DAFTAR ISI

Halaman

JUDUL........................................................................................................... i

HALAMAN PENGESAHAN ....................................................................... ii

KATA PENGANTAR ................................................................................... iii

ABSTRAK .................................................................................................... v

DAFTAR ISI ................................................................................................. vi

DAFTAR TABEL ......................................................................................... ix

DAFTAR GAMBAR .................................................................................... x

DAFTAR LAMPIRAN.................................................................................. xi

BAB I PENDAHULUAN ............................................................................. 1

1.1 Latar Belakang.............................................................................. 1

1.2 Perumusan Masalah ..................................................................... 3

1.3 Hipotesis ...................................................................................... 4

1.4 Tujuan Penelitian ......................................................................... 4

1.5 Manfaat Penelitian ....................................................................... 4

BAB II METODOLOGI PENELITIAN ....................................................... 6

2.1 Jenis Penelitian............................................................................. 6

2.2 Waktu dan Tempat Penelitian....................................................... 6

2.3 Determinasi Tumbuhan ............................................................... 6

2.4 Alat-alat, Bahan-bahan dan Sampel ............................................ 6

2.4.1 Alat-alat.............................................................................. 6

2.4.2 Bahan-bahan....................................................................... 6

2.4.3 Sampel................................................................................ 7

2.5 Pembuatan Larutan Pereaksi ....................................................... 7

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 2.5.1 Asam klorida 10%............................................................ 7

2.5.2 Larutan o-fenantrolin 0,1% b/v........................................ 7

2.5.3 Larutan buffer asetat......................................................... 7

2.5.4 Larutan hidroksilamin 10%.............................................. 7

2.5.5 Larutan asam sulfat 10%.................................................. 8

2.5.6 Larutan standar kalium permanganat 0,1 N .................... 8

2.5.7 Larutan standar asam oksalat 0,1 N ................................. 8

2.5.8 Larutan asam nitrat 5 N ................................................... 8

2.5.9 Larutan kalium heksasianoferat (II) ................................ 8

2.5.10 Pembuatan akuades bebas karbon dioksida...................... 8

2.5.11 Larutan natrium hidroksida ............................................ 9

2.6 Pembakuan Larutan Standar Kalium Permanganat 0,1 N ........... 9

2.7 Rancangan Penelitian................................................................... 9

2.7.1 Penyiapan sampel............................................................... 9

2.7.2 Destruksi sampel secara destruksi basah............................ 9

2.7.3 Pembuatan larutan sampel ................................................ 10

2.8 Analisis Kualitatif Besi .............................................................. 10

2.9 Analisis Kuantitatif Besi

............................................................................................................

............................................................................................................

10

2.9.1 Penetapan kadar / pemurnian fero (II) amonium sulfat

baku secara permanganometri
...................................................................................................

2.9.2  Pembuatan larutan induk baku fero (II) amonium sulfat... 11

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 2.9.3  Pembuatan kurva serapan maksimum larutan fero
fenantrolin
..............................................................................................
..............................................................................................
12

2.9.4   Penentuan waktu kerja ..................................................... 12

2.9.5   Pembuatan kurva kalibrasi larutan fero fenantrolin ........ 13

2.9.6 Pengukuran absorbansi sampel .......................................... 13

2.10 Analisis Data .............................................................................. 14

2.10.1 Menghitung simpangan baku (Standar Deviasi) ............. 14

2.10.2 Uji validasi metode analisis ............................................. 15

2.10.2.1 Uji akurasi ......................................................... 15

2.10.2.2 Uji keseksamaan (precision) ............................. 16

2.10.2.3 Uji Limit of Detection (LOD) dan Limit of

Quantitation (LOQ)........................................ 16

2.10.3 Menghitung analisa varian .............................................. 17

BAB III HASIL DAN PEMBAHASAN ....................................................... 20

3.1  Penentuan Kemurnian Fero (II) Amonium Sulfat Sebagai

       Baku Pembanding ......................................................................... 20

3.2 Identifikasi Besi (Uji Kualitatif).................................................. 20

3.3 Penetuan Panjang Gelombang Maksimum.................................. 20

3.4 Penentuan Waktu Kerja .............................................................. 21

3.5 Penentuan Linieritas Kurva Kalibrasi.......................................... 22

3.6 Penetapan Kadar Besi dalam Sampel ......................................... 24

3.7 Uji Analisa Varian (ANAVA) dan Uji Beda Nyata Terkecil
(BNT) ………………………………………………………….

25

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 3.8 Validasi Metode Analisis ............................................................ 27

3.8.1 Uji perolehan kembali (Recovery).................................... 27

3.8.2 Simpangan baku relatif..................................................... 29

3.8.3 Penentuan batas deteksi (Limit of Detection) dan batas

kuantitasi (Limit of Quantitation)
.........................................................................................
.........................................................................................
.........................................................................................
29

BAB IV KESIMPULAN DAN SARAN ....................................................... 30

4.1 Kesimpulan .................................................................................. 30

4.2 Saran ............................................................................................ 30

DAFTAR PUSTAKA .................................................................................... 31

LAMPIRAN .................................................................................................. 32

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 DAFTAR TABEL

Halaman

Tabel 1. Hasil Pengukuran Kurva Kalibrasi Larutan Baku ........................ 23

Tabel 2. Hasil Analisis Kadar Besi Pada Daun Bayam Hijau ....................

