Bioresource Technology 101 (2010) 965969

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Bioresource Technology
journal homepage: www.elsevier.com/locate/biortech

A glycerol-free process to produce biodiesel by supercritical methyl acetate technology: An optimization study via Response Surface Methodology
Kok Tat Tan, Keat Teong Lee *, Abdul Rahman Mohamed
School of Chemical Engineering, Universiti Sains Malaysia, Engineering Campus, Seri Ampangan, 14300 Nibong Tebal, Pulau Pinang, Malaysia

a r t i c l e

i n f o

a b s t r a c t
In this study, fatty acid methyl esters (FAME) have been successfully produced from transesterication reaction between triglycerides and methyl acetate, instead of alcohol. In this non-catalytic supercritical methyl acetate (SCMA) technology, triacetin which is a valuable biodiesel additive is produced as side product rather than glycerol, which has lower commercial value. Besides, the properties of the biodiesel (FAME and triacetin) were found to be superior compared to those produced from conventional catalytic reactions (FAME only). In this study, the effects of various important parameters on the yield of biodiesel were optimized by utilizing Response Surface Methodology (RSM) analysis. The mathematical model developed was found to be adequate and statistically accurate to predict the optimum yield of biodiesel. The optimum conditions were found to be 399 C for reaction temperature, 30 mol/mol of methyl acetate to oil molar ratio and reaction time of 59 min to achieve 97.6% biodiesel yield. 2009 Elsevier Ltd. All rights reserved.

Article history: Received 21 July 2009 Received in revised form 31 August 2009 Accepted 1 September 2009 Available online 20 September 2009 Keywords: Supercritical uids Biodiesel Optimization Response Surface Methodology

1. Introduction Generally, biodiesel is a mixture of fatty acid methyl esters (FAME) which is derived from a variety of vegetable oils, animal fats or waste oils and has similar physico-chemical properties compared to conventional diesel (Demirbas, 2008; Georgogianni et al., 2009). Hence, biodiesel is compatible with existing diesel engines and can be utilized directly without any major engine modication. Furthermore, this renewable and environmental-friendly biofuel has the potential to ensure the sustainability of human development and energy sources in the future by replacing exhaustible fossil fuels as the main energy supply. Despite the enormous benets of biodiesel, this renewable energy source is yet to be commercialized comprehensively throughout the world, which is attributed to its high processing costs and expensive feedstock (Bautista et al., 2009; Kulkarni and Dalai, 2006; Peng et al., 2008). Moreover, a huge amount of glycerol is produced as side product which leads to excessive supply and devaluation in the market price (Galan et al., 2009; Johnson and Taconi, 2007; Sabourin-Provost and Hallenbeck, 2009). Apart from that, the poor performance of biodiesel at low temperature in terms of viscosity, pour point and oxidation stability are also some of the contributing factors towards its limited commercial application (Liao et al., 2009). Hence, biodiesel additives are commonly utilized to improve the properties of biodiesel to accommodate the demand in cold climate countries.
* Corresponding author. Tel.: +60 4 5996467; fax: +60 4 5941013. E-mail address: chktlee@eng.usm.my (K.T. Lee). 0960-8524/$ - see front matter 2009 Elsevier Ltd. All rights reserved. doi:10.1016/j.biortech.2009.09.004

Consequently, the focus of research has been shifted towards nding new additives to improve the quality of biodiesel and revalorizing glycerol to other value-added products, which is important to generate side income to biodiesel biorenery. Recently, there are numerous articles reporting the conversion of glycerol into biodiesel additives, which not only solve the problem of glycerol glut in the market but also has the potential to improve the properties of biodiesel. For instance, Garca and co-workers reported a new class of acetal derived from glycerol and acetone which has the potential to be biodiesel additive (Garca et al., 2008). This new acetal (2,2dimethyl-1,3-dioxolan-4-yl)methyl acetate has been proven to enhance biodiesel properties such as viscosity, ash point and oxidation stability. On the other hand, Melero et al. carried out acetylation of glycerol by utilizing acidic mesoporous silica to produce triacetylglycerol (TAG) or commonly known as triacetin, which has been shown to be a valuable antiknocking additive (Melero et al., 2007). However, this method suffers from low selectivity of TAG compared to monoacetylglycerol (MAG) and diacetylglycerol (DAG). Consequently, Liao et al. proposed a two-step process which consists of esterication and acetylation to enhance TAG selectivity in the reaction by using amberlyst catalysts (Liao et al., 2009). In their work, glycerol is subjected to esterication with acetic acid to produce a mixture of MAG, DAG and TAG in the rst step. Subsequently, MAG and DAG are acetylated with acetic anhydride by consuming the water produced during esterication reaction and this shifts the reaction equilibrium towards producing TAG. However, acetylation reactions involving mesoporous silica or amberlyst catalysts required hours of reaction time for completion which makes these processes uneconomical.

