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Study on car shampoo formulation using D-optimal statistical design

Article · November 2012

DOI: 10.1186/2228-5547-3-31

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Krishnaiah et al. International Journal of Industrial Chemistry 2012, 3:31
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RESEARCH Open Access

Study on car shampoo formulation using

D-optimal statistical design
Duduku Krishnaiah*, Rosalam Sarbatly, SM Anisuzzaman and Enddy Madais

Abstract
Background: In this investigation car shampoo formulation was studied. The quality of car shampoo is directly
linked to the basic material used in the formulation. By varying the ratio of ingredients such as sodium metasilicate
(SMS), sodium lauryl ether sulphate (SLES), coco dimethyl betaine (betaine), coconut fatty acid diethanolamide
(CDE) and linear alkyl benzene sulphonate (LABS), the final product characteristics were determined. A common
problem in pre-formulation is the optimization of the mixture composition which is aimed to obtain a product with
the required characteristics.
Results: In this work, various composition surfactants were used to prepare the car shampoo formulations. The
D-optimal mixture design was performed to obtain the optimum formulation. Twenty-five combination
components were selected according to the D-optimal criterion. Physical properties of the car shampoo such as
pH, power of removal and foaming ability were studied. Contour graphics were formed to assess the change in the
response surface in order to understand the effect of the mixture composition on car shampoo characteristics.
Conclusion: The statistical study shows that the fitted model was adequate to describe the viscosity response. The
optimum composition formulation was SMS 1.48%, SLES 3.52%, betaine 4.0%, CDE 4.5% and LABS 1.5%.
Keywords: Surfactant, Car shampoo formulation, D-optimal mixture design, Foaming

Background work, statistical experimental design is commonly used

The production of new cars is increasing year by year. to obtain a product with the required characteristics.
The detergent demand for car washing is also increasing The primary goal of designing an experiment statisti-
in parallel with production of cars. Car shampoo is pro- cally is to obtain valid results at minimum of effort, time
duced from the combination of surfactant, fragrance, and resources [5]. There were several experimental de-
stabiliser and other materials [1]. The good formulation sign techniques used for formulation work such as fac-
consists at least of five components. Surfactant is the torial design and mixture design. However, it should be
base material of the car shampoo formulation. It is the noted that factorial design cannot be used to study in
chemical species that is active and has a preference for a such mixtures since the variables are not independent.
surface or interface which is the boundary between two The sum of all fractions of the components used must
phases. When the surfactant is used as emulsifier, it be equal to 1 [6-10]. The mixture design represents an
decreases the energy differences between the two phases efficient approach for solving such optimisation prob-
to allow a relative stable mixture of oil and water. Gen- lem. It was found to be an effective tool to select the
erally, surfactant can be divided into four main groups: best liquid detergent formulation [11].
anionic, nonionic, cationic and amphoteric based on the This research was based on the five main surfactants,
chemical group [2-4]. namely, sodium metasilicate (SMS), sodium lauryl ether
The problem faced in the car shampoo formulation sulphate (SLES), coco dimethyl betaine (betaine), coconut
development is to achieve the optimum performance fatty acid diethanolamide (CDE) and linear alkyl benzene
with good appearance and stability. In the formulation sulphonate (LABS). These surfactants are widely used in
detergent industry as these are biodegradable. The for-
* Correspondence: [email protected] mulations were based on the composition designed by
Chemical Engineering Programme, School of Engineering and Information
Technology, Universiti Malaysia Sabah, Kota Kinabalu, Sabah 88400, Malaysia D-optimal mixture method. Physical properties of the car

