UV-VISIBLE SPECTROSCOPIC AND IODOMETRIC BACK TITRATION

ANALYSIS OF TOTAL CAFFEINE CONTENT OF TEA, COFFEE AND

ENERGY DRINKS

Determination of Caffeine content by UV-Vis Spectroscopy:

Caffeine extraction from the sample solution was performed by mixing 5 mL of

filtrate with 5 mL of dichloromethane and stirring the liquid for one minute using a
vortex mixer. Finally, the absorbance of caffeine in dichloromethane was measured
by the UV-Vis spectrophotometer (Shimadzu-UV-1900i) within the range of 200–
500 nm against the corresponding blank reagent (dichloromethane) and—as per to
the Beer-Lambert law—at a maximum wavelength of λ = 273 nm (Table 1). The
caffeine content was calculated in percent on a dry weight (dw) basis (Table 1).

a b
 c d

e f
Fig.1- (a) Show 5 samples, (b) Tea extraction, (c) Smart extraction, (d) Maxiki
extraction, (e) Redbull extraction process and (f) Shows Shimadzu-UV-1900i
Table-1

percentage of caffeine for five independent measurements for (5) samples.

Sample Amount of Mass of caffeine Percentage of

sample in sample (mg) caffeine in sample
(%w\w)
Tea (Mahmood) 0.028 (mg) 6.22 × 10-5 0.22
Coffee (Nescafe Gold) 0.028 (mg) 0.3139 × 10-3 1.12
Redbull 50 (ml) 8.39 × 10-5 0.1678
Smart 50 (ml) 8.13 × 10-5 0.1626
Maxiki 50 (ml) 7.29 × 10-5 0.1458

Table.2: UV-Vis spectrophotometer for each sample at different temperature:

Temperature 50 60 70 80 90
range (±1
Co)
Tea 0.224 0.235 0.246 0.251 0.254
Maxiki 0.065 0.068 0.069 0.07 0.067
smart 0.105 0.105 0.105 0.104 0.101
Redbull 0.087 0.087 0.088 0.088 0.089
coffee 0.211 0.211 0.21 0.209 0.211
 0.35 0.20
50 Co 273

0.30 60 Co 0.18
smart 70 Co
70 Co 0.16 smart
0.25
Absorbance (a.u)

Absorbance (a.u)
80 Co
0.14
0.20
0.12
0.15
0.10
0.10
0.08
0.05
0.06
0.00
200 225 250 275 300 325 50 60 70 80 90

Wavelength (nm) Temperature (Co)

Determination of Caffeine by Iodometric Back Titration:

Experimental Procedure:

Preparations of solutions

Starch solution;

1.0g of starch was poured into 10ml of distilled water, stirred well, and then
transferred into a 100 ml boiling water. The solution was stirred and boiled for one
minute, then it was allowed to cool at room temperature and filtered.
Acid solutions; 1.0M solution of HCl was prepared by measuring 8.3 mL of 37%
HCl and pouring into a 100 mL volumetric flask containing small amount of
distilled water and making up the solution to the mark with the distilled water.

Iodine solution; 0.634.4g of iodine crystal was dissolved in 1000cm3 distilled

water to produce a 0.01M solution of iodine.

Thiosulphate solution; 3.16g of Na2S2O3 was dissolved in 1000cm3 distilled water

to get a 0.02M thiosulphate solution. The water used here was boiled and cooled
before use.

Determination of Caffeine by Iodometric Back Titration:

Blank Titration:

25 ml of the 0.01 M iodine solution was measured and poured into a 100 mL
Erlenmeyer flask, 2.5 ml of 1.0 M HCl solution was added to the iodine solution
and it was immediately titrated with the 0.02 M thiosulphate solution until the
yellow color was almost gone (pale yellow). A few drops of starch indicator (three
drops) were added and titration was continued until the blue color of the solution
was gone. The procedure was repeated three times and the results recorded.

Determination of Caffeine levels in the Energy Drinks:

The energy drinks were used as supplied by manufacturers. 25 ml solution of 0.01

M iodine solution was measured and poured into a 100 ml Erlenmeyer flask, 2.5
ml of 1.0 M HCl solution was added to it and 25 ml of each brand of energy drink
was also added to the mixture. The excess iodine solution was then titrated against
a 0.02 M thiosulphate solution until the yellow color of the iodine was almost
gone. A few drops of starch indicator were added and titration was continued until
the blue color was gone. The results were recorded and the process repeated thrice
for each sample of energy drink. The difference between the blank and each of the
titration in a sample was used to determine the caffeine content found in each
titration.

a b
Fig.2.(a) Iodometric titration before end point, (b) Iodometric titration after end
point

Iodometric Back titration results

Table 3: Caffeine Content in Energy Drinks from Iodometric Back Titration.

Sample Caffeine content in Caffeine content in

(mg/mL) (g/L)
Redbull 0.3356 0.0003356
Smart 0.3252 0.0003252
Maxiki 0.2916 0.0002916

Dr.Sirwan Taha Uthman MSc. Hawta Kastro Abdulla Abdulbasit Hakim

Salahaddin University Salahaddin University Salahaddin University

Chemistry Department Chemistry Department Chemistry Department