Term
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Definition
chemically inert gas such as He, CO2 or Ar that acts as the mobile phase in GC |
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Term
Draw the Gas chromatography block diagram |
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Definition
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Term
Draw the sample injection port |
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Definition
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Term
What are the 2 types of injectors |
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Definition
1)Split junction 2)Splitless junction |
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Term
Describe split junction injection |
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Definition
Ratio the amount of sample that goes to column vs waste
Provides better resolution then splitless |
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Term
Describe splitless injection |
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Definition
everything injected goes straight on the column Lower detection limits Higher sensitivity |
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Term
What are 2 types of columns |
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Definition
1)packed column 2)capilary column |
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Term
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Definition
1-5 meter long 2-4mm inside diameter not widely used, need more sample |
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Term
Describe capillary column |
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Definition
30m long .25-.32 incid diameter more theoretical plates |
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Term
What are the characteristics of ideal column? |
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Definition
1)Inert
2)Thermally stable
3)Low volatility |
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Term
Describe GC stationary phase in general |
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Definition
-Polyalkylated silanes are most common -resolution must be great enough to separate similar things out -Alternating R groups on silanes changes column characteristics |
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Term
Draw general structure for polyalkylate silane |
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Definition
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Term
Describe Chiral stationary phase |
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Definition
Separates out stereoisomers |
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Term
Draw the structure of a chiral stationary phase |
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Definition
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Term
Describe Thermostate oven |
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Definition
heats the column and sample either isocratically or by a gradient |
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Term
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Definition
Oven stays on one temperature the entire time |
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Term
Define gradient heating oven |
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Definition
Oven starts low and increases in temp over time better resoluton possibility for degradation |
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Term
What are the 4 types of detector for GC and their relative sensitivities |
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Definition
1)Mass spec 10ppb 2)Flame ionization (FID) 0.1ppm 3)Thermal conductivity (TCD) 10ppm 4)Electron capture (ECD) 0.1ppb |
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Term
Draw a flame ionization detector |
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Definition
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Term
Describe flame ionization detector |
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Definition
-Hydrocarbons ionized in the flame -measures current -Insensitive to to non combustible gases -Mass sensitive: responds to number of carbons entering per unit time |
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Term
What are the characteristics of an ideal detector? |
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Definition
- adequate sensitivity
- good stability
- linear response over several orders of magnitude
- Thermostable Rt->400+
- Short response independant of flow rate
- high reliability and easy to use
- similar response to all solutes
- non destructive
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Term
Draw a thermal conductivity detector |
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Definition
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Term
Describe thermal conductivity detector |
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Definition
Made of set of resistor for the ref and the sample. Measures difference in current Non destructive Low sensitivity, requires a lot of sample Global use |
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Term
Draw electron capture detector |
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Definition
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Term
Describe electron capture detector |
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Definition
used for environmental samples (halogenated nitrogen, phosphorous, more electronegative makes for better e- acceptor)
63Ni->63Cu+e- (beta emitter) sample accepts electrons changing current in detector
excellent sensitivity 0.1ppb |
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Term
Write out the b-emission process of an ECD. |
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Definition
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Term
Describe the principle operation of the thermal conductivity detector |
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Definition
based on the decrease in thermal conductivity of the helium or hydrogen carrier gas brought about by analyte molecules |
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Term
Describe the principle operation of the flame ionization detector |
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Definition
based on the ionization of the analyte in a small air/hydrogen flame. the ions and electrons produced are collected by a pair of biased electrodes giving rise to current |
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Term
Describe the principle operation of the electron capture detector |
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Definition
based on the attenuation by analyte molecules of a standing ion current generated in the effluent by ionization of mobile phase molecules with a beta-emitter. Electronegative functional groups are particularly effective at capturing electrons and reducing the ion current |
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