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

(b) What is the advantage of pressure programming?

Short Answer

Expert verified

(a.) as the temperature continue to increase, the solutes become less retained and are eluted which then emerge as sharp peaks.

Decomposition of the stationary phase and "bleeding" of column can result from high temperatures. Peak broadening, tailing, and changing retention times are some indications of column degradation.

(b.) an advantage of programmed pressure is that is can be used for analytes that cannot withstand high temperatures.

Step by step solution

01

Step 1: To find the the advantages and disadvantages of temperature programming in gas chromatography 

(a)

Temperature programming in gas chromatography is performed by increasing the temperature of the column during the separation to raise analyte vapor Pressure and reduce retention times of late-eluting components. In this procedure, the solutes are strongly retained at the head of the column. Furthermore, as the temperature continue to increase, the solutes become less retained and are eluted which then emerge as sharp peaks.

Temperature limits in most gas chromatography columns indicate at which temperature the device must operate. Operating the column at the lower temperature limit may result to poor peak shape and other performance related complications. In terms of the upper temperature limit, two maximum values are considered. One is the isothermal temperature limit, which is the lower value, at which the column can be operated for extended durations. The upper value, the programmed temperature, is the condition at which the column should only be exposed for a few minutes at the end of a programmed temperature run. Decomposition of the stationary phase and "bleeding" of column can result from high temperatures. Peak broadening, tailing, and changing retention times are some indications of column degradation

02

Step :2  Find the  advantage of pressure programming

(b).

Pressure programming in gas chromatography is executed by applying pressure control for the carrier gas. An increase in inlet pressure results to increase in mobile phase flow rate and reduction in retention time. Pressure programming can be used as an alternative to temperature programming to decrease the retention times of late-eluting components. In this procedure, the pressure can be quickly reduced to its initial value at the end of the run and be instantly ready for the next run. Thus, waiting for the hot column to cool down before the next process is not required. Furthermore, an advantage of programmed pressure is that is can be used for analytes that cannot withstand high temperatures.

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Most popular questions from this chapter

When 1.06 mmol of 1-pentanol and 1.53 mmol of 1-hexanol were separated by gas chromatography, they gave peak areas of 922 and 1570 units, respectively. When 0.57 mmol of pentanol was added to an unknown containing hexanol, the peak areas were 843:816 (pentanol:hexanol). How much hexanol did the unknown contain?

(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?

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?

Consider the chromatography of n-c12H26on a 25 m 脳 0.53 mm open tubular column of 5% phenyl鈥95% methyl polysiloxane with a stationary phase thickness of 3.0 渭尘and He carrier gas at 125潞C. The observed retention factor for n-c12H26is 8.0. Measurements were made of plate height, H, at various values of linear velocity,xm/s. A least-squares curve through the data points is given by

localid="1654864230381" H(m)=(6.010-5m2/s)/x+(2.0910-3s)xthecoefficientsofthevanDeemterequation,findthediffusioncoefficientofn-c12H26inthemobileandstationaryphases.Whyisoneofthesediffusioncoefficientssomuchgreaterthantheother?

(a) When would you use split, split less, or on-column injection in gas chromatography?

(b) Explain how solvent trapping and cold trapping work in split less injection.

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