Lampiran 1 Uji SSA sampel

LAMPIRAN 35

36 Lampiran 1 Uji SSA sampel Action Sample ppm Cons Abs. BG WF VF DF cons. Con. unit BLK-1 BLK -0.0005-0.002 BLK-2 BLK -0.0005-0.0033 BLK-3 BLK -0.0004-0.0045 BLK- BLK -0.0005-0.0033 12.4 1 Standar 1 1 1.0006 0.1829-0.0063 2 Standar 1 1 0.9945 0.182-0.0074 3 Standar 1 1 1.0019 0.1831-0.0079 Standar 1 1 0.9992 0.1827-0.0072 0.32 1 Standar 2 2 2.0353 0.3361-0.0082 2 Standar 2 2 2.0347 0.336-0.0092 3 Standar 2 2 2.0266 0.3348-0.0096 Standar 2 2 2.032 0.3356-0.009 0.22 1 Standar 3 3 3.0161 0.4813-0.0095 2 Standar 3 3 3.01 0.4804-0.01 3 Standar 3 3 2.9925 0.4778-0.0103 Standar 3 3 3.006 0.4798-0.0099 0.38 1 Standar 4 4 3.9118 0.6139-0.0108 2 Standar 4 4 3.9178 0.6148-0.011 3 Standar 4 4 3.9246 0.6158-0.0109 Standar 4 4 3.9178 0.6148-0.0109 0.15 1 Standar 5 5.5 5.5443 0.8556-0.0097 2 Standar 5 5.5 5.5572 0.8575-0.01 3 Standar 5 5.5 5.5329 0.8539-0.0098 Standar 5 5.5 5.545 0.8557-0.0098 0.21 UNK1-1 UNK1-2 UNK1-3 UNK1- UNK2-1 UNK2-2 UNK2-3 UNK2- BLK - 0.2254 0.0014-0.0052 1 1 1-0.2254 ppm BLK -0.222 0.0019-0.0069 1 1 1-0.222 ppm BLK -0.22 0.0022-0.0083 1 1 1-0.22 ppm BLK - 0.2227 0.0018-0.0068 1 1 1-0.2227 ppm 22 Sampel Fixer 2.6615 0.4288-0.0221 1 1 2500 6000.737 ppm Sampel Fixer 2.6689 0.4299-0.0225 1 1 2500 6000.312 ppm Sampel Fixer 2.6608 0.4287-0.0224 1 1 2500 6000.048 ppm Sampel Fixer 2.6635 0.4291-0.0223 1 1 2500 6000.365 ppm 0.16 % Rsd

37 Lampiran 2 Uji SSA endapan dengan variasi konsentrasi Action Sample True value Konsentrasi Abs. BG WF VF DF cons. cons. unit BLK-1 BLK -0.0005-0.002 BLK-2 BLK -0.0005-0.0033 BLK-3 BLK -0.0004-0.0045 BLK- BLK -0.0005-0.0033 12.4 1 Standar 1 1 1.0006 0.1829-0.0063 2 Standar 1 1 0.9945 0.182-0.0074 3 Standar 1 1 1.0019 0.1831-0.0079 Standar 1 1 0.9992 0.1827-0.0072 0.32 1 Standar 2 2 2.0353 0.3361-0.0082 2 Standar 2 2 2.0347 0.336-0.0092 3 Standar 2 2 2.0266 0.3348-0.0096 Standar 2 2 2.032 0.3356-0.009 0.22 1 Standar 3 3 3.0161 0.4813-0.0095 2 Standar 3 3 3.01 0.4804-0.01 3 Standar 3 3 2.9925 0.4778-0.0103 Standar 3 3 3.006 0.4798-0.0099 0.38 1 Standar 4 4 3.9118 0.6139-0.0108 2 Standar 4 4 3.9178 0.6148-0.011 3 Standar 4 4 3.9246 0.6158-0.0109 Standar 4 4 3.9178 0.6148-0.0109 0.15 1 Standar 5 5.5 5.5443 0.8556-0.0097 2 Standar 5 5.5 5.5572 0.8575-0.01 3 Standar 5 5.5 5.5329 0.8539-0.0098 Standar 5 5.5 5.545 0.8557-0.0098 0.21 UNK1-1 BLK -0.2024 0.0048-0.004 1 1 1-0.2024 ppm UNK1-2 BLK -0.2018 0.0049-0.0051 1 1 1-0.2018 ppm UNK1-3 BLK -0.195 0.0059-0.0064 1 1 1-0.195 ppm UNK1- BLK -0.1997 0.0052-0.0052 1 1 1-0.1997 ppm 11.7 UNK2-1 300 1.6287 0.2759-0.0074 0.6 100 1 270.5522 ppm UNK2-2 300 1.674 0.2826-0.0082 0.6 100 1 278.0697 ppm UNK2-3 300 1.6233 0.2751-0.0085 0.6 100 1 269.6545 ppm UNK2-300 1.6422 0.2779-0.008 0.6 100 1 272.7962 ppm 1.48 UNK3-1 400 0.2751 0.0755-0.0142 0.57 100 1 48.4694 ppm UNK3-2 400 0.2852 0.077-0.015 0.57 100 1 50.2544 ppm UNK3-3 400 0.2812 0.0764-0.0158 0.57 100 1 49.5404 ppm UNK3-400 0.2805 0.0763-0.015 0.57 100 1 49.4214 ppm 0.99 UNK4-1 500 0.7473 0.1454-0.0155 0.55 100 1 136.1865 ppm UNK4-2 500 0.7648 0.148-0.0165 0.55 100 1 139.3871 ppm % Rsd

