Analysis sample dissolution

In addition to the spark emission methods, quantitative analysis directly on soHds can be accompHshed using x-ray fluorescence, or, after sample dissolution, accurate analyses can be made using plasma emission or atomic absorption spectroscopy (37). 

At present time the use of oxide single erystals sueh as bismuth germanate (Bi Ge O, ) and pai atellurite (TeO,) as deteetors in opto-eleetronies stimulate produetion of high purity Bi, Te, Ge and their oxides Bi O, GeO, TeO,. This requires development of analytieal teehniques for purity eontrol of these materials. For survey traee analysis atomie emission speetrometry (AES) and mass speetrometry (MS) with induetively eoupled plasma (ICP) is widely used. However, the deteetion limits of impurities aehievable by these methods for the analysis of high purity solids are limited by neeessity of sample dissolution in pure aeids and dilution up to 5 10 times for ICP-MS and 50-100 for ICP-AES. One of the most effeetive ways to improve the analytieal performanees of these methods is pre-eoneentration of miero-elements. 

Investigated is the influence of the purity degree and concentration of sulfuric acid used for samples dissolution, on the analysis precision. Chosen are optimum conditions of sample preparation for the analysis excluding loss of Ce(IV) due to its interaction with organic impurities-reducers present in sulfuric acid. The photometric technique for Ce(IV) 0.002 - 0.1 % determination in alkaline and rare-earth borates is worked out. The technique based on o-tolidine oxidation by Ce(IV). The relative standard deviation is 0.02-0.1. 

In trace organic analysis there is usually an extraction or clean-up process, rather than a sample dissolution. Here not only must the matrix effect be considered, but also the recovery yield of the extraction. Frequently an external spike standard is added, but there is often no way of knowing if the recovery of the spike standard matches the analyte in question. There is considerable evidence that the U S E P A method for VOA analysis (Minnich 1993) is subject to such error, as reported by Schumacher and Ward (7997). The analyst must always consider the possibility of such an error, especially when using CRMs to control methods that are applied in routine mode. 

For the analysis of organic additives in polymeric materials, in most cases, prior extraction will be necessary. Depending on the nature of the additive, many different approaches are employed. These include soxhlet extraction with organic solvent or aqueous media, total sample dissolution followed by selective precipitation of the polymer leaving the additive in solution, assisted extraction using pressurised systems, ultrasonic agitation and the use of supercritical fluids. In trace analysis, solid phase extraction (SPME) from solution or solvent partition may be required to increase the analyte concentration. 

The earliest applications for quantitative analysis of liquid samples and solid preparations entailed sample dissolution in an appropriate solvent. A number of moisture determinations in APIs and pharmaceutical preparations based on both reflectance and transmission measurements have been reported. Their results are comparable to those of the KF method. The high sensitivity provided by the NIR technique has fostered its use in the determination of moisture in freeze-dried pharmaceuticals. ° The noninvasive nature of NIR has been exploited in determination of moisture in sealed glass vials. " " ... 

Sample Dissolution — Sample introduction into most ICP systems, is by liquid nebuli-zation. This constraint partially limits the quality of the emission analysis to be dependent on the digestion, in the case of solid samples. The fact that several elements are easily monitored simultaneously places a greater demand on the care and choice of sample preparation. Also there are both advantages and disadvantages to the use of dissolved samples in analysis. Some disadvantages are ... 

Dissolution testing involves a two-step process sample preparation and sample analysis. In this chapter sample preparation denotes the actual sample dissolution procedure, including sample collection. The samples collected from the dissolution apparatus may be analyzed directly or may be subject to further manipulation (e.g., dilution) to give the final sample solutions. 

The validation requirements are discussed as they apply to both the sample preparation and sample analysis aspects of a dissolution method. The focus of the discussion in this chapter is on the validation considerations that are unique to a dissolution method. Validation is the assessment of the performance of a defined test method. The result of any successful validation exercise is a comprehensive set of data that will support the suitability of the test method for its intended use. To this end, execution of a validation exercise without a clearly defined plan can lead to many difficulties, including an incomplete or flawed set of validation data. Planning for the validation exercise must include the following determination of what performance characteristics to assess (i.e., strategy), how to assess each characteristic (i.e., experimental), and what minimum standard of performance is expected (i.e., criteria). The preparation of a validation protocol is highly recommended to clearly define the experiments and associated criteria. Validation of a test method must include experiments to assess both the sample preparation (i.e., sample dissolution) and the sample analysis. ICH Q2A [1] provides guidance for the validation characteristics of the dissolution test and is summarized in Table 4.1. 

The earliest applications for quantitative analysis of liquid samples109 and solid preparations107 entailed sample dissolution in an appropriate solvent and using an MLR calibration. MLR calibration models can also be applied in methods based on reflectance measurement of spectra. 

The use of ICP-MS for trace analysis in sediments has recently been reviewed [326]. The advantages and disadvantages of acid digestion versus fusion-based sample dissolution were discussed. The problems involved in ICP-MS analysis of... 

