Determination of heavy metals in soil byatomic absorption spectrometry(AAS)
Name: XuFei Group: The 3rd group
Date: Sep. 20th 20xx
Part 1 The introduction
1.1The purposes
(1)Learn how to operate the atomic absorption spectrometry;
(2)Learn how to do the pretreatment of soil samples;
(3)Get familiar with the application of atomic absorption spectrometry.
1.2The principles
Atomic Absorption Spectrometry (AAS) is a technique for measuring quantities of chemical elements present in environmental samples by measuring the absorbed radiation by the chemical element of interest. This is done by reading the spectra produced when thesample is excited by radiation. The atoms absorb ultraviolet or visible light and make transitions to higher energy levels .
Atomic absorption methods measure the amount of energy in the form of photons of light that are absorbed by the sample. A detector measures the wavelengths of light transmitted by the sample, and compares them to the wavelengths which originally passed through the sample. A signal processor then integrates the changes in wavelength absorbed, which appear in the readout as peaks of energy absorption at discrete wavelengths. The energy required for an electron to leave an atom is known as ionization energy and is specific to each chemical element. When an electron moves from one energy level to another within the atom, a photon is emitted with energy E. Atoms of an element emit a characteristic spectral line. Every atom has its own distinct pattern of wavelengths at which it will absorb energy, due to the unique configuration of electrons in its outer shell. This enables the qualitative analysis of a sample.
The concentration is calculated based on the Beer-Lambert law. Absorbance is directly proportional to the concentration of the analyte absorbed for the existing set of conditions. The concentration is usually determined from a calibration curve, obtained using standards of known concentration. Calibration Curve Method: Prepare standard solutions of at least three different concentrations, measure the absorbance of these standard solutions, and prepare a calibration curve from the values obtained. Then measure the absorbance of the test solution adjusted in concentration to a measurable range, and determine the concentration of the element from the calibration curve.
Part 2 The materials and apparatus
Atomic absorption spectrometry; Cu hollow cathode lamp; AC voltage stabilizer; oil-free gas compressor; acetylene cylinder; oscillator; sample boat; Erlenmeyer flask with stopper (100 ml); beaker; graduate cylinder; pipette.
Part 3 The procedure
3.1 operating procedure for AAS
(1) inspect major components to ensure operating normal.
(2) Install required hollow cathode lamp. Select “T” before turning to the power and hollow cathode lamp. Then select appropriate la mp current and preheat for 30min.
(3) Make sure electrical meter to point to zero and then turn on high-voltage power.
(4) Select appropriate slit width.
(5) Rotate monochromator and select required wavelength. If the power meter is too high or low, adjust negative high voltage until the meter reads full scale.
(6) Adjust light point and wavelength so that the meter represents the maximum value.
(7) Turn on air compressor and acetylene gas and ignite flame. Adjust the flame appropriately and preheat the burner.
(8) Inject distilled water into the flame and continue to preheat the burner. Inject distilled water into the flame after each sample.
(9) Select “E”, inject blank solution into the flame and adjust the meter to zero.
(10) Optimize analysis conditions and measure standard solution and samples.
(11) After completion of measurement, turn off acetylene gas valve and then air compressor, cut off gas supply a moment later.
(12) Select “T” before turning off high voltage power, decrease lamp current and then turn off the lamp. At the same time, all buttons should be on original positions.
(13) Check the equipment before leaving the laboratory.
3.2 Determination of soil samples
(1) Preparation of extracting solution (0.05 mol/l EDTA solution)
18.6 g of EDTA is dissolved with water in a beaker (500 ml). The PH is adjusted to 7.0 using dilute ammonia. The mixture is transferred into a volumetric flask (1000ml), dilute to the mark and mixed well.
(2) Treatment of soil samples
2.50 g of air-dried soil (60- 100 mesh) is put into an Erlenmeyer flask with stopper (100 ml). 12.5 ml of EDTA solution is added. The mixture is shaken for 1h and then filtered. The filtrate is preserved for analysis.
(3) Preparation of Cu standard stock solution
0.10 g of Cu is dissolved in 15 ml of (1:1) nitric acid solution. The mixture is transferred into a volumetric flask (1000 ml) and diluted to the mark with re-distilled water. The concentration of the stock standard solution is 100g/ml. (The concentration should be calculated according to the mass of Cu).The working Cu standard solution (10μg/ml) is obtained by diluting 10 ml of Cu standard stock solution to 100 ml with
re-distilled water.
(4) Plotting of the standard curve
0 ml, 1 ml, 2 ml, 3 ml, 4 ml and 5 ml of Cu standard solution (10μg/ml) are added respectively to 6 volumetric flask (10 ml) with 1 ml of 5 mol/l hydrochloric acid. The mixture is diluted with re-distilled water and mixed well to give 0μg/ml, 1.00μg/ml,2.00μg/ml, 3.00μg/ml, 4.00μg/ml, 5.00μg/ml of Cu, respectively. The absorbance is measured at wavelengths of 3247 ?. The standard curve is constructed by plotting absorbance vs. concentration.
(5) Determination of samples
The sample solution is analyzed using the same procedure and conditions as for the standard curve. The concentration of Cu is obtained from the standard curve based on the absorbance.
Part 4 The results
4.1 The raw data
4.2 AAS standard curve
4.3 Calculation
The absorbance of sample is 0.0511.
According to the formula above :y=0.0446x+0.0024,R2=0.9997
The concentration of Cu in the sample is:1.091mg/L.
Part 5 Discussion
In this experiment, we use the AAS to determine Cu in soil. I learn how to operate the AAS and the limitation. In the experimental process, standard solution was prepared in strict accordance with the experimental requirements and I learn how to deal with the data. Finally we get the standard curve, then, the sample concentration is calculated according to the absorbance of the sample.
In the experiment we have nine members in our group, so we can do our best in every work we need to do. For my work, I am responsible for the preparation of solution and titration. What’s more, I learn how to use and operate the AAS on the computer later.
Ultimately, we get the linear formula is y = 0.0446x + 0.0024 and R2=0.9997. From According to the formula and the absorbance of Cu in the sample is 0.0511, we draw the concentration of Cu in the sample is 1.091μg/ml. We have known that the concentration of test sample measured by instrument is 1.091mg/L.
We can say our result of experiment is so very accurate from the standard curve of Cu and the value of R(R2=0.09997). The accurate data is due to the efforts of we everyone. Thanks for every members of our group.
I have some suggestions for our experiments. Firstly when we’ll do an experiment, we must prepare our pre-lab by ourselves and translate it into Chinese .Only do like this, we can understand the experiment well. Secondly we should prefer to solute the problems in the experiment rather than ask for TA. Finally, everyone should understand his own task in the experiment.