Quantitative Gas

Chromatography
Chem 2223 Lab Prep

1
 Goals and Objectives
• Goals
– To become familiar with basic methods of
quantitative analysis by gas chromatography

• Specific Objectives
– Use the standard additions technique to determine
the identities and concentrations of the
components in a mixture of volatile organic
compounds

2
Setup

4
Solutes and Internal Standard

Compound Structure or Formula Boiling Point, oC Relative Polarity

Methanol
CH3OH 64.6 Polar
(solvent)

Toluene 110.6 Nonpolar

Ethylbenzene 135.2 Nonpolar

p-Xylene 138.4 Nonpolar

Br
Bromobenzene
156.0 Polar
(internal standard)

9
 Internal Standard Method
• Description
– In this approach, an internal standard is added to the
sample, and the response from the analyte peak is
compared to the internal standard. This approach
corrects for minor variations in the injection volume.

• Response Factor (RF)

– The response factor accounts for differences in the
detector response between the analyte and standard.

11
Sample Chromatogram and Integration Report

IS
X
Ax Ais
Rx / is 
c x cis

AX = 27.01
AIS = 17.80
13
 Calibration Curve with Internal Standard

Standards GC Calibration Curve for Cocaine with Internal Standard

• Each contains fixed mass of internal Cocaine Int. Std.

standard, various masses of std Standard
1
mg/mL
2.50
mg/mL
5.00
cx/cis
0.500
Ax
120
Aix
600
Ax/Ais
0.200
analyte 2 5.00 5.00 1.000 241 601 0.401
3 10.00 5.00 2.000 480 600 0.800
• Calibration curve shows linear 4 25.00 5.00 5.000 1198 600 1.997

response. Slope = response factor*

Cocaine with Interal Standard
1.0 microliter injections
Ax Ais
Rx / is  2.500

c x cis 2.000
y = 0.3991x + 0.0013

1.500

Ax/Ais
Unknown
1.000
• Add known amount of internal standard
• Inject and measure Ax/Ais 0.500

• Determine cx/cis for your unknown from 0.000

0.000 1.000 2.000 3.000 4.000 5.000 6.000
calibration curve. Since cis is known, cx for cx/cis
your unknown is simply
*This expression for the response factor is not used directly in your
cx = (cx/cis)cis calculations. The following expression which accounts for the intercept is
more rigorous (in practice the intercept is very near zero). Calculations
based on the calibration data do take the intercept into account.

Ax Ais  ( y intercept) 14
Rx / is 
c x cis