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Although revalorizing glycerol into triacetin can improve the quality of biodiesel, the cost required to produce FAME and triacetin independently will be enormous. Hence, from economic point of view, it is a very promising and interesting prospect if FAME and triacetin can be produced simultaneously in a one-step reaction. This ideal scenario not only solves the poor quality of biodiesel but also minimizes the cost of processing biodiesel additives. This reaction can be made possible by transesterication reaction between triglycerides and methyl acetate to produce FAME and triacetin as the side product, instead of glycerol. This leads to simplied downstream processes compared to conventional catalytic reactions and the mixture of FAME and triacetin can be utilized as biodiesel, rather than FAME only. To the best of our knowledge, study on the reaction between triglycerides and methyl acetate is still very limited in the literature. Xu and co-workers proposed an enzymatic reaction to produce FAME and triacetin simultaneously by utilizing commercial immobilized enzymes and the biodiesel mixture was found to comply with international standards but suffers from long reaction time (Xu et al., 2003). Subsequently, Saka and Isayama carried out feasibility study to investigate the potential of utilizing non-catalytic supercritical methyl acetate (SCMA) to produce mixture of FAME and triacetin in a shorter amount of reaction time (Saka and Isayama, 2009). By utilizing a single-factor experiment design, it was found that supercritical treatment can reduce the reaction time signicantly and the properties of the product mixture were found to full international standards as well. Hence, mixture of FAME and triacetin has been proven to be a feasible option to address the weaknesses of biodiesel production which are poor performance in cold climate country and high production costs. However, there is still no optimization study concerning SCMA in the literature which is important for scale-up and commercialization purposes. For instance, optimization of SCMA by utilizing Response Surface Methodology (RSM) analysis allows a more comprehensive analysis on the interactions between experimental variables than a single-factor experimental design. Consequently, this leads to a better understanding and knowledge of the process and subsequently maximizes the yield of biodiesel. Apart from that, it also reduces the number of experimental runs required to generate statistically-validated results (Box and Hunter, 1976; Montgomery, 2001). RSM has been successfully applied in optimizing numerous biodiesel processing methods which include enzymatic catalysation of tallow kernel oil, homogeneous reaction involving animal fats and ultrasound-assisted methanolysis of soybean oil (Gao et al., 2009; Ghadge and Raheman, 2006; Jeong et al., 2009; Santos et al., 2009; Shieh et al., 2003). Therefore, in this study, optimization of SCMA process by using RSM has been carried out with three important variables which include reaction temperature (x1), methyl acetate/oil molar ratio (x2) and reaction time (x3). The effects of these variables on the yield of biodiesel (response) were studied concurrently in a rotatable central composite design (RCCD) and subsequently an empirical mathematical model correlating the response to the variables was developed and presented as well.

methyl oleate, methyl linoleate were also obtained from Fluka Chemie. 2.2. SCMA transesterication SCMA transesterication reaction was carried out by using a batch-type tube reactor (12 ml) made of Stainless Steel Super Duplex which can sustain high temperature and pressure needed in supercritical treatment as reported by Tan and co-workers (Tan et al., 2009). Initially, methyl acetate and oil were charged into the tube reactor without any prior mixing and subsequently immersed in a furnace heated at pre-determined temperature. To allow volume expansion, the amount of reactants was limited to 90% of total tube volume. A thermocouple and a pressure gauge were utilized to monitor the reaction temperature and pressure, respectively. After a xed reaction period, the reaction tube will be transferred into the water bath to quench the reaction immediately. Finally, the product mixtures will be subjected to evaporation process by using rotary evaporator at 60 C for 20 min to recover excessive methyl acetate and subsequently pure biodiesel sample can be obtained. 2.3. Product analysis The analysis of FAME content in sample was carried out by using gas chromatography (PerkinElmer, Clarus 500) with NukolTM capillary column (15 m 0.53 mm, 0.5 lm lm thickness) and Flame Ionization Detector (FID) as the detector. Helium was used as carrier gas with the initial oven temperature at 110 C held for 0.5 min and subsequently increased to 220 C (hold 8 min) at 10 C/min. Temperatures of the injector and detector were set at 220 C and 250 C, respectively. In each run, 1 lL of sample was injected into the column. Methyl heptadecanoate was used as internal standard. The yield of FAME was calculated by the following Eq. (1):

