Report of laboratory

exercises
 Atomic absorption specroscopy is analytical method characterized with high
selectivity,sensitivity and fast speed.

Application of flame atomic absorption

spectrometric techniques to pharmaceuticals
and waters
 Three different brands of multivitamins (effervescent tablets) were taken from the market
and the levels of some elements (total amount) were determined (Ca, Mg, Zn, Cr, Mn)

 One tablet from each of the three pharmaceutical products was dissolved in 100ml (mother
solution) water and one milliliter of each solution was diluted 25 times. So were prepared the
working sample solutions and were marked as follows:
Sample 1 (samp1) - ABO Pharma A-Z ®;
Sample 2 (samp2) - Supradyn ®;
Sample 3 (samp3) - Supravit Active ®;

 A brand of mineral water - Gorna Banja ® was tested for any Mg and the concentration of
the metal was under the detection limit of the instrument

 For each different element was made a standard calibration curve, using freshly prepared
standard solutions from 0,5; 1; 3; 5; 10; 20ppm containing all the mentioned elements in water
(deionized)

 For the last sample results were obtained both after automated calibration and a manually
made calibration curve.

 Differences in the absorption using reducing and oxidizing flames were observed
 Ca calibration curve Measured
Given values
# Sample values
300 Mgycalibration curve Measured [mg/tablet]
= 4,8951x + 22,446 [mg/tablet] Given values
250 Zn
2
R = 0,9939 curve
calibration # Sample values
y = 190,51x + 76,783 Measured [mg/tablet]
200
1200 [mg/tablet] Given values
absorance

yR
Mn
2
= 0,984 + 65,358
calibration
= 73,959x curve #
1 Sample 102 ± values
Measured
10% 160
1000
150 900 [mg/tablet]
Given values
800
800
2
yR= 25,781x
= 0,9706+ 11,941
# Sample [mg/tablet]
values
1 150±10% 100
absorbtion

100 700600 Cr calibrationRcurve(reductive flame) Measured [mg/tablet]

2
λ =422,7
= 0,9971
nm [mg/tablet] Given values
absorbance

50 600
600
y = 6.4178x + 5.7374 # Sample values
500
500 160
400
2 1 167 ± 10%
5,25±10% 120 5[ug/tablet]
100±10%[mg/tablet]
0 400400
λ =285,2
R2 = 0.9935
nm
absorbance

0 300
200
140
10 20 30 40 50 60 2 1 0.9±10% 80 2
300120
λ =213.9 nm
absorbance

200
0
100200100
concentration [ppm] 3 2 1 - 7±10% - - 8 25
00
100
80 1 2 3
λ4 8=279.5
5
nm6
3 2 1.6±10%
12,5±10% 20 1.8
0 60
0 40
2 4 6 [ppm]
concentration λ =213.9 nm
10 12
3 1,75±10% - 3
20
0 5
concentration [ppm]
10 15 20 25 2 25
0 concentration [ppm]
3 1.0±10% 1
0 5 10 15 20 25
3 - -
concentration [ppm]

Cr calibration curve (oxidation flame)

20 y = 0.8219x + 1.6256
18
R2 = 0.9996
16
14
12
10
8
6
4 λ =213.9 nm
2
0
0 5 10 15 20 25
 Pb calibration curve (ET AAS) Measured
# Sample values
350
y = 3,775x + 8,3333 [ug/tablet]
300 R2 = 0,9909
250
absorption

200 1 1.9±10%
150
100
50 λ =283.3 nm 2 2.4±10%
0
0 20 40 60 80 100

Et AA S
concentration [ppb] 3 2.1±10%

Cd calibration curve (ETAAS) Measured

# Sample values
300
y = 144,38x + 8,8333 [ug/tablet]
250
R2 = 0,9828
200
absoption

1 8.9±10%
150
100
50 λ =228.8 nm 2 1.6±10%
0
0 0,5 1 1,5 2
concentration [ppb]
3 1.9±10%
Sample 1 (samp1) - ABO Pharma A-Z ®;
Manufacturer: ABO Pharma AG

Sample 2 (samp2) - Supradyn ®;

Manufacturer: Bayer AG

Sample 3 (samp3) - Supravit Active ®;

Manufacturer: Kendy Ltd Bulgaria
Patented by Swisse AG
IR spectra of benzocaine
 CH3 (end)
CH3, CH2 def. vibr.
C-H str. vibr def. vibr.
 KBr Spectra benzocaine

-CH2
C-C
-NH2

-Ar
-C=O
-NH2
 Thank You for Your
attention
Lora Georgieva
Denitsa Atanasova
Krum Bardarov