Wednesdiay,06 March 2024
Practical 4:Inductively Coupled Plasma-Optical Emission Speetroscop}
AIM
This experiment aims to determine the concentration of Copper, Iron, and Mee ea feo
Magnesium content in tea samples, namely green tea, Rooibos te, and five roses. ad
determine the concentrations of the following elements in standard solution, to prep
element standard solution to obtain quantitative measurements for the ICP-OES.
Abstract
Concentrations of the following selected metals (Cu, Fe, Mg, Mn) in tea leaves were investigated.
Samples included green tea, Rooiboos, and Sroses tea. Metal determinations were performed
using Inductively Coupled Plasma-Optical Emission Spectroscopy. Where the standard solutions
and their intensities were identified using the ICP-OES and used to plot calibration curves. In
green tea it was found to have high amounts of iron, and manganese content compared to other
samples, whereas Sroses has a significant concentration content of magnesium, it was found that
rooibos has the least metal concentration out of all 3 samples. Taking this into consideration,
green tea must be the most beneficial beverage in terms of human health as it contains the most
necessary metals namely iron, mangattese and magnesium, while 5 roses have significant
concentrations of these metals too, green tea is still at an advantage.
Results
|. Ifthe samples were to dry out, this would lead to the loss of volatile elements, thus
Guusing sample volailisation, additionally, allowing the sample to dry out will alle wv
{fe sample to return to its original solid state which will impact analyte recovery.
] 2. Since this is a wet digestion technique, nitric acid is required to digest the samples to
analyse the metals that will be in the solution, with this the ‘sample scan be analyzed by
ICP.
Table 1:preprared multi-clement standards(ppm)
[Elements | Standard 1 | Standard Standard 3 | Standard 4
0.05 0.2 04 0.8 i ; Eas :
0.25 10 2.0 4.0 5.0 10
1.25 5.0 10 20 25 40
0.5 2.0 40 8.0 10.0 20.0
Powered by CamScannerThe multi-working standard contains 10 x concentrations of standard 5 from the table |
above.
CiVieC2V2
cu
(1000ppm)(V)=(10ppm)(100mL)
V=ImL
Which means, ImL of the copper solution is used to make 10ppm copper that is in the
multi
clement working standard, The same was done for Mg, Mn, and Iron to caleulate 250ppm-
100ppm and 50 ppm of the elements respectively.
Fe
(1000ppm)(V1)=(S0ppm)(100mL)
V=5
Mg
(1000ppm)(V1)=(250ppm)(100mL)
Vi=25mL
Mn
(1000ppm)(V)=(100ppm)(100mL)
Vi=10mL
‘Table 2: Concentrations of the elements in the multi-clement working standard and
volumes of the 1000ppm standards to prepare the multi-element working standard.
ELEMENT, Concentration of elements _| Volume of elements.
Fe SOppm. SmL.
[Mg_ 250ppm, 25mL
Mn 100ppm 10mL.
Cu 10ppm imL 7 y
From the multi-element working standard, 6 standard solutions had to be mixed. Where
the volume from the multi-element solutions was determined,using CiV1-C2V2
Standard 1.
CIVi =C2v2
10ppm V1 = (0.05pm) (100mL)
V1 =0.5ml of working solution
Fe standard 2
10ppm V1 = (0.2ppm) (100mL)
V1 =2 mL of working solution
Powered by CamScannerPowered by CamScannerPowered by CamScannerPowered by CamScannerEmission intensity vs concentration
|
|
a
mee
Emission Intensity
ee 2s 2
¥=S2473x4 3187.
