Use of sealed tubes for the preparation of acid solutions of samples for analysis, or for small-scale refining: pressures of acids heated above 100 degrees C

Abstract

This paper describes special technics suita ble for the use of sealed tubes in treating refractory materials with hydrochloric acid and other acid mixtures at eievated temperatures. Methods for filli ng, fo r sealing, and for opening tubes are discussed. The feasibility of re use of tubes of Pyrex glass is discussed with some observed phenomena of the attack of the glass by the acids. A protecting shell is described together with a method of using solid carbon dioxide to provide the compensating pressures needed to protect the sealed t ubes from bursting. The pressures developed on heating hydrochloric acid and mixtures of hydrochloric acid with nitric or perchloric acids were measured in a special gage, which is described.

Analytical Methods for Os Isotope Ratios and Re-PGE Mass Fractions in Geological Samples

“… Shirey and Walker (1995) first adopted the Carius tube method ( Gordon, 1943 ; Wichers, et al, 1944 ; Gordon et al, 1944 ) for Re-Os isotopic analysis. The Carius tube method permits the dissolution of samples in oxidizing solutions (usually reverse aqua regia) at high temperatures without the loss of volatile OsO 4 .…”

Determination of copolymer composition by combustion analysis for carbon and hydrogen

“…In the determination of sulfur, a 0.2-g sample of the purified polymer is decomposed by the Carius method [ 19 , 20 ]. The sulfur is precipitated and weighed as barium sulfate by the conventional microtechnique.…”

Siderophile Elements in Tracing Planetary Formation and Evolution

“…The technique had been updated specifically for noble metals at the NBS by Gordon et al (1944) and Wichers et al (1944). So, in collaboration with Steve Shirey at DTM, in 1993 I had some tubes fabricated and added sample powder to them.…”