Persulphate systems

Aromatic nitriles are now also available in good yields from aryl iodides by reaction with sodium cyanide impregnated on alumina/ from primary aralkyl-amines by oxidation with a potassium ruthenate-potassium persulphate system/ ... 

Polymerization was brought about by a water-emulsion persulphate system. The two most well-known types were Poly-lF4 and Poly-2F4 (known earlier as PolyFBA and PolyFMFPA respectively) ... 

Since poly(vinyl acetate) is usually used in an emulsion form, the emulsion polymerisation process is commonly used. In a typical system, approximately equal quantities of vinyl acetate and water are stirred together in the presence of a suitable colloid-emulsifier system, such as poly(vinyl alcohol) and sodium lauryl sulphate, and a water-soluble initiator such as potassium persulphate. 

In aqueous solutions the persulphate ion is known as a strong oxidizing agent, either alone or with activators. Thus, it has been extensively used as the initiator of vinyl polymerization [43-47]. However, only later, Kulkarni et al. [48] reported the graft copolymerization of AN onto cellulose using the Na2S203/K2S20s redox system. 

Grafting of polyacrylamide onto guar gum [431] and Ipomoea gum [178] in aqueous medium initiated by the potassium persulphate/ascorbic acid redox system was performed in the presence of atmospheric oxygen and Ag" " ions. After grafting, a tremendous increase of the viscosity of both gum solutions was achieved, and the grafted gums were found to be thermally more stable. 

FIGURE 9.10 In vitro cytotoxicity testing of individual components of recombinant resilin curing polymer system. The light gray areas represent green fluorescence, evidence of live cells, (a) Ammonium persulphate... 

Needles, H.L. and Whitfield, R.E. "Crosslinking of Collagens Employing a Redox System Comprising Persulphate and a Reducing Agent," US Patent 3,427,301(1969). 

In this case, a moderately water-soluble amphiphilic N-vinylcaprolaclam (NVC1) played the role of a fl-unit, and a well-water-compatible N-vinyl-imidazole (NVIAz) served as a P-unil. The polymerization was carried out in a medium of 10% aqueous dimethylsulfoxide (DMSO). The addition of DMSO to the reaction solvent was necessary because of insufficient NVC1 solubility in pure water. It was also shown that in this solvent mixture, the NVCl-homopolymers and NVCl/NVIAz-copolymers retained their LCST-behaviour [26,28]. Hence, the DMSO in the reaction solvent did not significantly suppress the hydrophobic interactions of the NVC1 units. The polymerization was initiated by the redox system (N,N,N, N -tetramethylethylenediamine (TMEDA) + ammonium persulphate (APS)) and was carried out at 65 °C (1st step). This condition was very important, since admittedly the temperature was higher than the phase separation threshold of the reaction bulk when the polymeric products were formed that is, under these thermal conditions, hydrophobically-induced folding as the NVCl-blocks appear was ensured. After completion of the reaction, the... 

As mentioned above, many variants of the Dohrmann total organic carbon analyser are available, ranging from low-cost non-automated analysers based on sample combustion in a platinum boat (DC8JA) or using persulphate oxidation/ultraviolet irradiation (DC 88) to top-of-range fully automated and computerized systems based on combustion in a ceramic tube (DC 90) or combined simultaneous persulphate-ultraviolet oxidation (DC 180). Only one of these systems, the DC 180, is discussed below in any detail. 

Ferguson and Shah described polymerization of AA in the presence of polyCethylene oxide), PEG, having mol. weight of 1,500 and 6,000. Polymerizations were carried out in water at 55 and 74°C. Potassium persulphate was used as an initiator. Having examined the influence of template concentration on the rate of polymerization, it was found that the maximum rate appears not at equimolar ratio of monomer to template, but at much lower concentration of the template. Polymerization of AA in the presence of PEG in water at 74°C was treated by the authors as an example of the system in which the interaction between template and the monomer is rather weak. Indeed, only tern-... 

By far the most studied PolyHIPE system is the styrene/divinylbenzene (DVB) material. This was the main subject of Barby and Haq s patent to Unilever in 1982 [128], HIPEs of an aqueous phase in a mixture of styrene, DVB and nonionic surfactant were prepared. Both water-soluble (e.g. potassium persulphate) and oil-soluble (2,2 -azo-bis-isobutyronitrile, AIBN) initiators were employed, and polymerisation was carried out by heating the emulsion in a sealed plastic container, typically for 24 hours at 50°C. This yielded a solid, crosslinked, monolithic polymer material, with the aqueous dispersed phase retained inside the porous microstructure. On exhaustive extraction of the material in a Soxhlet with a lower alcohol, followed by drying in vacuo, a low-density polystyrene foam was produced, with a permanent, macroporous, open-cellular structure of very high porosity (Fig. 11). 

