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To which kinds of analyses do the following gas chromatography detectors respond?

(a) thermal conductivity

(b) flame ionization

(c) electron capture

(d) flame photometric

(e) nitrogen-phosphorus

(f) photo ionization

(g) sulfur chemiluminescence

(h) atomic emission

(i) mass spectrometer

(j) vacuum ultraviolet

Short Answer

Expert verified

(a.) Thermal conductivity detectors are simple and universal, which means that they react to all analyses. This makes these detectors to be frequently used in gas chromatography in the past. The thermal conductivity of the carrier gas must be completely different from the analyses, for thermal conductivity detection to proceed.

(b.)CH+Oโ†’CHO++e-

(c.) Electron capture detectors respond to halogen-containing molecules, conjugated carbonyls, nitrites, nitro compounds, and organ metallic compounds

(d.) Flame photometric detectors can control optical emission from phosphorus, sulfur, lead, tin, or other elements. The excited electrons of these elements emit characteristic light when the elute passes through a H2-air flame

(e.) Nitrogen-phosphorus detector (or alkali flame detector) is a type of flame ionization detector that is modified in such a way that it is sensitive to and -including compounds. It responds 104-106timesgreater to N and P than to carbon. Its applications include drug, pesticide, and herbicide analyses.

(f.) It has relatively low sensitivity to saturated hydrocarbons or halocarbons. The electrons produced by the ionization are collected and calculated.

(g) The intensity of the emission is proportional to the Mass of sulfur eluted and the detector responds107 times greater to S than to C.

(h) An atomic emission detector detects the characteristic emission of elements through a photodiode array polychromatic. Its sensitivity for sulfur is up to 10 times greater than the sensitiveness of flame photometric detection.

(i) Mass spectrometers are sensitive to most analytes. It can detect chromatographic peak by comparing its spectrum with a library of spectra.

(j) A vacuum ultraviolet absorbance can detect most analytes, with a detection limit of 15-250 pg.

Step by step solution

01

thermal conductivity

(a)

Thermal conductivity detectors are simple and universal, which means that they respond to all analyses. This makes these detectors are frequently used in gas chromatography in the past. The thermal conductivity of the carrier gas must be completely different from the analyses, for thermal conductivity detection to proceed. The most frequently used carrier gas is helium because it has the second highest thermal conductivity next toH2 , thus the conductivity of the gas stream is reduced with any analyte mixed with H2.

02

Step 2: flame ionization

(b)

Flame ionization detectors respond to most hydrocarbons with near constant response per carbon atom , but with lesser response for C bonded N to O . Flame ionization does not respond to no hydrocarbons such asH2,He,N2,O2,CO,CO2,H2O,NH3,NO,H2SandSiF4 . When this detector operates, the elute is burned in a mixture of H2 and air. The carbon atoms create CH radicals which are then converted toCHO+ ions and electrons in the flame, as shown in the reaction below:

CH+Oโ†’CHO++e-

03

electron capture

(c).

Electron capture detectors respond to halogen-containing molecules, conjugated carbonyls, nitrites, nitro compounds, and organ metallic compounds. However, they are relatively insensitive to hydrocarbons, alcohols, and ketoses. These detectors are applied to chlorinated pesticides and fluorocarbons in environmental samples.

04

Step 4: flame photometric

(d).

Flame photometric detectors can measure optical emission from phosphorus, sulfur, lead, tin, or other elements. The excited electrons of these elements emit characteristic light when the elute passes through a H2 -air flame. The emission of phosphorus at 526nm or sulfur at 394nm is isolated by a narrow-band interference filter and detected with a photomultiplier tube. The detector responds 105 times greater to sulfur and phosphorus compounds than to hydrocarbons. This enables the recognition of trace sulfur compounds that contribute to the aroma of beer.

05

Step 5: nitrogen-phosphorus

(e).

Nitrogen-phosphorus detector (or alkali flame detector) is a type of flame ionization detector that is modified to become sensitive to N and P -containing compounds. It responds 104-106times greater to N and P than to carbon. Its applications include drug, pesticide, and herbicide analyses.

06

Step 6: photo ionization

(f)

A photo ionization detector ionizes aromatic and unsaturated compounds by employing a vacuum ultraviolet source. It has relatively low sensitivity to saturated hydrocarbons or halocarbons. The electrons produced by the ionization are collected and measured.

07

Step 7: sulfur chemiluminescence

(g).

A sulfur chemiluminescence detector analyzes the exhaust from a flame ionization detector, wherein sulfur is oxidized toSO, and mixes it with ozoneO3to form an excited state of SO2 that emits blue and ultraviolet radiation. The intensity of the emission is proportional to the Mass of sulfur eluted and the detector responds times greater to S than to C.

08

Step 8: atomic emissionatomic emission

(h).

An atomic emission detector detects the characteristic emission of elements thru a photodiode array polychromatic. Its sensitivity for sulfur is up to 10 times greater than the sensitivity of flame photometric detection.

09

Step 9: mass spectrometer

(i).

Mass spectrometers are sensitive to most analytes. It can identify a chromatographic peak by comparing its spectrum with a library of spectra.

10

vacuum ultraviolet

(J).

A vacuum ultraviolet absorbance can detect most analytes, with a detection limit of 15-250 pg.

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Most popular questions from this chapter

(a) When a solution containing234mg of pentanol (FM 88.15) and237mg of 2,3 -dimethyl-2-butanol (FM 102.17) in10.0ml was separated, relative peak areas were pentanol: 2,3 -dimethyl-2-butanol = 0.913 : 1.00. Considering pentanol to be the internal standard, find the response factor for 2,3 -dimethyl-2-butanol.

(b) Use Equation 24-8 to find the areas for pentanol and 2,3 -dimethyl-2-butanol in Figure 24-8.

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The antitumor drug gimatecan is available as nearly pure (S)-enantiomer. Neither pure (R)-enantiomer nor a racemic (equal) mixture of the two enantiomers is available. To measure small quantities of (R)-enantiomer in nearly pure (S)-gimatecan, a preparation was subjected to normal-phase chromatography on each of the enantiomers of a commercial, chiral stationary phase designated (S,S)- and (R,R)-DACH-DNB. Chromatography on the (R,R)-stationary phase gave a slightly asymmetric peak at tr 5 6.10 min with retention factor k 5 1.22. Chromatography on the (S,S)- stationary phase gave a slightly asymmetric peak at tr 5 6.96 min with k 5 1.50. With the (S,S) stationary phase, a small peak with 0.03% of the area of the main peak was observed at 6.10 min.

Chromatography of gimatecan on each enantiomer of a chiral stationary phase. Lower traces have enlarged vertical scale. [Data from E. Badaloni, W. Cabri, A. Ciogli, R. Deias, F. Gasparrini, F. Giorgi, A. Vigevani, and C. Villani, โ€œCombination of HPLC โ€˜Inverted Chirality Columns Approachโ€™ and MS/MS Detection for Extreme Enantiomeric Excess Determination Even in Absence of Reference Samples.โ€ Anal. Chem. 2007, 79, 6013.]

(a) Explain the appearance of the upper chromatograms. Dashed lines are position markers, not part of the chromatogram. What Problems 709 would the chromatogram of pure (R)-gimatecan look like on the same two stationary phases?

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(c) Find the relative retention (a) for the two enantiomers on the (S,S)-stationary phase.

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(b) What is the instrumental method used?

(c) What type of column was used?

(d) What quantification method is used?

(e) What are the precision, limit of detection, limit of quantification, and linear range of the method?

(f) For how long could a standard solution be used?

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