38 Lampiran 2 (lanjutan) Action Sample True value Konsentrasi Abs. BG WF VF DF cons. cons. unit UNK4-3 500 0.7432 0.1448-0.0155 0.55 100 1 135.4479 ppm UNK4-500 0.752 0.1461-0.0158 0.55 100 1 137.0482 ppm 1.16 UNK5-1 600 0.3785 0.0908-0.019 0.66 100 1 56.9536 ppm UNK5-2 600 0.3649 0.0888-0.0184 0.66 100 1 54.9207 ppm UNK5-3 600 0.3582 0.0878-0.0177 0.66 100 1 53.9042 ppm UNK5-600 0.367 0.0891-0.0184 0.66 100 1 55.2256 ppm 1.71 UNK6-1 700 1.9732 0.3269-0.0171 0.9 100 1 218.8803 ppm UNK6-2 700 1.9698 0.3264-0.0167 0.9 100 1 218.5057 ppm UNK6-3 700 2.0063 0.3318-0.0167 0.9 100 1 222.5517 ppm UNK6-700 1.9833 0.3284-0.0168 0.9 100 1 220.0042 ppm 0.91 UNK7-1 800 0.2386 0.0701-0.0203 0.65 100 1 36.9924 ppm UNK7-2 800 0.2434 0.0708-0.0201 0.65 100 1 37.7253 ppm UNK7-3 800 0.2373 0.0699-0.0199 0.65 100 1 36.7829 ppm UNK7-800 0.24 0.0703-0.0201 0.65 100 1 37.2018 ppm 0.67 % Rsd

39 Lampiran 3 Uji SSA endapan dengan variasi ukuran elektrode karbon Action Sample True value Cons Abs. BG WF VF DF. cons Cons. BLK-1 BLK -0.0005-0.002 BLK-2 BLK -0.0005-0.003 BLK-3 BLK -0.0004-0.005 BLK- BLK -0.0005-0.003 12.37 1 Standar 1 1 1.0006 0.1829-0.006 2 Standar 1 1 0.9945 0.182-0.007 3 Standar 1 1 1.0019 0.1831-0.008 Standar 1 1 0.9992 0.1827-0.007 0.32 1 Standar 2 2 2.0353 0.3361-0.008 2 Standar 2 2 2.0347 0.336-0.009 3 Standar 2 2 2.0266 0.3348-0.01 Standar 2 2 2.032 0.3356-0.009 0.22 1 Standar 3 3 3.0161 0.4813-0.01 2 Standar 3 3 3.01 0.4804-0.01 3 Standar 3 3 2.9925 0.4778-0.01 Standar 3 3 3.006 0.4798-0.01 0.38 1 Standar 4 4 3.9118 0.6139-0.011 2 Standar 4 4 3.9178 0.6148-0.011 3 Standar 4 4 3.9246 0.6158-0.011 Standar 4 4 3.9178 0.6148-0.011 0.15 1 Standar 5 5.5 5.5443 0.8556-0.01 2 Standar 5 5.5 5.5572 0.8575-0.01 3 Standar 5 5.5 5.5329 0.8539-0.01 Standar 5 5.5 5.545 0.8557-0.01 0.21 UNK1-1 BLK -0.191 0.0065-0.004 1 1 1-0.191 ppm UNK1-2 BLK -0.191 0.0065-0.005 1 1 1-0.191 ppm UNK1-3 BLK -0.1876 0.007-0.006 1 1 1-0.1876 ppm UNK1- BLK -0.1896 0.0067-0.005 1 1 1-0.1896 ppm 4.33 UNK2-1 Sampel A 1.8672 0.3112-0.005 2.007 100 1 93.0324 ppm UNK2-2 Sampel A 1.8537 0.3092-0.005 2.007 100 1 92.3593 ppm UNK2-3 Sampel A 1.8604 0.3102-0.006 2.007 100 1 92.6958 ppm UNK2- Sampel A 1.8604 0.3102-0.005 2.007 100 1 92.6958 ppm 0.32 UNK3-1 Sampel B 0.2224 0.0677-0.01 2.003 100 1 11.1047 ppm UNK3-2 Sampel B 0.2109 0.066-0.011 2.003 100 1 10.5314 ppm UNK3-3 Sampel B 0.2285 0.0686-0.011 2.003 100 1 11.4082 ppm UNK3- Sampel B 0.2204 0.0674-0.011 2.003 100 1 11.0035 ppm 1.96 UNK4-1 0 10.912 1.6502 0.0036 2.007 100 1 543.672 ppm UNK4-2 0 10.893 1.6475 0.003 2.007 100 1 542.764 ppm UNK4-3 0 10.914 1.6506 0.0031 2.007 100 1 543.807 ppm UNK4-0 2.007 100 1 ppm UNK5-1 Sampel C 4.7419 0.7368-0.008 2.007 100 5 1181.34 ppm UNK5-2 Sampel C 4.7324 0.7354-0.009 2.007 100 5 1178.98 ppm UNK5-3 Sampel C 4.7101 0.7321-0.008 2.007 100 5 1173.43 ppm UNK5- Sampel C 4.7284 0.7348-0.008 2.007 100 5 1177.97 ppm 0.33 % Rsd