© 2012 Krishnaiah et al.; licensee BioMed Central Ltd. This is an Open Access article distributed under the terms of the Creative
Commons Attribution License (http://creativecommons.org/licenses/by/2.0), which permits unrestricted use, distribution, and
reproduction in any medium, provided the original work is properly cited.
Krishnaiah et al. International Journal of Industrial Chemistry 2012, 3:31 Page 2 of 8
http://www.industchem.com/content/3/1/31

shampoo such as pH, foaming ability and power of re- Power of removal test
moval were studied. The responses of these components The power of removal of car shampoo formulation was
were analysed and optimised. Contour graphics were estimated by using weighed soil before and after washing.
formed to assess the change in the response surface in The soil used in this research is the motor oil waste
order to understand the effect of the mixture compos- (degraded motor oil). The substrate used in the laboratory
ition on car shampoo characteristics. test is steel plate. One layer of soil (motor oil) was spread
in the entire surface of the plate before the test was per-
formed (initial weight). The mechanical stirrer assisted the
Methods removal of the oil. After washing, the plate was dried in
Chemicals the oven and the final weight was measured. The formula
All the chemicals (analaytical grade), sodium metasilicate used in this test is shown in Equation 2 [12,13].
(SMS), sodium lauryl ether sulphate (SLES), coco dimethyl
betaine (betaine), coconut fatty acid diethanolamide W ¼ W F  Wi ; ð2Þ
(CDE) and linear alkyl benzene sulphonate (LABS) were
where W is the soil removed, WF is the final weight, and
purchased from Sigma-Aldrich (St. Louis, MO, USA).
Wi is the initial weight.

Detergency evaluation: pH test Results and discussion

The pH test is the one of the detergency evaluation para- Relationship between composition and pH
meters in car shampoo formulation. The pH metre was Tables 1 and 2 represent the results of mean, linear,
calibrated before the pH test was performed. Five read- quadratic, special cubic and full cubic models of the data
ings were taken to get the average pH data for each obtained. The computations were performed using Design
formulation. Expert computer programme (version 6.09, Stat-Ease Inc.,
Minneapolis, MN, USA). The sequential F-tests in these
Foaming ability test tables indicate that the contribution of the mean, linear
The foaming was measured based on the height of the and special cubic model is significant. However, the
foam in the used container. The mechanical stirrer has terms in special cubic and cubic model are aliased and
been used to produce the foam. The volume of the foam were ignored. Furthermore, the quadratic model is
was calculated by using Equation 1. chosen because it has a larger adjusted R value compared
to the other models.
Foam volume ¼ π r 2 H ð1Þ The model for D-optimal is based on the following
quadratic model in Scheffé equation:
where r is the radius of beaker and H is the height of
X
q XX
q
foam in millimetres. E ðyÞ ¼ βi X i þ βij Xi Xj : ð3Þ
i¼1 i<j¼2

Viscosity test
Final equation in terms of pseudo components
The viscosity measurement was carried out using Cole-
becomes:
Palmer Rotational Viscometer (Cole-Palmer, Chicago, IL,
USA) with R2 spindle. A volume of 250 ml of car sham- Y ¼ 89:52X1 þ 6:52X2  3:74X3 þ 116:75X4
poo is poured into a beaker. The viscometer speed was þ 32:72X5 þ 176:40X1 X3 þ 169:91X1 X4
set at 10 rpm. The process was allowed for about 20 min þ 106:31X1 X5 þ 21:28X2 X3  36:16X2 X4
before the reading is taken. The reading was taken after  25:47X2 X5  20:56X3 X4  18:89X3 X5
20 min.  58:39X4 X5 ð4Þ

Table 1 Sequential model sum of squares

Source Sum of squares Degrees of freedom Mean square F-value Probability > F
Mean 1,841.10 1 1,841.10 - -
Linear 291.02 4 72.76 34.22 <0.0001
Quadratic 31.84 10 3.18 2.98 0.0499
Special cubic 9.58 5 1.92 8.67 0.0167
Cubic 0.000 0 - - -
Residuals 1.11 5 0.22 - -
Total 2,174.64 25 86.99 - -
Krishnaiah et al. International Journal of Industrial Chemistry 2012, 3:31 Page 3 of 8
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Table 2 ANOVA summary statistics of model fit

Source Standard R2 Adjusted Predicted PRESS 3.00
deviation value R2 value R2 value
Linear 1.46 0.8725 0.8470 0.7996 66.83
Quadratic 1.03 0.9680 0.9231 0.6615 112.91
1.50

