Absorption spectrometer

While a laser beam can be used for traditional absorption spectroscopy by measuring / and 7q, the strength of laser spectroscopy lies in more specialized experiments which often do not lend themselves to such measurements. Other techniques are connnonly used to detect the absorption of light from the laser beam. A coimnon one is to observe fluorescence excited by the laser. The total fluorescence produced is nonnally proportional to the amount of light absorbed. It can be used as a measurement of concentration to detect species present in extremely small amounts. Or a measurement of the fluorescence intensity as the laser frequency is scaimed can give an absorption spectrum. This may allow much higher resolution than is easily obtained with a traditional absorption spectrometer. In other experiments the fluorescence may be dispersed and its spectrum detennined with a traditional spectrometer. In suitable cases this could be the emission from a single electronic-vibrational-rotational level of a molecule and the experimenter can study how the spectrum varies with level. 

The use of more complex or more costly articles of equipment, such as catalytic hydrogenation apparatus, autoclaves, polari-meters, ultraviolet absorption spectrometers, etc., has not been described, because the type of such apparatus employed indifferent laboratories varies considerably, and students must be taught the use of their own laboratory equipment. 

Atomic Absorption Spectroscopy. Mercury, separated from a measured sample, may be passed as vapor iato a closed system between an ultraviolet lamp and a photocell detector or iato the light path of an atomic absorption spectrometer. Ground-state atoms ia the vapor attenuate the light decreasiag the current output of the photocell ia an amount proportional to the concentration of the mercury. The light absorption can be measured at 253.7 nm and compared to estabUshed caUbrated standards (21). A mercury concentration of 0.1 ppb can be measured by atomic absorption. 

In this work, atmospheric particles (PM 10 and PM 2.5) were collected by a dichotomos air sampler. Several leaching procedures were investigated for decomposition of heavy metals. The digests were pre-concentrated with sodium diethyldithiocarbamate. The determinations were canted out on a Vartan Model AA-220 atomic absorption spectrometer. The instrarment was equipped with a GTA-110 graphite furnace system. Table 1 shows the concentrations of heavy metals associated with PM 10 and PM 2.5 particles. Table 1. Concentrations of heavy metals in PM 10 and PM 2.5 atmospheric particles (ng/m )... 

I3.5.4.S Optica) Muttigas Analysis Techniques Differential Opticoi Absorption Spectrometer... 

The differential optica) absorption spectrometer (DOAS) is based on the differential absorption of gaseous atoms or molecules.The Lamherr-Beer law gives the concentration... 

Applications The differential optical absorption spectrometer has been used to monitor concentrations of gases or intermediate compounds such as SO, NO, O5, HCHO, HNO, CS, NO, and OH in the atmosphere.In atmospheric measurements with open paths of 100 to 1000 m, a detection limit of about 1 ppb can be achieved. In the emission measurements, the path length across the duct or the plume can range in meters. 

Magnesium may conveniently be determined by atomic absorption spectroscopy (Section 21.21) if a smaller amount (ca 4 mg) is used for the separation. Collect the magnesium effluent in a 1 L graduated flask, dilute to the mark with de-ionised water and aspirate the solution into the flame of an atomic absorption spectrometer. Calibrate the instrument using standard magnesium solutions covering the range 2 to 8 ppm. 

At present, however, the usual flame emission method is obtained by simply operating a flame atomic absorption spectrometer in the emission mode (see Fig. 21.3). 

Although flame emission measurements can be made by using an atomic absorption spectrometer in the emission mode, the following account refers to the use of a simple flame photometer (the Coming Model 410 flame photometer). Before attempting to use the instrument read the instruction manual supplied by the manufacturers. 

Fig. 5—6. Geiger-counter output currents recorded by Dow automatic x-ray absorption spectrometer. Superposed records on left are x-ray absorptiometric curves for iso-octane and a solution containing ethylene dibromide, whereas traces at right illustrate recording of transmitted intensities at fixed wavelengths. Apparent change in x-ray absorption of solvent in going through bromine absorption edge is result of marked slope of white radiation distribution curve at 0.9 A. 16 (Liebhafsky, Anal. Chem., 21, 17. Courtesy of Dow Chemical Company.)...

Visible and ultraviolet absorption spectra are measured in an absorption spectrometer. The source gives out intense visible light or ultraviolet radiation. The wavelengths can be selected with a glass prism for visible light and with a quartz prism or a diffraction grating for ultraviolet radiation (which is absorbed by glass). A typical absorption spectrum, that of... 

Atomic absorption spectrometers with dual monochromators are commercially available from Jarrell-Ash Division of Fisher Scientific Co.9 and from Instrumentation Laboratories Inc. 

