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Disusi 10

1. The document describes the preparation and calculation of standard working solutions from a stock solution with a concentration of 5034 ppm. Six working standard solutions were prepared with concentrations ranging from 201.36 to 805.44 ppm. 2. A 500 ppm standard solution was also prepared for recovery calculations. Three samples were weighed and found to have masses ranging from 0.0213 to 0.0219 g. 3. Three recovery samples were also weighed and had masses ranging from 0.0209 to 0.0217 g. Linear regression of the standard solutions yielded a correlation coefficient of 0.9324. Concentrations of the samples and recoveries were calculated from the regression equation.

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Zaqina Erin Setya Fazri
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28 views8 pages

Disusi 10

1. The document describes the preparation and calculation of standard working solutions from a stock solution with a concentration of 5034 ppm. Six working standard solutions were prepared with concentrations ranging from 201.36 to 805.44 ppm. 2. A 500 ppm standard solution was also prepared for recovery calculations. Three samples were weighed and found to have masses ranging from 0.0213 to 0.0219 g. 3. Three recovery samples were also weighed and had masses ranging from 0.0209 to 0.0217 g. Linear regression of the standard solutions yielded a correlation coefficient of 0.9324. Concentrations of the samples and recoveries were calculated from the regression equation.

Uploaded by

Zaqina Erin Setya Fazri
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as DOCX, PDF, TXT or read online on Scribd
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1.

Kosentrasi Larutan Baku


botol timbang + ekstrak = 13,3952 g
Botol timbang = 13,1435 g _
Bobot ektrak = 0,2517 g

Penimbangan dan konsentrasi Baku induk


Baku induk 1 = 0,2517 g ~251,7 mg
251 ,7 mg
= × 1000=5034 ppm
50 ml
Baku induk 2 = N1 x V1 = N2 x V2
5034 ppm x 4,0 ml = N2 x 10,0 ml
N2 = 2013,6 ppm
Konsentrasi baku kerja
BK 6 : N1 x V1 = N2 x V2
2013,6 ppm x 4,0 ml = N2 x 10,0 ml
N2 = 805,44 ppm
BK 5 : N1 x V1 = N2 x V2
2013,6 ppm x 3,0 ml = N2 x 10,0 ml
N2 = 604,08 ppm
BK 4 : N1 x V1 = N2 x V2
5034 ppm x 5,0 ml = N2 x 50,0 ml
N2 = 503,4 ppm
BK 3 : N1 x V1 = N2 x V2
805,44 ppm x 5,0 ml = N2 x 10,0 ml
N2 = 402,72 ppm
BK 2 : N1 x V1 = N2 x V2
604,08 ppm x 5,0 ml = N2 x 10,0 ml
N2 = 302,04 ppm
BK 1 : N1 x V1 = N2 x V2
402,72 ppm x 5,0 ml = N2 x 10,0 ml
N2 = 201,36 ppm
2. Perhitungan Konsentrasi Larutan Standar EPMS (dibuat 500 ppm untuk recovery)
botol timbang + ekstrak = 13,2013 g
Botol timbang = 13,1495 g _
Bobot ektrak = 0,0518 g ~ 51,8 mg
51, 8 mg
= × 1000=518 ppm
100 ml

3. Penimbangan sampel 20 mg → 0,02±10% (0,018 g -0,022 g )


 Sampel 1 → botol timbang + ekstrak = 12,8108 g
Botol timbang = 12,7895 g _
Bobot ektrak = 0,0213 g
 Sampel 2 → botol timbang + ekstrak = 12,6956 g
Botol timbang = 12,6737 g _
Bobot ektrak = 0,0219 g
 Sampel 3 → botol timbang + ekstrak = 13,1110 g
Botol timbang = 13,0906 g
Bobot ektrak = 0,0204 g

4. Penimbangan recovery 20 mg → 0,02±10% (0,018 g -0,022 g )


 Recovery 1 → botol timbang + ekstrak = 12,9669 g
Botol timbang = 12,9460 g _
Bobot ektrak = 0,0209 g
 Recovery 2 → botol timbang + ekstrak = 12,2763 g
Botol timbang = 12,2548 g _
Bobot ektrak = 0,0215 g
 Recovery 3 → botol timbang + ekstrak = 13,1123 g
Botol timbang = 13,0906 g _
Bobot ektrak = 0,0217 g
Tabel Konsentrasi dan Luas Area baku Kerja
Konsentrasi (ppm) Luas Area (AV) Sampel dan
BK Luas Area (AV)
Recovery
Teoritis Praktis (x) (y)

1 200 201,36 14455,3 S1 20429,0

2 300 302,04 25549,4 S2 21865,1

3 400 402,72 21885,7 S3 21704,4

4 500 503,40 22380,2 R1 18853,2

5 600 604,08 22750,5 R2 20104,8

6 800 805,44 25964,7 R3 19992,1

Regresi 6 BK
a : 16439,74
b : 12,18406
r hitung : 0,64 < r table (0,917)
1 sampel direject (BK2)
a : 12639,03
b : 17,576976 ~ 17,577
r hitung : 0,9324 < r table untuk 5 data

