Professional Documents
Culture Documents
C6H5 O N N CH 3 O
C6H5 N N H3C CH 3
CH 3 H3C
Antipirin
C6H5 O N N CH 3
CH 3
Amidopirin
C6H5 O N N CH 3
Metampiron
Isopropilantipirin = Isopropylphenazone
C6H5 O N N CH3
H Antipirin
CH3
Penetapan Kadar 1. N- total/ Kjeldahl metode destruksi 2. Gravimetri dasar: bobot konstan I2 ke C no.4 monoiodoantipirin standar: selisih <0.5 mg/gram endapan 3. Iodometri dasar: reaksi redoks
I2 sisa + 2 Na2S2O3
2 NaI + Na2S4O6
1 mol antipirin ~ 1 mol I2 ~ 2 atom I- ~ 2 evalensi = 2 Indikator : CHCl3 I2 + CHCl3 ungu Titran : Na2S2O3 TA : tidak berwarna
Reaksi kolorimetri
H HONO + H+
C6H5 O N N CH3
O H
NO
NO+ + H2O
C6H5
N N CH3
+ NO+
CH3 C6H5
N N -H+
N N CH3
NO
CH3
NO
CH3
Nitosoantipirin
C6H5 O N N CH3
H3C
N CH3
CH3
garam
3. Asidimetri dasar : Rx netralisasi Amiopirin + HCl pelarut : etanol 4. TBA dengan HClO4 pelarut : asam asetat glasial
5. Kompleksometri dasar : Amidopirin membentuk komplek dg Cd(NH4)(SCN)4 Titran : EDTA 6. Bromatometri (titrasi langsung) Dasar : oksidasi amidopirin titran : KBrO3 KBrO3 + HCl bromin + amidopirin
TA : amido habis, tersisa warna kekuningan dari bromin (autoindikator) Indikator : a. CHCl3 - ->CHCl3 + Br2coklat b. Autoindikator (Br2)
+ amidopirin + FeCl3
violet ( = 570 nm)
c. TBA
d. Kompleksometri
e. Bromatometri
mm
f. Kolorimetri
+ KBrO3 + HCl
g. Spektrofotometri
III.
O
C6H5 N N CH 3
H3C
N CH 2SO 3Na
CH 3
Metampiron
a. Iodimetri
C6H5 O N N CH3 + H2O H3C N CH2SO3Na CH3 HCl 0,02 N HN CH2SO3Na O C6H5 N N CH3 + HCHO + Na2HSO3 CH3
NaHSO3 + I2
Metampiron
H3C
N CH2SO3Na C6H5 O N N
CH3
HN
CH3
O2 HN +, H
CH3 NH 4OH
H3C
N N O
CH3
H3C
CH3
IV.
O
Isopropilantipirin = Isopropylphenazone CH3 + FeCl3 orange Lieberman test H2O biru merah 100oC TLC fase diam Silika Gel G
HC CH3
fase gerak Rf
71
a. HPLC
Kolom : ODS Fase gerak : isopropilalkohol : as formiat : KH2PO4 0,1 M (540 : 1 : 1000)