The document describes procedures for preparing standard solutions and using UV-Vis spectroscopy and iodimetry to determine the concentration of samples. Specifically:
1. It details how to make a 500 ppm stock solution of paracetamol and generate a calibration curve by taking absorbance measurements of standards ranging from 3.5-6.5 ppm.
2. The absorbance of a sample is measured and used to determine its concentration via the linear regression equation from the calibration curve.
3. Iodimetry is also described to determine the concentration of vitamin C and iodine via titration with sodium thiosulfate of known concentration. Concentrations are calculated based on the titration volumes
The document describes procedures for preparing standard solutions and using UV-Vis spectroscopy and iodimetry to determine the concentration of samples. Specifically:
1. It details how to make a 500 ppm stock solution of paracetamol and generate a calibration curve by taking absorbance measurements of standards ranging from 3.5-6.5 ppm.
2. The absorbance of a sample is measured and used to determine its concentration via the linear regression equation from the calibration curve.
3. Iodimetry is also described to determine the concentration of vitamin C and iodine via titration with sodium thiosulfate of known concentration. Concentrations are calculated based on the titration volumes
The document describes procedures for preparing standard solutions and using UV-Vis spectroscopy and iodimetry to determine the concentration of samples. Specifically:
1. It details how to make a 500 ppm stock solution of paracetamol and generate a calibration curve by taking absorbance measurements of standards ranging from 3.5-6.5 ppm.
2. The absorbance of a sample is measured and used to determine its concentration via the linear regression equation from the calibration curve.
3. Iodimetry is also described to determine the concentration of vitamin C and iodine via titration with sodium thiosulfate of known concentration. Concentrations are calculated based on the titration volumes
V1 . N1 = V2 . N2 1. Pembuatan Larutan Stok V1 . 500 ppm = 10 mL . 3,5 ppm 50 mg parasetamol p.a dilarutkan dalam 100 mL etanol 96% 35 V1 = 500 50 mg x = 0,07 mL = 70 µL = 100 mL 1000 b. Konsentrasi 4 ppm V1 . N1 = V2 . N2 50.000 x = V1 . 500 ppm = 10 mL . 4 ppm 100 40 V1 = x = 500 ppm 500 = 0,08 mL = 80 µL Konsentrasi Absorbansi Standar (ppm) c. Konsentrasi 4,5 ppm 3,5 0,34 V1 . N1 = V2 . N2 4 0,41 V1 . 500 ppm = 10 mL . 4,5 ppm 45 4,5 0,48 V1 = 500 5 0,56 = 0,09 mL = 90 µL 5,5 0,68 d. Konsentrasi 5 ppm 6 0,75 V1 . N1 = V2 . N2 V1 . 500 ppm = 10 mL . 5 ppm 6,5 0,83 50 V1 = 500 = 0,10 mL = 100 µL Kurva Kalibrasi Paracetamol e. Konsentrasi 5,5 ppm 1 V1 . N1 = V2 . N2 V1 . 500 ppm = 10 mL . 5,5 ppm Absorbansi