Yield of FAME; %

Total weight of methyl esters 100% Total weight of oil in the sample 1

Moreover, since both FAME and triacetin can be utilized as biodiesel, the total weight of FAME and triacetin generated per unit weight of oil in the sample was used to dene the yield of biodiesel. As shown in Fig. 1, in reversible transesterication reaction, 1 mol of triglyceride reacted with 3 mol of methyl acetate to produce 3 mol of FAME and 1 mol of triacetin where R1, R2 and R3 are the long chain alkyl compound. Equivalently, the mass ratio of FAME to triacetin was found to be approximately 4:1 in weight percent basis. Consequently, the total theoretical weight of biodiesel (FAME and triacetin) was found to be 125%, instead of 100% (FAME only). 2.4. Design of experiments The experimental design for SCMA reaction was carried out by utilizing RCCD as mentioned previously. In a RCCD consisting of three independent variables and ve levels, the total number of

2. Methods 2.1. Materials Puried palm oil (density = 0.755 kg/m3, molecular weight = 857 g/mol) was purchased from Yee Lee Edible Oils Sdn. Bhd., Malaysia. Methyl acetate (99%) was used as the solvent (Tc = 234 C, Pc = 4.69 MPa). Methyl heptadecanoate (used as internal standard) and standard references for FAME analysis which include methyl myristate, methyl palmitate, methyl stearate,

Fig. 1. Reaction stoichiometry for transesterication reaction between triglycerides and methyl acetate to produce fatty acid methyl esters (FAME) and triacetin.

K.T. Tan et al. / Bioresource Technology 101 (2010) 965969 Table 1 Constraints of process variables and the respective levels for RCCD. Variables Symbols Levels (2) Reaction temperature (C) Molar ratio (mol/mol) Reaction time (min) x1 x2 x3 340 20 15 (1) 360 30 30 (0) 380 40 45 (+1) 400 50 60 (+2) 420 60 75

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uate the statistical signicance of the model by the values of regression and mean square of residual error. 3. Results and discussion 3.1. Development of regression model equation The results obtained in the experiments are summarized in Table 2. As shown in the table, the biodiesel yield ranged from 18% to 102%, depending on the conditions of experiments. These results can be tted into a second order quadratic model of coded units as given in Eq. (3):
2 Y 77:48 20:94x1 2:19x2 10:44x3 5:01x2 1 2:89x2

experiments needed was determined to be 20 which included eight factorial points (2n = 8), six axial points (2n = 6) and six central points (nc = 6). The chosen variables in this study were reaction temperature (x1), methyl acetate/oil molar ratio (x2) and reaction time (x3). Table 1 summarizes the range and levels of the three variables investigated in this study. The value of a (alpha) which is important for a rotatable design was xed at 2. All variables at zero level constitute to the centre points while combination of variables consisting of one at its lowest (2) level or highest (+2) level with other variables at zero level constitutes the axial points. Table 2 shows the complete design matrix and yield of the experiments employed in this study. 2.5. Statistical analysis Design Expert software version 6.0.6 (STAT-EASE Inc., Minneapolis, USA) was used for regression analysis of the experimental data. The responses (Y) of the transesterication process were used to develop a quadratic polynomial equation that correlates the yield of biodiesel as a function of the independent variables and their interactions as shown in the following Eq. (2):

3:39x2 3 1:88x1 x2 1:87x1 x3 0:13x2 x3

Y b0

3 X i 1

b i xi

3 X i 1

bii x2 i

2 3 X X i1 ji1

bij xi xj

where Y is the predicted yield of biodiesel, xi is the ith independent variable, b0 is the intercept, bi is the rst order model coefcient, bii is the quadratic coefcient for the variable i and bij is the linear model coefcient for the interaction between variables i and j. The quality of developed model was determined by the value of correlation (R2) while analysis of variance (ANOVA) was used to eval-

