The effects of inlet liner configuration and septum purge flow rate on discrimination in splitless injection

Hinshaw, John V.

doi:10.1002/jhrc.1240160409

Cited by 12 publications

(3 citation statements)

References 16 publications

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“…chamber (1 mL) is often too small to reliably hold the sample vapor. 25,26 mixing with carrier gas increases capacity more than proportionally to the volume and should enable injection of about 2 µL of methanol (1.5 mL of vapor at 30 kPa and 250 °C), 1 µL of water (1500 µL), 3.5 µL of dichloromethane (1600 µL), or 6 µL of hexane (1550 µL). With an inlet pressure of 160 kPa, the capacity is approximately doubled.…”

Section: Consequences For the Injector Designmentioning

confidence: 99%

“…It has been known for a long time that the internal volume of a 80 × 4 mm i.d. chamber (1 mL) is often too small to reliably hold the sample vapor. , At modest inlet pressures it does not even house the vapor of 1 μL of a solution in methanol. Overloading is frequent and serious effects on quantitative analysis have been reported (e.g., refs and ).…”

Section: Consequences For the Injector Designmentioning

confidence: 99%

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The Two Options for Sample Evaporation in Hot GC Injectors: Thermospray and Band Formation. Optimization of Conditions and Injector Design

Grob¹,

Biedermann²

2001

Anal. Chem.

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Although classical split and splitless injection is more than 30 years old, we only start to understand the vaporization process in the injector. Solvent evaporation determines much of the process and is the first obstacle to overcome. Videos recorded on devices imitating injectors showed that sample (solvent) evaporation is often a violent process which is poorly controlled and might well explain many of the puzzling quantitative results often obtained. We do not adequately take into account that two vaporization techniques are in use. Partial solvent evaporation inside the syringe needle (optimized as "hot needle injection") produces thermospray: the sample liquid is nebulized upon leaving the needle. The resulting fog is rapidly slowed and moves with the gas. Solute evaporation largely occurs from microparticles suspended in the gas phase. Empty liners are most suitable. Fast autosamplers suppress vaporization in the needle, i.e., nebulization, and shoot a band of liquid into the chamber that must be stopped by a packing or obstacles suitable to hold the liquid in place during the 0.2-5 s required for solvent evaporation. Solute evaporation largely occurs from the surfaces onto which the sample is deposited. Insights into these mechanisms help optimize conditions in a more rational manner. Methods should specify whether they were optimized and validated for injection with thermospray or band formation. The insights should also enable a significant improvement of the injector design, particularly for splitless injection.

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Section: Consequences For the Injector Designmentioning

confidence: 99%

Section: Consequences For the Injector Designmentioning

confidence: 99%

The Two Options for Sample Evaporation in Hot GC Injectors: Thermospray and Band Formation. Optimization of Conditions and Injector Design

Grob¹,

Biedermann²

2001

Anal. Chem.

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“…Evaporates are divided into the GC column and the high flow split gas path to establish short injection times. There have been many efforts to optimize this technique by optimal syringe operation 3, special design of the inlet 4 and flow control procedures (e.g. split/splitless injection 5).…”

Section: Introductionmentioning

confidence: 99%

Construction of a thermodesorption injector for gas chromatography

Schröder

2011

J of Separation Science

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A detailed description for the do-it-yourself construction of a high-performance thermodesorption GC injector (HPTI) is presented. The injector consists of a heated desorption chamber, a cooled loop for focusing the desorbed volatiles as well as a heating control for sample injection into the separation column. The gas flow is controlled by valve switching during the steps of the operation. Two versions of the injector function either for the injection of highly volatile compounds or for compounds with extremely low volatility, e.g. lubricants. The sophisticated gas flow management allows injection of highly concentrated samples without memory effects in a sample gas split mode, while traces may be injected with virtually 1:1 sample transfer. A wide range of adsorbents appropriate for the compounds can be chosen due to homemade adsorbent tubes and the achievability of high desorption temperature. Solutions may be injected from a carrier material after solvent evaporation. The HPTI fulfills all multipurpose GC injector requirements and with the support of downloadable instruction files can be built by anyone working with conventional GC devices.

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Determination of absolute amount extracted by solid-phase microextraction: Different approaches under examination

2000

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The effects of inlet liner configuration and septum purge flow rate on discrimination in splitless injection

Cited by 12 publications

References 16 publications

The Two Options for Sample Evaporation in Hot GC Injectors: Thermospray and Band Formation. Optimization of Conditions and Injector Design

The Two Options for Sample Evaporation in Hot GC Injectors: Thermospray and Band Formation. Optimization of Conditions and Injector Design

Construction of a thermodesorption injector for gas chromatography

Determination of absolute amount extracted by solid-phase microextraction: Different approaches under examination

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