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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%)