f(x) = 0.17 x − 0.26
0.5 R² = 0.99 55 Linear () V1 = 500 0 2 3 4 5 6 7 = 1,1 mL = 110 µL Konsentrasi (ppm) f. Konsentrasi 6 ppm V1 . N1 = V2 . N2 V1 . 500 ppm = 10 mL . 6 ppm 60 V1 = 500 2. Perhitungan Pengenceran = 1,2 mL = 120 µL g. Konsentrasi 6,5 ppm V1 . N1 = V2 . N2 IODIMETRI V1 . 500 ppm = 10 mL . 6,5 ppm 65 Pembakuan Vitamin C dengan K2Cr2O7 V1 = Dik : K2Cr2O7 = 50 mg, BM K2Cr2O7 = 249 500 = 1,3 mL = 130 µL Percobaan Ke- VNa2S2O3 NNa2S2O3 3. Perhitungan Kadar Sampel 1 20,6 ml 0,049 N Diketahui : 2 20,5 ml 0,049 N a = 0,2607 3 20,6 ml 0,049 N b = 0,1679 Rata-rata 0,049 N Absorbansi sampel = 0,4125 Perhitungan : Perhitungan Persamaan Regresi Linear : 1) Mgek Na2S2O3 = Mgek K2Cr2O7 y = bx + a mg K 2 Cr 2 O7 VNa2S2O3 . NNa2S2O3 = 0,4125 = 0,01679x + 0,2607 BE K 2Cr 2O 7 0,4125- 0,2607 = 0,01679x mg K 2 Cr 2 O7 NNa2S2O3 = x = 4,0095 BE K 2Cr 2O 7 .VNa 2 S 2 O3 50 mg Konsentrasi = 4,0095 x factor pengenceran = 49 . 20,6 ml NNa2S2O3 = 0,0495 N Konsentrasi = 4,0095 x 10 mg K 2 Cr 2 O7 2) NNa2S2O3 = Konsentrasi = 40,095 ppm BE K 2Cr 2O 7 .VNa 2 S 2 O3 50 mg = 49 . 20,5 ml NNa2S2O3 = 0,0497 N mg K 2 Cr 2 O7 3) NNa2S2O3 = BE K 2Cr 2O 7 .VNa 2 S 2 O3 50 mg = 49 . 20,6 ml NNa2S2O3 = 0,0495 N
Pembakuan Larutan Iodium (I2) dengan larutan Na2S2O3 (0,049 N)
Pecobaan Ke- VI VNa2S2O3 NI 1 10 ml 9,6 ml 0,047 N 2 10 ml 9,8 ml 0,048 N 11,5ml . 0,047 N = 3 10 ml 9,7 ml 0,047 N 10 ml Rata-rata 0,047 N NVitC = 0,054 N Perhitungan : ¿ 2) NVitC = VI .∋ VVitC ¿ 1) VI . NI = VNa2S2O3 . NNa2S2O3 11,7 ml . 0,047 N = VNa 2 S 2 O3 . NNa 2 S 2 O3 10 ml NI = VI NVitC = 0,055 N 9,6 ml . 0,049 N 3) NVitC ¿ = VI .∋ VVitC ¿ = 10 ml NI = 0,047 N 11,5ml . 0,047 N = VNa 2 S 2 O3 . NNa 2 S 2 O3 10 ml 2) NI = NVitC = 0,054 N VI 9,8 ml . 0,049 N 0,054 N +0,055 N +0,054 N = Rata-rata = = 0,054 N 10 ml 3 NI = 0,048 N VNa 2 S 2 O3 . NNa 2 S 2 O3 g VitC = NVitC x BE VitC x VVitC 3) NI = VI = 0,054 N x 88,065 x 0,05 L 9,7 ml . 