Studentized Residuals
Special cubic 0.47 0.9967 0.9841 - -

where X1 = SMS, X2 = SLES, X3 = betaine, X4 = LABS and

X5 = CDE. 0.00 2 2

Figures 1 and 2 present a normal probability of the

studentized residuals and residual values. Based on this
analysis, the probability plot of the studentized residuals -1.50
was determined for the standard deviation of the actual
values from their respective predicted values [5,6]. The
second analysis has been plotted with the residuals versus
-3.00
the predicted responses. As shown in the Figures 1 and 2,
there is no systematic pattern, and the points must be 2.26 4.76 7.26 9.76 12.26
within a horizontal band centred at zero [5,14]. Depart- Predicted
ure from this may suggest a violation of the constant
variance assumption. The size of the studentized residual Figure 2 Plot of pH residuals versus predicted values. (red lines
should be independent of its predictive value, which represent limits of variables).
means that the spread should be the same across all
levels of the predicted values [11]. Figures 1 and 2 also composition of A (SMS), D (LABS) and E (CDE) is the
present the normal probability plot of the studentized re- main factor to influence the pH value. The LABS and
sidual and plot of the studentized residuals versus the CDE increased the pH of the car shampoo. Meanwhile
prediction of this model. These plots are satisfactory and for the SMS, when this surfactant is increased, the pH
it is concluded that the quadratic model is suitable to de- decreases in the formulation.
scribe the pH by response surface of the car shampoo
formulation. Figure 3 presents the three-dimensional re- Relationship between composition and foaming ability
sponse surface plot of pH. These plots are very important Tables 3 and 4 present the results of mean, linear, quadratic,
in interpreting the results. At this stage the prediction of special cubic and full cubic models of the data obtained.
the model is being used to generate the response surface The sequential F-tests in Table 3 indicate that the contribu-
graphs and the contour plots of the combination of tion of the mean, linear, and quadratic is significant. In this
the each component mixture [5]. Based on Figure 3, the analysis also the two models, the linear and quadratic, were

DESIGN-EXPERT Plot Normal Plot of Residuals

pH

99
Norm al % Probability

95
90
80
70

50

30
20
10
5

-1.63 -0.61 0.41 1.43 2.45

Studentized Res iduals

Figure 1 The normal probability plot of studentized residual. Figure 3 Three-dimensional surface plot of pH data.
Krishnaiah et al. International Journal of Industrial Chemistry 2012, 3:31 Page 4 of 8
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Table 3 Sequential model sum of squares

DESIGN-EXPERT Plot Normal Plot of Residuals
Source Sum of Degrees of Mean F- Probability Foaming Ability

squares freedom square value >F

99
Mean 1.79 × 1 1.793E + - -
107 007

Norm al % Probability
95
90
Linear 5.715 × 4 1.429E + 4.70 0.0078
105 005 80
70

Quadratic 4.928 × 10 49,275.37 4.27 0.0157 50

105 30
20
Special 75,656.66 5 15,131.33 1.90 0.2483
10
cubic
5
Cubic 0.000 0 - - -
1
Residuals 39,730.50 5 7,946.10 - -
Total 1.911 × 25 7.645E + - -
107 005 -2.40 -1.28 -0.16 0.96 2.07

Studentized Res iduals

significant. However, the quadratic model fits well because

Figure 4 The normal probability plot of studentized residuals.
it has a larger R squared value compared to other models.
However, the terms in special cubic and cubic models are
aliased and should be ignored. Therefore, the fitted quad-
ratic model has been chosen from D-optimal model
Relationship between composition and viscosity
(Scheffé equation).
Tables 5 and 6 present the result of mean, linear, quad-
Final equation in terms of pseudo components becomes:
ratic, special cubic and full cubic models of the data
Y ¼ 5; 896:65X1  743:75X2 þ 1; 775:74X3 obtained. The sequential F-tests in Table 5 indicate that
þ 4; 669:52X4 þ 571:94X5 þ 9; 335:53X1 X2 the contribution of the linear model is significant since
þ 8; 403:48X1 X4 þ 4; 059:83X1 X5 the adjusted R value is larger and better than the other
þ 2; 831:20X2 X3  2; 987:98X2 X4 models. However, terms in special cubic and cubic
þ 3; 142:32X2 X5  8; 401:44X3 X4 model are aliased and should be ignored.
 4; 230:65X4 X5 ð5Þ Therefore, the fitted linear model based on Scheffé
where X1, X2, X3, X4, and X5 refer to SMS, SLES, betaine, equation is
LABS and CDE, respectively. X q

