Coal is the world’s largest energy source as a result of its wealth and comparatively minimal

cost. In the new era, it is essential to utilize low-grade coal for satisfying energy demands
because of the shortage in the supply of high-grade coal. Anyhow, this low-grade coal exerts
significant effect on their utilization such as pyrolysis, liquefaction, gasification, and combustion
process due to its high ash and moisture content. Hence, a study is carried to build up the
effective strategy for the production of clean coal by optimizing the relevant variables with the
aid of response surface methodology.

A quadratic model was proposed to coordinate the relevant variables for maximum ash reduction
at the optimum process condition by applying central composite design (CCD) method. CCD
was utilized to build up the model for ash reduction from coal. In this investigation, 3
independent variables were chosen for the statistical model design which is:

i. Leachant concentration (%)

ii. Temperature (˚C)
iii. Time (min)

The range and dimension of the factors differed correspondingly to the model design. These
three parameters are observed to be the vital parameters for effective ash reduction from low-
grade coal. The goal of this design was to optimize the responsible variable (Ash Reduction). It
is expected to find an optimum approximation for the relationship between the independent
factors and the response surface. The experimental run was randomized so as to reduce the error
and the impact of the uncontrolled factors.

The statistical “Design-Expert 11.1.2.0” software has been utilized to study the regression
analysis of the experimental data. The statistical parameters were assessed by utilizing ANOVA.
For the leaching study, the necessary experimental range and coded level of factors are tabulated
in tables below followed by the experimental results. As the output proposed by the software, the
quadratic model was not aliased. The final equation in terms of coded factor for ash reduction is:

𝐴𝑠ℎ 𝑅𝑒𝑑𝑢𝑐𝑡𝑖𝑜𝑛 (%)

= 74.23 − 0.550245𝐴 + 0.853778𝐵 + 2.3773𝐶 − 0.10875𝐴𝐵 − 0.06375𝐴𝐶
− 0.07125𝐵𝐶 + 13177𝐴2 + 0.417193 𝐵 2 − 13177.5𝐶 2
Table of Experimental independent variables and their coded levels for the central composite design.

Factor Name Units Change Type Min Max

Coded Coded Mean Std.
Low High Dev.
A Time min. Hard Numeric 89.59 180.41 -1 ↔ +1 ↔ 135.00 22.89
108.00 162.00
B Temperature deg Hard Numeric 59.82 100.18 -1 ↔ +1 ↔ 80.00 10.17
C 68.00 92.00
C Leachant % Hard Numeric 9.95 20.05 -1 ↔ +1 ↔ 15.00 2.54
Conc. 12.00 18.00

Table of Experimental factors in actual units and experimental response.

Std. Run Space Factor 1 Factor 2 Factor 3 Response 1

Type A: Time B: Temperature C: Leachant Conc. Ash Reduction
(min) (deg C) (%) (%)
1 20 Factorial 108 68 12 69.25
2 18 Factorial 108 68 18 75.93
3 13 Factorial 108 92 12 70.68
4 3 Factorial 108 92 18 78.36
5 2 Factorial 162 68 12 70.15
6 12 Factorial 162 68 18 77.86
7 6 Factorial 162 92 12 72.43
8 19 Factorial 162 92 18 78.57
9 14 Center 135 80 15 65.27
10 5 Center 135 80 15 78.21
11 15 Axial 135 59.8185 15 73.98
12 1 Axial 135 100.182 15 76.84
13 7 Unknown 89.59 80 9.95462 74.93
14 8 Unknown 180.41 80 20.0454 75.61
15 4 Center 135 80 15 74.64
16 16 Center 135 80 15 74.58
17 9 Center 135 80 15 74.24
18 17 Center 135 80 15 74.74
19 10 Center 135 80 15 74.16
20 11 Center 135 80 15 78

Table of Response obtained

Respons Name Uni Observatio Analysis Minimu Maximu Mean Std. Ratio Transfor Model
e ts ns m m Dev. m
R1 Ash % 20 Polynomial 65.27 78.57 74.42 3.47 1.20 None Quadratic
Reduction
ANOVA for Quadratic model

Response 1: Ash Reduction

Source Sum of Squares df Mean Square F-value p-value

Model 80.90 9 8.99 0.6083 0.7663 not significant
A-Time 3.43 1 3.43 0.2318 0.6405
B-Temperature 9.95 1 9.95 0.6737 0.4309
C-Leachant Conc. 63.94 1 63.94 4.33 0.0642
AB 0.0946 1 0.0946 0.0064 0.9378
AC 0.0325 1 0.0325 0.0022 0.9635
BC 0.0406 1 0.0406 0.0027 0.9592
A² 2.22 1 2.22 0.1501 0.7066
B² 2.23 1 2.23 0.1508 0.7059
C² 2.22 1 2.22 0.1501 0.7066
Residual 147.77 10 14.78
Lack of Fit 36.88 3 12.29 0.7761 0.5434 not significant
Pure Error 110.89 7 15.84
Cor Total 228.67 19

