Chemistry 439
I. Objectives:
III. Procedure:
Obtain an aqueous unknown containing ethanol from your TA. You are to measure
the percent of ethanol, on a percent by volume basis, in the sample and report
both the percent and the 95% confidence limits for your determination. You will
then convert your results to a percent by weight and report that number.
Prepare a series of calibration standards by adding a known volume of absolute
(pure) ethanol to enough water to provide a known volume of solution. The most
frequently used concentration for the stock solution is 1.00%. Since the legal
limit of ethanol in blood in most states is 0.08% by volume, the working calibration
standards should be well below and above that number. Again, a convenient way to
prepare the calibration standards is to dilute the 1% stock solution to concentrations
from 0.05% to 0.20% ethanol in a water solution. You are to prepare a calibration
curve of peak area (instrument units) vs ethanol concentration using a GC to obtain the ethanol
peak areas. The instrument should be equipped with a capillary column
specifically designed to separate low molecular weight alcohols. However, alcohols
are hard to separate on gas chromatograph columns so you should expect some peak
tailing. You should also be aware that you will be working close to the method
detection limit so your best analytical technique will be required. The procedures
for operating the different instruments are inside the instrument log book.
Choose the settings for the injector, oven and detector based on your knowledge of
GC and the boiling point of ethanol (78.4 degrees C).
After making 10-15 injections, heat the detector to 275 C and the column to 250 C
to clean the column and then return to the settings above for subsequent analyses.
Heat the column as the last thing you do on the instrument
so the next group will have a clean column to start their analyses.
Report
Report the equation for the calibration curve (Y = mX + b) where mg etoh/ml of
solution is the Y coordinate and the peak area is the X coordinate. The numerical
value of the slope and intercept will be graded so be sure your units are as
specified. Determine the amount of error in your measurements and