International Conference on Agriculture, Environment and Biological Sciences (ICFAE’14) June 4-5, 2014 Antalya (Turkey) Properties of Soaps Produced From Selected Seed Oils Warra, A. A., Babayemi, A. W., and Buga, M. L. I. INTRODUCTION Abstract—Some traditional and hexane extracts of selected indigenous seed oils were chemically analyzed to justify their utilization for soap production and the following values were obtained; The neem seed oil had saponification, iodine and acid values of 148. 8 ± 1. 168 mgKOH/g, 73. 76 ± 0. 397g I2/100g and 22. 37 ±1. 168 mgKOH/g respectively. The chemical analysis of shea nut fat revealed that it had saponification, iodine and acid values of 136. 32 ±1. 943 mgKOH/g, 50. 50 ± 8. 023 gI2/100g and 14. 77 ± 0. 065 mgKOH/g respectively. The parameters analyzed for Jatropha seed oil were Acid value, (1. 20 ± 0. 065 mgKOH/g) Iodine value,(73. 46 ± 5. 00g I2/100g) and saponification value (122. 49 ± 2. 59 mgKOH/g). The chemical characteristics of Castor seed oil were: saponification, iodine and acid values of 123. 3 ± 3. 428 mgKOH/g, 76. 93 ± 0. 397g I2/100g and 2. 39 ±0. 065 mgKOH/g respectively The oils were saponified and skin friendly pH was obtained from most of the prepared soaps which were within the range accepted by National Agency for Food and Drug Administration and Control (NAFDAC). The foam height of the soaps showed variations which were discussed. The properties exhibited by the soap solutions indicated their suitability for commercial production. For the statistical analysis DMRT was used, homogenous subset testing alpha value was at 0. 05 level of significance, the saponification value of Castor seeds oil was p=0. 712 and Jatropha seeds oil p=0. 712 which showed no significant difference between the mean since p=0. 712>0. 05, Shea nut fat(p<0. 05), and Neem seed oil (p<0. 05) showed significant difference For iodine value, Castor p= 0. 413, Jatropha seeds oil p= 0. 413, Neem seed oil p= 0. 413 all showed no significant difference since p= 0. 413>0. 05 except Shea nut fat that showed significant difference (p<0. 05). For acid value, Castor seeds oil (p<0. 05), Jatropha seeds oil (p<0. 05), Neem seed oil (p<0. 05), Shea nut fat (p<0. 05), all showed significant difference. For the pH of the soap samples, the DMRT showed that there was significant difference among all the seed oil soaps Castor seed oil soap (p<0. 05), Jatropha seed oil soap(p<0. 05), Neem seed oil soap (p<0. 05), Shea nut fat soap (p<0. 05), likewise the Foam ability, Castor seed oil soap (p<0. 05), Jatropha seed oil soap(p<0. 05), Neem seed oil soap (p<0. 05), Shea nut fat soap (p<0. 05), they all showed significant difference (p<0. 05). This means that their pH and foam ability were not equally effective. The results obtained conclusively indicated that the selected oils are utilizable for soap making and other cosmetic preparations. The importance of fats and oils to the global economy becomes clear when considering the amount of oilseed and fruit grown worldwide. The importance of these oils and fats will increase considerably in the future because they represent a vast potential of naturally regenerating raw materials in which the chemical and pharmaceutical industries have a special interest. Until the previous century, the utilization of fats and oils as food went hand in hand with their use as fuel, predominantly for purposes of illumination. Even today, the name “lampante” for certain qualities of olive oil refers to this. As a base for ointments and cosmetics, they are still in use today, just as in the earliest periods [1]. There are many areas where oils and fats are used for non-food purposes. Thus, detergents, soaps, glycerine and polymers, inks, lubricants, and biodiesel may be derived from fatty acids and their derivative [2]. This work is aimed at extraction and physicochemical analysis of some selected indigenous seed oils in order to justify their industrial utilization for soap production. II. PROCEDURE FOR PAPER SUBMISSION 2. 1. Source of Research materials The indigenous Azadiracta Indica seed oil was obtained from Saberg International Ltd. producers of Nigeria Naija Neems (Neem oil) at Technology Incubation Centre, Birnin Kebbi, Kebbi State, Nigeria. Indigenous Jatropha Curcas L. seeds were obtained from Jatropha Curcas plant in a test plot in Warra town Ngaski local government area of Kebbi State, Nigeria. The plant was identified and authenticated by a Botanist at the Biological Sciences Department, Bayero University, and Kano, Nigeria. Confirmation of taxonomic identity of the plant was achieved by comparison with voucher specimen (voucher No. 110) kept at the Herbarium of the Department of Biological Sciences and use of documented literature [3]. Indigenous Castor (Ricinus communis) beans were plucked directly from plant. The