CConcentration(ppm)
23 3 3s 4
as
Figure 11; Calibration curve of Mg standards Emission intensity/au plotted as
the function of concentration/ppm
‘Table 12: Mass of samples(g) _
‘Samples Runt Run2 Run3
GreenTea, 0.1029, 0.1049) 0.1099
Rooibos 0.1002 0.103 0.1001
Five Roses 0.1017 0.1013 0.1001
Table 9: Samples of teas with Emission intensity/au for Cu
Sample Emission Intensity
Greenteal (6376.447617
Greentea2 5941217418
Greentea3 6195.00249
Rooibos! 3607.274633,
Rooibos? 4360.281484
Rooibos3 4768.142255
FiveRoses] 7891.442282
Fiveroses2 16939.09476
[Fiveroses3 10183.06375
Table 10: Samples of teas with emission intensity for Fe
Sample
Emission Intensity
Greenteal
41095.911480
3.7615 .
Calculation for greentea 1 for iron
Y=31503x-1095.1
Y=41095.91
X=1.3393 mg/L,
1.3393 x0,25
0.3348 mg x 1000
334.8173,
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X=2.196 me «1000
2196.25
Table 12 : Table 13: Masses calculated from the calibration curves (ug/g)
Sample copper Fe Mg __ Mn 1
Greenteal | 3.76 334.817 _| 4996.75 i
z 2196.25
Rooibos 1 2S 36.39 4215 788
SRoses 1 4.287 174.5 5748.079 | 755.47
4. Yes, the tea samples have a significant difference. Green tea has the most metal
content followed by five roses then lastly by rooiboos. The metal content of the tea is
differentiated by the regions at which the tea leaves are grown, and the degree of
oxidation it undergoes. Depending on where the tea leaves are grown, factors such as
soil type, and the environment, the metal content will vary. Thus the tea leaves will be
different. There’s a high amount of manganese and
agnesium present in green teas as compared to all other elements while copper and
Of in dominate in Five Roses tea samples 4, So, the samples are different in terms of
¥ composition concerning the trace elements, Cu, Mg, Mn and Fe.
5. Prepare multi-element standards can be di, since element compatibility, and
solubility will be affected and will result in the possible precipitation of one or more
elements in the standard, and the elements can cause interference with each other
vy them difficult to analyze them because they combine.Figure; Drawing of ICP-AES and components.
Peristaltic Pump; The fluid sample is pumped into the nebulizer via the peristaltic pump
certs the sample to aerosol, which will be transferred to the spray chamber and
ito the spray chamber along with the sample.Spray chamber filters
from the aerosol, where the large mist particles settle down as
swept into the torch assembly into the plasma. The
meray source: to get atoms sufficiently energised that they emit light RF generators generates an
oscillating electro-magnetic field where the radiation is sent to the load coil, the load oil is where
yhich then transfers the radiation to the torch. p
Nebuliser: conv
injects humidified Argon gas
out the uneven, large droplets
waste into the rain, and the finest particles are
the radiation from the RF generator travels to w1
‘hich has argon flowing into it and will form an plasma in the RF field. Transducer - converts
gneray from one form to another. Usually, it converts a signal in one form of energy to a signal in
nother. Torch: makes the gas pass through at a high velocity. The transfer optics focuses the
nce slit whereas the detector reads out the intensity measured from the
plasma image on the entra
sample.A monochromator/wavelength isolation device is responsible for directing the wanted
light or focusing it by blocking the unwanted wavelengths therefore providing monochromatic
Tight or it transmits a mechanically selectable narrow band of wavelengths of light or other
radiation
Powered by @ CamScannerecause it has excellent
Rives the Freedom from matrix effects and provides a
Tight View for any sample 8. Furthermore, using bo
g b using both
neta ine have found a very wide dynamic range, As the dynamic range shifts lower
‘view. Italso has a tolerance to dissolved solids like that of a dedicated axial. The
torch lifetimes are shorter, and the torch is longer than the radial design. The slots or holes get a
radial view.
8. References
1) Anna Szymezycha-Madeja(2015) - Determination of essential and non-essential elements in
green and black teas by FAAS and ICP OES simplified — multivariate classification of different
tea products, Microchemical Journal
2)Charles, B., & Fredeen,|k. J. (1997). Concepts, instrumentation and techniques in inductively coupled
plasma optical emission spectrometry. Perkin Elmer Corp, 3(2), 115.