Luận án Nghiên cứu biến tính vật liệu Zif - 8 và một số ứng dụng

Ảnh hưởng của thời gian hấp phụ trên ZIF-8 và Fe-ZIF-8 ở nồng độ đầu RDB thay đổi trong khoảng 30-50 mg.L-1 được thể hiện trên Hình 3.24. Kết quả cho thấy, dung lượng hấp phụ tăng lên khi nồng độ phẩm nhuộm tăng. Cùng nồng độ đầu, dung lượng hấp phụ RDB của Fe-ZIF-8 cao hơn của ZIF-8. Khi nồng độ phẩm nhuộm tăng từ 30 mg.L-1 đến 50 mg.L-1 thì dung lượng hấp phụ tăng lên, tương ứng với 30,2 - 42,1 mg.g-1 trên ZIF-8; 50,4 - 76,8 mg.g-1 trên Fe-ZIF-8(10%); 44,9 - 88,7 mg.g-1 trên Fe-ZIF-8(20%) và 41,1 - 72,0 mg.g-1 trên Fe-ZIF-8(30%). Khi nồng độ đầu của phẩm nhuộm tăng cao, sẽ cung cấp một lực động (driving force) để vượt qua sự truyền khối của RDB từ dung dịch vào bề mặt chất hấp phụ [185]