plant was identified and authenticated by a Botanist at the Biological Science Department, Bayero University, Kano Nigeria. Confirmation of taxonomic identity of the plant was achieved by comparison with voucher specimen (voucher No. 225) kept at the Herbarium of the Department of Biological Sciences, and use of documented literature [3]. Castor bean Keywords— Indigenous oils, local extraction, soxhlet extraction, analysis, soaps. Warra, A. A. , Dept. of Biochemistry, Kebbi State University of Science and Technology, Aliero, Nigeria. Email: aliyuwarra@yahoo. com Babayemi, A. W. , Dept. of Mathematics, Kebbi State University of Science and Technology, Aliero, Nigeria. Buga, M. L Raw Materials Research and Development Council, Abuja, Nigeria. http://dx.doi.org/10.17758/IAAST.A0614019 44 International Conference on Agriculture, Environment and Biological Sciences (ICFAE’14) June 4-5, 2014 Antalya (Turkey) variety, which ripens from late October until late December, was obtained from a test Garden in Warra town of Ngaski Local Government Area of Kebbi State, Nigeria. Good seeds were selected, cleaned, de-shelled and dried and ground using laboratory plastic pestle and mortar prior to extraction as done for other seeds. The shea butter was obtained from local market at Warra town of Ngaski Local Government Area of Kebbi State, Nigeria. Good seeds were carefully selected cleaned, de-shelled and sundried. It was identified and authenticated by Dr. Dhramemdra Singh of the Botany unit Biological Sciences Department, Kebbi State University of Science and Technology Aleiro. Confirmation of taxonomic identity of the shea nut (Vitellaria paradoxa) leaves and stems (voucher No. 320) was achieved by comparing them with the specimens kept in the Herbarium of Department of Biological Sciences, Kebbi State University of Science and Technology, Aliero, Nigeria. The seeds were selected and damaged ones were discarded. The seeds were cleaned, de-shelled, dried and ground using laboratory plastic pestle and Mortar prior to extraction. . using soaps produced from each fat or oil. . III. RESULTS TABLE I PHYSICO- CHEMICAL CHARACTERISTICS OF THE SELECTED INDIGENOUS SEED OILS*. * The values are expressed as mean ± standard deviations of triplicates determinations. TABLE II PH OF THE SOAP SAMPLES*. Soap sample pH value Castor seed oil soap 8. 70±0. 057b 2. 2 Oil extraction The extraction of 50g of the ground seed kernels of Jatropha and Castor and was conducted in a soxhlet extractor using n-hexane (boiling point of 40–60 ◦C) for six hours. The extracted lipid was obtained after the solvent was removed under reduced temperature and pressure and refluxing in a boiling water bath. The oil was recovered from the mixture by drying the residual extracting solvent in an oven set at 60°C for 1h and stored in the bottle. Extracted seed oil was stored in freezer at−20 ◦C for subsequent physicochemical analyses. Oil analysis The chemical analysis of the oils was carried out using standard methods. Iodine value was estimated as reported [4], while saponification value was determined according the method [5]. Acid value was calculated as described in literature [6]. Saponification procedure was carried out as described in literature [7]. . 9. 11±0. 057d Neem seed oil soap 8. 90±0. 200c Shea nut fat soap 8. 33±0. 200a *The values are expressed as mean ± standard deviations of triplicates determinations TABLE 3: FOAM ABILITY AS A FUNCTION OF FOAM HEIGHT OF THE VARIOUS SOAP SAMPLES*. Soap sample Foam height (cm3) Castor seed oil soap 1. 6±0. 100a Jatropha oil soap 5. 4±0. 200d Neem seed oil soap 2. 0±0. 057b Shea nut fat soap 4. 2±0. 057c *The values are expressed as mean ± standard deviations of triplicates determinations. The same superscript letter indicates that there is no significant difference while different superscript letter indicates that there is significant difference in the Foam ability of the seed oil soaps. 2. 3. pH Determination The pH was determined using a pH meter (827 pH lab Model). 10g of the soap shavings was weighed and dissolved in distilled water in a 100ml volumetric flask. This was made up to prepare 10% soap solution in line with literature report [8]. The electrode of the pH meter was inserted into the solution. The pH reading was recorded. IV. DISCUSSION The physicochemical analysis (TABLE 1), for the soxhlet extracted indigenous Jatropha seed oil revealed; Saponification value of 122. 49 ± 2. 591 mgKOH/g the value obtained was lower than that of Dennettia tripatala fruit oil (Pepper fruit) 159. 33±1-20 suitable for soap making [10] but higher than that of beeswax (93mgKOH/g), which are commonly used in soap making [11]. This indicates that the oil could be used in soap making since its saponification value falls within the range of these oils. Higher saponification justifies the usage of fat or oil for soap production. Iodine value of 73. 