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The graph shows van Deemter curves for n-nonane at . in the 3.0-m-long microfabricated column in Box 24-2 with a -thick stationary phase.

van Deemter curves. [Data from G. Lambertus, A. Elstro, K. Sensenig, J. Potkay, M. Agah, S. Scheuening, K. Wise, F. Dorman, and R. Sacks, "Design, Fabrication, and Evaluation of Microfabricated Columns for Gas Chromatography," Anal. Chem. 2004, 76, 2629.]

(a) Why would air be chosen as the carrier gas? What is the danger of using

air as carrier gas?

(b) Measure the optimum velocity and plate height for air and for carrier

gases.

(c) How many plates are there in the 3 -m-long column for each carrier gas at

optimum flow rate?

(d) How long does unretained gas take to travel through the column at

optimum velocity for each carrier gas?

(e) If stationary phase is sufficiently thin with respect to column diameter, which of the two mass transfer terms (23-40 or 23-41) becomes negligible?

Why?

(f) Why is the loss of column efficiency at high flow rates less severe for

than for air carrier gas?

Short Answer

Expert verified

(a.) better resolution can be achieved with the application of H2. Using air as carrier gas can degrade the stationary phase because it contains traces of O2,H2O, and organic compounds. The ideal carrier gas must be of high quality and should not contain the compounds mentioned.

VH2=7mm50cm/s16.5mmb..=21.21cm/sVAir=3mm50cm/cm16.5mm=9.09cm/sNH2=LHAirc=3m0.04cm1m100cm=7500tH2=3m21.21cms1m100cmd.=14.14stAir=3m9.09cms1m100cm33.0sCm=1+6k+11k224(k+1)2r2Dme.Cs=2k3(k+1)2d2Dm

(f.) The loss of column efficiency at high flowrates is less severe for than Air because the former can be run much faster than its optimal velocity with small depreciation in resolution. This is because solutes can diffuse more rapidly in H2than in Air.

Step-by-step-solution

List the given:

-T=Temperature=70-L=Columnlengh=3.0m-Thicknessofstationaryphase=1-2渭尘

Step by step solution

01

To finding the danger of using air as carrier gas

(a)

Based on the given plot,H2 has a higher optimal velocity than Air. Thus, a faster separation can be achieved by using H2as carrier gas than Air. Furthermore, better resolution can be achieved with the application of H2 . Using air as carrier gas can degrade the stationary phase because it contains traces of O2,H2O, and organic compounds. The ideal carrier gas must be of high quality and should not contain the compounds mentioned.

02

To Measure the optimum velocity and plate height for air and for carrier gases

(b).

To acquire the optimum velocity, get the minimum point of the curves forH2VH2and AirVAirthen read the corresponding value in the x-axis.

Perform approximations by measuring the length of a known velocity in the graph and solve for the unknown values by measuring the length and applying ratio and proportion.

The length of a retention time

50cm/sis16.5mm=xintheplot.ThedistanceofVH2andVAirfromthestartingpointare7mmand3mm,respectively.

Compute for the corresponding values of optimum velocity of H2and Air by ratio and proportion:

VH2=7mm50cm/s16.5mm=21.21cm/sVAir=3mm50cm/s16.5mm=9.09cm/s

03

To finding plates are there in the 3 -m-long column for each carrier gas at optimum flow rate

(c)

To acquire the number of platesN, first get the plate heightHrom the

corresponding values in the y-axis based on the minimum point of the curves for

H2HH2andAirHAir.

The length of a retention time of 0.05 cm is 7 mm. The distances ofHH2andHAirfrom the starting point are 7 mm and 5 mm, respectively.

Compute for the corresponding values of the plate height of H2and Air by ratio and

proportion:

localid="1655028203697" HH2=7mm0.5cm7mm=0.05cmHAir=5mm0.05cm7mm=0.04cm

Calculate the number of plates of H2NH2 :

NH2=LHH2=3m0.05cm1m100cm=6000

Calculate the number of plates of AirNAir:

NH2=LHAir=3m0.04cm1m100cm=7500

04

unretained gas take to travel through the column at optimum velocity for each carrier gas

(d).

To compute for the time of unretained H2tH2andAirtAirto travel through the

column at optimum velocity, divide the length of the column by the velocity of each

carrier gas:

tH2=3m21.21cms1m100cm=14.14stAir=3m9.09cms1m100cm=33.0

05

To finding the  two mass transfer terms (23-40 or 23-41) becomes negligible

(e).

For a thin stationary phase ,(^0.5渭尘) ,the mass transfer is dominated by slow diffusion through the mobile phase(CCm)( than through the stationary phase CSThatis, Cs<<Cmin Equations 23-40 and 23-41.

The expressions for Cmand CSare shown below:

Cm=1+6k+11k224(k+1)2r2Dm

where:

-K=retentionfactor-r=columnradius-d=thicknessofstationaryphase-Dm=diffusioncoefficientofsoluteinmobilephase-Ds=diffusioncoefficientofsoluteinstationaryphase

By examining the expressions, we can observe that CSis directly proportional

to the thickness of the stationary phase. Thus, this term becomes negligible as compared

to Cmwhen the stationary phase is sufficiently thin with respect to column diameter.

06

Finding  the loss of column efficiency at high flow rates less severe for H2 than for air carrier gas

(f).

The loss of column efficiency at high flowrates is less severe for H2than Air because the former can be run much faster than its optimal velocity with small depreciation in resolution. This is because solutes can diffuse more rapidly in H2than in Air.

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Most popular questions from this chapter

Astandard solution containing 6.310-8Miodoacetone and 2.010-7Mp-dichlorobenzene (an internal standard) gave peak areas of 395 and 787, respectively, in a gas chromatogram. A 3.00-mlunknown solution of iodoacetone was treated with 0.100mLof 1.610-5Mp-dichlorobenzene and the mixture was diluted to. Gas chromatography gave peak areas of 633 and 520 for iodoacetone and p-dichlorobenzene, respectively. Find the concentration of iodoacetone in the 3.00mLof original unknown.

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(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?

Retention time depends on temperature, T, according to the equation log t鈥r =(a/T) + b, where a and b are constants for a specific compound on a specific column. A compound is eluted from a gas chromatography column at an adjusted retention time t鈥r =15.0 min when the column temperature is 373K. At 363 K, t9r 5 20.0 min. Find the parameters a and b and predict t鈥r at 353K

(a) How can you improve the resolution between two closely spaced peaks in gas chromatography?

(b) What approach from (a) would be most cost effective (not involve a purchase)?

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