Figures 4 and 5 present the normal probability plot of E ðyÞ ¼ βi X i : ð6Þ

studentized residual and plot of studentized residuals versus i¼1

the predicted values of the model. These plots are satis-

factory, and the quadratic model is suitable to describe
the foaming ability response surface of the car shampoo
formulation. Figure 6 presents the three-dimensional re-
sponse surface plot of foaming ability. Based on the contour
plot, the composition of A (SMS), C (betaine) and D
(LABS) is the main factor to influence of the foaming abil-
ity. The betaine and LABS will influence the foaming ability
of the car shampoo formulation. When both surfactant
composition is increased, the foaming ability also
decreased. However, for the SMS, when this surfactant is
increased, the foaming ability also increased in the car
shampoo formulation. The optimum foaming ability was
found to be 1,038 mm.
Table 4 ANOVA summary statistics of model fit
Source Standard R2 Adjusted Predicted PRESS
deviation value R2 value R2 value
Linear 174.38 0.4845 0.3814 0.1599 9.910 × 105
Quadratic 107.42 0.9022 0.7652 0.0628 1.106 × 106 Figure 5 Plot of foaming ability residual versus predicted
Special cubic 89.14 0.9663 0.8383 - - values. (red lines represent limits of variables).
Krishnaiah et al. International Journal of Industrial Chemistry 2012, 3:31 Page 5 of 8
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Table 6 ANOVA Summary statistics of model fit

Source Standard R2 Adjusted Predicted PRESS
deviation value R2 value R2 value
Linear 1,610.90 0.3999 0.2799 0.0825 7.936 × 107
Quadratic 1,668.50 0.6781 0.2275 −3.6470 4.019 × 108
Special cubic 1,149.46 0.9236 0.6334 - +
Cubic - - - - +

the viscosity. The betaine and CDE will influence the

viscosity of the car shampoo formulation. When both
surfactant are increased, the viscosity decreases. Mean-
while for the SLES, when the surfactant composition is
increased, the viscosity also increased in the car shampoo
formulation.
Figure 6 Three-dimensional surface plot of foaming ability
data. Relationship between composition and the power
of removal
The final equation in terms of pseudo components Tables 7 and 8 present the results of mean, linear, quad-
becomes ratic, special cubic and full cubic models of the data
obtained. The sequential F-tests in Table 7 indicate the
significant contribution of linear model. In this analysis,
∧
Y ¼ 3196:70X1  4176:66X2 þ 3284:97X3 the linear model has been suggested because the value
 1223:92X4 þ 6028X5 ð7Þ of the predicted residual sums of squares (PRESS) is
lower compared to the quadratic model. However, terms
where X1, X2, X3, X4, and X5 are SMS, SLES, betaine, in special cubic and cubic model are aliased and should
LABS and CDE respectively. be ignored.
Figures 7 and 8 present a normal probability of the The final equation in terms of pseudo components
studentized residuals and residual plotted versus pre- becomes
dicted responses from the quadratic model. The figures
also present the normal probability plot of studentized Y ¼ 0:64X1 þ 0:46X2 þ 0:37X3 þ 0:31X4 þ 0:26X5
residual and plot of studentized residuals versus pre-
ð8Þ
dicted values. These plots are satisfactory, and the linear
model is suitable to describe the viscosity of response
surface of the car shampoo formulation. Figure 9 presents where X1 X2, X3, X4, and X5 are SMS, SLES, betaine,
the three-dimensional response surface plot of viscosity. LABS and CDE respectively.
Based on the plot, the composition of B (SLES), C
(betaine) and E (CDE) is the main factor to influence of DESIGN-EXPERT Plot
Viscosity
Normal Plot of Residuals