Pour the gels in a fume hood. The total gel volume depends on the electrophoresis system used. Mix acrylamide solutions with ammonium persulphate (6 pl/ml gel)... 

Sulphuric acid [7664-93-9] M 98.1, d 1.83. Sulphuric acid, and also 30% fuming H2SO4, can be distilled in an all-Pyrex system, optionally from potassium persulphate. Also purified by fractional crystn of the monohydrate from the liquid. It ha pKa values of -3 and +1.96 in water. 

The thin-layer gel system used for resolving the different fragments produced by the chemical degradation method is essentially that of Sanger, Nicklen and Coulson (1977) as described in Chapter 4. An 8% polyacrylamide gel is usually used though for special purposes a 10 or 12% gel can give an improved resolution of the smallest fragments. For the standard 8% gel the polymerization mixture contains 7.6% (wt/vol) acrylamide, 0.4% (wt/vol) bisacrylamide, 50% (wt/vol) urea, 100 mM Tris-borate, pH 8.3, 2mM EDTA, 0.07% (wt/vol) ammonium persulphate and TEMED catalyst. This solution is poured or injected into a 0.4 x 200 x 400 mm mold to form a gel slab. 

The persulphate solution is hydrolysed and distilled at a reduced pressure in two systems of distillation tubes which are parallely connected (see Fig. 143). 

As expected, the pH of the latex produced by the reaction correlates closely with the Initial pH of the reaction system. However, rather unexpectedly It was found (see Figure 4) that the final pH Is always about two units lower than the Initial pH. Similar effects are observed In persulphate - Initiated emulsion polymerisations, where the reduction in pH Is attributed to the formation of blsulphate Ions by reaction between water molecules and sulphate radical Ions formed by decomposition of the persulphate. No such ready explanation Is available In this Instance. 

Several oxidants were tested in an epoxidation reaction in the presence of iminium salt catalysts to determine which offers the best profile in the absence of water [42]. These reactions were carried out at 0 °C with 1-phenylcyclohexene as substrate and (17) and /or (24) as catalysts (5-20 mol%), in dichloromethane as solvent. Most of the systems examined showed either high levels of background epoxidation (alkaline hydrogen peroxide, peracids, persulphates) or very low rates of reaction, even in the presence of 20 mol% of the catalysts (perselenates, percarbonates, perborates and iodosobenzene diacetate). Tetra-N-butylammo-nium Oxone, reported by Trost [43], was also unsuccessful as oxidant. 

The largest group of elements comprises those isolated from solution in the elemental form as a result of reduction, usually electrochemical. In acid solution, the electrolytic deposition of metal on a solid cathode is limited to noble and semi-noble metals. Trace analysis of copper and its compounds may serve as an example [100]. An anodic dissolution technique may be applied for the isolation of macroscopic amounts of copper. A sample in the form of a bar, plate, or wire is the anode in the electrolytic system. When current is passed through the electrolyte (nitric acid + persulphate), Cu is deposited on the graphite cathode, while most trace elements accumulate in the solution. In the trace analysis of platinum, the matrix has been also separated on a cathode [101]. 

The condensation method begins with molecular units, and the particles are built-up by a process of nucleation typical example is the preparation of polymer lattices, in which case the monomer (e.g., styrene or methylmethacrylate) is emulsified in water using an anionic or nonionic surfactant (e.g., sodium dodecyl sulphate or alcohol ethoxylate). A polymeric surfactant is also added to ensure the long-term colloid stabiHty of the resulting latex. An initiator such as potassium persulphate is then added and, when the temperature of the system has increased, initiation occurs that results in formation of the latex [polystyrene or poly(methylmethacrylate)]. 

Water-soluble initiators used in emulsion polymerization are preferentially sodium, potassium or ammonium persulphate operating at 50-80°C. Redox systems use hydrogen peroxide or a persulphate as the oxidizing moiety and sodium metabisulphite, sodium hydrosulphate (also known as hyposulphite or dithionite), sodium thiosulphate and sodium formaldehyde sulphoxylate as the reductant. 

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