Positive sign in front of the terms indicates synergistic effect while negative sign indicates antagonistic effect. From the equation, the yield of biodiesel has linear and quadratic effects by the three process variables. The model was found to have correlation value (R2) of 0.9891, which means that 98.91% of the total variation in the results was attributed to the independent variables investigated. The ideal value of R2 is unity which means a complete agreement between predicted and actual responses. Hence, the value in Eq. (3) is relatively high which indicates a good agreement between predicted and experimental yield of biodiesel in this regression model. Fig. 2 summarizes correlation between experimental values versus predicted values by using the developed model. Statistical analysis based on ANOVA for the response surface quadratic model is shown in Table 3. The value of P > F for the model is less than 0.05, which indicate that it is a signicant and desirable model. Besides, the value of P < 0.0001 indicates that there is only a 0.01% chance that a model F-value this large could occur due to noise in the experiments. Apart from that, the Lack of Fit F-value of 3.11 implies that Lack of Fit is not signicant relative to pure error. Hence, there is only a mere 11.93% chance that a Lack of Fit F-value this large could occur due to noise factor such as human errors or experimental errors. 3.2. Interactions between process variables The results in Table 3 show that interactions between variables have signicant effect on the yield of biodiesel. Therefore, instead of studying single variable (as in conventional method) the interactions will be investigated which is signicance and importance for a comprehensive optimization study. Fig. 3a and b shows the effects of different reaction temperature and molar ratio of methyl acetate to oil on the yield of biodiesel in three dimensional surface response and two dimensional interaction plots, respectively. From

Table 2 Experimental design matrix and the yields of biodiesel. Design points Point type Coded process variables Temperature (C) 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 Fact Fact Fact Fact Fact Fact Fact Fact Axial Axial Axial Axial Axial Axial Center Center Center Center Center Center 1 1 1 1 +1 +1 +1 +1 0 0 0 2 0 +2 0 0 0 0 0 0 Molar ratio (mol/mol) +1 +1 1 1 1 +1 +1 1 2 0 +2 0 0 0 0 0 0 0 0 0 Time (min) 1 +1 +1 1 1 1 +1 +1 0 2 0 0 +2 0 0 0 0 0 0 0 35 49 52 37 80 70 92 102 70 42 65 18 89 100 80 81 78 75 76 78 Yield (%)

103.63

Biodiesel yield, % (Predicted)

81.61

59.59

37.58

15.56 15.56 37.58 59.59 81.61 103.63

Biodiesel yield, % (Experimental)

Fig. 2. Predicted versus experimental yield of biodiesel.

968 Table 3 Anova for response surface quadratic model. Source Model x1 x2 x3 x2 1 x2 2 x2 3 x1x2 x1x3 x2x3 Residual Lack of t Pure error Cor. total Sum of square 9716.07 7014.06 76.56 1743.06 631.43 209.47 288.32 28.13 28.13 0.13 106.88 80.88 26.00 9822.95

K.T. Tan et al. / Bioresource Technology 101 (2010) 965969

Degree of freedom 9 1 1 1 1 1 1 1 1 1 10 5 5 19

Mean square 1079.56 7014.06 76.56 1743.06 631.43 209.47 288.32 28.13 28.13 0.13 10.69 16.18 5.20

F-value 101.01 656.25 7.16 163.08 59.08 19.60 26.98 2.63 2.63 0.012 3.11

Prof > F <0.0001 <0.0001 0.0232 <0.0001 <0.0001 0.0013 0.0004 0.1358 0.1358 0.9160 0.1193 Not signicant Signicant

94.8328 83.207 71.5812

102.33 86.642 70.9545

Yield (%)

Yield (%)
400.00 40.00 390.00 380.00 35.00 30.00 360.00 370.00

59.9554 48.3295

55.267 39.5795

50.00 45.00

60.00 52.50 45.00 390.00 380.00 30.00 360.00 370.00

400.00

Molar ratio, (Mol/Mol)

Reaction temperature, (Celcius)

Reaction time, (Minute) 37.50

Reaction temperature, (Celcius)

Fig. 3. Effect of reaction temperature and molar ratio on the yield of biodiesel in three dimensional response surface.