Dabeka, R. W. and McKenzie, A. D. (1991). Graphite furnace atomic absorption spectromet-ric determination of selenium in foods after sequential wet digestion with nitric acid, dry ashing and coprecipitation with palladium. Can. J. Appl. Spectrosc. 36,123-126. 

In the stripping voltammetry, in general it is anodic SV which, owing to its extreme sensitivity and selectivity together with its cheapness, has gained so much analytical importance that for instance the Kemforschungsanlage Jiilich (F.R.G.) recently (1983) replaced their atomic absorption spectrometer with an SV system for the simultaneous determination of Cu, Cd, Pb, etc. 

Silver acetylide is a more powerful detonator than the copper derivative, but both will initiate explosive acetylene-containing gas mixtures [1]. It decomposes violently when heated to 120-140°C [2], Formation of a deposit of this explosive material was observed when silver-containing solutions were aspirated into an acetylene-fuelled atomic absorption spectrometer. Precautions to prevent formation are discussed [3], The effect of ageing for 16 months on the explosive properties of silver and copper acetylides has been studied. Both retain their hazardous properties for many months, and the former is the more effective in initiating acetylene explosions [4],... 

XRD analyses were performed on oriented samples prepared by spreading of the sample suspension on a glass slide, followed by drying at room temperature. The XRD patterns were obtained with a PW 1130/00/60 Philips diffractometer using CuKa radiation (/, = 1,5405 A). Chemical analysis was carried out on a Perkin Elmer 3100 atomic absorption spectrometer after dissolution of the sample with several acids (HF, HCIO4, HC1) for 24h, and HN03 in a second time. 

Gill and Fitzgerald [481] determined picomolar quantities of mercury in seawater using stannous chloride reduction and two-stage amalgamation with gas-phase detection. The gas flow system used two gold-coated bead columns (the collection and the analytical columns) to transfer mercury into the gas cell of an atomic absorption spectrometer. By careful control and estimation of the blank, a detection limit of 0.21 pM was achieved using 21 of seawater. The accuracy and precision of this method were checked by comparison with aqueous laboratory and National Bureau of Standards (NBS) reference materials spiked into acidified natural water samples at picomolar levels. Further studies showed that at least 88% of mercury in open ocean and coastal seawater consisted of labile species which could be reduced by stannous chloride under acidic conditions. 

The sensitivity achieved should enable seawater samples to be analysed for molybdenum, because the concentration of molybdenum in seawater is usually 2.1 -18.8 pg/1. The selected temperature of 1700-1850 °C during the charring stage permits separation of the seawater matrix from the analyte prior to atomisation with the Perkin-Elmer Model 603 atomic absorption spectrometer equipped with a heated graphite atomiser (HGA-2100). 

Andreae [564] coprecipitated tellurium (V) and tellurium (VI) from seawater and other natural waters with magnesium hydroxide. After dissolution of the precipitate with hydrochloric acid, the tellurium (IV) was reduced to tellurium hydride in 3 M hydrochloric acid. The hydride was trapped inside the graphite tube of a graphite furnace atomic absorption spectrometer, heated to 300 °C, and tellurium (IV) determined. Tellurium (VI) was reduced to tellurium (IV) by boiling with hydrochloric acid and total tellurium determined. Tellurium (VI) was then calculated. The limit of detection was 0.5 pmol per litre and precision 10-20%. 

Huang and Shih [616] used a graphite furnace atomic absorption spectrometer with a stabilised platform furnace involving atomisation from a graphite surface pretreated with vanadium to determine down to 24 ppt of zinc in seawater. 

Figure 5.17. Dual-column ion exchange preconcentration valve. Sa, Sb samples A and B Ca, Cb ion exchange columns A and B Ea, Eb eluant (2 M nitric acid) for columns A and B Wa, Wb waste lines for samples and eluants A and B W waste lines AAS atomic absorption spectrometer. The dimensions of the base plate of the valve are 70 x 45 x 10 mm. See text for details of operation. Source [661]...

The primary requirement for all equipment (whether it be a volumetric flask, an oven used for drying samples or an atomic absorption spectrometer used for determining trace metal concentrations) is that it must be fit for its intended... 

The heart of a traditional atomic absorption spectrometer is the burner, of which the most usual type is called a laminar flow burner. The stability of the flame is the most important factor in AAS. Typical working temperatures are 2200 2400°C for an air-acetylene flame, up to 2600-2800°C for acetylene-nitrous oxide. The fraction of species of a particular element that exist in the excited state can be calculated at these temperatures using the Boltzmann equation ... 

The design of a conventional atomic absorption spectrometer is relatively simple (Fig. 3.1), consisting of a lamp, a beam chopper, a burner, a grating monochromator, and a photomultiplier detector. The design of each of these is briefly considered. The figure shows both single and double beam operation, as explained below. 

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