Lampiran 1 Uji SSA sampel

35

36

Lampiran 1 Uji SSA sampel

Action Sample ppm Cons

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

37

Lampiran 2 Uji SSA endapan dengan variasi konsentrasi

Action Sample True value (ppm) Konsentrasi (ppm) Abs. BG WF VF DF Actual cons. Actual cons. unit % Rsd BLK-1 BLK -0.0005 -0.002 BLK-2 BLK -0.0005 -0.0033 BLK-3 BLK -0.0004 -0.0045 BLK-AV BLK -0.0005 -0.0033 12.4 STD-1 Standar 1 1 1.0006 0.1829 -0.0063 STD-2 Standar 1 1 0.9945 0.182 -0.0074 STD-3 Standar 1 1 1.0019 0.1831 -0.0079 STD-AV Standar 1 1 0.9992 0.1827 -0.0072 0.32 STD-1 Standar 2 2 2.0353 0.3361 -0.0082 STD-2 Standar 2 2 2.0347 0.336 -0.0092 STD-3 Standar 2 2 2.0266 0.3348 -0.0096 STD-AV Standar 2 2 2.032 0.3356 -0.009 0.22 STD-1 Standar 3 3 3.0161 0.4813 -0.0095 STD-2 Standar 3 3 3.01 0.4804 -0.01 STD-3 Standar 3 3 2.9925 0.4778 -0.0103 STD-AV Standar 3 3 3.006 0.4798 -0.0099 0.38 STD-1 Standar 4 4 3.9118 0.6139 -0.0108 STD-2 Standar 4 4 3.9178 0.6148 -0.011 STD-3 Standar 4 4 3.9246 0.6158 -0.0109 STD-AV Standar 4 4 3.9178 0.6148 -0.0109 0.15 STD-1 Standar 5 5.5 5.5443 0.8556 -0.0097 STD-2 Standar 5 5.5 5.5572 0.8575 -0.01 STD-3 Standar 5 5.5 5.5329 0.8539 -0.0098 STD-AV 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-AV 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-AV 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-AV 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

38

Lampiran 2 (lanjutan)

Action Sample True value (ppm) Konsentrasi (ppm) Abs. BG WF VF DF Actual cons. Actual cons. unit % Rsd UNK4-3 500 0.7432 0.1448 -0.0155 0.55 100 1 135.4479 ppm UNK4-AV 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-AV 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-AV 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-AV 800 0.24 0.0703 -0.0201 0.65 100 1 37.2018 ppm 0.67

39

Lampiran 3 Uji SSA endapan dengan variasi ukuran elektrode karbon

Action Sample True value (ppm) Cons (ppm) Abs. BG WF VF DF. Actual cons Actual Cons. (ppm) % Rsd BLK-1 BLK -0.0005 -0.002 BLK-2 BLK -0.0005 -0.003 BLK-3 BLK -0.0004 -0.005 BLK-AV BLK -0.0005 -0.003 12.37 STD-1 Standar 1 1 1.0006 0.1829 -0.006 STD-2 Standar 1 1 0.9945 0.182 -0.007 STD-3 Standar 1 1 1.0019 0.1831 -0.008 STD-AV Standar 1 1 0.9992 0.1827 -0.007 0.32 STD-1 Standar 2 2 2.0353 0.3361 -0.008 STD-2 Standar 2 2 2.0347 0.336 -0.009 STD-3 Standar 2 2 2.0266 0.3348 -0.01 STD-AV Standar 2 2 2.032 0.3356 -0.009 0.22 STD-1 Standar 3 3 3.0161 0.4813 -0.01 STD-2 Standar 3 3 3.01 0.4804 -0.01 STD-3 Standar 3 3 2.9925 0.4778 -0.01 STD-AV Standar 3 3 3.006 0.4798 -0.01 0.38 STD-1 Standar 4 4 3.9118 0.6139 -0.011 STD-2 Standar 4 4 3.9178 0.6148 -0.011 STD-3 Standar 4 4 3.9246 0.6158 -0.011 STD-AV Standar 4 4 3.9178 0.6148 -0.011 0.15 STD-1 Standar 5 5.5 5.5443 0.8556 -0.01 STD-2 Standar 5 5.5 5.5572 0.8575 -0.01 STD-3 Standar 5 5.5 5.5329 0.8539 -0.01 STD-AV 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-AV 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-AV 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-AV 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-AV 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-AV Sampel C 4.7284 0.7348 -0.008 2.007 100 5 1177.97 ppm 0.33