Table 5 Sequential model sum of squares 99

Source Sum of Degrees of Mean F- Probability

Norm al % Probability

95
squares freedom square value >F 90

Mean 3.948 × 1 3.948 × 107 80

107 70

50
Linear 3.459 × 4 8.647 × 106 3.33 0.0303
107 30
20
6
Quadratic 2.406 × 10 2.406 × 10 0.86 0.5889 10

107 5

6
Special 2.123 × 5 4.246 × 10 3.21 0.1129 1

cubic 107
Cubic 0.000 0 - + +
-1.98 -0.60 0.79 2.18 3.56
6
Residuals 6.606 × 5 1.321 × 10 - -
106 Studentized Res iduals

Total 1.260 × 25 5.039 × 106 - -

Figure 7 The normal probability plot of studentized residual.
108
Krishnaiah et al. International Journal of Industrial Chemistry 2012, 3:31 Page 6 of 8
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Table 7 Sequential model sum of squares for power of

removal
Source Sum of Degrees of Mean F- Probability
squares freedom square value >F
Mean 3.90 1 3.90 - -
Linear 0.037 4 9.293 × 10 5.07 0.0055
−3

Quadratic 0.027 10 2.696 × 10 2.78 0.0610

−3

Special 6.839 × 10 5 1.368 × 10 2.40 0.1794

−3 −3
cubic
Cubic 0.000 0 - + +
Residuals 2.850 × 10 5 5.70 × 10−4 - -
−3

Total 3.98 25 0.16 - -

Figure 8 Plot of viscosity residuals versus predicted value. (red

Optimization of car shampoo formulation
lines represent limits of variables).
For pH the expected values were in the range of 7 to 12,
since at low pH, very acidic condition causes skin irrita-
tion [15]. Thus, the viscosity test is very important. Be-
Figures 10 and 11 present a normal probability of the sides, the optimum foaming ability is also needed in the
studentized residuals and residual plotted versus predicted formulation, since the optimum removal of the soil
responses from the quadratic model. The figures also depends on the foaming ability. Nevertheless, heavy
present plot of studentized residuals versus predicted foaming can cause overflowing in the machinery and
values. These plots are satisfactory, and we concluded that often accompanied by considerable loss of active ingre-
the quadratic model is suitable to describe the power of dients. The function of the foaming in each formulation
removal response surface of the car shampoo formulation. is to assist the surfactant itself especially LABS and
Figure 12 presents a three-dimensional response sur- SLES to remove the soil in every substrate and in any
face in power of removal. The composition of A (SMS), surface. The optimum power of removal is needed to
B (SLES) and C (betaine) is the main factor to influence determine the effectiveness of the formulation formed.
of power of removal. The betaine and SLES influenced The optimization process was conducted by using nu-
the power of removal of the car shampoo formulation. merical values as shown in Table 9. The optimization and
When both compositions of these surfactants increased, analyses of all the parameters such as pH, viscosity,
the power of removal also increased. However for the power of removal and foaming ability were done using
SMS, when its surfactant composition is increased, the D-optimal method. Table 10 shows the optimal compos-
power of removal decreased. ition of each component to achieve the response desired.

Experimental
The experimental settings were performed by mixture
experimental design. The experimental design of five-
component system was conducted by using Design
Expert (version 6.10, Stat-Ease Inc., Minneapolis, MN,
USA). A set of candidate points in the design space
were selected using the D-optimal criterion [5,16-19].

Table 8 ANOVA summary statistics of model fit for power

of removal
Source Standard R2 Adjusted Predicted PRESS
deviation value R2 value R2 value
Linear 0.043 0.5035 0.4042 0.1964 0.059
Quadratic 0.031 0.8688 0.6850 −0.8483 0.14
Special cubic 0.024 0.9614 0.8147 - +
Figure 9 Three-dimensional surface plot of viscosity data.
Cubic - - - - +
Krishnaiah et al. International Journal of Industrial Chemistry 2012, 3:31 Page 7 of 8
http://www.industchem.com/content/3/1/31

DESIGN-EXPERT Plot Normal Plot of Residuals

Power of Removal

99
Norm al % Probability

95
90

80
70

50

30
20

10
5

-2.43 -1.39 -0.35 0.69 1.73

Studentized Res iduals

Figure 10 The normal probability plot of studentized residual. Figure 12 Three-dimensional surface plot of power of removal
data.