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Các thông số cố định trong phương pháp CV STT Thông số Kí hiệu Giá trị Giá trị 1 Tốc độ quay điện cực Ω 2000 vòng/phút 2 Khoảng quét thế Erange -1000 – 300 mV 3 Thời gian nghỉ trest 10 s 4 Thế làm giàu Eacc -1000 mV 5 Thời gian làm giàu tacc 120 s 6 Tốc độ quét ν 100 mV/s Nghỉ 10 s 1. Giai đoạn làm giàu: - Dung dịch phân tích: đệm pH, V1 mL Pb(II), V2 mL Bi(III) và thêm nước cất 2 lần vừa đủ 10 ml (V0 mL); - Áp thế và thời gian làm giàu: Eacc (- 1200 mV) và tacc (120 s);  (2000 vòng/phút). 2. Giai đoạn hòa tan: - Quét thế theo chiều anode, khoảng quét thế từ - 1000 (mV) →300 (mV); - Sử dụng kỹ thuật DP để đo tín hiệu hòa tan (Ep,Pb và Ip,Pb); - Tín hiệu hòa tan: Ip và Ep, trong đó Ip,Pb  CPb. - Tiến hành định lượng bằng phương pháp thêm chuẩn. Phụ lục 3. Quy trình thí nghiệm của phương pháp DP-ASV Phụ lục 4. Các thông số cố định trong phương pháp DP-ASV STT Thông số Kí hiệu Đơn vị Giá trị 1 Tốc độ quay điện cực Ω 2000 vòng/phút 2 Khoảng quét thế Erange -1000 – 300 mV 3 Thời gian nghỉ trest 10 s 4 Thế làm giàu Eacc -1200 mV 5 Thời gian làm giàu tacc 120 s 6 Biên độ xung ∆E 50 mV 7 Thời gian mỗi bước thế tstep 0,3 s 8 Bước nhảy thế Ustep 6 mV 9 Tốc độ quét ν 20 mV/s Phụ lục 5. Tín hiệu hòa tan của Pb(II) ở các nồng độ Bi(III) khác nhau STT [Bi(III)] (ppb) Ep,Pb (V) Ip, Pb (1) (μA) SdIp (μA) RSDI p (%) (n=4) 1 10 -0,586 20,17 0,931 4,62 2 50 -0,589 24,16 0,143 0,59 3 100 -0,601 29,19 0,512 1,76 4 300 -0,580 36,21 0,355 0,98 5 500 -0,604 31,24 0,258 0,83 6 700 -0,612 25,16 0,046 0,18 7 1000 -0,622 14,61 0,622 4,26 Phụ lục 6. Tín hiệu hòa tan của Pb(II) ở các tốc độ quét thế khác nhau STT ν (mV/s) Ip,Pb (1) (μA) SdIp (μA) Ep,Pb (V) SdEp (V) Ep/2,Pb (V) SdEp/2 (V) 1 20 6,393 0,228 -0,570 0,002 -0,593 0,001 2 40 14,58 0,210 -0,553 0,001 -0,582 0,001 3 50 19,26 0,230 -0,548 0,001 -0,579 0 4 75 28,86 0,204 -0,538 0,001 -0,573 0,001 5 100 37,13 0,497 -0,533 0 -0,571 0,001 6 200 66,40 0,489 -0,514 0,002 -0,562 0 7 300 88,66 1,091 -0,506 0,003 -0,559 0 8 400 103,6 0,902 -0,500 0 -0,562 0 9 500 117,3 1,470 -0,492 0 -0,562 0 ĐKTN: WE = BiF/Naf-ZIF-8/GCE; mZIF-8 = 12,5 μg; đệm B-R 0,5 M (pH = 3,2); [Pb(II)] = 500 ppb; [Bi(III)] = 300 ppb; Ip là kết quả trung bình 4 lần đo lặp lại Phụ lục 7: Giản đồ XRD của ZIF-8 Phụ lục 8: Giản đồ XRD của Fe-ZIF-8(10%) Faculty of Chemistry, HUS, VNU, D8 ADVANCE-Bruker - ZIF8 File: ThanhQN ZIF8.raw - Type: 2Th/Th locked - Start: 1.000 ° - End: 60.010 ° - Step: 0.030 ° - Step time: 0.5 s - Anode: Cu - WL1: 1.5406 - Generator kV: 40 kV - Generator mA: 40 mA - Creation: 19/09/2016 1:23:02 PM L in ( C p s ) 0 1000 2000 3000 4000 5000 2-Theta - Scale 1 10 20 30 40 50 60 d = 1 2 .0 8 4 d = 8 .5 4 2 d = 6 .9 6 2 d = 6 .0 1 6 d = 5 .3 7 4 d = 5 .1 3 4 d = 4 .9 1 7 d = 4 .7 3 5 d = 4 .5 4 6 d = 4 .0 2 8 d = 3 .6 2 7 d = 3 .4 6 5 d = 3 .3 3 7 d = 3 .0 8 1 d = 3 .0 0 7 d = 2 .9 1 8 d = 2 .8 3 5 d = 2 .7 6 2 d = 2 .6 2 6 d = 2 .5 6 3 d = 2 .4 5 6 Faculty of Chemistry, HUS, VNU, D8 ADVANCE-Bruker - Fe-ZIF8-9:1 File: ThanhQN Fe-ZIF8-91.raw - Type: 2Th/Th locked - Start: 1.000 ° - End: 60.010 ° - Step: 0.030 ° - Step time: 0.5 s - Anode: Cu - WL1: 1.5406 - Generator kV: 40 kV - Generator mA: 40 mA - Creation: 19/09/2016 2:04:51 L in ( C p s ) 0 100 200 300 400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700 1800 1900 2000 2100 2200 2300 2400 2500 2600 2700 2800 2900 3000 2-Theta - Scale 1 10 20 30 40 50 60 d = 1 2 .0 7 6 d = 8 .5 0 6 d = 6 .9 4 1 d = 5 .9 6 1 d = 5 .6 3 0 d = 5 .3 9 8 d = 4 .9 0 6 d = 4 .5 3 4 d = 3 .9 9 9 d = 3 .6 2 0 d = 3 .3 3 6 d = 2 .9 9 5 d = 2 .9 1 6 d = 2 .8 3 5 d = 2 .7 5 1 d = 2 .5 6 0 Phụ lục 9: Giản đồ XRD của Fe-ZIF-8(20%) Phụ lục 10: Giản đồ XRD của Fe-ZIF-8(30%) Faculty of Chemistry, HUS, VNU, D8 ADVANCE-Bruker - Fe-ZIF8-8:2 File: ThanhQN Fe-ZIF8-82.raw - Type: 2Th/Th locked - Start: 1.000 ° - End: 60.010 ° - Step: 0.030 ° - Step time: 0.5 s - Anode: Cu - WL1: 1.5406 - Generator kV: 40 kV - Generator mA: 40 mA - Creation: 19/09/2016 1:41:00 L in ( C p s ) 0 100 200 300 400 500 600 700 800 900 1000 1100 1200 1300 1400 1500 1600 1700 1800 1900 2000 2100 2200 2300 2400 2500 2600 2700 2800 2900 3000 2-Theta - Scale 1 10 20 30 40 50 60 d = 1 2 .1 3 3 d = 8 .5 5 5 d = 6 .9 4 3 d = 6 .4 9 2 d = 6 .0 4 2 d = 5 .7 9 4 d = 5 .4 2 2 d = 4 .9 2 1 d = 4 .3 5 4 d = 4 .0 1 1 d = 3 .6 3 1 d = 3 .3 2 8 d = 3 .0 1 3 d = 2 .9 2 1 d = 2 .8 4 2 Faculty of Chemistry, HUS, VNU, D8 ADVANCE-Bruker - Fe-ZIF8-7:3 File: ThanhQN Fe-ZIF8-73.raw - Type: 2Th/Th locked - Start: 1.000 ° - End: 60.010 ° - Step: 0.030 ° - Step time: 0.5 s - Anode: Cu - WL1: 1.5406 - Generator kV: 40 kV - Generator mA: 40 mA - Creation: 19/09/2016 1:05:52 L in ( C p s) 0 100 200 300 400 500 600 700 800 900 1000 2-Theta - Scale 1 10 20 30 40 50 60 d = 1 2 .0 8 2 d = 8 .4 7 2 d = 6 .9 4 5 d = 6 .0 4 2 d = 5 .4 0 5 d = 4 .9 1 7 Phụ lục 11 :Giản đồ phân tích nhiệt TG - TGA của ZIF-8 Phụ lục 12 :Giản đồ phân tích nhiệt TG - TGA của Fe-ZIF-8(10%) Phụ lục 13 :Giản đồ phân tích nhiệt TG - TGA của Fe-ZIF-8(20%) Phụ lục 14 :Giản đồ phân tích nhiệt TG - TGA của Fe-ZIF-8(30%)

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