0,049 N = 0,237 gram/50 ml = 10 ml g VitC NI = 0,047 N % Vit C = x 100% VVitC 0,237 g 0,047 N +0,048 N +0,047 N = x 100% NI rata-rata = = 0,047 N 50 ml 3 % Vit C = 0,474 % Penetapan Kadar Analit (Vitamin C) Pecobaan Ke- VVitC VI NVitC 1 10 ml 11,5 ml 0,054 N 2 10 ml 11,7 ml 0,055 N 3 10 ml 11,5 ml 0,054 N Rata-rata 0,054 N Perhitungan : 1) VVitC . NVitC = VI . NI ¿ ¿ NVitC = VI .∋ VVitC 0,048 N + 0,049 N + 0,048 N MEDTA rata-rata = = 0,048 N 3 Titrasi Blanko Percobaan Ke- VPelarut VEDTA MPelarut KOMPLEKSOMETRI 1 10 ml 0,4 ml 0,002 M 2 10 ml 0,6 ml 0,003 M Pembakuan EDTA menggunakan ZnSO4 0,05 M 3 10 ml 0,4 ml 0,002 M Rata-rata 0,0023 M Percobaan VNa2EDTA MNa2EDTA Ke- 1 12,8 ml 0,048 M Perhitungan : 2 12,6 ml 0,049 M 3 12,8 ml 0,048 M 1. VPelarut . MPelarut = VEDTA . MEDTA Rata-rata 0,048 M VEDTA . MEDTA MPelarut1 = Perhitungan : VPelarut 0,4 ml . 0,048 M = 1. mmol EDTA = mmol ZnSO4 10 ml mg ZnSO 4 MPelarut1 = 0,002 M VEDTA . MEDTA = Mr ZnSO 4 VEDTA . MEDTA 2. MPelarut2 = mg ZnSO 4 VPelarut MEDTA = Mr ZnSO 4 . VEDTA 0,6 ml . 0,048 M = 100 mg 10 ml = 161. 12,8 ml MEDTA = 0,048 M MPelarut2 = 0,003 M mg ZnSO 4 VEDTA . MEDTA 2. MEDTA = 3. MPelarut3 = Mr ZnSO 4 . VEDTA VPelarut 100 mg 0,4 ml . 0,048 M = = 161. 12,6 ml 10 ml MEDTA = 0,049 M MPelaurt3 = 0,002 M mg ZnSO 4 0,002 M +0,003 M +0,002 M 3. MEDTA = MPelarut rata-rata = = 0,0023 M Mr ZnSO 4 . VEDTA 3 100 mg = 161. 12,8 ml Penetapan Kadar Analit (Asam Mefenamat) dengan Titrasi Komplesometri Refreshment MEDTA = 0,048 M Percobaan VAsam VZnSO4 yang VTitrasi VEDTA VZnSO4 VZnSO4 8,7 ml . 0,048 M = Ke- Mefenamat ditambahka Blanko (VEDTA berlebih yang 0,05 M n yang bereaksi VZnSO4 berlebih = 8,35 ml bereaksi dengan dengan analit - Menghitung VZnSO4 yang bereaksi dengan analit ZnSO4) 1. VZnSO4 analit = VZnSO4 yang ditambahkan – Vtitrasi Blanko – VZnSO4 1 10 ml 10 ml 0,4 ml 8,8 ml 8,45 1,15 ml berlebih ml 2 10 ml 10 ml 0,6 ml 8,7 ml 8,35 1,05 ml = 10 ml – 0,4 ml – 8,45 ml ml VZnSO4 analit = 1,15 ml 3 10 ml 10 ml 0,4 ml 8,7 ml 8,5 ml 1,25 ml 2. VZnSO4 analit = 10 ml – 0,6 ml – 8,35 ml = 1,05 ml
3. VZnSO4 analit = 10 ml – 0,4 ml – 8,5 ml
VZnSO4 analit = 1,25 Perhitungan :
- Menghitung VZnSO4 berlebih
1. VZnSO4 . MZnSO4 = VEDTA. MEDTA Penetapan Kadar Asam Mefenamat menggunakan Titrasi VEDTA . MEDTA VZnSO4 berlebih = Kompleksometri Refrreshment MZnSO 4 1. VAsam Mefenamat . MAsam Mefenamat = VZnSO4 . MZnSO4 8,8 ml . 0,048 M VZnSO 4 . MZnSO 4 = MAsam Mefenamat = 0,05 M VAsam Mefenamat 1,15 ml .0,05 M = VZnSO4 berlebih = 8,45 ml 10 ml MAsam Mefenamat = 0,006 M VEDTA . MEDTA 2. VZnSO4 berlebih = MZnSO 4 VZnSO 4 . MZnSO 4 8,7 ml . 