Laboratory electrodes

FIGURE 1.26 Three-electrode laboratory cell. (A) Porous carbon electrode film (carbon + binder) (B) treated A1 current collectors (C) porous separator (D) Teflon plates (for stack pressure) and (E) stainless steel clamps (not shown, see arrows). (From Gamby, J., et al., J. Power Sources, 101,109, 2001.)... 

In order to know the performances of individual electrodes working in the conditions of actual cells, it is necessary to add a reference electrode. Laboratory cells have been designed for that... 

The other two SMETs datasets evaluated for nitrate analysis in RM13 were obtained by one other laboratory, again with two different methods 1, MERCK Specktroquant Kit (Spectrophotometry - colorimetry) (laboratory code 09a) and 2, YSI Multiparameter Probe 6900 nitrate specific electrode (laboratory code 09b). The two results are presented encircled on Figure 5.2.1. 

These are items which cannot be made in-house like spares for pumps, conveyers, special lubricants, graphite electrodes, laboratory reagents and other analytical grade chemicals, thermocouples, electrical spares) since the know-how and/or facilities for making them are not available,... 

A microelectrode is an electrode with at least one dimension small enough that its properties are a fimction of size, typically with at least one dimension smaller than 50 pm [28, 29, 30, 31, 32 and 33]. If compared with electrodes employed in industrial-scale electrosynthesis or in laboratory-scale synthesis, where the characteristic dimensions can be of the order of metres and centimetres, respectively, or electrodes for voltannnetry with millimetre dimension, it is clear that the size of the electrodes can vary dramatically. This enonnous difference in size gives microelectrodes their unique properties of increased rate of mass transport, faster response and decreased reliance on the presence of a conducting medium. Over the past 15 years, microelectrodes have made a tremendous impact in electrochemistry. They have, for example, been used to improve the sensitivity of ASV in enviroiunental analysis, to investigate rapid... 

Of course, in order to vary the mass transport of the reactant to the electrode surface, the radius of the electrode must be varied, and this unplies the need for microelectrodes of different sizes. Spherical electrodes are difficult to constnict, and therefore other geometries are ohen employed. Microdiscs are conunonly used in the laboratory, as diey are easily constnicted by sealing very fine wires into glass epoxy resins, cutting... 

The preparation of an ion-selective electrode for salicylate is described. The electrode incorporates an ion-pair of crystal violet and salicylate in a PVC matrix as the ion-selective membrane. Its use for the determination of acetylsalicylic acid in aspirin tablets is described. A similar experiment is described by Creager, S. E. Lawrence, K. D. Tibbets, C. R. in An Easily Constructed Salicylate-Ion-Selective Electrode for Use in the Instructional Laboratory, /. Chem. Educ. 1995, 72, 274-276. 

In the laboratory, it has been found that similar effects can be produced if a voltage is applied between two electrodes immersed in a gas. The nature of the laboratory or instrumental discharge depends critically on the type of gas used, the gas pressure, and the magnitude of the applied voltage. The actual electrical and gas pressure conditions determine whether or not the discharge is called a corona, a plasma, or an arc. 

National Institute of Standards and Technology (NIST). The NIST is the source of many of the standards used in chemical and physical analyses in the United States and throughout the world. The standards prepared and distributed by the NIST are used to caUbrate measurement systems and to provide a central basis for uniformity and accuracy of measurement. At present, over 1200 Standard Reference Materials (SRMs) are available and are described by the NIST (15). Included are many steels, nonferrous alloys, high purity metals, primary standards for use in volumetric analysis, microchemical standards, clinical laboratory standards, biological material certified for trace elements, environmental standards, trace element standards, ion-activity standards (for pH and ion-selective electrodes), freezing and melting point standards, colorimetry standards, optical standards, radioactivity standards, particle-size standards, and density standards. Certificates are issued with the standard reference materials showing values for the parameters that have been determined. 

Laboratory experiments have shown that IGSCC can be mitigated if the electrochemical potential (ECP) could be decreased to —0.230 V on the standard hydrogen electrode (SHE) scale in water with a conductivity of 0.3 ]lS/cm (22). This has also been demonstrated in operating plants. Equipment has been developed to monitor ECP in the recirculation line and in strategic places such as the core top and core bottom, in the reactor vessel during power operation. 

Individual polyethers exhibit varying specificities for cations. Some polyethers have found appHcation as components in ion-selective electrodes for use in clinical medicine or in laboratory studies involving transport studies or measurement of transmembrane electrical potential (4). The methyl ester of monensin [28636-21 -7] i2ls been incorporated into a membrane sHde assembly used for the assay of semm sodium (see Biosensors) (5). Studies directed toward the design of a lithium selective electrode resulted in the synthesis of a derivative of monensin lactone that is highly specific for lithium (6). 

In the area of consumer products, amperometric glucose sensors hold high potential. Industrially, process monitors for the manufacture of consumer chemicals are under development. However, replacement of defective reference electrodes, which in a laboratory environment may be trivial, may be prohibitively difficult m vivo or in an industrial process environment. 

Electrodes. At least three factors need to be considered ia electrode selection as the technical development of an electroorganic reaction moves from the laboratory cell to the commercial system. First is the selection of the lowest cost form of the conductive material that both produces the desired electrode reactions and possesses stmctural iategrity. Second is the preservation of the active life of the electrodes. The final factor is the conductivity of the electrode material within the context of cell design. An ia-depth discussion of electrode materials for electroorganic synthesis as well as a detailed discussion of the influence of electrode materials on reaction path (electrocatalysis) are available (25,26). A general account of electrodes for iadustrial processes is also available (27). 

Tank Cells. A direct extension of laboratory beaker cells is represented in the use of plate electrodes immersed into a lined, rectangular tank, which may be fitted with a cover for gas collection or vapor control. The tank cell, which is usually undivided, is used in batch or semibatch operations. The tank cell has the attraction of being both simple to design and usually inexpensive. However, it is not the most suitable for large-scale operation or where forced convection is needed. Rotating cylinders or rotating disks have been used to overcome mass-transfer problems in tank cells. An example for electroorganic synthesis is available (46). 

It is of special interest for many applications to consider adsorption of fiuids in matrices in the framework of models which include electrostatic forces. These systems are relevant, for example, to colloidal chemistry. On the other hand, electrodes made of specially treated carbon particles and impregnated by electrolyte solutions are very promising devices for practical applications. Only a few attempts have been undertaken to solve models with electrostatic forces, those have been restricted, moreover, to ionic fiuids with Coulomb interactions. We would hke to mention in advance that it is clear, at present, how to obtain the structural properties of ionic fiuids adsorbed in disordered charged matrices. Other systems with higher-order multipole interactions have not been studied so far. Thermodynamics of these systems, and, in particular, peculiarities of phase transitions, is the issue which is practically unsolved, in spite of its great importance. This part of our chapter is based on recent works from our laboratory [37,38]. 

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... 

Praktikum, n. practice practical course, laboratory course laboratory manual, praktisch, a. practical applied practised, praktizieren, v.t. practice, prall, a. tight, taut, stretched, tense plump. Prall, m. shock rebound reflection, -blech, n. deflecting plate, baffle, -elektrode, /. reflecting electrode. 

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