40 Lampiran 4 Uji SSA endapan dengan variasi voltase Action Sample True value Cons. Abs BG WF VF DF cons UNK8- Electrolisis C - 1 0.5298 0.1132 0.0104 2.03 100 1 26.058 ppm 3.04 UNK9-1 Electrolisis C - 2 0.1083 0.0508 0.0103 2.13 100 1 5.0786 ppm UNK9-2 Electrolisis C - 2 0.1056 0.0504 0.0106 2.13 100 1 4.9518 ppm UNK9-3 Electrolisis C - 2 0.1083 0.0508 0.0105 2.13 100 1 5.0786 ppm UNK9- Electrolisis C - 2 0.1076 0.0507 0.0105 2.13 100 1 5.0469 ppm 0.46 UNK10-1 Electrolisis C - 3 0.0441 0.0413 0.0117 2.15 100 1 2.0486 ppm UNK10-2 Electrolisis C - 3 0.0428 0.0411 0.0112 2.15 100 1 1.9859 ppm UNK10-3 Electrolisis C - 3 0.0414 0.0409 0.0108 2.15 100 1 1.9231 ppm UNK10- Electrolisis C - 3 0.0428 0.0411 0.0112 2.15 100 1 1.9859 ppm 0.49 UNK11-1 Electrolisis C - 4 2.1866 0.3585 0.0147 2.3 100 1 94.989 ppm UNK11-2 Electrolisis C - 4 2.1042 0.3463 0.015 2.3 100 1 91.409 ppm UNK11-3 Electrolisis C - 4 2.1063 0.3466 0.015 2.3 100 1 91.497 ppm UNK11- Electrolisis C - 4 2.1326 0.3505 0.0149 2.3 100 1 92.642 ppm 1.99 UNK11- Electrolisis C - 4 2.1326 0.3505 0.0149 2.3 100 1 92.642 ppm 1.99 UNK12-1 Electrolisis C - 5 2.4102 0.3916 0.0156 2.25 100 1 107.12 ppm UNK12-2 Electrolisis C - 5 2.4123 0.3919 0.0152 2.25 100 1 107.21 ppm UNK12-3 Electrolisis C - 5 2.5014 0.4051 0.0153 2.25 100 1 111.17 ppm UNK12- Electrolisis C - 5 2.4413 0.3962 0.0154 2.25 100 1 108.5 ppm 1.95 Act. Con unit % Rsd

41 Lampiran 5 Diagram alir elektrolisis ke-2 Fixer dgn elektroda A Fixer dgn elektroda B Fixer dgn elektroda C Elektrolisis Sampel lain Sampel terpilih A = 68.4422 g Ekstraksi +HNO 3 pekat 2 jam, lalu panasi dgn api kecil (60 C). Stop saat keluar uap putih. Penyaringan/ pemerasan Dgn kain paracut, diambil filtratnya Penggodogan larutan Suhu 70 C, 1 jam Penambahan NaCl AgNO 3 + NaCl AgCl + NaNO 3 Pemurnian + H 2 O t = 100 C AgCl masih bercampur dengan pengotor maka dibilas Dijemur di bawah Matahari Gas klor lepas pada tahap ini. Menghasilkan Ag