In this study, there are restrictions on the component

proportions Xj that take the form of lower Lj and upper
Uj constraint. Constraints in this research are shown in
Table 11. In this work, 25 car shampoo formulations
were prepared in laboratory scale according to the com- Table 9 The criteria used in numerical optimization
position designed by the D-optimal criterion. The ingre- Response Target Range
dients used in car shampoo formulation were water as Low High
solvent, colour, fragrance and surfactants such as SMS, pH In range 7 12
SLES, betaine, CDE and LABS. The components, starting Viscosity Maximum 7 7,483
with water and followed by SMS, SLES, betaine, CDE
Power of removal Maximum 0.23 0.48
and LABS, were added together in a reactor. The mixture
Foaming ability Maximum 316 1,097
was then homogenised by using mechanical stirrer at

Table 10 The optimised formulation of car shampoo

Component Percentage
SMS 1.48
SLES 3.52
Betaine 4.00
LABS 1.50
CDE 4.50
Total of mixture (%) 15.00

Table 11 Constraints of the component proportion

Component Low limit (%) High limit (%)
SMS, X1 0.50 3.0
SLES, X2 1.5 4.5
Betaine, X3 0.0 4.0
Figure 11 Plot of foaming ability residuals versus predicted LABS, X4 1.5 4.5
values. (red lines represent limits of variables). CDE, X5 1.5 4.5
 Krishnaiah et al. International Journal of Industrial Chemistry 2012, 3:31 Page 8 of 8
http://www.industchem.com/content/3/1/31

280 rpm. The car shampoo produced was stored in a bot- 11. Kamoun K, Chaabouni M, Sergent M, Roger PTL (2002) Mixture design
tle for 24 h at 30°C. applied to the formulation of hydrotropes for liquid detergents. Chemom
Intell Lab Syst 63:69–79
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Marcel Dekker, New York
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Twenty-five samples were prepared and four responses Marcel Dekker, New York
14. Bono A, Duduku K, Rajin M (2008) Products and Process Optimization Using
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tested in this study were pH test, foaming ability test, 15. Hall-Manning TJ, Holland GH, Rennie G, Revell P, Hines J, Barratt MD,
viscosity test and power of removal test. The analysis Basketter DA (1997) Skin irritation potential of mixed surfactant systems.
Food Chem. Toxicol. doi:10.1016/S0278-6915(97)00144-0
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best model, based on the results of pH test, foaming and melting point of natural ingredient based lipstick. Studies in Surface Sci
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the quadratic model. However, for viscosity test, the lin- the gel viscosity and gel strength of semi-refined carrageenan (SRC)
ear model has been chosen. The results indicate that the produced from seaweed (Kappaphycusalvarezii). J King Saud Uni - Eng Sci
performance and characteristics of the car shampoo can (in press)
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be manipulated by changing the composition of the sur- biopolymer (polyhydroxyalkanoates: PHAs) production from industrial
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the each desired response. From the analysis, the optimal
formulation consists of 1.48% SMS, 3.52% SLES, 4.00% doi:10.1186/2228-5547-3-31
betaine, 1.50% LABS, and 4.5% CDE, which gives the vis- Cite this article as: Krishnaiah et al.: Study on car shampoo formulation
using D-optimal statistical design. International Journal of Industrial
cosity of 2481.61 cP, power of removal of 0.44 g and Chemistry 2012 3:31.
foaming ability at 1,038 mm.
Competing interests
All the authors declare that they have no competing interests.

Authors’ contributions
EM carried out the experiments and analysed the data with D-optimal mixer
design. DK has supervised the research work. RS and SMA helped in the data
interpretation and analysis. All the authors have read and approved the final
manuscript.

Acknowledgements
Authors would like to thank Universiti Malaysia Sabah for providing the
research facilities.

Received: 3 October 2012 Accepted: 18 November 2012

Published: 10 December 2012

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