Perhitungan Konsentrasi kadar Sampel dan Recovery


a. S1
y = 17,577x + a
20429,0 = 17,577x + 12639,03
x = 443,19 ppm
b. S2
y = 17,577x + a
21865,1 = 17,577x + 12639,03
x = 524,89 ppm
c. S3
y = 17,577x + a
21704,4 = 17,577x + 12639,03
x = 515,75 ppm
d. R1
y = 17,577x + a
18853,2 = 17,577x + 12639,03
x = 353,54 ppm
e. R2
y = 17,577x + a
20104,8 = 17,577x + 12639,03
x = 424,75 ppm
f. R3
y = 17,577x + a
19992,1 = 17,577x + 12639,03
x = 418,335 ppm

Perhitungan sampel untuk penetapan kadar EPMS dalam ekstrak kering


% kadar cab-o-sil = bobot cab-o-sil/ bobot ekstrak kering x 100%
= 20 gram / 55,16 gram x 100% = 36,26%

Penimbangan sampel
Sampel 1 ektrak tanpa cab-o-sil = 21,3 mg - (36,26% x 21,3 mg) = 13,58 mg
Sampel 2 ektrak tanpa cab-o-sil = 21,9 mg - (36,26% x 21,9 mg) = 13,96 mg
Sampel 3 ektrak tanpa cab-o-sil = 20,4 mg - (36,26% x 20,4 mg) = 13,00 mg

Pengenceran 3 ml
3
Sampel 1 : x 443 , 19 ppm = 1329,57 ppm
1
3
Sampel 2 : x 524 , 89 ppm = 1574,67
1
3
Sampel 3 : x 515 , 75 ppm =1547,25 ppm
1
Bobot sampel dalam 5 ml
1329 ,57 mg
Sampel 1 : x 5 ml = 6,6479 mg
1000 ml
1574 , 67 mg
Sampel 2 : x 5 ml = 7,8734 mg
1000 ml
1547 ,25 mg
Sampel 3 : x 5 ml = 7,7363 mg
1000 ml

(%) EPMS dalam sampel


6,6479 mg
Sampel 1 : x 100 % = 48,95%
13 ,58 mg
7,8734 mg
Sampel 2 : x 100 % = 56,40%
13 , 96 mg
7,7363 mg
Sampel 3 : x 100 % = 59,51%
13 , 00 mg

Penentuan Presisi
48 , 95 %+ 56 , 40 %+ 59 ,51 %
Rata-rata : = 54,95%
3
SD : 5,4266
SD 5,4266
KV : x 100 % = x 100 % = 9,88%
rata−rata 54 , 95
Penimbangan recovery
Recovery 1 ektrak tanpa cab-o-sil = 20,9 mg - (36,26% x 20,9 mg) = 13,32 mg
Recovery 2 ektrak tanpa cab-o-sil = 21,5 mg - (36,26% x 21,5 mg) = 13,70 mg
Recovery 3 ektrak tanpa cab-o-sil = 21,7 mg - (36,26% x 21,7 mg) = 13,83 mg

Pengenceran 4 ml
4
Recovery 1 : x 353 , 54 ppm = 1414,16 ppm
1
4
Recovery 2 : x 424 , 75 ppm = 1699,00 ppm
1
4
Recovery 3 : x 418,335 ppm = 1673,34 ppm
1

Bobot recovery dalam 5 ml


1414 , 16 mg
Recovery 1 : x 5 ml = 7,0708 mg
1000 ml
1699 ,00 mg
Recovery 2 : x 5 ml = 8,4950 mg
1000 ml
1673 ,34 mg
Recovery 3 : x 5 ml = 8,3667 mg
1000 ml

(%) EPMS dalam recovery


7,0708 mg
Recovery 1 : x 100 % = 53,08%
13 , 32mg
8,4950 mg
Recovery 2 : x 100 % = 62,01%
13 , 70 mg
8,3667 mg
Recovery 3 : x 100 % = 60,50%
13 , 83 mg

453 , 08 %+ 62 ,01 % +60 ,50 %


Rata-rata : = 58,53%
3
Penentuan akurasi
 Ct : Kadar recovery dalam 5 ml
rata−rata sampel x bobot penimbangan recovery
 Cp :
100
Ct
 Recovery : x 100 %
Cp+ Cst

Ct Cp Cst recovery

54 , 95 x 13 , 32 7,0708
7,0708 mg Cp1 = =7 , 32 0,518 R1 = x 100 %=90 ,21 %
100 7 ,32+ 0,518

54 , 95 x 13 , 70 8,4950
8,4950 mg Cp2 = =7 , 53 0,518 R2 = x 100 %=105 ,55 %
100 7 ,53+ 0,518

54 , 95 x 13 , 83 8,3667
8,3667 mg Cp3 = =7 , 60 0,518 R3 = x 100 %=103 , 06 %
100 7 , 60+0,518

90 , 21% +105 , 55 %+103 , 06 %


Rata-rata : = 99,61%
3

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