UV analysis

The development of rehable uv analysis permitted the dependable detection and assay of the provitamins and vitamins. Prior to this, the Lieberman-Bouchard chemical test was used, but the color reaction gave many false positives and was relatively inaccurate. 

The first bioanalytical application of LC-GC was presented by Grob et al. (119). These authors proposed this coupled system for the determination of diethylstilbe-strol in urine as a replacement for GC-MS. After hydrolysis, clean-up by solid-phase extraction and derivatization by pentafluorobenzyl bromide, the extract was separated with normal-phase LC by using cyclohexane/1 % tetrahydrofuran (THE) at a flow-rate of 260 p.l/min as the mobile phase. The result of LC-UV analysis of a urine sample and GC with electron-capture detection (ECD) of the LC fraction are shown in Ligures 11.8(a) and (b), respectively. The practical detection limits varied between about 0.1 and 0.3 ppb, depending on the urine being analysed. By use of... 

This aminium radical salt in aqueous solution in the form of solvated radical salt is very stable and will not polymerize acrylonitrile even with CeHsCOONa to form the corresponding benzoate. Therefore, we believe that in the nucleophilic displacement, there must be some intermediate step, such as intimate ion pair and cyclic transition state, which will then proceed the deprotonation to form the active aminium radical ion [14], as shown in Scheme 1. The presence of the above aminomethyl radical has also been verified [15] through ultraviolet (UV) analysis of this polymer formed such as PAN or PMMA with the characteristic band as the end group. 

Formation of an intimate ion pair of OH " and aminium radical cation was also proposed for the intermediate step before deprotonation. The presence of the above radical was verified through UV analysis of the polymer formed with the characteristic band on the end group. Through chromatographic analysis of the TBH-DMT reaction products, H2O was detected as the above mechanism proposes after deprotonation. 

Besides on-line UV analysis, off-line HPLC analysis was performed after about 48 h dark reaction [72, 74]. In this period, the photoinduced reaction proceeds by radical paths in the dark. 

With the development of more and more additives with closely similar absorbance bands UV analysis has lost its original role as a premier additive analysis technique. However, UV analysis can still be a very useful technique if one knows the exact additive package in a sample and there are no unknowns. Then the concentrations of the additives can be determined from the absorbance using Beer s law. 

On-line SFE-pSFC-FTD, using formic or acetic acid modified CO2 as an extraction solvent, was used to analyse a dialkyltin mercaptide stabiliser in rigid PVC (Geon 87444) [114]. Hunt et al. [115] reported off-line SFE-pSFC-UV analysis of PVC/(DIOP, chlorinated PE wax, Topanol CA), using methanol as a modifier. Individual additives are unevenly extracted at lower pressures and temperatures, where extraction is incomplete. Topanol CA, the most polar of the three PVC additives studied, could not be fully extracted in the time-scale required (15-20min), even at the highest CO2 temperature and pressure obtainable. However, methanol-modified CO2 enhances extraction of Topanol CA. PVC film additives (DEHP, fatty acids, saturated and aromatic hydrocarbons) were also separated by off-line SFE-preparative SFC, and analysed by PDA and IR [116]. 

Applications Off-line SFE-HPLC appears to be applicable and quantitative for a variety of samples in many real -world matrices. The main challenge lies in the use of this technique for the more polar compounds. Quantitative off-line SFE-SFC-UV analysis of HDPE/Ethanox 330 was described after extensive method development (varying modifiers, modifier concentration, temperature) [129]. Soxhlet extraction and SFE-RPLC-UV of PE samples were compared [127]. A sample size (inhomogeneity) problem was pointed out when a SFE reproducibility study was performed on five 3-mg samples of PE. This points to limits... 

The scope of UV analysis of dissolved polymer/additive matrices is thus quite restricted and mainly limited to special cases in which the additive package is known, e.g. the determination of Irganox 1098 in GFR-PA4.6 after dissolution in H2SO4/HNO3. Fibre-optic dissolution analysis by means of a UV diode array spectrometer is well known. In comparison to IR spectroscopy, UV spectrophotometry is better equipped to provide quantitative data. 

The functionality of the end groups were also determined by NMR or UV analysis which should provide identical molecular weights for perfectly monofunctional materials. As can be seen in Table I, a good correspondence was obtained. Incorporation of the macromonomers into copolymers via free radical copolymerization can also be used as a check on functionality since nonfunctional materials obviously will not be incorporated. Proton NMR was used to confirm the amount of PSX... 

A UV analysis of the products formed upon photolysis of 2a at 280 nm in ethyl propionate, PMMA, and PPMA further illustrates the effect of the matrix stiffness on the photodecomposition process (Table III). The ratio 0C to b +, j [ c/( b+ d)) is determined by the ratio of absorbance of product 2c to the absorbances of products 2b and 2d [A2c/(A2b+A2d)1 n this case, since the results were tabulated from the actual absorption spectra (difference spectra), the ratio of the products formed in the solvent ethyl propionate can be directly compared to the ratios in PPMA and PMMA. From Table III, it is readily seen that the ratio increases on going from the ethyl propionate solution,... 