46 ± 5. 00 I2/100g (less than 100) was obtained, which shows that the oil belongs to the class of Non-drying 2. 4. Foam ability Tests The method reported [9] for synthetic detergent was adopted. About 2. 0g each of soap (shavings) was added to a 500ml measuring cylinder containing 100ml of distilled water. The mixture was shaken vigorously so as to generate foams. After shaking for about 2 minutes, the cylinder was allowed to stand for about 10 minutes. The height of the foam in the solution was measured and recorded. The steps were repeated http://dx.doi.org/10.17758/IAAST.A0614019 Jatropha seed oil soap 45 International Conference on Agriculture, Environment and Biological Sciences (ICFAE’14) June 4-5, 2014 Antalya (Turkey) and makes it suitable for soap production. For the Jatropha oil soap the pH was 9. 11 (TABLE 2) comparably within the higher pH range of 9-11 but favourably higher than the pH range of 3-5, which are considered as high and low levels respectively by the National Agency for Food and Drug Administration and Control [18] mostly due to incomplete alkali hydrolysis resulting from the saponification process. This can be overcome by the addition of excess fat or oil or any other superfatting agent to reduce the harshness of the soap. Superfatting soaps with 1-2% neutral oils or glycerine also resulted in the better quality of soaps that were free of cracks [19]. The foam height of the soap was 5. 4cm3 (TABLE 3) higher than that of all other soap solutions analysed. The soap forms a clear solution and was and slightly soluble in distilled water. Although foam generation has little to do with cleansing ability [20], it is of interesting importance to the consumer and is therefore considered as a parameter in evaluating soaps and detergents. Commonly used test protocols for foam test was mentioned [20]. The pour foam test was developed [21], which for long has been accepted method for measuring foaming performance. Measurement of lather drain times was reportedly preferred [22], whereas rotating a shampoo solution in a glass stoppered cylinder was called for [23]. Kitchen blender was also used to produce foam and found that the foam characteristics were similar to those observed in practice [24]. For the prepared Castor oil soap the pH was 9. 7 (TABLE 2) comparably within the higher pH range of 9-11 but favourably higher than the pH range of 3-5, which are considered as high and low levels respectively by the National Agency for Food and Drug Administration and Control [18] mostly due to incomplete alkali hydrolysis resulting from the saponification process. This can be overcome by the addition of excess fat or oil or any other superfatting agent to reduce the harshness of the soap. Superfatting soaps with 1-2% neutral oils or glycerine also resulted in the better quality of soaps that were free of cracks [19]. The foam height of the soap was 1. 6 cm (TABLE 3) lower than that of all other soap solutions analysed. The soap solution was yellow, transparent and completely soluble in distilled water. The pH value of the prepared sheanut fat soap was measured. Soap being salt of strong base and weak acids should be weakly alkaline in aqueous solution. However, soap with free alkali (pH 11-14) can cause irritation to the skin. The pH value of 8. 33 was obtained for the prepared soap. The value is lower than the pH range of 9-11 and higher than the pH range of 3-5, which are considered as high and low levels respectively by National Agency for Food and Drug Administration and control [18]. The foam ability was 4. 2cm higher than that of 2. 0 for Neem oil soap, 1. 6 cm for Castor oil based soap. For the prepared neem oil soap the pH was 9. 90, within the higher pH range of 9-11 but higher than the pH range of 35, which are considered as high and low levels respectively by the National Agency for Food and Drug Administration and Control [18] due to incomplete alkali hydrolysis resulting oils, which are useful in the manufacture of soaps [3]. An Acid value of 14. 77 ± 0. 065mgKOH/g was obtained which is lower than that of olive oil 17 mgKOH/g[12] higher than the 10. 49 3mgKOH/g reported [13], which signifies a maximum purity and made it suitable for soap production. The results of the physicochemical analysis (Table 1), for the soxhlet extracted indigenous castor seed oil includes; Saponification value of 123. 3 ±3. 428 mgKOH/g the value obtained was lower than that of Terminalia catappa seed oil 207± 0. 13 suggested for use in the production of liquid soap, shampoos and lather shaving creams [14] but higher than that of beeswax (93 mgKOH/g), which are commonly used in soap making [11]. This indicates that the oil could be used in soap making since its saponification value falls within the range of these oils. Higher saponification justifies the usage of fat or oil for soap production. Iodine value of 76. 