Fit Statistics

Std. Dev. 3.84 R² 0.3538

Mean 74.42 Adjusted R² -0.2278
C.V. % 5.17 Predicted R² -2.1159
Adeq Precision 2.8949

Lack of Fit Tests

Source Sum of Squares df Mean Square F-value p-value

Linear 41.31 9 4.59 0.2898 0.9560 Suggested
2FI 40.36 6 6.73 0.4246 0.8418
Quadratic 36.88 3 12.29 0.7761 0.5434
Cubic 0.0000 0 Aliased
Pure Error 110.89 7 15.84

Final Results

Run Actual Predicted Residual Leverage Influence on Fitted Standard Order

Order Value Value Value DFFITS
1 76.84 76.85 -0.0059 0.707 -0.004 12
2 70.15 70.47 -0.3237 0.823 -0.411 5
3 78.36 78.04 0.3237 0.823 0.411 4
 4 74.64 74.23 0.4100 0.125 0.041 15
5 78.21 74.23 3.98 0.125 0.424 10
6 72.43 72.11 0.3238 0.823 0.411 7
7 74.93 72.20 2.73 0.793 3.335⁽¹⁾ 13
8 75.61 78.34 -2.73 0.793 -3.335⁽¹⁾ 14
9 74.24 74.23 0.0100 0.125 0.001 17
10 74.16 74.23 -0.0700 0.125 -0.007 19
11 78.00 74.23 3.77 0.125 0.398 20
12 77.86 75.24 2.62 0.677 1.776 6
13 70.68 73.30 -2.62 0.677 -1.776 3
14 65.27 74.23 -8.96 0.125 -1.451 9
15 73.98 73.97 0.0059 0.707 0.004 11
16 74.58 74.23 0.3500 0.125 0.035 16
17 74.74 74.23 0.5100 0.125 0.051 18
18 75.93 76.25 -0.3238 0.823 -0.411 2
19 78.57 76.59 1.98 0.677 1.297 8
20 69.25 71.23 -1.98 0.677 -1.297 1

Point Prediction

Response Predicted Predicted Observed Std Dev SE 95% CI 95% CI 95% TI 95% TI
Mean Median Mean low for high for low for high for
Mean Mean 99% Pop 99% Pop
Ash 74.23 74.23 3.84414 1.35911 71.2017 77.2583 55.9923 92.4677
Reduction

Fig. 1. Combined effect of temperature and time on ash reduction at 15% HF acid concentration.
Fig. 2. Combined effect of concentration and temperature on ash reduction at time 135 min.

Fig. 3. Combined effect of concentration and time on ash reduction at temperature 80 °C
Figure 1, Figure 2, and Figure 3 illustrate the interactions between the variables in three-
dimensional response surface plots. The combined effect of time (A) and temperature (B) on ash
reduction at 15% HF acid concentration and corresponding three-dimensional response surface
were illustrated in Figure 1. From the results obtained, it is observed that the time and
temperature have fewer effects on ash reduction from coal because of the low value
of F statistics. Meanwhile, the combined effect of temperature (B) and concentration (C) on ash
reduction at constant time is shown in Figure 2. The interaction between the concentration and
temperature was the most effective parameter for ash removal in the leaching process. Whereas
in Figure 3, the combined effect of time (A) and concentration(C) on ash reduction at constant
temperature was studied. On the other hand, it can be seen that the ash reduction increase with
the rise of temperature from Figure 1 and Figure 2. This may be due to an increase in
temperature results in the increase of the rate of reaction and the activation energy of the
reaction. The maximum ash reduction of 74.24% was obtained by the effect of time and
temperature at 15% HF concentration.

Figure 4. The actual cube of ash reduction in CCD

References

Behera S. K., Meena H., Chakraborty S., Meikap B. C. (2018) “Application of response surface
methodology (RSM) for optimization of leaching parameters for ash reduction from low-grade
coal” retrieved from
https://www.sciencedirect.com/science/article/pii/S209526861830257X#e0040

Stat-Ease, Inc (2018) “Response Surface” retrieved from

https://www.statease.com/docs/v11/tutorials/multifactor-rsm.html

Stat-Ease, Inc. (2018) “Central Composite Design (CCD)” retrieved from

https://www.statease.com/docs/v11/designs/ccd.html