On-line data acquisition system for Perkin-Elmer 240 carbon,hydrogen, and nitrogen analyzer

The Perkin-Elmer 240 CH and N analyzer was adapted for on-line data acquisition with a remote computer. Sample weights from a Cahn electrobalance are directly entered into the computer via a power supply and interrupt system. The outputs from the three thermal conductivity detectors are monitored for 10 sec and signal averaged by the computer. The computer takes all data necessary for the calculation of percent CH and N and prints out a final report on a Silent 700 remote terminal. The report is suitable for direct transmission to the sample submitter. Duplicate reports are printed for permanent analytical records. The precision of results obtained with on-line data acquisition compare favorably to results calculated manually, and provides a 38% improvement in efficiency. The on-line systems employ a PDP-15/76 computer, which is available for other tasks. This provides an additional cost savings compared to the alternate approach of purchasing a small dedicated computer.     

Synthesis and novel reactivity of halomethyldimethylsulfonium salts

Iodomethyl-, chloromethyl-, and fluoromethyldimethylsulfonium salts, 4b-d, have been synthesized and are observed to be highly reactive molecules that exhibit extraordinary diversity with respect to the nature of their reactivity, undergoing facile direct substitution (S(N)2) reactions, but also being highly susceptible to electron-transfer reactions. Cyclic voltametry experiments indicated that the iodomethyldimethylsulfonium compound, 4b, is a potent electron acceptor, even surpassing the reactivity of perfluoro-n-alkyl iodides in that capacity. The iodo- and chloromethyldimethylsulfonium salts, 4b,c, as well as the analogous iodomethyltrimethylammonium salt, 3a, are shown to be reactive SET acceptors.     

Determination of ruthenium and iridium in anode coatings by atomic-absorption spectroscopy

A method is described for the determination of ruthenium and iridium coated on an electrode surface. The coating is chemically removed from the electrode by fusion with alkali, and the resulting solution prepared for analysis. Interelement interferences are eliminated by using a titanium-potassium matrix solution as a releasing agent. Recovery and precision data are given for ruthenium and iridium. The AAS determination of ruthenium compares favourably with a standard colorimetric method.     

Determination of ruthenium and tin on electrochemical anodes by energy-dispersive X-ray fluorescence

"Dimensionally Stable Anodes" (DSA)(R) have gained wide acceptance in electrochemical production of chlorine and caustic soda. The DSAs are usually composed of electrocatalytic layers of precious and non-precious metal oxides produced by thermal decomposition of salts on a valve-metal substrate (e.g., titanium). They have long lifetimes (some years) in commercial service, and accelerated aging is used in testing them. In these tests the cell potential is stable for most of the anode life. Failure of an anode is characterized by a rapid increase in potential to beyond the point of practical operation of the cell. Non-destructive X-ray techniques have been utilized to investigate the mechanism involved. It has been established that the precious metal content has been reduced by 50-60% when the anodes fail. Although present DSA coatings are more than adequate for commercial applications, there is continuing interest in improving them. The materials for DSA formulation include the precious metals iridium, ruthenium and rhodium, the non-precious metals tin, antimony and manganese, and the valve metals titanium and tantalum.     

Determination of acid-soluble and total rhodium on alumina-supported catalysts

Characterization of alumina-supported catalysts required determination of rhodium by atomic-absorption spectroscopy (AAS). Catalysts were loaded with 0.1-2.0% rhodium chloride and calcined at 400 degrees . Rhodium remaining as the chloride was regarded as the soluble form, while that converted into the oxide or bonded to the alumina was regarded as the bonded form. By selective dissolution procedures, soluble rhodium was leached from the substrate and determined by AAS. Total rhodium was determined after the catalyst had been fused with sodium peroxide. Bonded rhodium can be determined by difference or by analysing leached residue. Optimization of AAS conditions, use of spectroscopic buffer solution and elimination of interelement interferences are discussed.     

Closing the automation loop for carbon,hydrogen and nitrogen analyses

Summary The automation of carbon, hydrogen, and nitrogen (CHN) microanalysis has been extended to include software control of two Perkin Elmer Elemental Analyzers (a 240A and 240C), electronic weight transfer from a Mettler UM3 Ultra-Microbalance, and electronic preparation of formalized reports. This highly automated closed loop system minimizes the sources of human error and maximizes the efficiency of CHN analyses. The precision and accuracy of data is comparable to values previously reported.

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Vervollständigung der Automatisierung der C-, H-und N-Bestimmung

Zusammenfassung Die Automatisierung der CHN-Mikrobestimmung wurde durch Software-Kontrolle zweier Perkin-Elmer Analysatoren (240 A und 240 C), durch elektronische Übertragung der Daten einer Mettler-Waage UM 3 sowie elektronische Herstellung der Resultat-Formulare erweitert. Dadurch werden die Fehlerquellen vermindert und der Gütegrad der CHN-Analysen erhöht. Richtigkeit und Genauigkeit der Ergebnisse entsprechen den an anderer Stelle angegebenen Werten.