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Configuring the GC/MS System for Pesticide Analysis Configuring the GC/MS System for Pesticide Analysis The analytical setup and method parameters in this document describe the basic setup for the quantitative analysis of pesticides using the TSQ Quantum GC mass spectrometer, TRACE GC Ultra gas chromatograph, and TriPlus autosampler. The method parameters have been selected to balance the analytical requirements for a large number of pesticides covering a wide range of volatility, chemical and chromatographic characteristics. Analyzing limited subsets of pesticides only with partial optimization for specific compound classes will improve separation and allow you to analyze faster. Customize the method template to include the particular compounds you are specifically looking for. The use of consumable components, such as insert liners, pre-columns and analytical column, has been tested by Thermo Fisher Scientific application laboratories for optimum analytical performance and sample throughput. TRACE GC Ultra The TRACE GC Ultra can be configured for Split/Splitless (SSL) or Programmable Temperature Vaporizing (PTV) injection techniques. The SSL injector can be used to analyze pesticide compounds in very low concentrations and for relatively dirty matrices. The PTV injector, however, allows you to vary the injection volume and temperature, which can lower detection limits and better analyze thermally sensitive compounds. Thermo Scientific Pesticide Analyzer Reference 29
Configuring the GC/MS System for Pesticide Analysis PTV Injector There are two types of PTV injectors that can be used for pesticide analysis: • The Brightly Enhanced Sample Transfer (BEST) PTV injector contains very low thermal mass components and can achieve very fast heating and cooling rates. This type of PTV injector maintains unprecedented sample integrity using the specially designed inert liners and the long vaporizing chamber with reduced internal diameter. It can provide a virtual discrimination-free sample transfer in any situation, even when using high boiling-point samples. The PTV injector’s compatibility with dirty samples makes it the ideal complement to the cold on-column injector. • The Large Volume BEST PTV injector has the same capabilities of the standard PTV injector, but it can accept larger injection volumes. This type of injector is compatible with dirty sample matrices. It is recommended for injection volumes > 10 μL, which can be injected all at once, while larger volumes can be programmed to inject slowly. Note The injection of larger solvent volumes strongly reduces the effect of active surfaces during the injection process, which is caused by the surrounding solvent vapor momentarily protecting the labile pesticide compounds. For example, when using Endrin breakdown as a tool for diagnosing issues with excessive injection port activity. Sample preparation time is greatly reduced by shortening the extract evaporation times. The use of a pre-column for matrix samples is recommended for pesticide analysis. Typically, a pre-column is an empty 0.53 mm inner diameter column of standard length, as determined by the type of injection volume. When injected, matrix samples are typically deposited in the insert liner and pre-column. The analytical column is protected from the entry of low volatile matrix components, which preserves the calibrated retention times and extends the life of the column. We recommend that you occasionally clean and maintain the injector, replace the insert liner, and replace the pre-column. Always use the appropriate mini-unions or a glass press-fit connector to connect the pre-column. Be aware that leaks can occur when using glass press-fit connectors with temperature programmed methods. For increased efficiency when injecting samples, you can upgrade the TRACE GC Ultra with a PTV backflush system, which eliminates the irrelevant parts of a dirty sample during the cleaning phase. Depending on your injection volume preference, there are two types of backflush systems available: 30 Pesticide Analyzer Reference Thermo Scientific
Page 1 and 2: Pesticide Analyzer Reference
Page 3 and 4: © 2009 Thermo Fisher Scientific In
Page 5 and 6: Contents 4 Pesticide Analyzer Refer
Page 7 and 8: Introduction Modern analytical meth
Page 9 and 10: About This Manual This manual also
Page 11 and 12: What is a Pesticide? Pesticide Chem
Page 13 and 14: What is a Pesticide? Table 2. Pesti
Page 23 and 24: Preparing Samples Preparing Samples
Page 25 and 26: Preparing Samples Extracting Sample
Page 27 and 28: Preparing Samples 5. Place the tube
Page 29 and 30: Preparing Samples Exchanging Solven
Page 31 and 32: Preparing Samples 5. Centrifuge the
Page 33: Setting Up a Method 9. Now you can
Page 37 and 38: Configuring the GC/MS System for Pe
Page 53 and 54: List of Pesticide Compounds Table 2
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List of Pesticide Compounds Table 2
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SRM Method Library Table 27. Compou
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References References 1. Anastassia
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