rd  - 1962 - ENC Conference

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"T~L PROBE INSERT ASSEMBLY MODIFICATIONS FOR VARIAN V-4340 VARIABLE TEMPERATURE ACCESSORY" R. H. Elsken Western Regional Research Laboratory, l_/ Albany, California ABSTRACT In our wide-line NMRwork, we need to obtain spectra of solids prepared in sealed containers. For convenience of handling, these sealed containers should also be the NMR sample tubes. We have modified extensively the ~.KLprobe insert for the VarianModel V-4340 Variable Temperature NMR Probe Accessory to accept sealed samples and, in t~e process, have also increased the filling factor by approximately h. In brief, the supplied combination dewar probe insert and sample holders were disca<strong>rd</strong>ed, and techniques suggested by S. Brownstein (Can. J. Chem., B7, 1119, 1939) and Paul Shafer (Mellon NMR Letters, #30, April 1961) w--~re followed to obtain a compatible system. As shown in the attached illustration, a two-component dewar and coil insert replaces the Varian dewar probe insert, and a 9 x 30 mm shell vial replaces the Varian sample holder. The sample tube assembly is designed to minimize vibration with high gas flow rates. In operation, tank nitrogen flows down between the walls of the coil insert and dewar insert, through holes in the lower section of the coil insert, up past the sample tube, and out the upper end of the coil insert tubing. We have used this system primarily for low temperature work. Average stability is + 0.5 ° C when tank nitrogen flows through a con- stant flow regulator and copper coil -- liquid nitrogen type heat ex- changer. Maximum flow rate is approximately 16 liters per minute for -195 ° C sample temperature. ~/A laboratory of the Western Utilization Research and Development Division, Agric itural Research Service, U. S. Department of Agriculture. Reference to a company or product by name does not imply approval or recam- mendation of the product by the Department of Agriculture to the exclusion of others which may also be suitable.
F Z- 3 MM TUBE ,.,, PROJECTS THRU ,: ~! HOUSING ' '~;":~~HOLD DOW-'~-~-N JMODIFIEO TWL VARIABLE TEMPERATURE " : 2 ~ ' f f , :,~.~ ~,RIAN_/ ;..~,~:~.. DEWAR INSERT ,:~,:~,,;:,'~ :" ~MATCHING CAP _J ASSEMBLY~ TC LEADS ADAPTER RING .3 MM O.[).~ GLASS TUBING INSERT HOLDER (TEFLON)" ~[ CORK SEAI ~ Ox30 MM SHELL VIAL q GLASS ROD ION SHELL VIAL :OIL INSERT TC LEADS SNUG FIT ON 3 MM TUBING| PROBE ADAPTER HOUSING NITROGEN m m~m 90 )EWAR INSERT A EXIT NITROGEN i COIL INSERT 121) mm DETAILS I ' TEFLON BNC SPACER CONNECTOR t II mm Iq mm BOTTOM INSERT SEAL (TEFLON) "'"~ ~:~t-~ mm ~ UG FIT ON 'LL___:J--v- C01L INSERT
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3 rd - 1962 Pittsburgh Chair: Davi
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C 13 NMR Studies Using the Absorpti
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SPIN DECOUPLER by Daniel D. Elleman
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rd  - 1962 - ENC Conference

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