Materials and methods 1 PROS Merry P, Masruri, Mohammad FR Study catalytic fulltext
M. Pradhita, Masruri, M.F. Rahman
SWUP
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al., 2005. Reaction was generally undertaken in room temperature until 50
o
C Maksimchuk et al., 2005. However, low selectivity and yield was always reported see Figure 1.
Figure 1. Scheme of oxidation reaction of -pinene.
Oxidation using hydrogen peroxide is interesting process since the by-product resulted is water. It is known as a green oxidator. It has efficiency of oxygen atom to convert organic
substances by 47 Noyori et al., 2003. According to Hasan and co-worker, oxidation using hydrogen peroxide is economically and ecologically advantageous. It was easily to manage,
handle, low cost, and only provided water as by product Hasan et al., 2011. Thus, applying hydrogen peroxide basically follows the principles of green oxidation. This study will report
oxidation of -pinene using hydrogen proxide and catalyzed by ironIII chloride. The result was expected can open the way to control selectivity and further application of Indonesian
turpentine oils.
2. Materials and methods 2.1
Materials
The materials used for research including turpentine oils given from PT Perhutani Anugerah Kimia, Trenggalek, East Java. Procedure and method for
-pinene purification was undertaken following Masruri et al. 2007. Other materials was some chemicals used as
bought from the manufacturer or as mentioned, including hydrogen peroxide 30 Merck, ironIII chloride Merck, ethyl acetate Smart Lab, n-hexane Smart Lab, magnesium sulfate
anhydrate Merck, pre-coated silica TLC F60 Merck, and aquadest.
2.2 Instrumentation and glassware
Some instrumentation for analysis was used such as ultraviolet-visible spectrophotometer Shimadzu UV-1601, infrared spectrophotometer Shimadzu FTIR-
8400S, and gas chromatography-mass spectrometry Shimadzu GCMS-QP2010S, refractometer Abbe, analytical balance Ohaus, and magnetic stirrer-heater. Meanwhile
some glassware applied such as a set of vacuum fractional distillation, pycnometer, TLC development glass, and other minor glassware.
2.3 Procedure for distillation of turpentine oils
Turpentine oil was distillated follow procedure from Masruri et al. 2007. A 100 mL of dried turpentine oil was placed in a round-flask from a setting of vacuum fractional
distillation apparatus. Stirring and vacuuming was undertaken until the oil boiled. The pressure and boiling point were monitored and kept constant until first fraction collected.
- Pinene was collected in the first fraction, and further analysis for its density, purity, index
refractive.
Study catalytic oxidation of
-pinene using hydrogen peroxide-ironIII chloride
SWUP
BC.92
2.4 Procedure for study oxidation reactions
A pure of -pinene 4.85 mL; 30.0 mmol in a 100-mL of round bottom flask was added ironIII chloride 8.11 g; 30.0 mmol. This mixture was setting up on the reflux
apparatus, and further added dropwise of with hydrogen peroxide 30 30.67 mL; 300 mmol. This was undertaken during 10 min, and it was further stirring at 80
o
C for 2 h. Reaction progress was monitor by spotting the reaction sampling on TLC. Disappearing of
- pinene on TLC plate as indication that reaction completed. Then, the reaction mixture was
washed with water 2 x 10 mL, and was extracted with ethyl acetate 3 x 10 mL. Combined the ethyl acetate layers was dried under magnesium sulfate anhydrate and decanted for
further concentrated using rotary evaporator. The product was further analyzed and haracterized by using GCMS and FTIR.