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Possible questions for the short test

1. Principle of flame spectrometric methods (emission, absorption, fluorscence).


Atomic Emission
In atomic emission, the processes of excitation and decay shown in Figure 1 are both involved. The sample is subjected to a high-energy thermal environment in order to produce excited-state atoms. This environment can be provided by a flame or, more recently, a plasma. However, since the excited state is unstable, the atoms spontaneously return to the "ground state" and emit light. The emission spectrum of an element consists of a collection of emission wavelengths called emission lines because of the discrete nature of the emitted wavelengths. The intensity at an emission line will increase as the number of excited atoms of the element increases. Using atomic emission, the flame serves a dual purpose: it converts the sample aerosol into an atomic vapor and then thermally elevates the atoms to an excited state. When these atoms return to the ground state, they emit light which is detected by the instrument. The intensity of lig. ht emitted is related to the concentration of the element of interest in solution.

Atomic Absorption
The "ground state" atom absorbs light energy of a specific wavelength as it enters the "excited state." As the number of atoms in the light path increases, the amount of light absorbed also increases. By measuring the amount of light absorbed, a quantitative determination of the amount of analyte can be made. The use of special light sources and careful selection of wavelengths allow the specific determination of individual elements. In atomic absorption, the only function of the flame is to convert the sample aerosol into atomic vapor which can then absorb light from the primary light source (hollow cathode lamp or electrodeless discharge lamp).
Single-Beam

The light source (hollow cathode lamp or electrodeless discharge lamp) emits a spectrum specific to the element of which it is made, which is focused through the sample cell into the monochromator. The light source must be electronically modulated or mechanically chopped to differentiate between the light from the source and the emission from the sample cell. The monochromator disperses the light, and the specific wavelength of light isolated passes to the detector, which is usually a photomultiplier tube. An electrical current is produced depending on the light intensity and processed by the instrument electronics. The electronics will measure the amount of light attenuation in the sample cell and convert those readings to the actual sample concentration. With single-beam systems, a short warmup period is required to allow the source lamp to stabilize.

Double-Beam

The light from the source lamp is divided into a sample beam, which is focused through the sample cell, and a reference beam, which is directed around the sample cell. In a double-beam system, the readout represents the ratio of the sample and reference beams. Therefore, fluctuations in source intensity do not become fluctuations in instrument readout, and stability is enhanced. Generally, analyses can be performed immediately with no lamp warm-up required

2. What kind of processes occur when a metal salt is introduced to flame? What kind of particles are used for flame absorption spectrometry and for flame emission spectrometry? 3. What are the main parts of FES instruments? What is the function of the units? 4. What are the main parts of FAAS instruments? What is the function of the units? 5. Give a general description about the most commonly used flames in flame spectromettry 6. What is the way of sample introduction to the spectrometers? 7. Give the main parts of hollow cathode lamp, the principle of functioning of hollow cathode lamp.

8. What is the way of the resolution of light? How do the light resolving units work? 9. What is the way of the detection of light in spectrometers? 10. Describe the two most commonly used evaluation methods (comprehensive calibration, standard addition calibration) Method
Most convenient when Useful Preparation

comprehensive calibration
a large number of similar samples are to be analyzed. Facilitates calculation of Figures of Merit. 1. Prepare a series of standard solutions (analyte solutions with known concentrations). 2. Plot [analyte] vs. Analytical Signal. 3. Use signal for unknown to find [analyte].

standard addition calibration


a small number of samples are to be analyzed. Useful when the analyte is present in a complicated matrix and no ideal blank is available 1. Add one or more increments of a standard solution to sample aliquots of the same size. Each mixture is then diluted to the same volume. 2. Prepare a plot of Analytical Signal versus: volume of standard solution added, or concentration of analyte added. 3. The x-intercept of the standard addition plot corresponds to the amount of analyte that must have been present in the sample (after accounting for dilution). b) the curve is linear over the concentration range c) the y-intercept of a calibration curve would be

method assumes

a) the curve is linear over the concentration range

0 Equation S = mC + b S = mVs + b