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AAS Manual

This document describes an experiment to determine the concentration of iron and cadmium in a vegetable sample using flame atomic absorption spectroscopy (FAAS). The procedure involves digesting the dried and milled vegetable sample, preparing standard solutions of iron and cadmium, measuring absorbances of the sample with and without standard additions to generate calibration curves, and calculating the concentrations of iron and cadmium in the sample based on the curves. The goals are to identify and quantify the levels of these heavy metals in the plant tissue if present and compare the results to reported literature values.

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126 views

AAS Manual

This document describes an experiment to determine the concentration of iron and cadmium in a vegetable sample using flame atomic absorption spectroscopy (FAAS). The procedure involves digesting the dried and milled vegetable sample, preparing standard solutions of iron and cadmium, measuring absorbances of the sample with and without standard additions to generate calibration curves, and calculating the concentrations of iron and cadmium in the sample based on the curves. The goals are to identify and quantify the levels of these heavy metals in the plant tissue if present and compare the results to reported literature values.

Uploaded by

fatihah mujahid
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as DOC, PDF, TXT or read online on Scribd
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CHM580 SPECTROSCOPIC METHODS OF ANALYSIS

EXPERIMENT 1: DETERMINATION OF THE AMOUNT OF IRON AND CADMIUM


IN VEGETABLE USING FLAME ATOMIC ABSORPTION SPECTROSCOPY (FAAS)

LABORATORY OUTCOMES
On successful completion of this experiment the student will be able to:
1. Explain the principle of atomic absorption (AA) spectrophotometry and its application.
2. Explain the operation of AA spectrophotometry and function of each main components in
AA spectrometer.
3. Know what kind of data produced from AAS instrument.
4. Analyze the AA data
5. Identify what kinds of samples are appropriate for AAS analysis.
6. Draft the procedure for analysis of solid samples using AA spectrometer.

INTRODUCTION

Pollution is correlated with the degree of industrialization and the intensity of chemical usage.
Past and present industrial activities have often resulted in the pollution of underlying soils
where these activities take place, either by leaching of water from landfills or direct discharge of
industrial waste water into soils. The most common toxic soil pollutants include heavy metals
and their compounds, organic chemicals, oils, tars and pesticides. Soil pollution by heavy metals
such as mercury, cadmium, chromium and lead are of great concern to public health. The source
of heavy metal in plant is the environment in which they grow and their growth medium (soil)
from which heavy metals are then taken up by roots or foliage of plants. Plant growing in
polluted environment can accumulate heavy metals at high concentration causing serious risk to
human health when consumed. Moreover, heavy metals are dangerous because they tend to
accumulate in plants and animals thereby causing deleterious effects and bioaccumulation in the
food chain.

Ingesting large amount of heavy metals like chromium, cadmium and lead can cause reduce litter
size and weight, liver, and kidney damage. Cadmium can also accumulate in kidney where it
damages filtering and causes excretion of essential proteins and sugar from the body. In
herbaceous plants, roots and leaves retain higher metal concentration of heavy metal than stem
and fruits.

Iron is an essential part of the proteins that transport oxygen in the body. Iron deficiency limits oxygen
delivery to the cells leading to fatigue, poor work performance and decreased immunity.
However, the body cannot easily get rid of excess of iron in the system. Excess iron gets deposited in
the liver, heart and pancreas, where it can cause cirrhosis, liver cancer, cardiac arrhythmias and diabetes.
Therefore, there is a need to know the concentration of heavy metals in crops particularly leafy
vegetables which are consumed by human.

TASK: You will be given a sample of one type of vegetable (i.e Cantella Asiatica). Your task is
to carry out an experiment to identify the presence of cadmium and iron in the plant tissue
sample. If presence, you are also required to determine the concentration of cadmium and iron in
the provided sample.
CHM 580 SPECTROSCOPIC METHODS OF ANALYSIS

PROCEDURE

A. Preparation of sample (Wet digestion method)

1. Dry the sample in the oven at 60 – 70 C overnight.


2. Mill the sample and weigh accurately 2-3 g of the milled plant sample. (#the sample
weight = 2.5246 g)
3. Transfer the sample into a 250 mL conical flask.
4. Add in 20 - 30 mL HNO3.
5. Place the conical flask in the fumehood and allow the sample to digest overnight.
6. Using a hot plate, heat the digested sample until the red fumes evolving from the conical
flask turn to brown.
7. Cool down the digestion flask to room temperature.
8. Add 2 – 3 mL H2O2 and heat again until the volume of the solution is reduced and a
clear solution is obtained.
9. Proceed with filtration process through a Whatman’s filter paper, leaving a whitish
residue into a 250 mL volumetric flask, dilute the volume with deionized water and
keep it for further analysis.

B. Preparation of 10 ppm standard solution


You will be provided with 100 ppm of stock solution of cadmium and iron.

1. Using 100 ppm of stock solution of cadmium and iron, prepare 10 ppm standard
solution of each of the target analyte in a 50 mL volumetric flask.

C. Preparation of standard solutions of iron for determination of iron contents using


standard addition method
1. Calculate the volume of 10 ppm standard solutions of iron that is needed to prepare 1.0,
1.5, 2.0, 2.5 and 3.0 ppm standard solutions of iron in 50 mL volumetric flasks.
2. Transfer the calculated volume into five separate 50 mL volumetric flasks.
3. Add 10 mL of the prepared sample solutions into each flask and dilute to the mark with
distilled water.

D. Preparation of standard solutions of cadmium for determination of cadmium contents


using standard addition method
1. Calculate the volume of 10 ppm of standard solution of cadmium needed to prepare 0.2,
0.4, 0.6, 0.8 and 1.0 ppm standard solution of cadmium in 50 mL volumetric flasks.
2. Transfer the calculated volume into five separate 50 mL volumetric flasks.
3. Add 10 mL of the prepared sample solutions into each flask before diluting to the mark
with distilled water.

NOTE: Please refer to the section on standard addition method for the procedure and
calculations.

E. Preparation of sample without addition of standard solutions used in C and D

2
CHM 580 SPECTROSCOPIC METHODS OF ANALYSIS

1. Add 10 ml of the prepared sample into a 50 ml volumetric flask and mark up the solution
with deionized water only.

F. Measurements for all solutions required to construct standard addition calibration


curve.
1. Measure absorbance of sample without addition of standard solutions for three times.
2. Measure absorbance of a series standard additions prepared by measuring from the lowest
to the highest concentration.

Include in the report

a. Procedures for analysis of the analyte in the sample using flame-AAS.


b. Calculations for the preparation of the standard solution of chromium and cadmium.
c. Standard addition curve with the linear equation and R2 value.
d. Calculate the analyte concentration (in mg/L unit) and expressed their content in weight
percent.
e. Compare and comment on the concentration obtained with the ones reported in journal
articles.

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