One of the most challenging aspects of atomic spectrometry is the incredibly wide variety of sample types that require elemental analysis. Samples cover the gamut of solids, liquids, and gases. By the nature of most modem spectrochemical methods, the latter two states are much more readily presented to sources that operate at atmospheric pressure. The most widely used of these techniques are flame and graphite furnace atomic absorption spectrophotometry (FAAS and GF-AAS) [1,2] and inductively coupled plasma atomic emission and mass spectrometries (ICP-AES and MS) [3-5]. As described in other chapters of this volume, ICP-MS is the workhorse technique for the trace element analysis of samples in the solution phase—either those that are native liquids or solids that are subjected to some sort of dissolution procedure. 

The vast majority of environmental analyses completed by flame spectrometry either involve direct analysis of aqueous samples or analysis of solid samples after sample dissolution. It is appropriate at this point, therefore, to consider briefly the implications which the requirement to have the sample in solution form has in flame spectroscopic analysis, and that is the prime purpose of this chapter. However, it is also important never to lose sight of the fact that appropriate sampling and sub-sampling techniques are a crucial prerequisite to the generation of meaningful environmental data. The analytical process often starts in the field, and that is the stage at which we should begin to look at sample preparation.1... 

Because of the difficulty and inconvenience of sample dissolution for soil and geological samples prior to analysis by atomic spectrometry, a number of authors have investigated the possibility of direct nebulization of slurry samples into flames or plasmas.20,21 However Ebdon et al.22 reported problems... 

Solid foods in powder form can be analyzed directly by means of LA- or ETV-ICP-MS to eliminate time-consuming sample dissolution procedures (see Table 8.2). However, this requires the preparation of homogeneous powdered samples and the subsequent analytical determination is not as straightforward as the one based on liquid sample introduction. Another way to perform direct analysis of solid foods is to grind and suspend them into slurries. The viability of slurry nebulization relies on the ability to prepare samples of fine particle size in a reproducible manner and on the adoption of suitable (e.g., high-solids) nebulizers. Otherwise, slurries can be analyzed by ETV-ICP-MS resorting to the ultrasonic slurry sampling technique [72-74]. 

Several methods are in general use for introduction of a material into the flame. These include solution aspiration, gas (hydride) evolution and entrainment into the flame, and direct introduction of solid substrates. All three have been used for flame-AAS analysis of trace elements from air sampling however, most work is carried out by use of the first two methods. In each case a suitable solution is first obtained by the dissolution of the elements of interest from the sample. Sample dissolution will be discussed in greater detail in a following section. 

The book begins with a discussion of the basic physico-chemical aspects of reactions utilised in qualitative inorganic analysis. A description of laboratory equipment follows, and operations which include semimicro and micro techniques, and simple electrochemical, spectroscopic and chromatographic methods. The reactions of the most important cations and anions are described, followed by a treatment of systematic qualitative analysis. Sample preparation, dissolution and fusion of insoluble materials are treated in detail. A separate chapter deals with the reactions of less common ions, with guidelines to their separation and identification in the course of systematic analysis. Finally, a simplified course of qualitative analysis is given this chapter will be particularly useful where the time allocated to qualitative analysis is limited. 

Barbiturates can be prepared for HPLC analysis by dissolution of the drug sample in methanol at a chosen concentration, followed by removal of any sofid particulate material by filtration, etc. A typical set of HPLC operating conditions used for the analysis of barbiturates is shown in Table 9.4. 

Matusiewicz, H., Sturgeon, R.E. Present status of microwave sample dissolution an decomposition for elemental analysis. Prog. Analyt. Spectrosc. 12, 21-39 (1989)... 

Burguera, J.L., Burguera, M. Flow injection systems for on-line sample dissolution/decom-position. In Sanz-Medel, A. (ed.) Flow Analysis with Atomic Spectrometric Detectors, pp. 135-149. Elsevier, Amsterdam (1999)... 

Developing an HPLC method requires a clear specification of the goals of the separation. The primary objective could be (1) resolution, detection and characterisation or quantitation of one or a few substances in a product, so that it is important to separate only a few sample components and complete separation of the sample is not necessary (2) complete resolution, characterisation and quantitation of all sample components (3) isolation of purified sample components for spectral identification or for other assays. Further points that should be considered include the required sensitivity (especially for trace analysis), accuracy, precision, character of sample matrices (which determines sample dissolution, extraction or pretreatment necessary for possible concentration of sample analytes or for removing interference), expected frequency of analyses and the HPLC equipment available. 

The simplest methods of HTSC analysis are based on the determination of the products of sample dissolution in acidic media. Potentiometric, amperometric, or coulometric titrations are frequently used (mainly for YBCO ceramics [525-527] and their analogs with other rare-earth elements [528, 529], and also for BSCCO [530]). We note particularly the method of potentiostatic coulometric analysis [531], which allows one to analyze thallium cuprate samples over a wide range of the Tl/Cu ratio, and also the method of flow-through coulometry for determining the effective valence of copper [532]. The polarographic determination of Cu content in the samples obtained by dissolving HTSCs in concentrated alkaline solutions with special... 

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