Platinum seals

Platinum is a beautiful silvery-white metal, when pure, and is malleable and ductile. It has a coefficient of expansion almost equal to that of soda-lime-silica glass, and is therefore used to make sealed electrodes in glass systems. The metal does not oxidize in air at any temperature, but is corroded by halogens, cyanides, sulfur, and caustic alkalis. 

Anhydrous, monomeric formaldehyde is not available commercially. The pure, dry gas is relatively stable at 80—100°C but slowly polymerizes at lower temperatures. Traces of polar impurities such as acids, alkahes, and water greatly accelerate the polymerization. When Hquid formaldehyde is warmed to room temperature in a sealed ampul, it polymerizes rapidly with evolution of heat (63 kj /mol or 15.05 kcal/mol). Uncatalyzed decomposition is very slow below 300°C extrapolation of kinetic data (32) to 400°C indicates that the rate of decomposition is ca 0.44%/min at 101 kPa (1 atm). The main products ate CO and H2. Metals such as platinum (33), copper (34), and chromia and alumina (35) also catalyze the formation of methanol, methyl formate, formic acid, carbon dioxide, and methane. Trace levels of formaldehyde found in urban atmospheres are readily photo-oxidized to carbon dioxide the half-life ranges from 35—50 minutes (36). 

Several compounds such as BaZrS [12026-44-7], SrZrS [12143-75-8], and CaZrS [59087-48-8], have been made by reacting carbon disulfide with the corresponding zirconate at high temperature (141), whereas PbZrS [12510-11-1] was produced from the elements zirconium and sulfur plus lead sulfide sealed in a platinum capsule which was then pressurized and heated (142). Lithium zirconium disulfide [55964-34-6], LiZrS2, was also synthesized. Zirconium disulfide forms organometaUic intercalations with a series of low ionization (<6.2 eV)-sandwich compounds with parallel rings (143). 

Odon acetate Odon, Saran polyethylene Teflon steel wood amber sealing wax hard mbber nickel, copper, brass, silver, old platinum sulfur acetate rayon polyester... 

This method involves very simple and inexpensive equipment that could be set up m any laboratory [9, 10] The equipment consists of a 250-mL beaker (used as an external half-cell), two platinum foil electrodes, a glass tube with asbestos fiber sealed m the bottom (used as an internal half-cell), a microburet, a stirrer, and a portable potentiometer The asbestos fiber may be substituted with a membrane This method has been used to determine the fluoride ion concentration in many binary and complex fluondes and has been applied to unbuffered solutions from Willard-Winter distillation, to lon-exchange eluant, and to pyrohydrolysis distil lates obtained from oxygen-flask or tube combustions The solution concentrations range from 0 1 to 5 X 10 M This method is based on complexing by fluonde ions of one of the oxidation states of the redox couple, and the potential difference measured is that between the two half-cells Initially, each cell contains the same ratio of cerium(IV) and cerium(tll) ions... 

It consists of a boiling-tube, thiough the bottoni-stout platinum wire is sealed, which is intenclcd... 

In outline the procedure consists of carefully weighing about 5-10 mg of sample on to a shaped piece of paper (Fig. 3.11c) which is folded in such a way that the tail (wick) is free. This is then placed in a platinum basket or carrier suspended from the ground-glass stopper of a 500 mL or 1 litre flask. The flask, containing a few millilitres of absorbing solution (e.g. aqueous sodium hydroxide), is filled with oxygen and then sealed with the stopper with the platinum basket attached. 

The introduction of the sample into the adsorbent layer is a critical process in HPTLC. For most quantitative work a platinum-iridium capillary of fixed volume (100 or 200 nL), sealed into a glass support capillary of larger bore, provides a convenient spotting device. The capillary tip is polished to provide a smooth, planar surface of small area (ca 0.05 mm2), which when used with a mechanical applicator minimises damage to the surface of the plate spotting by manual procedures invariably damages the surface. 

One form of calomel electrode is shown in Fig. 15.1(a). It consists of a stoppered glass vessel provided with a bent side tube fitted with a three-way tap which carries a short upper and a long lower tube the latter is drawn out to a constriction at the bottom end. A short platinum wire is fused into the bottom of the vessel so that it protrudes into the interior, and a narrow glass tube sealed to the bottom of the vessel is bent round parallel to the vessel. A little mercury placed in the bottom of this tube provides electrical connection with the interior of the vessel through the sealed-in platinum wire. Mercury and mercury compounds must be handled with care (see Section 16.8). 

A length of 6-7 mm of platinum wire of 0.5 mm diameter sealed into a glass tube is satisfactory electrical connection is made by means of a copper wire dipping into a little mercury in contact with the platinum wire. 

Batsanov et al. 23) reacted sulfur with PtCU and PtBr2 by heating mixtures of the reactants in evacuated, sealed ampoules. At 100 -200°C after 12-24 h, sulfide chlorides PtCljS (1.70 < x < 2 0.6 s y < 3.35) and sulfide bromides PtBr S (1.87 < x 2.06 0.84 y s 1.80) were formed. The compositions depended on the initial PtX2 S ratio, and the temperature. At 320-350°C, loss of chlorine led to the compounds PtClS (1.7 y 1.9). According to their X-ray powder patterns, all of these products retained the main structural features of the original platinum halides. From considerations of molar volumes, the authors deduced the presence of polysulfide anions. 

P, Petri dish TS, PTFE supports PP, polymerized packing (Lukopren ) G, glass seal, E, platinum planar electrodes TW, thermostated water [68. ... 

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