0,048 M 2. MAsam Mefenamat = = VAsam Mefenamat 0,05 M 1,05 ml .0,05 M VZnSO4 berlebih = 8,35 ml = 10 ml MAsam Mefenamat = 0,005 M VEDTA . MEDTA 3. VZnSO4 berlebih = MZnSO 4 VZnSO 4 . MZnSO 4 3. MAsam Mefenamat = VAsam Mefenamat 1,25 ml .0,05 M mg AsamOksalat = 1. VNaOH . NNaOH = 10 ml BE AsamOksalat MAsam Mefenamat = 0,006 M mg Asam Oksalat 0,006 M + 0,005 M +0,006 M NNaOH = BE AsamOksalat . VNaOH MAsam Mefenamat rata-rata = = 0,006 M 3 63 mg NNaOH = g Asam Mefenamat = MAsam Mefenamat x BM Asam Mefenamat x VAsam 63 .10 , 8 ml Mefenamat NNaOH1 = 0,092 N = 0,006 M x 241,29 x 0,05 L mg Asam Oksalat 2. NNaOH2 = BE AsamOksalat . VNaOH g Asam Mefenamat = 0,07 g 63 mg = g Asam Mefenamat 63 .10,5 ml % Asam Mefenamat = x 100% VAsam Mefenamat NNaOH2 = 0,095 N 0,07 g = x 100% 50 ml mg Asam Oksalat 3. NNaOH3 = BE AsamOksalat . VNaOH % Asam Mefenamat = 0,14% b/v 63 mg = 63 .10,6 ml NNaOH3 = 0,094 N 0,092 N + 0,095 N +0,094 N NNaOH rata-rata = = 0,094 N 3 Pembakuan HCl menggunakan NaOH hasil pembakuan (0,094 N) Percobaan Ke- VNaOH VHCl NHCl ASAM BASA TIDAK LANGSUNG 1 10 ml 10,4 ml 0,090 N 2 10 ml 10,6 ml 0,090 N Sampel : 18 3 10 ml 10,4 ml 0,090 N Pembakuan NaOH menggunakan Asam Oksalat 0,1 N Rata-rata 0,090 N Percobaan Ke- VAsam Oksalat VNaOH NNaOH Perhitungan : 1 10 ml 10, 8 ml 0,092 N 1. VHCl . NHCl = VNaOH . NNaOH 2 10 ml 10,5 ml 0,095 N VNaOH . NNaOH 3 10 ml 10,6 ml 0,094 N NHCl1 = VHCl 1 Rata-rata 0,094 N 10 ml . 0,094 N Perhitungan : = 10,4 ml Mgek NaOH = Mgek Asam Oksalat NHCl1 = 0,090 N VNaOH . NNaOH VHCl . NHCl 2. NHCl2 = 3. NPelarut3 = VHCl 2 VPelarut 3 0,1 ml .0,090 N 10 ml . 0,094 N = = 10 ml 10,6 ml NPelarut3 = 0,0009 N NHCl2 = 0,090 N 0,0018 N + 0,0018 N + 0,0009 N NPelarut rata-rata = = 0,0015 N VNaOH . NNaOH 3 3. NHCl3 = VHCl 3 10 ml . 0,094 N = 10,4 ml Penetapan Kadar Analit (Asetosal) dengan Titrasi Asam Basa Tidak NHCl3 = 0,090 N Langsung 0,090 N + 0,090 N + 0,090 N Percobaa VAsetosal VNaOH yang VTitrasi VHCl (VNaOH VNaOH VNaOH yang NHCl rata – rata = = 0,090 N 3 n Ke- ditambahkan Blanko yang berlebih bereaksi bereaksi dengan Titrasi Blanko (Pelarut yang digunakan etanol 96%) dengan analit Percobaan Ke- VPelarut VHCl NPelarut HCl) 1 10 ml 0,2 ml 0,0018 N 1 10 ml 25 ml 0,2 ml 20,8 ml 19,91 4,89 ml ml 2 10 ml 0,2 ml 0,0018 N 2 10 ml 25 ml 0,2 ml 20,5 ml 19,63 5,17 ml 3 10 ml 0,1 ml 0,0009 N ml Rata-rata 0,0015 N 3 10 ml 25 ml 0,1 ml 20,6 ml 19,72 5,18 ml Perhitungan : ml 1. VPelarut . NPelarut = VHCl . NHCl VHCl . NHCl Keterangan : VNaOH yang bereaksi dengan analit = VNaOH yang ditambahkan - NPelarut1 = VTitrasi Blanko – VNaOH berlebih VPelarut 1 NNaOH = 0,094 N 0,2 ml .0,090 N = 10 ml Perhitungan : NPelarut1 = 0,0018 N 1. VNaOH berlebih . NNaOH = VHCl . NHCl VHCl . NHCl 2. NPelarut2 = VHCl . NHCl VPelarut 2 VNaOH berlebih = NNaOH 0,2 ml .0,090 N = 20,8 ml . 