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Objectives:
Introduction:
Instrumentation:
Beaker250ml, volumetric flask 250ml, filter paper, filter funnel, pipette, hot plate
Chemicals:
Procedures:
Sample preparation:
The anchovies was cut in small pieces and dried in oven at 110℃ for 24 hours. Three
portion of the sample was weigh ranging from 0.5 to 1.0 g and transfer into a beaker.
7ml of concentrated HNO3 and 1ml of H2O2 was added into each beaker. The beaker
was put onto a hot plate for 20 minutes. After that, the solution was filtered using a filter
funnel equipped with filter paper and combining. The sample was run for three times to
obtained the calibration points. The calibration curve was plot and the concentration of
Pb2+ in the sample was determined.
Standard preparation:
M1V1 = M2V2
(1000mg/L)(x) = (100mg/L)(0.25L)
X = 0.025 L
25ml of 1000ppm of Pb2+ stock solution was pipette into 250ml of volumetric flask. The
solution diluted by using deionized water.
2. Preparation of Pb2+ standard solution
M1V1 = M2V2
(100mg/L)(x) = (2mg/L)(0.25L)
X = 0.005 L
M1V1 = M2V2
(100mg/L)(x) = (4mg/L)(0.25L)
X = 0.01 L
M1V1 = M2V2
(100mg/L)(x) = (6mg/L)(0.25L)
X = 0.15 L
M1V1 = M2V2
(100mg/L)(x) = (10mg/L)(0.25L)
X = 0.25 L
Result and Discussion:
Based on the result from the experiment, the absorbance of light increased with
increasing concentration of Lead. The calibration curve clearly shows the linear
relationship between absorbance and concentration. From this curve the concentration
of lead in anchovies was determine is 4.169 ppm.
In this experiment, fish was used in determine the concentration of Lead. The objective to
determine the Lead in fish was achieved. The concentration of Lead from the experiment is
4.169 ppm.
References:
1. http://www.galbraith.com/spectroscopy.htm
2. http://www.kau.edu.sa/files/130002/files/6785_aas.pdf
Experiment 4: Background and Correction Method for the Determination of
Caffeine in Tea Samples by using Ultraviolet Spectroscopy.
Objectives:
Introduction:
Structure of Caffeine
Instrumentation:
Apparatus:
Beaker 250ml, volumetric flask 100ppm, hot plate, pipette, filter paper, filter funnel
Chemicals:
Procedure:
10mL of the tea sample solution was transfer into a separating funnel. 20mL of CHCl3
solution was added into the separating funnel and the mixture then shake. The mixture
will separate into two aqueous layer at the bottom and organic layer at the upper layer.
1 ml of the extract was pipette into 5 different of 10ml volumetric flask. 0.2, 0.4, 0.6, 0.8
and 1.0mL of NaOH added in respective flasks. The distilled water added to the mark.
Sample preparation:
2gm of dried tea sample was dissolved in 100ml of distilled water. After that, the
solution boiled using hot plate. After the sample cold, the sample transfer into volumetric
flask (100ppm) and diluted with distilled water. 5ml of the diluted solution was transfer
into another volumetric flask (100ml) and diluted again with distilled water.
Standard solution:
M1V1 = M2V2
(100mg/L) (x) = (2mg/L) (0.1L)
X = 0.002 L
M1V1 = M2V2
(100mg/L) (x) = (4mg/L) (0.1L)
X = 0.004 L
M1V1 = M2V2
(100mg/L) (x) = (6mg/L) (0.1L)
X = 0.006 L
M1V1 = M2V2
(100mg/L) (x) = (8mg/L) (0.1L)
X = 0.008 L
M1V1 = M2V2
(100mg/L) (x) = (10mg/L) (0.1L)
X = 0.01 L
Preparation of 0.005 M of NaOH:
𝑚𝑎𝑠𝑠
0.005 𝑀 𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠
=
𝐿 𝑣𝑜𝑙𝑢𝑚𝑒
𝑚𝑎𝑠𝑠
0.005 𝑚𝑜𝑙 22.09 𝑔/𝑚𝑜𝑙
=
𝐿 0.25 𝐿
Mass = 0.028 g
∴ Dissolve about 0.028 g of NaoH in distilled water. Transfer the solution into 250 ml of
volumetric flask and fill up with distilled water.