93 ± 0. 397 I2/100g (less than 100) was obtained, which shows that the oil belongs to the class of Non-drying oils, which are useful in the manufacture of soaps [3 ]. Castor oil has only one double bond in each fatty acid chain and so is classified as nondrying oil. An Acid value of 2. 39 ± 0. 065 mgKOH/g was obtained which is lower than that of Demettia tripetala fruit oil(Pepper fruit) 5. 34± 0. 04 mgKOH/g [10] and Shea butter 10. 3mgKOH/g [15], higher than that of Palm kernel seed oil 0. 834± 0. 004mgKOH/g reported [16] suitable for soap production. For the sheanut fat, the physicochemical analysis, relatively similar to the literature values [11]-[ 13 ] was determined for the indigenous crude shea fat. Saponification value of 183. 1 mgKOH/g obtained was lower than that of olive oil (192 mgKOH/g) and sunflower oil (188. 7 mgKOH/g) but higher than that of beeswax (93 mgKOH/g), which are commonly used in soap making [11]. This indicates that the oil could be used in soap making since its saponification value falls within the range of these oils. Iodine value of 53. 6 I2/100g (less than 100) was obtained, which shows that the oil belongs to the class of Non-drying oils, which are useful in the manufacture of soaps [3]. An Acid value of 10. 3mgKOH/g was obtained and was similar to the 10. 49 3mgKOH/g reported [13], which signifies a minimum purity. The results of the physicochemical analysis of Neem seed oil Saponification value of 148. 8 ± 1. 168 mgKOH/g which is lower than that of Dennettia tripatala fruit oil (Pepper fruit) 159. 33±1. 20 suitable for soap making [10] but higher than that of African pear oil 143. 76 mgKOH/g which could be good for soap making [17]. This indicates that the oil could be used in soap making since its saponification value falls within the range of these oils. Higher saponification justifies the usage of fat or oil for soap production. Iodine value of 73. 76 ± 0. 397 I2/100g (less than 100) was obtained, which shows that the oil belongs to the class of Non-drying oils, which are useful in the manufacture of soaps [3]. An Acid value of 22. 37 ± 1. 168 mg KOH/g was obtained which is higher than that of olive oil 17 mgKOH/g [12] and shea nut fat 10. 49mgKOH/g reported [17], which signifies a maximum purity http://dx.doi.org/10.17758/IAAST.A0614019 46 International Conference on Agriculture, Environment and Biological Sciences (ICFAE’14) June 4-5, 2014 Antalya (Turkey) [6] from the saponification process. This can be overcome by the addition of excess fat or oil or any other superfatting agent to reduce the harshness of the soap. Superfatting soaps with 12% neutral oils or glycerine resulted in the better quality of soaps that were free of cracks [19]. The foam height of the soap was 2. 0 cm lower than that of Jatropha, sheanut fat soaps analyzed higher than that of castor soap. The soap was milky in colour and slightly soluble in water. Using Duncan Multiple Range Test (DMRT), the physicochemical analysis results of the seed oils when subjected to homogenous subset testing alpha value at 0. 05 level of significance, the saponification value of Castor seeds oil was p=0. 712 and Jatropha seeds oil p=0. 712 which showed no significant difference between the mean since p=0. 712>0. 05, but there was significant difference between shea nut fat(p<0. 05), and Neem seed oil (p<0. 05). For iodine value, Castor p= 0. 413, Jatropha seeds oil p= 0. 413, Neem seed oil p= 0. 413 all showed no significant difference since p= 0. 413>0. 05 except Shea nut fat that showed significant difference (p<0. 05). For acid value, there were significant difference among all the seed oils; Castor seeds oil (p<0. 05), Jatropha seeds oil (p<0. 05), Neem seed oil (p<0. 05), Shea nut fat (p<0. 05), hence they are not equally effective. For the pH of the soap samples, the DMRT showed that there was significant difference among all the seed oil soaps Castor seed oil soap (p<0. 05), Jatropha seed oil soap(p<0. 05), Neem seed oil soap (p<0. 05), Shea nut fat soap (p<0. 05), likewise the Foam ability when the homogenous subsets were displayed, Castor seed oil soap (p<0. 05), Jatropha seed oil soap(p<0. 05), Neem seed oil soap (p<0. 05), Shea nut fat soap (p<0. 05), they all showed significant difference (p<0. 05). This means that their foam ability were not equally effective [7] [8] [9] [10] [11] [12] [13] [14] [15] [16] [17] [18] [19] V. CONCLUSION [20] From the results obtained after the chemical analysis of the oils it can be concluded that the selected oil is utilizable for soap making. The properties exhibited by the soap solutions indicated their suitability for commercial production. 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