latest Blog Posts from Separation Science

Separation Science offers free learning from the experts covering methods, applications, webinars, eSeminars, videos, tutorials for users of liquid chromatography, gas chromatography, mass spectrometry, sample preparation and related analytical techniques.

Subscribe to our eNewsletter with daily, weekly or monthly updates: Food & Beverage, Environmental, (Bio)Pharmaceutical, Bioclinical, Liquid Chromatography, Gas Chromatography and Mass Spectrometry.

Liquid Chromatography

Gas Chromatography

Mass Spectrometry