A contribution to common Carius tube distillation techniques

Abstract

In this paper, we introduce an economic electrothermal timing steamer for common Carius tube Os in situ distillation. It is suitable for analysing several batches of samples. Its configuration allows the Carius tubes to be properly fixed and bathed in steam into which the tubes are immersed. The top of each Carius tube is sealed with a stretchy rubber head through which a pair of teflon tubes pierce, serving as inlet and outlet for clean air and OsO 4 respectively. At steam temperatures of 99-100 C, OsO 4 in the sample solutions inside the Carius tubes is evaporated out and subsequently carried by clean air to the trapping water in an ampoule bottle, immersed in a box filled with ice. In the present study the steamer allowed for the convenient, efficient and simultaneous distillation of Os from seven samples with near ninety percent recovery. The blank values were 0.42 AE 0.15 pg and 0.26 AE 0.05 for 187 Os and 187 Os/ 188 Os (n ¼ 4). The dating results of reference materials (RMs) namely Henderson, HLP and JDC were in accordance with reference and certified values within the range of uncertainties. The special steamer has successfully been used in the analysis of pyrite samples for the distillation of Os.

High-efficiency photooxidation vapor generation of osmium for determination by inductively coupled plasma-optical emission spectrometry

“…The volatility (boiling point: 130 C) of osmium tetraoxide has long been used to separate osmium from a matrix for analytical practices. 15,[28][29][30][31][32][33][34][35][36][37][38] In these studies, the generation of volatile osmium tetraoxide is usually achieved by using a large amount of strong oxidizing agents, such as HNO 3 , 32,37 H 2 O 2 , 31 H 5 IO 6 28,32,33 and K 2 Cr 2 O 7 . 15 In our previous study, we have realized the generation of osmium tetraoxide without any oxidant based on a novel solution cathode glow discharge (SCGD) induced vapor generation method.…”

Re-Os dating of galena and sphalerite from lead-zinc sulfide deposits in Yunnan Province, SW China

“…The pre-concentration methods for both Os (Jin et al, 2013(Jin et al, , 2011Li et al, 2012;Paul et al, 2009;Hassler et al, 2000;Birck et al, 1997;Cohen and Waters, 1996) and Re (Tagami and Uchida, 2000;Morgan et al, 1991) in geologic samples have been extensively investigated. Anion exchange chromatography (Qi et al, 2010(Qi et al, , 2007Meisel et al, 2003a;Malinovsky et al, 2002;Morgan et al, 1991) and extraction with organic solvent Yang et al, 2006;Du et al, 2001Du et al, , 1994Birck et al, 1997) are usually used for separation of Re.…”

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

“…Some authors developed in situ Caius tube distillation methods without the use of distillation flask to further reduce the Os blank (e.g., Qi et al, 2010 ). Jin et al (2013) developed a device for a batch of simultaneous Carius tube in situ distillations, which can offer significantly higher sample throughput. Woodhouse et al (1999) developed a method for the direct distillation of Os from large volumes of seawater (1–1.5 L, addition of H 2 O 2 in H 2 SO 4 to oxidize the spiked Os) for subsequent Os isotopic analysis.…”