Analytical Lab Exp.1

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Calculation and discussion:

 What is the λmax for Paracetamol?


λmax =243 nm; we chose this value according the maximum peak that UV device
measured it.

 For diluent preparation:

Methanol: water (30ml: 70ml) for 100ml.

To prepare 1Liter:

30 ml∗1000ml
Volume of methanol= = 300ml.
100 ml

70 ml∗1000 ml
Volume of water= = 700ml.
100 ml

 For solution of standard and sample preparation:

weight of four tablet


Weight tablet₁= 0.5651g
Weight tablet₂= 0.5664g
Weight tablet₃= 0.5678g
Weight tablet₄= 0.5687g
Total weight of four tablet= 2.268g
Average weight=

∑ total weight of 4 tablet


=0.567 g
4

The average weight of four tablet= 567mg of paracetamol tablets contains≈ 500 mg
paracetamol API

567 mg∗100 mg
The Weight of powder from tablet contains 100mg= =113.4 mg.
500
Concentration of sample =

100 mg
∗1 ml
100 ml
∗1 ml
1 2 100 ml mg
concentration of stock ’ s solution∗dilution ∗dilutio n = =0.0004 =0.4 ppm
25 ml ml
.

 Measure the absorbance of the standard and sample solutions at wavelength


of 243 nm using diluent as blank.

Concentration of sample= 0.0004 mg/ml Absorbance of sample= 0.036


Concentration of standard= 0.0002 Absorbance of standard= 0.019
mg/ml

the Assay (%) of paracetamol in the samples=

absorbance of sample AS∗conc . of standard 0.036∗0.0002


∗100 %=¿ ∗100 %=¿
absorbance of standard Astd .∗conc . of sample 0.019∗0.0004
94.74%

II. Determination of paracetamol by using calibration curve


 Calculation for different concentration of standard:

10 mg 0.1 mg
From the stock’s solution of STD ( = =100 ppm ¿ take four dilution
100 ml ml

1. The conc. Of STD₁=

10 mg
∗0.1ml
1 100 ml mg
concentration of stock ’ s solution∗dilution = =0.0002 =0.2 ppm
50 ml ml
.
2. The conc. Of STD₂=

10 mg
∗0.5 ml
100 ml mg .
concentration of stock ’ s solution∗dilution ₂= =0.001 =1 ppm
50 ml ml
3. The conc. Of STD₃=

10 mg
∗1ml
₃ 100 ml mg .
concentration of stock ’ s solution∗dilution = =0.002 =2 ppm
50 ml ml
4. The conc. Of STD₄=

10 mg
∗3 ml
100 ml mg .
concentration of stock ’ s solution∗dilution ₄= =0.006 =6 ppm
50 ml ml
 The Measurement of the absorbance for the standard solutions at wavelength
of 243 nm using diluent as blank.

Concentration (mgl100 ml) Concentration ppm Absorbance at 243 nm


Blank = 0 0 0
STD₁= 0.0002 0.2 0.019
STD₂= 0.001 1 0.071
STD₃= 0.002 2 0.145
STD₄= 0.006 6 0.417
Sample= 0.0004 0.4 0.036
The assay%= 94.7%

 Plot Absorbance vs. concentration using Excel software.


calibration curve for STD paracetamol

0.45
0.4 f(x) = 0.07 x + 0
0.35 R² = 1
0.3
absorbance

0.25
0.2
0.15
0.1
0.05
0
0 1 2 3 4 5 6 7
concentration of STD paracetamol ppm

Figure 1: the calibration curve BTW conc. and absorbance for standard solution.

 Check the linearity of the calibration curve (do regression analysis:


regression equation, and correlation coefficient 0.998.

As noted in the figure1, the calibration curve is linear, the equation is


y=0.0691 x +0.0032and R2=0.9997.

As express Beer-Lambert law A= Є b C that main A= constant* C to the same length


of cell in UV (quartz cells (1 cm)). So, the absorbance is directly proportional to the
concentration C (when the concentration of the sample increases, absorption increases
directly) and the relationship is linear ( R2=0.9997).

- If the concentration of sample is unknown it can use the calibration curve to know
this concentration by applied on calibration equation

The Absorbance for unknown sample at 243 nm= 0.036

By applied in calibration curve or slope of calibration curve:

y=0.0691 x +0.0032

Y is absorbance value and x are the concentration.

0.036=0.0691 x +0.0032
X= 0.474ppm.

∆ y 0.036−0.019
And can determine the unknown concentration by slope= = =0.0691
∆x x−0.2

X by slope= 0.45ppm ‫هاد الي بالصفر اضافه مني‬

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