40

Lampiran 4 Uji SSA endapan dengan variasi voltase

Action Sample True

value Cons. (ppm) Abs BG WF VF DF Actual cons Act. Con unit % Rsd UNK8-AV 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-AV 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-AV 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-AV Electrolisis C - 4 2.1326 0.3505 0.0149 2.3 100 1 92.642 ppm 1.99 UNK11-AV 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-AV Electrolisis C - 5 2.4413 0.3962 0.0154 2.25 100 1 108.5 ppm 1.95

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Lampiran 5 Diagram alir elektrolisis ke-2

Elektrolisis

A = 68.4422 g

AgCl masih bercampur dengan pengotor maka dibilas

AgNO3 + NaCl

AgCl + NaNO3

Dgn kain paracut, diambil filtratnya +HNO3 pekat 2 jam, lalu

panasi dgn api kecil (60 ˚C). Stop saat keluar uap putih.

Fixer dgn elektroda B

Fixer dgn elektroda C

Fixer dgn elektroda A

Sampel terpilih

_Ekstraksi

Penyaringan/

pemerasan

Penambahan NaCl

Dijemur di bawah

Matahari

Penggodogan

larutan

Sampel lain

Suhu 70 ˚C, 1 jam

Pemurnian

+ H2O t = 100

˚C

Gas klor lepas pada tahap ini.

42

Lampiran 6 Diagram alir elektrolisis ke-3

Elektrolisis

F= 47.4575 gram

Fixer B Pot A

Sampel terpilih

Ekstraksi

Penambahan NaCl

Penggodogan larutan

Fixer B Pot B

Fixer B Pot C

Fixer B Pot E

_{Fixer B Pot F}

Fixer B Pot D

Pemurnian

+ H2O t = 100

˚C

Sampel lain

+HNO_{panasi dgn api kecil (60 ˚C).} 3 pekat 2 jam, lalu

Stop saat keluar uap putih.

Penyaringan/

pemerasan

Dgn kain paracut, diambil filtratnya Suhu 70 ˚C, 1 jam AgNO3 + NaCl AgCl + NaNO3

AgCl masih bercampur dengan pengotor maka dibilas

Dijemur di bawah

Matahari

Gas klor lepas pada tahap ini.

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 (1 gram)

1 gram

27.27 mg X bobot endapan

27.27 mg X 17.47 g

1 gram

= 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 (1 gram)

1 gram

117.7 mg X bobot endapan

117.7 mg X 68.2 g

1 gram

= 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 (1 gram)

1 gram

10.85 mg X bobot endapan

10.85 mg X 46.1 g

1 gram

= 500 mg (0.5 gram)

44

Lampiran 10 Pengolahan ANNOVA lengkap limbah fixer encer

Voltase

(volt)

Waktu (Jam)

Kuadrat

1

2

3

4

S

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

SS

A

678.59527

A - B

B

2900.70

SS

B

245.58999

C - B

C

_3146.29

_SS

_R

_57.38238

_{(D + B) - (A + C)}

D

_3882.27

_SS

_total

_981.56764

_{SSA + SSB + SSR}

A

=(10737.9/3)

B

_=(186.57)

2

/12

C

=(12585.17/4)

D

=3882.3

F

F

tabel

23.652

A

6.60

F

B

12.840

7.26

45

Lampiran 11 Pengolahan ANNOVA lengkap limbah fixer pekat

Voltase

(volt)

Waktu (Jam)

Kuadrat

1

2

3

4

S

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

q

3

119.81

257.28

798.14 1181.36

p

4

241.5

577.2

1366.0

2250.7

4435.4

N

12

A

4112.23

SSA

532.86491

A - B

B

3579.36

SSB

248.15978

C - B

C

_3827.52

_SS

_R

_75.01064

_{(D + B) - (A + C)}

D

_4435.40

_SS

_total

_856.03533

_{SSA + SSB + SSR}

A

=(10737.9/3)

B

_=(186.57)

2

C

/12

=(12585.17/4)

D

=3882.3

F

tabel

F

A

14.208

6.60

(α = 0.025)

F

B

9.925

7.26

(α = 0.025)