0,090 N 10 ml = 0,094 N NPelarut2 = 0,0018 N VNaOH berlebih = 19,91 ml
1. VAsetosal . NAsetosal = VNaOH. NNaOH
VNaOH . NNaOH berlebih g Asetosal NAsetosal = % Asetosal = x 100% VAsetosal VAsetosal 4,89 ml . 0,094 N 0,43 g = = x 100% 10 ml 50 ml NAsetosal = 0,046 N % Asetosal = 0,86 % b/v VHCl . NHCl 2. VNaOH berlebih = NNaOH 20,5 ml . 0,090 N = 0,094 N ARGENTOMETRI VNaOH berlebih = 19,63 ml Dik : BM Tramadol HCl = 299,84 BM HCl = 36,5 VNaOH . NNaOH berlebih 2. NAsetosal = BE NaCl = 58,5 VAsetosal Pembakuan AgNO3 dengan NaCl p.a 5,17 ml . 0,094 N = Dik : Bobot NaCl p.a = 50 mg 10 ml NAsetosal = 0,049 ml Percobaan Ke- VAgNO3 NAgNO3 1 17,4 ml 0,049 N VHCl . NHCl 2 17,3 ml 0,049 N 3. VNaOH berlebih = NNaOH 20,6 ml . 0,090 N 3 17,4 ml 0,049 N = Rata-rata 0,049 N 0,094 N VNaOH berlebih = 19,72 ml Perhitungan : 1) Mgek AgNO3 = Mgek NaCl VNaOH . NNaOH berlebih mg NaCl 3. NAsetosal = VAgNO3 . NAgNO3 = VAsetosal BE NaCl 5,18 ml .0,094 ml mg NaCl = NAgNO3 = 10 ml BE NaCl .VAgNO 3 NAsetosal = 0,049 N 50 mg = 58,5. 17,4 ml 0,046 N +0,049 N + 0,049 N NAgNO3 = 0,049 N NAsetosal rata-rata = = 0,048 N 3 mg NaCl 2) NAgNO3 = BE NaCl .VAgNO 3 g Asetosal = NAsetosal x BE Asetosal x VAsetosal 50 mg = 0,048 N x 180,16 x 0,05 L = 58,5. 17,3 ml g Asetosal = 0,43 g NAgNO3 = 0,049 N mg NaCl g HCl = NHCl x BE HCl x VHCl 3) NAgNO3 = BE NaCl .VAgNO 3 = 0,047 N x 36,5 x 0,05 L 50 mg = g HCl = 0,086 gram 58,5. 17,4 ml NAgNO3 = 0,049 N BM Tramadol HCl g Tramadol HCl = x g HCl 0,049 N + 0,049 N + 0,049 N BM HCl NAgNO3 rata-rata = = 0,049 N 3 299,84 = x 0,08 g Penetapan Kadar Tramadol HCl dengan Titrasi Argentometri Metode Mohr 36,5 g Tramadol HCl = 0,71 g/50 ml Percobaan Ke- VHCl VAgNO3 NHCl 1 10 ml 9,7 ml 0,048 N g Tramadol HCl 2 10 ml 9,5 ml 0,046 N % Tramadol HCl = x 100% V Tramadol HCl 3 10 ml 9,8 ml 0,048 N Rata-rata 0,047 N 0,71 g = x 100% Perhitungan : 50 ml
VAgNO3 . NAgNO 3 NHCl = VHCl 9,7 ml . 0,049 N = 10 ml NHCl = 0,048 N VAgNO3 . NAgNO 3 2) NHCl = VHCl 9,5 ml . 0,049 N = 10 ml NHCl = 0,046 N VAgNO3 . NAgNO 3 3) NHCl = VHCl 9,8 ml . 0,049 N = 10 ml NHCl = 0,048 N 0,048 N + 0,046 N +0,048 N NHCl rata-rata = = 0,047 N 3