Result and Discussion:
The standard linear calibration curve was obtained from standard solutions
analysis and it showed a good linear relationship between absorbance and
concentrations of the standard solutions. The caffeine content in the tea sample showed
a minimum caffeine level which range from 8.6 to 9.3 ppm. The average caffeine
quantity in the tea sample was found to be ppm. Moderate caffeine consumption of
300 mg/day, is considered generally safe (Rogers and Dernoncourt, 1998; Smith,
2005). This amount typically corresponds to 4 cans of energy drink. Caffeine content in
beverage drinks varies by brand from 10 to 60 mg of caffeine per serving (Violeta et al.,
2010); however the US Food and Drug Administration (FDA, 2006) limits the maximum
amount in carbonated beverages to 6 mg/oz (200 ppm). Therefore caffeine content
allowed in soft drinks may be in the range between 30 and 72 mg/355 mL (12 oz) or
8.45-20.28 mg/100 mL (NSDA, 1999).
Conclusion:
References:
Objectives:
Introduction:
Instrumentation:
Solutions to prepare:
Sample:
Energy drink
Procedure:
A series of 5 standard solutions was prepared ranging from 0.02ppm- 0.1 ppm by using
the stock Riboflavin solution containing 100ppm of Riboflavin. After that, the solution
was diluted with 1% (v/v) acetic acid solution. A calibration Curve was plotted using the
standard concentrations (x-axis) and their fluorescence values (y-axis). From this curve,
the amount of riboflavin was determined in sample.
M1V1 = M2V2
V1 = 10 ml
M1V1 = M2V2
(100mg/L)(x) = (2mg/L)(0.25L)
X = 0.005 L
M1V1 = M2V2
(100mg/L)(x) = (4mg/L)(0.25L)
X = 0.01 L
M1V1 = M2V2
(100mg/L)(x) = (6mg/L)(0.25L)
X = 0.15 L
M1V1 = M2V2
(100mg/L)(x) = (10mg/L)(0.25L)
X = 0.25 L
Result and Discussion:
References:
1. http://dc.etsu.edu/cgi/viewcontent.cgi?article=3352&context=etd
2. http://www.vernier.com/innovate/monitoring-vitamin-b2-in-energy-drinks/
Experiment 1: Analysis of Aspirin in Commercial APC Tablet FTIR Spectroscopy
Objectives:
Introduction:
Fourier Transform Infrared (FTIR) is most useful for identifying chemicals that are
either organic or inorganic. It can be utilize to quantitate some components of an
unknown mixture and can be applied to the analysis of solid, liquid and gases. FTIR is
instrument to identifying types of chemical bond or functional groups. The wavelength of
light absorbed is show the characteristic of the chemical bond. The chemical bonds can
ce determine by interpreting the infrared absorption spectrum. For most common
materials, the spectrum of an unknown can be identified by comparison to the library of
known compound. Samples for FTIR can be prepared in number of ways. For this
experiment we use solid sample. Solid samples can be milled with potassium bromide
(KBr) to form fine powder. This powder is then compressed into a thin pellet which can
be analyzed. KBr is transparent to infrared light.
1. Instrument model:
a) Pelkin Elmer- Spectrum One (FTIR)
b) Bruker 300 UltraShelid (NMR)
2. Serial No: 55705 / ZH042703
3. Location: 306 / 307
Apparatus:
Chemicals:
KBr, sample,
Method:
2) KB pellets
One fourth of the KBr mixture was taking into the collar of the hand press. The
anvil placed along with the loger die pin to make sure it comes into contact with
samples. The die set lift carefully by holding the lower anvil. The collar must stay
in place. The handle of the hand press slowly open and the die set insert into the
hand press. After the handle closed, the dial pressure rotated until the upper ram
of the hand press slightly touches the upper anvil on the die assembly. The unit
tilt back in order to hold the die set from falling off. After the handle open, the
pressure dial rotated clockwise in one half turn. The mixture compress slowly
while closing the handle in 2 minutes. The unit tilt back, the handle open and the
die set remove from the unit carefully.
Result and discussion:
Based on the spectrum obtained from the experiment, there is no significant difference
in the fingerprinting between spectra obtained from prepared KBr disk and the standard. Since
an IR spectrum is a plot of % transmittance vs. wavenumber, the bond vibration energies vary
as moved horizontally on the graph. The IR spectra contain information about the structures of
compounds. The absorption peak at 3600 cm-1 – 2500 cm-1 arises from the stretching of
carboxylic acids group of acetylsalicylic acid. In the structure of acetylsalicylic acid, there is
aromatic compound. The aromatic compound gives absorption peak at 870 cm-1 and 735 cm-1.
The peaks in 2800- 3000 cm-1 region suggest stretching of the C-H bonds of alkyl group either
CH2 or CH3. The strong, broad absorbance in the 2500-3600 cm-1 region suggests a hydroxyl
group arising from a carboxylic acid. The strong peak around 1710-1780 cm-1 is consistent with
this since it could arise from the carbonyl group of carboxylic acid.
