Sample digestion techniques

In his reviews, Olson (1973 and 1976) covers most of the earlier, commonly used sample preparation procedures. More recently, Raptls et al. (1983) and Ihnat (1992) have discussed most sample digestion techniques, together with a comprehensive list of references. Reamer and Veillon (1981a) and Robberecht et al. (1981) reviewed the losses... 

As can be seen, the temperature rose to 115 "C after the first 15 minutes and to 152 "C at 0.3 MPa after the final 15 minutes of heating. With both reagent systems, element recoveries are in good agreement with the values obtained using a hot plate total sample digestion technique, which typically requires 4-6 hours. 

Nagoumey and Madan [20] have considered both AAS and ICP-AES as reliable measurement techniques for the determination of metal components in mixed-metal/phosphite stabiliser systems in PVC. For reasons given elsewhere (Section 8.3.2.4), in this case ICP-AES was considered the technique of choice for most metal stabiliser determinations, while AAS remains a useful method to corroborate the ICP-AES results. For the determination of tin in rigid PVC by means of HG-AAS, the main effort has been to develop a sample digestion procedure [118]. Tin and Ti from a PVC potable... 

A 68 element ICP-MS scan was performed on one dried white-colored paint sample. The chemical elements scanned for during the ICP analysis and the detection limits are provided in Table 5. Approximately 0.5 g of each sample was prepared by an acid digestion technique prior to conducting the ICP-MS analysis. Shown in Table 6 are the quantified ICP-MS results for the sample. Elements scanned for but not detected are either not present in the sample or may be present below the detection limit. 

Thallium has been determined in 10 ml of ashed serum or in urine by extracting with sodium diethyldithiocarbamate into MIBK n°). More recently, Savory and co-workers 1131 described a wet digestion procedure for 50 ml of urine or 5 ml of serum in which the thallium is separated by extracting the bromide into ether, evaporating the ether and then taking up in dilute acid for aspiration. As little as 0.1 ppm is determined in urine. Curry et al.114) determined less than 1 ng of thallium in 200 /d of urine by using the tantalum sample boat technique. The sample in the boat is dried by holding the boat 1 cm from the flame and then it is inserted into the flame where it is vaporized. A similar procedure is used for >3 ng of thallium in 50-100/al of blood, except that the blood is preashed with 3 drops of nitric acid. Since the tantalum boat method is susceptible to interelement interferences, the method of standard additions is used for calibration. 

A chloric acid digestion was used by Backer 2 391 for the preparation of tissue samples. The digest is simply diluted to determine iron, zinc, and copper. The tantalum sampling boat technique was used by Emmermann and Luecke 2531 to measure lead, zinc, and silver in prepared soil solutions. White 1S81 treated ashed plants with hydroxylamine in IN hydrochloric acid to reduce and dissolve oxides of manganese, prior to its determination by atomic absorption spectroscopy. 

The micropipette tip containing solid phases is a relatively new sample preparation technique that permits handling of microliter to submicroliter amounts of liquid samples, using the techniques of SPE, dialysis, and enzyme digestion. Various phases (reversed-phase, affinity, size-exclusion, etc.) are packed, embedded, or coated on the walls of pipette, permitting liquid samples to be transferred without undue pressure drop or plugging (Fig. 2.5). 

Pressure dissolution and digestion bombs have been used to dissolve samples for which wet digestion is unsuitable. In this technique the sample is placed in a pressure dissolution vessel with a suitable mixture of acids and the combination of temperature and pressure effects dissolution of the sample. This technique is particularly useful for the analysis of volatile elements which may be lost in an open digestion [24]. 

The advantages of this digestion technique are the large number of samples that can be processed at one time, the simple and cheap glassware involved, and the fact that the digest may be used for the subsequent determination of not only nitrogen, but calcium, magnesium, potassium, sodium, phosphorus and iron. 

Analysis of major elements (except Si) and total phosphorus on bomb-digested samples was accomplished by inductively coupled plasma emission spectrometry (ICP, ARL model 34,000). Silicon was analyzed colorimetrically (14). Phosphorus in total digests was also determined colorimetrically by the method of Murphy and Riley (15), as modified by Erickson (16). To avoid interference from fluoride ion used in the digestion technique, sample volumes were restricted to <1.5 mL in the standard P analytical protocol. 

Digestion Techniques For nonvascularized or low-water-content tissues such as bone, cartilage, or hair, a mechanical technique may do little to disrupt cellular structure and extract analytes. Extreme measures such as digestion with strong acid (i.e., 12 N HC1) are routinely used for DNA or nucleic acids, which can tolerate the harsh conditions. Alternatively, certain enzymes can be used to digest tissue samples. Commercial devices are available which contain digestion bombs fabricated from material resistant to corrosive media. 

An alternative to MSA in ICP-MS analysis is the internal standard technique. One or more elements not present in the samples and verified not to cause an interelement spectral interference are added to the digested samples, standards, and blanks. Yttrium, scandium, and other rarely occurring elements or isotopes are used for this purpose. Their response serves as an internal standard for correcting the target analyte response in the calibration standards and for target analyte quantitation in the samples. This technique is very useful in overcoming matrix interferences, especially in high solids matrices. 

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