Normal phase LC-ES-MS was used for the analysis. In a previous work by the same authors, an interesting comparison was made between LC-FL, LC-UV and LC-ES-MS analysis of the same (spiked and unspiked) marine sediments [29]. The concentrations measured by LC-FL and LC-UV were consistently higher by about a factor of two than concentrations analysed by LC-ES-MS (however, with LC-UV analysis, for the unspiked sediments concentrations were all below the detection limit). This was attributed to the limited specificity of the LC-FL and UV techniques. 

In this study, synthetic aqueous solutions of phenol were treated with ozone. The reaction of ozone with phenol was investigated at several conditions, such as different phenol and ozone concentrations, and contact times. Total Organic Carbon (TOC) and UV analysis of the aromatic by-products formed during and after the ozonation reaction were employed. The reaction rates calculated from TOC analysis were investigated. 

Abstract In the beginning, the mixed potential model, which is generally used to explain the adsorption of collectors on the sulphide minerals, is illustrated. And the collector flotation of several kinds of minerals such as copper sulphide minerals, lead sulphide minerals, zinc sulphide minerals and iron sulphide minerals is discussed in the aspect of pulp potential and the nature of hydrophobic entity is concluded from the dependence of flotation on pulp potential. In the following section, the electrochemical phase diagrams for butyl xanthate/water system and chalcocite/oxygen/xanthate system are all demonstrated from which some useful information about the hydrophobic species are obtained. And some instrumental methods including UV analysis, FTIR analysis and XPS analysis can also be used to investigated sulphide mineral-thio-collector sytem. And some examples about that are listed in the last part of this chapter. 

From the flotation results in Fig. 4.21 and the voltammogram in Fig. 4.22, it is derived that the hydrophobic entity of collector on marmatite is mainly of disulphide of xanthate and dithiocarbamate, which is further confirmed by the above UV analysis. However, the UV analysis also suggested the coexistence of collector salts. We propose that the initial oxidation products of xanthate and dithiocarbamate on marmatite should be mainly of disulphide. At higher potential, the adsorbed disulphide may be decomposed and react with surface zinc species to form some parts of collector salts as in the following reactions ... 

Figure 4.41 presents the FTIR reflection spectra of ethyl xanthate adsorption on marmatite at different pH. The characteristic absorption peaks 1210, 1108, 1025 cm occurred. It has been reported that the characteristic absorption bands of dixanthogen are 1260, 1240, 1020 and 1105 cm and those bands of zinc xanthate are 1030, 1125 and 1212 cm (Mielezarski, 1986 Leppinen, 1990). It is derived from Fig.4.41 that there may exist the mixture of dixanthogen and zinc xanthate because both distinct peaks of dixanthogen and xanthate salt appeares in Fig. 4.41, which further confirms the results from the UV analysis in Fig. 4.36 and Fig. 4.37. It can also be seen from Fig. 4.41 that the intensity of the IR peaks is strong indicating the stronger adsorption of xanthate on marmatite accounting for its good floatability in weak pH media. When pH increased above 7, only a very weak peak appeared in the spectra indicating very weak or no adsorption of xanthate on marmatite accounting for its very poor floatability in alkaline pH media.

For the determination of organotin compounds (tributyltin, triphenyltin, triethyltin, and tetra-ethyltin) a MAE is proposed before the normal phase (NP) HPLC/UV analysis [35], In organotin and arsenic speciation studies, hydride generation is the most popular derivatization method, combined with atomic absorption and fluorescence spectroscopy or ICP techniques [25,36], Both atmospheric pressure chemical ionization (APCI)-MS and electrospray ionization ESI-MS are employed in the determination of butyltin, phenyltin, triphenyltin, and tributyltin in waters and sediments [37], A micro LC/ESI-ion trap MS method has been recently chosen as the official EPA (Environmental Protection Agency) method (8323) [38] it permits the determination of mono-, di-, and tri- butyltin, and mono-, di-, and tri-phenyltin at concentration levels of a subnanogram per liter and has been successfully applied in the analysis of freshwaters and fish [39], Tributyltin in waters has been also quantified through an automated sensitive SPME LC/ESI-MS method [40],... 

Toxic nitrophenols (4-nitrophenol, 2-nitrophenol, and 2,4-dinitrophenol) present in air samples are sampled on silica gel or XAD-2 polymeric resin, extracted, and analyzed by the HPLC/DAD technique [240], Nitrophenols are also determined in rain and snow precipitations through HPLC/ UV analysis after SPE [241]. 

More recently [635], a unique extraction step in supplemented foods, by using hot water and a precipitation solution, following by HPLC-ELD/UV analysis has been performed for the simultaneous determination of pyridoxine, thiamine, riboflavin, niacin, pantothenic acid, folic acid, cyanoco-balamin, and ascorbic acid. The mobile phase consisting of phosphate buffer and methanol has been modified in order to perform ion-liquid chromatography by adding l-octanesulfonic acid sodium salt. Furthermore, triethylamine has been also added to improve peak symmetry. 

To qualitatively determine phenyl placements in silicones, SEC-UV analysis was used at 254 nm, with methylene chloride mobile phase,... 

An example of the LC-NMR stop-flow procedure is provided in the analysis of polyphe-nolics from the Chilean plant Gentiana ottonis (Gentianaceae). Preliminary LC-UV analysis... 

If the amounts of the two forms are similar, determination of KT for the mixture of tautomers becomes feasible by direct UV analysis, given that extinction coefficients for the two forms may be satisfactorily substituted by the extinction coefficients for the model compounds, as in equation (12). 

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