....................................................................................................24

Tabel 3. Data Hasil Uji ANAVA (Analisa Varian) .................................... 26

Tabel 4. Data Hasil Uji BNT (Beda Nyata Terkecil) .................................. 26

Tabel 5. Data Hasil Uji Validasi Penetapan Kadar Besi Di Dalam Sampel
Daun Bayam Hijau.........................................................................
...................................................................................................28

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 DAFTAR GAMBAR

Halaman

Gambar 1. Kurva serapan larutan baku fero dengan konsentrasi 2,4

µg/ml
...................................................................................................
...................................................................................................
21

Gambar 2. Kurva penentuan waktu kerja larutan baku fero ...................... 22

Gambar 3. Kurva kalibrasi larutan baku fero.............................................. 23

Gambar 4. Histogram kadar besi pada daun bayam hijau ......................... 24

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 DAFTAR LAMPIRAN

Halaman

Lampiran 1. Surat Hasil Identifikasi Tanaman Bayam Hijau

................................................................................................

................................................................................................

................................................................................................

32

Lampiran 2. Gambar Sampel Tanaman Bayam Hijau

................................................................................................

................................................................................................

................................................................................................

33

Lampiran 3. Hasil Uji Kualitatif Besi Di Dalam Sampel Daun Bayam

Hijau
................................................................................................
................................................................................................
................................................................................................
34

Lampiran 4. Pembuatan Dan Pembakuan Larutan Kalium Permanganat

................................................................................................
................................................................................................
35

Lampiran 5. Penetapan Kadar Baku Fero (II) Amonium Sulfat Secara

Permanganometri
................................................................................................
................................................................................................
................................................................................................
36

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Lampiran 6. Perhitungan Penimbangan Fero (II) Amonium Sulfat Untuk
Pembuatan Larutan Induk Baku
................................................................................................
................................................................................................
37

Lampiran 7. Gambar Bagan Kerja Mencari Panjang Gelombang

Maksimum, Operating Time, Dan Kurva Kalibrasi Larutan
Fero Fenantrolin
................................................................................................
................................................................................................
................................................................................................
38

Lampiran 8. Bagan Kerja Penetapan Kadar Besi Di Dalam Sampel Daun

Bayam Hijau Secara Spektrofotometri Sinar Tampak
................................................................................................
................................................................................................
39

Lampiran 9. Kurva Absorbansi Maksimum Larutan Fero (II) Fenantrolin

................................................................................................
................................................................................................
40

Lampiran 10. Kurva Waktu Kerja (Operating Time) Larutan Fero

Fenantrolin
................................................................................................
................................................................................................
................................................................................................
41

Lampiran 11. Kurva Kalibrasi Larutan Fero Fenantrolin

................................................................................................

................................................................................................

................................................................................................

42

Lampiran 12. Perhitungan Persamaan Garis Regresi Larutan Baku Besi

................................................................................................

................................................................................................

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 ................................................................................................

43

Lampiran 13. Contoh Perhitungan Kadar Besi Di Dalam Sampel Daun

Bayam Hijau
................................................................................................
................................................................................................
................................................................................................
44

Lampiran 14. Perhitungan Data Secara Statistik Hasil Penetapan Kadar

Besi Di Dalam Sampel Daun Bayam Hijau Mentah
................................................................................................
................................................................................................
................................................................................................
44

Lampiran 15. Perhitungan Data Secara Statistik Hasil Penetapan Kadar

Besi Di Dalam Sampel Daun Bayam Hijau Kukus
................................................................................................
................................................................................................
................................................................................................
47

Lampiran 16. Perhitungan Data Secara Statistik Hasil Penetapan Kadar

Besi Di Dalam Sampel Daun Bayam Hijau Rebus
................................................................................................
................................................................................................
................................................................................................
49

Lampiran 17. Data Hasil Penetapan Kadar Besi Di Dalam Sampel Daun
Bayam Hijau
................................................................................................
................................................................................................
................................................................................................
51

Lampiran 18. Uji ANAVA dan BNT

................................................................................................

................................................................................................

................................................................................................

52

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Lampiran 19. Perhitungan Analit Dan Bahan Baku Untuk Uji Persen
Recovery
................................................................................................
................................................................................................
................................................................................................
55

Lampiran 20. Contoh Perhitungan Persen Recovery

................................................................................................

................................................................................................

................................................................................................

58

Lampiran 21. Data Dan Hasil Perhitungan Persen Recovery Besi ............... 59

Lampiran 22. Perhitungan LOD dan LOQ Pada Penentuan Kadar Besi
Secara Spektrofotometri Sinar Tampak
................................................................................................
................................................................................................
................................................................................................
60

Lampiran 23. Hasil Pengukuran Absorbansi Sampel Daun Bayam Hijau

Mentah.................................................................................... 61

Lampiran 24. Hasil Pengukuran Absorbansi Sampel Daun Bayam Hijau

Kukus......................................................................................
................................................................................................
................................................................................................
62

Lampiran 25. Hasil Pengukuran Absorbansi Sampel Daun Bayam Hijau

Rebus
................................................................................................
................................................................................................
................................................................................................
63

Lampiran 26. Hasil Pengukuran Absorbansi Pada Penentuan Recovery

Besi Rentang 80% Pada Sampel Daun Bayam Hijau Mentah
................................................................................................
................................................................................................
................................................................................................
64

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Lampiran 27. Hasil Pengukuran Absorbansi Pada Penentuan Recovery
Besi Rentang 100% Pada Sampel Daun Bayam Hijau
Mentah
................................................................................................
................................................................................................
................................................................................................
65

Lampiran 28. Hasil Pengukuran Absorbansi Pada Penentuan Recovery

Besi Rentang 100% Pada Sampel Daun Bayam Hijau
Mentah
................................................................................................
................................................................................................
................................................................................................
66

Lampiran 29. Nilai distribusi t ..................................................................... 67

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