Fig. 4. Effect of reaction temperature and reaction time on the yield of biodiesel in three dimensional response surface.

the gures, it is obvious that at any designated quantity of molar ratio from 30 to 50, the yield of biodiesel increase proportionally with reaction temperature. In contrast, the yield augmented when the molar ratio was reduced from 50 to 30 at any constant temperature within the range of 360400 C. The observed phenomenon occurred as increasing the reaction temperature enhanced the reaction rate of transesterication reaction and eventually the yield of biodiesel. On the other hand, the same trend was not applicable for molar ratio of methyl acetate to oil. Although increasing the molar ratio will push this reversible reaction towards producing more products, but limitation of reaction equilibrium and difculties in separating excessive methyl acetate from FAME and triacetin will leads to lower yield (Tan et al., 2009). The effect of reaction temperature and reaction time on the yield of biodiesel at 30 M ratio is shown in Fig. 4a and b. At low reaction temperature of 360 C, the yield of biodiesel is only marginally affected by reaction time. However, at higher reaction temperature, its relevancy to the augmentation of yield is enormous. For instance, as can be seen in Fig. 4b, the yield increases steadily at 360 C but when the temperature was raised to 400 C, the yield escalates signicantly to achieve 102% after 60 min of reaction time. Reaction temperature plays a crucial role in determining the reaction rate in SCMA reaction which inuence the total yield of biodiesel produced. For instance, higher temperature induces faster reaction rate compared to lower temperature (Saka and Isayama, 2009). Hence, the optimum reaction temperature for SCMA is 400 C as shown in Figs. 3 and 4. Fig. 5a and b represents the effect of interaction between reaction time and molar ratio on the yield of biodiesel at constant reac-

84.9916 78.4198 71.8481

Yield (% )

65.2763 58.7045

60.00 52.50 45.00 45.00 40.00 35.00 30.00 30.00

50.00

Reaction time, (Minute) 37.50

Molar ratio, (Mol/Mol)

Fig. 5. Effect of reaction time and molar ratio on the yield of biodiesel in three dimensional response surface.

tion temperature of 400 C. Within the studied range of molar ratio, increment in reaction time enhanced the yield of biodiesel steadily as prolonging the duration allows higher reactivity between reactants. Besides, it also permits the reaction to reach equilibrium and stability which is important in a reversible reaction. In contrast, the yield of biodiesel decreases when the molar ratio was increased from 30 to 50. As mentioned previously, the presence of excessive methyl acetate in the reaction mixture required redundant separation process which is uneconomical and causes lower yield of biodiesel.

K.T. Tan et al. / Bioresource Technology 101 (2010) 965969 Table 4 Optimization constraints used to obtain the optimum value for biodiesel yield. Criteria Reaction temperature, x1 (C) Molar ratio, x2 (mol/mol) Reaction time, x3 (min) Yield, Y (%) Goal Is in range Is in range Is in range Maximize Lower limit 360 30 30 18 Upper limit 400 50 60 102

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Acknowledgements The authors would like to acknowledge Universiti Sains Malaysia (Research University Grant No. 1001/PJKIMIA//814047 and USM Fellowship) for the nancial support given. References
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Table 5 Results of three independent experiments to validate model adequacy. Run 1 2 3 x1 (C) 399 399 399 x2 (mol/mol) 30 30 30 x3 (min) 59 59 59 Predicted (%) 102 102 102 Experimental (%) 98 100 95

3.3. Process optimization The applications of RSM to optimize parameters which inuence transesterication process have been well reported by several researchers (Gao et al., 2009; Shieh et al., 2003; Yuan et al., 2008). In order to optimize the yield, numerical feature of the Design Expert 6.06 software was applied to nd the optimum combination conditions which resulted in maximum yield. In numerical optimization, the independent parameters which include molar ratio, reaction temperature and reaction time were set within the range between low (1) and high (+1) while the yield was set to maximum value. Table 4 summarizes the constraints used for the optimization study. Subsequently, 10 solutions for the optimum conditions were generated by the software and the solution with the highest desirability was selected to be veried by three independent experiments. The optimum conditions are shown in Table 5 coupled with the predicted and experimental yield of biodiesel. From the table, the obtained average optimum yield of 97.6% is well in agreement with the predicted value, with a relatively insignicant error of 4.2%. As the experimental error is less than 5%, it can be concluded that the proposed statistical model was adequate for predicting the yield of biodiesel in SCMA transesterication reaction. 4. Conclusion This study has shown that SCMA transesterication reaction is a very promising technology for biodiesel production. This glycerolfree process is more economical compared to conventional processes as the side product of triacetin can be utilized as biodiesel additive as well. Apart from that, separation and purication processes are simpler and less energy-intensive. On the other hand, optimization of biodiesel yield was successfully carried out by utilizing RSM analysis with optimum yield of 97.6%. The mathematical model developed was validated and proven to be statistically adequate and accurate to predict the optimal yield of biodiesel.