42 Lampiran 6 Diagram alir elektrolisis ke-3 Fixer B Pot A Fixer B Pot C Fixer B Pot E Fixer B Pot B Fixer B Pot D Fixer B Pot F Elektrolisis Sampel lain Sampel terpilih Ekstraksi +HNO 3 pekat 2 jam, lalu panasi dgn api kecil (60 C). Stop saat keluar uap putih. F= 47.4575 gram Penyaringan/ pemerasan Dgn kain paracut, diambil filtratnya Suhu 70 C, 1 jam Penggodogan larutan Penambahan NaCl AgNO 3 + NaCl AgCl + NaNO 3 Pemurnian + H 2 O t = 100 C AgCl masih bercampur dengan pengotor maka dibilas Dijemur di bawah Matahari Gas klor lepas pada tahap ini. Menghasilkan Ag

43 Lampiran 7 Perhitungan rendemen hasil elektrolisis variasi konsentrasi Kadar Ag awal = 6000 mg/l X 10 liter = 60000 mg (60 gram) Kadar Ag akhir= 272.7 mg/l X 0.1 liter=27.27 mg 27.27 mg dalam 1000 mg sampel () 27.27 mg X bobot endapan 27.27 mg X 17.47 g = 476.40 mg (0.476 gram) Jadi rendemen= hasil/awal X 100 = 0.476/60 X 100= 0.79%. Lampiran 8 Perhitungan rendemen hasil elektrolisis variasi elektrode karbon Kadar Ag awal = 6000 mg/l X 10 liter = 60000 mg (60 gram) Kadar Ag akhir= 1177 mg/l X 0.11 = 117.7 mg 117.7 mg dalam 1000 mg sampel () 117.7 mg X bobot endapan 117.7 mg X 68.2 g = 8027 mg (8 gram) Jadi rendemen= hasil/awal X 100 = 8/60 X 100 = 13.33% Lampiran 9 Perhitungan rendemen hasil elektrolisis elektrode tegangan Kadar Ag awal = 6000 mg/lx 10 liter = 60000 mg (60 gram) Kadar Ag akhir =108.5 mg/l X 0.1 liter = 10.85 mg 10.85 mg dalam 1000 mg sampel () 10.85 mg X bobot endapan 10.85 mg X 46.1 g = 500 mg (0.5 gram) Jadi rendemen = hasil/awal X 100 = 0.5/60 X 100 = 0.8%

44 Lampiran 10 Pengolahan ANNOVA lengkap limbah fixer encer Voltase (volt) Waktu (Jam) 1 2 3 4 S Kuadrat 3 3.53 7.77 13.46 16.60 41.36 1710.66 7.5 5.33 11.38 18.90 24.11 59.3 3567.68 9 7.56 16.02 27.33 34.57 85.48 7306.83 16.42 35.17 59.69 75.29 186.57 12585.17 Kuadrat 269.567 1237.26 3562.74 5668.3281 10737.9 Q 3 P 4 N 12 1 2 3 4 12.45 60.40 181.10 275.62 28.44 129.55 357.31 581.43 57.11 256.67 746.85 1195.35 98.0 446.6 1285.3 2052.4 3882,3 A 3579.30 SSA 678.59527 A - B B 2900.70 SSB 245.58999 C - B C 3146.29 SSR 57.38238 (D + B) - (A + C) D 3882.27 SStotal 981.56764 SSA + SSB + SSR A =(10737.9/3) B =(186.57) 2 /12 C =(12585.17/4) D =3882.3 Ftabel FA 23.652 6.60 FB 12.840 7.26

45 Lampiran 11 Pengolahan ANNOVA lengkap limbah fixer pekat Voltase Waktu (Jam) (volt) 1 2 3 4 S Kuadrat 3 6.93 9.04 13.21 16.21 45.39 2060.32 7.5 8.59 15.43 19.83 28.40 72.25 5220.16 9 10.95 16.04 28.25 34.37 89.61 8029.61 26.46 40.51 61.30 78.98 207.25 15310.09 Kuadrat 700.121 1641.22 3757.09 6238.2511 12336.7 1 2 3 4 47.99 81.70 174.54 262.87 73.73 238.19 393.33 806.46 119.81 257.28 798.14 1181.36 241.5 577.2 1366.0 2250.7 4435.4 A 4112.23 SSA 532.86491 B 3579.36 SSB 248.15978 q 3 p 4 N 12 A - B C - B C 3827.52 SSR 75.01064 (D + B) - (A + C) D 4435.40 SStotal 856.03533 SSA + SSB + SSR A =(10737.9/3) B =(186.57) 2 /12 C =(12585.17/4) D =3882.3 F tabel FA 14.208 6.60 (α = 0.025) FB 9.925 7.26 (α = 0.025)