CHAPTER THREE 3.
0 MATERIAL AND METHODS This chapter presents the various materials and methods that were used to carry out the extraction and characterization experiment. 3.1 INSTRUMENTATION AND EQUIPMENT 3.1.1 Materials [Link]. Raw materials Dried and powdered seed Dried and powered pulp
[Link]. Reagents N-Hexane Ethanol Benzene 0.1N Aqueous Potassium Hydroxide Phenolphthalein indicator
[Link]. Equipment Soxhlet extractor Heating mantle Oven Reflux condenser Thermostat water bath Weighing scale Grinder Beakers Conical flasks Measuring cylinder
Burette Pipette Retort stand
3.1.2 EXPERIMENTAL PROCEDURE All experiments carried out in this study are described in this chapter [Link] Process Description
Figure 3.1: Block Flow Diagram for Solvent Extraction of Golden Shower Seed and Pulp [Link] Seed Processing (Preparation) The golden shower seed and pulp undergo several processes in the course of its preparation for extraction. The unit operations involved are; Dehulling: This is the removal of the fruit which house the seeds. Hulls and shells of oilseeds do not contain a significant amount of oil so they need to be removed prior to extraction. Cleaning: The golden shower seeds and pulp have some foreign materials and dirt which is separated by hand picking. Drying: The cleaned seeds and pulp was oven dried, to reduce its moisture content. Size reduction: A grinder was used to crush the seeds in order to weaken or rupture the cell walls for better extraction.
[Link] Extraction Procedure 200ml of N-Hexane was poured into a round bottom flask and weighed. 30g of the sample was weighed and placed in the thimble and was inserted in the main chamber of the extractor. The Soxhlet was heated at 70oC. The timer was started. When the solvent was boiling, the vapour rose through the vertical tube into the condenser at the top. The liquid condensate drips into the filter paper thimble in the centre, which contains the solid sample to be extracted. The extract seeps through the pores of the thimble and fills the siphon tube, where it flows back down into the round bottom flask. This was allowed to continue for 2 hour.
Figure 3.2: Soxhlet Apparatus Setup for Extraction The solvent was removed from the tube and distilled to separate and recover the solvent. The oil extracted was placed in a sample bottle whose weight had already been taken. Weight of oil extracted = weight of sample bottle and content weight of empty sample bottle.. (3.1) The experiment was repeated for the same pulp samples using two hours interval until ten and twelve hours extraction time was obtained.
Figure 3.3: water bath setup for Extraction Determination of the percentage of golden shower oil extracted for seed and pulp %Oil extracted = 100 (W1/W2) (3.2) Where W1 = weight of oil extracted (or total weights of oil extracted); W2 = original weight of sample before extraction (or total weights of samples before extraction). [Link] Precautions The apparatus and equipments were washed and dried to avoid contamination of the experimental solutions. Care was taken with the measuring instruments to avoid error and parallax error. Special care was taken while handling the oven and heating mantle to avoid any unsafe situation. The sample bottles holding the hexane-oil mixture was closed and kept properly to avoid losing the contents.
The conical flask positioned for recovering the hexane during distillation was sealed to prevent the hexane from escaping. Special care was taken when handling volatile liquids.
3.2 Characterization of oil 3.2.1 Determination of acid value 0.5g of the oil is weighed accurately and transferred into a 250ml conical flask. 95% ethanol is taken and neutralized with very dilute NaOH solution using phenolphthalein indicator. 50ml of this neutral alcohol and 50ml of benzene are added to the oil in the flask. The contents of the flask are shaken well to dissolve the free fatty acids. This is immediately titrated using standardized potassium hydroxide solution phenolphthalein indicator. The end point was indicated by the appearance of a pale pink color. The acid value was calculated using the expression: Acid Value = Where: V = Volume in ml of standard Potassium Hydroxide N = Normality of standard Potassium Hydroxide solution W = Weight in grams of oil taken for test . (3.3)