A method of general applicability for the micro determination of chlorine,bromine and iodine

Summary A method is described for the combustion of halogen containing organic compounds in milligram quantities in a closed system. It has been found to have greater applicability than existing techniques. After combustion the halogen is determined by an amperometric titration, which permits the determination of Cl^–, Br^– and I^– either singly or in admixture. The accuracy is probably better than existing micro methods for single halides and comparable with these methods for mixed halides.

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Zusammenfassung Eine Methode zur Verbrennung von Milligrammengen halogenhaltiger organischer Verbindungen im geschlossenen System wurde beschrieben. Sie hat einen größeren Anwendungsbereich als bisher bekannte Verfahren. Nach der Verbrennung wird das Halogen durch eine amperometrische Titration bestimmt, womit Chlorid, Bromid und Jodid sowohl einzeln wie in Gemischen bestimmt werden können. Die Genauigkeit seheint besser zu sein als bei bekannten Mikromethoden für die Bestimmung einzelner Halogene und etwa gleich gut wie bei Methoden zur Analyse von Halogengemischen.

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Résumé On décrit une méthode de combustion en vase clos, des composés organiques contenant des halogènes en quantités de l'ordre du milligramme. Cette méthode a été trouvée comme ayant un domaine d'applications plus grand que celui des techniques existant déjà. Après combustion, l'halogène est dosé par titrage ampérométrique, ce qui permet le dosage de Cl^–, Br^– et I^– isolés ou en mélange. La précision est probablement meilleure que celle des microméthodes existant pour les halogénures isolés et comparable à celle de ces méthodes pour les mélanges d'halogénures.

     

The development of a versatile field program for measuring tritium in “real-time”

Robust sample handling and liquid scintillation counting (LSC) procedures have been developed to routinely monitor tritium in the field relative to the 20,000 pCi/L drinking water standard. This procedure allows tritium to be monitored hourly during 24 hour drilling operations at depths in the saturated zone potentially contaminated by sub-surface nuclear weapons testing at the Nevada Test Site. Using retrofitted, shock hardened, vibration damped counters and strict analytical protocols, tritium may be measured rapidly in the field under hostile conditions. Concentration standards and dead tritium backgrounds are prepared weekly in a central laboratory and delivered to remote drilling locations where they are recounted daily as a check on counter efficiency and calibration. Portable LSC counters are located in trailers and powered off a battery pack and line filter fed by mobile generator. The samples are typically groundwaters mixed with drilling fluids returned after circulation through a drill string. Fluids are aerated and de-foamed, filtered, mixed with scintillation cocktail and dark adapted before counting. Real-time monitoring affords drilling and field personnel early warning against intercepting down-gradient plumes of radioactivity. For routine operations, the tritium activity may not exceed a 10,000 pCi/L threshold.     

Measurement/data-processing method to improve the ruggedness of membrane-based sensors: Application to amperometric oxygen sensor

This paper describes alternative measurement and data-processing approaches that can reduce effects of experimental variables on results obtained with a membrane-based sensor for oxygen. In the new approaches, the membrane-based sensor is first equilibrated with the sample solution, after which a polarizing voltage is applied and current vs. time data are recorded as the response decays toward a steady-state condition. Current vs. time data are then processed by a fixed-time option and an integration option designed to determine the charge corresponding to the total amount of oxygen inside the membrane when a polarizing voltage is applied. The current measured at a fixed time and the total charge varied linearly with oxygen concentration between 0.05 and 0.26 mmol l(-1). Pooled relative standard deviations (N = 35) for the measurement/data-processing step were near 0.4% for the new pre-equilibrium options compared to a value of 0.3% for the steady-state option. Dependencies of the pre-equilibrium options on membrane thickness and stirring rate in the most sensitive regions were at least two orders of magnitude smaller than for the steady-state option.