Laboratory #1 Isolation of Carvone and Limonene from the Oil of Spearmint/Caraway Introduction The oils of spearmint and caraway are made of ch same principal components carvone, limonene, pinene but of different portions. They are used mainly in the pharmaceutical and flavor industry. Separation, Isolation, and Identification ofCarvone and Limonene The natural extract of oil will be separated to its components by using column chromatography with silica gel as stationary phase. Each fraction of eluent will be concentrated under reduced pressure to remove the solvent. The residue of each sample will be then identify using gas chromatography, mass spectrometry, and infrared spectroscopy. The separation of oils to its components will be completed by eluting the column with four different solvents in the following order: First: 30 ml petroleum ether Second: 60 ml., 19 =CH.Cl/petroleum ether Third: 25 ml, 1/4 - CH,CI/petroleum ether Fourth: 100 - 130 mL, 1/1- CH;Cl/petroleum ether Experimental Observation Fours fractions are collected corresponding to the volumes of cach solvent: Fraction A: 30 ml Fraction B: 60 ml. Fraction C: 25 ml. Fraction D: 100 – 130 ml The solvent is removed from cach fraction on the rotary evaporator. The residue mass of cach fraction is recorded. The following is observed: Residue fraction A: Probably wont yield or it will yield a very small amount. Residue fraction B: It has the first major component (assumed as pure first component). Residue fraction C: It is a mixture of the two main components Residue fraction D: It has the second major component (assumed as pure second component). Analysis and Report Analysis of Fractions: Infrared Spectroscopy and Mass Spectrometry A) From the fractions B and D, identify the functional groups using IR

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Laboratory #1
Isolation of Carvone and Limonene from the Oil of Spearmint/Caraway
Introduction
The oils of spearmint and caraway are made of ch same principal components carvone,
limonene, pinene but of different portions. They are used mainly in the pharmaceutical and
flavor industry.
Separation, Isolation, and Identification of Carvone and Limonene
The natural extract of oil will be separated to its components by using column chromatography
with silica gel as stationary phase. Each fraction of cluent will be concentrated under reduced
pressure to remove the solvent. The residue of each sample will be then identify using gas
chromatography, mass spectrometry, and infrared spectroscopy.
The separation of oils to its components will be completed by eluting the column with four
different solvents in the following order:
First: 30 ml petroleum ether
Second: 60 ml., 1/9 =CH;Cls/petroleum ether
Third: 25 mL, 1/4 - CH,Cl/petroleum ether
Fourth: 100 – 130 mL., 1/1 - CH;Cls/petroleum ether
Experimental Observation
Fours fractions are collected corresponding to the volumes of cach solvent:
Fraction A: 30 ml
Fraction B: 60 ml.
Fraction C: 25 ml
Fraction D: 100 – 130 ml.
The solvent is removed from each fraction on the rotary evaporator. The residue mass of each
fraction is recorded. The following is observed:
Residue fraction A: Probably wont yield or it will yield a very small amount.
Residue fraction B: It has the first major component (assumed as pure first component).
Residue fraction C: It is a mixture of the two main components
Residue fraction D: It has the second major component (assumed as pure second
component).
Analysis and Report
Analysis of Fractions: Infrared Spectroscopy and Mass Spectrometry
A) From the fractions B and D, identify the functional groups using IR
Transcribed Image Text:Laboratory #1 Isolation of Carvone and Limonene from the Oil of Spearmint/Caraway Introduction The oils of spearmint and caraway are made of ch same principal components carvone, limonene, pinene but of different portions. They are used mainly in the pharmaceutical and flavor industry. Separation, Isolation, and Identification of Carvone and Limonene The natural extract of oil will be separated to its components by using column chromatography with silica gel as stationary phase. Each fraction of cluent will be concentrated under reduced pressure to remove the solvent. The residue of each sample will be then identify using gas chromatography, mass spectrometry, and infrared spectroscopy. The separation of oils to its components will be completed by eluting the column with four different solvents in the following order: First: 30 ml petroleum ether Second: 60 ml., 1/9 =CH;Cls/petroleum ether Third: 25 mL, 1/4 - CH,Cl/petroleum ether Fourth: 100 – 130 mL., 1/1 - CH;Cls/petroleum ether Experimental Observation Fours fractions are collected corresponding to the volumes of cach solvent: Fraction A: 30 ml Fraction B: 60 ml. Fraction C: 25 ml Fraction D: 100 – 130 ml. The solvent is removed from each fraction on the rotary evaporator. The residue mass of each fraction is recorded. The following is observed: Residue fraction A: Probably wont yield or it will yield a very small amount. Residue fraction B: It has the first major component (assumed as pure first component). Residue fraction C: It is a mixture of the two main components Residue fraction D: It has the second major component (assumed as pure second component). Analysis and Report Analysis of Fractions: Infrared Spectroscopy and Mass Spectrometry A) From the fractions B and D, identify the functional groups using IR
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