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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.

Short Answer

Expert verified

Given:

- tm = time travelled in chromatography column by unretained solute

=3.7min

- role="math" localid="1654785649415" tr= retention time =8.4 min

Find:

role="math" localid="1654785698532" -tr'=adjustedretentiontime-kretentionfactor

Step by step solution

01

 a) adjusted retention time and factor

Compute the adjusted retention time(tr')by applying the formula below:

tr'=tr-tm

8.4min-3.7 min

4.7 min

The retention factor is the time required to elute that peak minusthe time from mobile phase to pass through the column, expressed in multiples oftm. Calculate the retention factor using the formula below:

k=tr-tmtm=8.4min-3.7min3.7min

02

b) phase ratio

GIVEN:

- Diameter of column =0.32mm

- Thickness of stationary phase =1.0渭尘

Find: phase ratiorole="math" localid="1654785803260"

The phase ratio role="math" localid="1654785811025" is the volume of the mobile phase divided by the volume of stationary phase. It can be deduced to the following expression:

=r2df

where:

-r=columnratio-df=stationaryfasefilmthickness

Solve for the phase ratio:

=0.32/2mm21.0渭尘1mm1000渭尘=80

03

c) partition coefficient

Find: partition coefficient(K)of the analyte

The retention factor (k)is related to the partition coefficient role="math" localid="1654783983446" (K)and phase ratio (), based on the following expression:

k=K

Thus, the partition coefficient (K)can be calculated by rearranging the expression:

K=k

=1.2780=101.6

04

d) retention time

Given:

- Diameter of column =0.32mm

- Thickness of stationary phase=0.5渭尘

Find: retention time(tr)of the same stationary phase and at the same temperature

Based on the formula of phase ratio role="math" localid="1654785312894" (), decreasing the thickness of the stationary phase, increases the role="math" localid="1654785292964" .

Calculating the new phase ratio role="math" localid="1654784786511" :

role="math" localid="1654785571991" '=0.32/2mm20.5m1mm1000m=160

Thenewphaseratio'is2timestheoriginalvalue.

'=2

Thus,theretentiontimetmisexpectedtodecrease.Then,computeforthenewretentionfactork':

k'=K'

thus,

k'=K2=121.27=0.635

Lastly, compute for the retention time tr:

k'=0.635=tr-3.73.7tr=6.05min

05

final answer

a)k=1.27b)=80c)K=101.6D)tr=6.05min

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Most popular questions from this chapter

(a) Use Trouton's rule, Hvap(88Jmol-1K-1)Tbp, to estimate the enthalpy of vaporization of octane (b.p. 126).

(b) Use the form of the Clausius-Clapeyron equation below to estimate the vapor pressure of octane at the column temperature in Figure 24-9(70C)

In(P1P2)=-(HvapR)(1T1-1T2)

(c) Calculate the vapor pressure for hexane (b.p. 69C) at70C

(d) What is the relationship between solute vapor pressure and retention?

(e) Why is the technique called "gas chromatography鈥 if retained analytes are only partially vaporized?

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

(a) What are the advantages and disadvantages of temperature programming in gas chromatography?

(b) What is the advantage of pressure programming?

(a) Why is it illogical to use a thin stationary phase (0.2 碌m) in a wide-bore (0.53-mm) open tubular column?

(b) Consider a narrow-bore (0.25 mm diameter), thin-film (0.10 碌m) column with 5 000 plates per meter. Consider also a wide-bore (0.53 mm diameter), thick-film (5.0 碌m) column with 1500 plates per meter. The density of stationary phase is approximately 1.0 g/mL. What mass of stationary phase is in each column in a length equivalent to one theoretical plate? How many nanograms of analyte can be injected into each column if the mass of analyte is not to exceed 1.0% of the mass of stationary phase in one theoretical plate?

Use Table 24-2 to predict the elution order of the following compounds from columns containing (a) poly (dimethyl siloxane), (b) (diphenyl)0.35(dimethyl)0.65polysiloxane, and (c) poly (ethylene glycol): hexane, heptane, octane, benzene, butanol, 2-pentanone.

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