Molecules can vibrate in a variety of ways. There bonds can vibrate with stretch motion
or bend motion. The movement of each ball toward or aways from the other ball along the line
of the spring represents a stretching vibration. Stretching can either be symmetric or
asymmetric. While a molecule with three or more atoms can experience a bendind vibration.
Conclusion:
In the experiment, FTIR spectroscopy was used to determine the spectrum of acetylsalicylic acid
in KBr. The objective of this experiment was achieved. By comparing to the standard spectrum,
it shows that there is no significant difference.
References:
1. http://www.wcaslab.com/tech/tbftir.htm
2. http://www.chem.ucla.edu/harding/notes/notes_14C_IR.pdf
Experiment 2: Determination of Cr2+ and Cd2+ in plant tissue samples using
Atomic Absorption Spectrometry (AAS)
Objectives:
Introduction:
Apparatus:
Chemicals:
Procedures:
1. Sample
The plant sample was cut into small pieces and about 50 g of the sample put in
oven to dry for 24 hours. Three portions of the samples weigh ranging from 0.5 g
to 1.0 g accurately. 7 ml of concentrated HNO3 added into each vessel. The
samples were heat on a hot plate about 20 minutes. the solution was added with
1 ml of H2O2 drop by drop and the precipitate formed. The solution was filtered
using a filter funnel equipped with filter paper. The solution was diluted into 100
ml of volumetric flask and make up with deionised water.
2. Standard preparation
M1V1 = M2V2
(1000mg/L)(x) = (1mg/L) (0.1L)
X = 0.0001 L
b) 2ppm standard solution
M1V1 = M2V2
(1000mg/L)(x) = (2mg/L) (0.1L)
X = 0.0002 L
M1V1 = M2V2
(1000mg/L)(x) = (3mg/L) (0.1L)
X = 0.0003 L
M1V1 = M2V2
(1000mg/L)(x) = (5mg/L) (0.1L)
X = 0.0005 L
M1V1 = M2V2
(1000mg/mL)(x) = (0.2mg/L) (100mL)
X = 0.02 ml
b) 0.4ppm standard solution
M1V1 = M2V2
(1000mg/mL)(x) = (0.4mg/L) (100L)
X = 0.04 mL
M1V1 = M2V2
(1000mg/L)(x) = (0.6mg/L) (100L)
X = 0.06 mL
M1V1 = M2V2
(1000mgm/L)(x) = (1.0mg/L) (100mL)
X = 0.10 mL
Result and discussion:
Based on the result from the experiment, the absorbance of light increased with
increasing concentration of Cadmium and Chromium. The calibration curve clearly
shows the linear relationship between absorbance and concentration. From this curve
the concentration of Cadmium in plant tissue was determine is 1.261 ppm while for
Chromium was 1.623 ppm.
In this experiment, wet digestion method was used for sample preparation. The
various acid and flux treatment was carried out in high temperature to help to minimize
contamination of sample with substance in the air, environment and vessel wall. The
use of closed system is completely isolated from the surroundings may help to prevent
both contamination and sample loss. The sample was covered with aluminium foil in this
experiment.
In this experiment, spinach was used in determination of Cadmiun and Chromiun in plant
tissue. The objective to determine the Cadmium and Chromiun in plant tissue was achieved.
The concentration of Cadmium in spinach is 261 ppm while for Chromium was 1.623 ppm.
References:
1. http://www.scribd.com/doc/88715301/CHM-580-EXP-AAS
2. http://www.galbraith.com/spectroscopy.htm
UNIVERSITI TEKNOLOGI MARA PERLIS
ARAU CAMPUS
FACULTY OF APPLIED CHEMISTRY
CHM 580
SPECTROCHEMICAL METHODS OF ANALYSIS
EXPERIMENT 1:
Analysis of Aspirin in Commercial APC Tablet FTIR
Spectroscopy
Group: ASB4Bg
CHM 580
SPECTROCHEMICAL METHODS OF ANALYSIS
EXPERIMENT 2:
Determination of Cr2+ and Cd2+ in plant tissue samples
using Atomic Absorption Spectrometry (AAS)
Group: ASB4Bg
CHM 580
SPECTROCHEMICAL METHODS OF ANALYSIS
EXPERIMENT 3:
Determination of Lead in Anchovies by Cold Vapors
Generation Atomic Absorption Spectrometry
Group: ASB4Bg
CHM 580
SPECTROCHEMICAL METHODS OF ANALYSIS
EXPERIMENT 4:
Background and Correction Method for the Determination
of Caffeine in Tea Samples by using Ultraviolet
Spectroscopy
Group: ASB4Bg
CHM 580
SPECTROCHEMICAL METHODS OF ANALYSIS
EXPERIMENT 5:
Determination of Riboflavin (vitamin B2) in Energy Drink
Group: ASB4Bg