In the analysis of odorants in tequila in Figure 24-21, tequila was diluted with water and extracted four times with dichloromethane(CH2Cl2) , b.p. 40CThe400mLof(CH2Cl2)was evaporated down to1mLand1μLof the extract was injected on-column onto a poly(ethylene glycol) open tubular column (30m×0.53mm,filmthickness=1μm), film thickness ) initially at and then ramped to 230C

(a) Why was the diluted tequila extracted four times with dichloromethane instead of once with a larger volume?

(b) Why was on-column injection used?

(c) Why was a poly(ethylene glycol) column chosen for this application?

(d) What was the phase ratio of the column?

(e) Why was a wide-bore 0.53-mm-diameter column chosen for this application?

Short Answer

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(a). As a result, diluted tequila is extracted four times with dichloromethane rather than once at a higher volume.

(b).On-column injection minimises the likelihood of heat degradation as well as the odour of a larger number of molecules.

(c). The use of poly (ethylene glycol) in the column is due to the fact that poly (ethylene glycol) is a polar column, which is ideal for polar analytes.

(d).The column's phase ratio βis 132.

(e).As a result, a wide-bore column with a diameter of0.53mm enables for bigger injections of compounds, the scent of the components can be recognised during elution.

Step by step solution

01

Definition of dichloromethane

  • Methylene chloride, often known as dichloromethane, is a colourless liquid with a slight pleasant odour that evaporates quickly and does not burn easily.
  • It's frequently used as a paint stripper and an industrial solvent.
02

Determine the diluted tequila extracted four times with dichloromethane instead of once with a larger volume

(a)

  • It must be explained why diluted tequila is extracted four times with dichloromethane rather than once with a larger volume.
  • To explain why diluted tequila is extracted four times with dichloromethane instead of once with a larger volume.
  • Small extractions repeated several times have been found to be more significant than a single extraction. As a result, diluted tequila is extracted four times with dichloromethane rather than once at a higher volume.
03

Determine the on-column injection

(b)

  • It is necessary to explain why on-column injection is used.
  • On-Column Injection: For thermally sensitive chemicals, on-column injection is the optimum method for quantitative analysis.
  • It's a low-resolution approach that won't work for columns smaller than a certain diameter0.2mm.
  • On-column injection can be used to handle both large and small amounts of dilute and concentrated solutions.
  • To describe how on-column injection is used.
  • On-column injection minimises the likelihood of heat degradation as well as the odour of a larger number of molecules.
04

Determine the poly(ethylene glycol) column chosen for this application 

(c)

  • It is necessary to explain why a poly (ethylene glycol) column was used.
  • To describe how to use a poly (ethylene glycol) column
  • The retention index of the compounds is determined by the total polarity phases as well as the selectivity of each column's polar interaction types.
  • The use of poly (ethylene glycol) in the column is due to the fact that poly (ethylene glycol) is a polar column, which is ideal for polar analytes.
05

Determine the phase ratio of the column

(d)

It is necessary to compute the phase ratio β

Phase ratio β

The dimensionless phase ratio is the volume of the mobile phase divided by the volume of the stationary phase. The phase ratio is determined as follows:

β=r2dr

Where,βphase ratio

r is the column's radius.

df=temporalthicknessofthestationaryphaseIncreaseinthicknessofstationaryphase,decreasesinβthatincreasestheretentiontimeandcapacityofsample.TofigureoutthephaseratioβGiven,Diameterofcolumn=0.53mmThickness=1μmThecolumn'sphaseratioiscomputedas,β=r2dtβ=0.265mm0.002mmβ=132Thecolumn'sphaseratioβis=132.

06

 Step 6: Determine the wide-bore 0.53-mm-diameter column chosen forthis application

(e)

  • The reason for the wide-bore column's0.53mm diameter must be explained.
  • To explain why a wide-bore column with a diameter of0.53mm was chosen.
  • Because a wide-bore column with a diameter of 0.53mmenables for bigger injections of compounds, the scent of the components can be recognised during elution.

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Most popular questions from this chapter

This problem reviews concepts from Chapter 23. An unretained solute passes through a chromatography column in 3.7 min and analyte requires 8.4 min.

(a) Find the adjusted retention time and retention factor for the analyte.

(b) Find the phase ratio b for a 0.32-mm-diameter column with a 1.0-mm-thick film of stationary phase.

(c) Find the partition coefficient for the analyte.

(d) Determine the retention time on a similar length of 0.32-mm diameter column with a 0.5-mm-thick film of the same stationary phase at the same temperature.

(a) Write the meaning of the retention factor, , in terms of time spent by solute in each phase. (b) Write an expression in terms of for the fraction of time spent by a solute molecule in the mobile phase. (c) The retention ratio in chromatography is defined as

R=timeforsolventtimeforsolutetopassthroughcolumn=tmtrShow that is related to the retention factor by the equationR=1/k+1

Genotoxic compounds damage DNA and cause mutations or cancer.Regulatory guidelines limit genotoxic impurities in pharmaceuticals. Mesityl oxide (4-methyl- 3-penten-2-one) is an intermediate product in the synthesis of some drugs. Search the literature for a gas chromatography method for the determination of mesityl oxide in the pharmaceutical enalapril maleate and answer the following questions.

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