Laboratorio De Analisis Instrumental: Quimica

University of Puerto Rico

Mayagüez Campus

Chemistry Department

Experiment # 1:

GC-FID: Analysis of a Non-acetone Polish Remover by Gas Chromatography with Flame Ionization Detector

Melanie Acevedo

Limarie Méndez

Andrea C. Rodríguez

QUIM 4015 L

Dr. Marcos A. De Jesús

I. Title: GC-FID: Analysis of a Non-acetone Polish Remover by Gas Chromatography with FlameIonization Detector

II. Dates:
Date experiment started: September 16, 2008
Date experiment ended: September 16, 2008
Date Report was submitted: September 26, 2008

III. Experimental:
Of the ethanol and ethyl acetate standard solutions, 4mL of each were quantitatively transferred to form the mixed standard stock in a 10mL beaker. This solution was thendissolved in toluene.

IV. Results and Discussion
In this experiment a Hewlett Packard Gas Chromatograph 5890 Series II with flame ionization detector and autosampler was used to qualitatively and quantitatively analyze the volatile components, ethanol and ethyl acetate, found in the non-acetone based nail polish remover using isothermal and gradient temperature methods. Perfectionnon-acetone nail polish remover was chosen as a model of pharmaceutical and personal care products because it contains various organic compounds that are considered emerging contaminants of environmental concern.

The column used for the experiment was a Supelco SPB-5 (30m x 0.25cm); a fused silica capillary column with a nonpolar stationary phase. The inert mobile phase carried 1µLof the solution, added by splitless injection, into the chromatographic column at a temperature of 190°C. The chromatogram of the individual identification standard of ethanol contained two large peaks. The retention time of the first peak was 3.227min and it contained an area of 2.43E5counts*s, while the largest peak had an area of 7.42E7counts*s and a retention time of 8.448min. The compoundsfound in the standard were the analyte of interest, ethanol (alcohol), and the solvent toluene (aromatic hydrocarbon). Since the stationary phase was nonpolar, and ethanol is more polar and has a smaller boiling point than toluene, it was determined that the first compound to elute was ethanol followed by toluene. This was also confirmed by the large area of the peak attributed to toluene,because as the solvent it had a much larger concentration than the analyte of interest.

Ethyl acetate was the other compound that was analyzed to determine the percentage of it in a non-acetone polish remover. The chromatogram of the ethyl acetate standard contained two large peaks as well; one at 4.415min and the other at 8.458min. The first peak was attributed to ethyl acetate since itwas previously established that the solvent eluted at around 8min.

The standards were prepared by a standard additions method with 0, 30, 40 and 50µL of the mixed standard solution and 1mL of non-acetone nail polish remover (NAP) dissolved in toluene. The first standard did not contain the mixed standard solution, only NAP. This was the only standard that was analyzed with both theisothermal and gradient temperature methods (figure 1). Using the isothermal method it was determined that NAP contained ethanol and ethyl acetate after comparing with the retention time of the respective identification standards. The retention time of ethanol in the first standard was of 3.315min and ethyl acetate eluted at 4.501min. The peaks of the analytes of interest and of toluene were thelargest peaks observed. This order of elution could also be determined based on polarity and boiling point. Ethanol is the most polar compound so it won’t react with the nonpolar stationary phase, therefore it eluted first. The second compound to elute was ethyl acetate because it is less polar than ethanol but more polar than toluene. The chromatogram also contained several small peaks that...