Detection limits spectroscopic procedures

Tao et al. [658] have described a procedure in which antimony and arsenic were generated as hydrides and irradiated with ultraviolet light. The broad continuous emission bands were observed in the ranges about 240-750 nm and 220 - 720 nm, and the detection limits were 0.6 ng and 9.0 ng for antimony and arsenic, respectively. Some characteristics of the photoluminescence phenomenon were made clear from spectroscopic observations. The method was successfully applied to the determination of antimony in river water and seawater. The apparatus used in this technique is illustrated in Fig. 5.16. 

Determination of uranium in soil samples can be carried out by nondestructive analysis (NDA) methods that do not require separation of uranium (needed for alpha spectrometry or TIMS) or even digestion of the soil for analysis by ICPMS, ICPAES, or some other spectroscopic methods. These NDA methods can be divided into passive techniques that utilize the natural radioactive mission (gamma and x-ray) of the uranium and progeny radionuclides or active methods where neutrons or electromagnetic radiation are used to excite the uranium and the resultant emissions (gamma, x-rays, or neutrons) are monitored. In many cases, sample preparation is simpler for these nondestructive methods but the requiranent of a neutron source (from a nuclear reactor in many cases) or a radioactive source (x-ray or gamma) and relatively complex calibration and data interpretation procedures make the use of these techniques competitive only in some applications. In addition, the detection limits are usually inferior to the mass spectrometric techniques and the isotopic composition is not readily obtainable. 

An example of direct examination is Ae examination of the polymer film by infrared or ultra-violet spectroscopy or of Aicker sections of polymer by attenuated total reflectance (ATR) infrared spectroscopy. Such techniques have severe limitations in that, because the additive is in effect heavily diluted with polymer, detection limits are usually well above the low concentration of additive present and Ais method is only applicable if the additive has distinct sharp absorption bands in regions where the polymer itself shows little or no absorption. In-situ spectroscopic techniques are not likely to be of value, then, in the analysis of samples of unknown composition. If known amounts of additive can be incorporated into additive-free polymer, however, these techniques are likely to be extremely useful in Ae study of solvent extraction procedures, and the study of additive ageing processes (ie. the effects of heat, light, sterilization, radiation, etc.), since the rate of disappearance of or decay can be measured directly by the decrease in absorbance of Ae sample at a suitable wave-lengA. 

By this procedure, contamination by hydrocarbons and oxidation can be reduced below the limit of spectroscopic detection. 

Like most spectroscopic analytical techniques, LEAF needs a calibration procedure. In common with other modern analytical techniques, determination of limits of detection (LOD) poses a new problem. Commonly, LOD are defined as the concentration (or absolute amount) of analyte that gives an analytical signal three times the standard deviation of the blank. The analyte con-... 

---