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NASA NTRS1973

Radiolytic preparation of anhydrous tin (2) chloride

Anhydrous tin (2) chloride (SnCl2) is prepared by radiolysis with high energy electrons of a tin (4) chloride (SnCl4) solution in heptane. The SnCl4 is reduced to insoluble SNCl2. The energy yield, G(SnCl2), molecules of SnCl2, produced per 100 eV, increases with SnCl4 concentration from 1.6 at 0.15 M SnCl4 to 3.1 at 3.0 M SnCl4. Other parameters such as temperature total dose and beam current have little influence on G(SnCl2). The method may be used to prepare other metal halides if the higher valence, more covalent metal halide is soluble in aliphatic hydrocarbons and the lower more ionic metal halide is insoluble. The reaction mechanism is discussed; the radiolysis of both heptane and SnCl4 is involved. At high SnCl4 concentration G(SnCl2) appears to be limited by the yield of SnC13 radicals.

Philipp, W. H.↗

NASA NTRS1979

Evaluation of high specific-heat ceramic for regenerator use at temperatures between 2-30 K

Specific heat, thermal conductivity (both in the range 2-30 K), and microhardness data were measured on the ceramics labelled LS-8, LS-8A, and LS-8A doped with CsI, SnCl2, and AgCl. A work hardened sample of LS-8A was also studied in an effort to determine the feasibility of using these types of LS-8 materials to replace Pb spheres in the regenerator of the JPL cryocooler. The LS-8A materials are all more than an order of magnitude harder than Pb, and the dopants do not significantly improve the hardness. However, the SnCl2 dopant has a remarkable effect in improving the specific heat and thermal conductivity of LS-8A. The SnCl2 doping level which maximized the regenerator enthalpy change in going from an unloaded to a loaded condition was found to be 0.2 percent SnCl2 in LS-8A. It was also found that the enthalpy change for a regenerator employing the LS-8A material is more than three times larger than for the Pb spheres case. The use of rods, rather than spheres, of optimally doped LS-8A in regenerators is discussed.

Lawless, W. N.↗

NASA NTRS1981

Evaluation of ceramic packed-rod regenerator matrices

An extensive evaluation of a modified cryocooler with various regenerator matrices is reported. The matrices examined are 0.015 in. diam. Pb spheres and 0.008, 0.015, and 0.030 in. diam. rods of a 0.2% SnCl2 doped ceramic labelled LS-8A. Specific heat and thermal conductivity data on these rod materials are also reported. The chronic pulverization/dusting problem common to Pb spheres was investigated. During a 1000 hr life test with 0.0008 in. diam. rods there was no degradation of the refrigerator performance, and a subsequent examination of the rods themselves revealed no evidence of breakage or pulverization. The load temperature characteristics for the rod packed regenerators were inferior to that for the Pb spheres, the effect being to shift the Pb spheres load curve up in temperature. This temperature shift was 5.0, 7.4, and 11.6K for the 0.0008, 0.015, and 0.030 in. diam. rods, respectively.

Lawless, W. N.↗

NASA NTRS2003

Determination of Mercury Content in a Shallow Firn Core from Summit, Greenland by Isotope Dilution Inductively Coupled Plasma Mass Spectrometry

The total mercury Hg content was determined in 6 cm sections of a near-surface 7 m firn core and in surrounding surface snow from Summit, Greenland (elevation: 3238 m, 72.58 N, 38.53 W) in May 2001 by isotope dilution cold-vapor inductively coupled plasma mass spectrometry (ID-CV-ICP-MS). The focus of this research was to evaluate the capability of the ID-CV-ICPMS technique for measuring trace levels of Hg typical of polar snow and firn. Highly enriched Hg-201 isotopic spike is added to approximately 10 ml melted core and thoroughly mixed. The Hg(+2) in the sample is reduced on line with tin (II) chloride (SnCl2) and the elemental Hg (Hg(0)) vapor pre-concentrated on to gold gauze using a commercial amalgam system. The Hg is then thermally desorbed and introduced into a quadrupole ICP-MS. The blank corrected Hg concentrations determined for all samples ranged from 0.25 ng/L to 1.74 ng/L (ppt) (average 0.59 ng/L plus or minus 0.28 ng/L) and fall within the range of those previously determined by Boutron et al., 1998 (less than or equal to 0.05 ng/L to 2.0 ng/L) for the Summit site. The average blank value was 0.19 ng/L plus or minus 0.045 ng/L (n=6). The Hg values specifically for the firn core range from 0.25 ng/L to 0.87 ng/L (average 0.51 ng/L plus or minus 0.13 ng/L) and show both values declining with time and larger variability in concentration in the top 1.8 m.

Mann, Jacqueline L.↗