Supplementary Data for:

Synthesis of N-TiO2-P25 Coated on Ceramic Foam by Modified Sol-gel Method for Acid Red 73 Degradation Under Visible-light Irradiation

Somayeh Alijania, AbdolsamadZarringhalam Moghaddama*, Mohammad Vaeza, Jafar Towfighia

a Department of Chemical Engineering, Tarbiat Modares University, Tehran, Iran

*Corresponding author. Tel.: +98 21 82883337; Fax: +98 21 82884931

E-mail address:

Contents

Table S1: Experimental designs and experimental results with predicted values………...... S2

Table S2: ANOVA Results for the Response Surface Quadratic Model…………………….S3

Table S3: Coefficients of regression and their significances………………………………...S4

Table S4: Optimization of the individual responses (di) to find the overall desirability response (D)………………………………………………………………………………….S5

Table S5: Optimum value of the process parameters for constraint conditions and their experimental values…………………………………………………………………………..S6

Table S6. Physical properties of undoped TiO2, N-TiO2 powders and films obtained from modified sol-gel method at optimal conditions derived from experimental design……….…S7

Table S7. Elemental Analysis data of N-TiO2-P25 samples obtained from modified sol-gel method at optimal conditions after 10 cycles…………………………………………...……S8

Table S1. Experimental designs and experimental results with predicted values

Run / Expereimental conditions / Acid Red 73 degradation (%)
x1 / x2 / x3 / Experimental / Predicative
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20 /
3.00
1.81
3.00
5.00
1.81
1.81
4.19
4.19
1.00
3.00
1.81
3.00
3.00
3.00
4.19
3.00
4.19
3.00
3.00
3.00 / 450.00
539.19
450.00
450.00
360.81
360.81
360.81
539.19
450.00
450.00
539.19
300.00
450.00
600.00
360.81
450.00
539.19
450.00
450.00
450.00 /
390.00
390.00
390.00
60.00
193.78
586.22
193.78
390.00
720.00
390.00
586.22
193.78
586.22
390.00
586.22
390.00
193.78
390.00
390.00
390.00
/
55
40
54
33
38
42
39
40
39
61
32
59
35
38
42
28
33
62
57
60 /
58.14
38.50
58.14
35.44
40.57
44.02
39.89
36.82
37.43
58.14
31.06
55.25
36.09
42.61
42.33
27.77
30.37
58.14
58.14
58.14


Table S2. ANOVA Results for the Response Surface Quadratic Model

Source / Sum of squares / Degree of
freedom / Mean squares / F value / p value
Model / 2234.99 / 9 / 248.33 / 18.88 / <0.0001
Residual / 131.56 / 10 / 13.16
Lack of fit / 76.73 / 5 / 15.35 / 1.4 / 0.3607
Pure error / 54.83 / 5 / 10.97
Total / 2366.55 / 19


Table S3. Coefficients of regression and their significances

Factor / Coefficient estimate / Degree of freedom / Standard error / F-value / 95% confidence interval Low / 95% confidence interval High / p-value
Intercept
x1
x2
x3
x1 x2
x1 x3
x2 x3
x12
x22
x23 / 58.14
-0.592
-3.76
-2.47
0.00
0.25
-1.00
-7.68
-3.26
-9.27 / 1
1
1
1
1
1
1
1
1
1 / 1.48
0. 98
0.98
0.98
1.28
1.28
1.28
0.95
0.95
0.95 / -
0.36
14.66
6.35
0.00
0.038
0.61
64.53
11.61
94.06 / 54.85
-2.78
-5.94
-4.66
-2.86
-2.61
-3.86
-9.80
-5.38
-11.4 / 61.44
1.59
-1.57
0.29
2.86
3.11
1.86
-5.55
-1.13
-7.14 / -
0.5596
0.0033
0.0304
1.00
0.8493
0.4536
< 0.0001
0.0067
< 0.0001


Table S4. Optimization of the individual responses (di) to find the overall desirability response (D)

Name / Goal / Lower Limit / Upper Limit / Lower weight / Upper weight / Importance
Molar ratio of urea to TTIP / In the range / 1 / 5 / 1 / 1 / 3
Calcination temperature (°C) / In the range / 300 / 600 / 1 / 1 / 3
Stirring time (min) / In the range / 60 / 720 / 1 / 1 / 3
Response (degradation %) / Maximize / 28 / 62 / 1 / 1 / 5


Table S5. Optimum value of the process parameters for constraint conditions and their experimental values

Variables / Optimum value
Molar ratio of urea to TTIP (x1) / 2.95
Calcination temperature (°C) (x2) / 400
Stirring time (min) (x3) / 375
Acid Red 73 degradation (%)
Run / Experimental / Predictive
1 / 59.40 / 59.33
2 / 60.00
3 / 58.11
Average / 59.17


Table S6. Physical properties of undoped TiO2, N-TiO2 powders and films obtained from modified sol-gel method at optimal conditions derived from experimental design

Method / 101 anatase crystallite size
(nm) / 110 rutile crystallite size
(nm) / Anatase content (%) / Rutile content
(%)
Undoped TiO2 powder prepared by PPMSG method / 43.06 / 36.92 / 78 / 22
N-TiO2 powder prepared by PPMSG method / 31.3 / 26.55 / 85 / 15
N-TiO2 Film prepared by PPMSG method / 35.2 / 30.39 / 82 / 18


Table S7. Elemental Analysis data of N-TiO2-P25 samples obtained from modified sol-gel method at optimal conditions after 10 cycles

Samples / C (w/w %) / N (w/w %)
N-TiO2-P25 samples before photocatalytic reaction / 0.305 / 0.248
N-TiO2-P25 samples after 10 photocatalytic cycles / 0.297 / 0.242

S6