SUPPORT FACILITIES

Below is a description of additional facilities available in relation to P-T-t-D research at Syracuse University.

Sample Preparation Facilities

Crushing facilities consist of a jaw crusher and Bico disk mill. Samples are washed and initially separated on a Rodgers Gemini Table. Mineral separation facilities consist of a heavy liquid set-up within a series of fume hoods, Frantz LB-1 Barrier magnetic separator, shaker table, sieves etc. Grinding and polishing facilities include a Buehler dual wheel variable speed polisher/grinder.

Handling of radioactive samples (e.g., 40Ar/39Ar and fission track irradiation packages) is done in a small room accessible through the noble gas mass spectrometry lab. This room is equipped with a lead safe, a glove box, appropriate radiation monitoring equipment and radioactive waste disposal facilities (through Syracuse University's Environmental Health and Safety Office). 40Ar/39Ar irradiations are carried out at either Oregon State University or McMaster University. We use GA 1550 biotite, Alder Creek and Fish Canyon sanidine, and 77600hornblende as flux monitors. Interferences from Ca and K are monitored by analyzing irradiated optical grade CaF2 and vacuum fused K2SO4 which are included in every irradiation package.

Fission Track Laboratory

The fission track laboratory comprises two Nikon Optiphot2 microscopes. One scope is fitted with a computer controlled Kinetek automated stage and Calcomp digitizing tablet. The other scope is a polarizing scope used for sample characterization and thin section analyses. Interchangeable between these two scopes is a video system with color monitor and a 35 mm camera set-up. The video system is particularly useful for teaching petrography and demonstrating fission track counting procedures. We use the external detector method and zeta calibration on CN5 glass for fission track thermochronology. Samples are irradiated in the Oregon State University Nuclear Reactor.

In addition, housed within the fission track lab is an Olympus SZX12 stereo microscope, used primarily for grain selection for (U-Th)/He analyses. This scope has a magnification range of 7x to 288x and a variable-slit transmitted base for variable angle illumination to help locate inclusions within grains under polarizing light. Attached to this scope (and also interchangeable with the Nikon scopes) is a digital camera allowing images to be captured and stored on an adjacent G3 desktop computer with a 40GB external hard drive.

Quadrupole and He extraction line

Helium determinations for (U-Th)/He analyses are made using a dedicated quadrupole mass spectrometer and gas handling system. A bakeable Balzers quadrupole mass spectrometer designed for UHV operation is used to determine 4He abundances. The instrument is fitted with electron multiplier detectors, providing it with a wide dynamic range. It has a mass resolution of 84 and 40Ar sensitivity of 1.7 A/mbar on the multiplier and 7.8x10-4A/mbar on the Faraday. Similar to the Micromass 5400 extraction line, the He extraction line utilizes a double vacuum resistance-heated furnace. Furnace temperatures of >1500°C are attainable with this design, sufficient for outgassing accessory phases. Our 4He blanks are routinely on the order of <0.001 ncc. An all metal sample holder with a linear motion feedthrough allows multiple samples to be loaded for sequential analysis in the furnace. Each run (i.e., sample, blank, standard) takes ~45 minutes.

Helium outgassed from samples is purified in the all-metal extraction line previously pumped by a turbomolecular pump and a rotary backing pump. Gettering of active gasses is handled by small, standard SAES getters. Reservoirs containing a 3He spike and a 4He standard are attached to the line behind all metal pipettes. A temperature stabilized capacitance manometer was used to make accurate pressure measurements during the preparation of the spikes and the 4He pipette was cross-calibrated on Prof. Ken Farley's line at Caltech. The 4He pipette delivers 9.84 +0.08 ncc STP 4He per aliquot. A Janis cryogenic cold trap system is interchangeable between the He extraction line and the 5400 extraction line when required. Measurement of 4He is done by isotope dilution, using a 3He spike. We use Durango apatite as mineral standards. Measurement of U and Th concentrations are presently performed by solution ICPMS at CSIRO.

Thermal Ionization Mass Spectrometry

The TIMS lab is equipped with a Micromass Sector 54 thermal ionization mass spectrometer for the determination of Sr, Nd, Sm, Pb, and U isotopic ratios. The Sector 54 features a magnetic sector analyzer with 90 degree extended geometry ion optics giving a dispersion length of 54 cm, a high sensitivity ion source of ‘quick release’ plug-in design with nominal operating 8 KV accelerating voltage, 20 sample turret on which both single and triple filaments may be utilized, vacuum system incorporating one 330 l/s turbomolecular pump, two 30 l/s ion pumps on the flight tube and a titanium sublimation pump on the collector block, liquid nitrogen cold trap, Multi-2 collector assembly featuring 7 motorized Faraday cups and a Daly multiplier detector with ion counting. The TIMS lab also features a newly designed filament degas bench.

Sample preparation facilities include an adjacent Class 100 Clean lab with individual Laminar Flow HEPA filtered hoods, custom designed HEPA filtered drydown boxes, Millipore Milli-Q water purification system, Quartz sub boiling and Savillex PFA sub boiling distillation stills. A recent addition to the TIMS lab is a Milestone Ethos high temperature (300°C) microwave digestion system used to dissolve zircon.

Stable Isotope Ratio Mass Spectrometry

The SIRMS lab is equipped with a Finnigan MAT 252 stable isotope mass spectrometer system for the determination of H/D, 13C/12C, 15N/14N, 18O/16O, and 34S/32S. The MAT 252 features a magnetic sector analyzer with stigmatic focusing, 460 mm effective deflection radius for C/N/O/S, 180 mm effective magnetic deflection radius for H/D, 10 kV accelerating voltage, electron impact ionization source, variable ion source conductance for S, einzel lens optics, UHV conditions through all-metal gaskets, and MEMCO Faraday collector array. The MAT252 is interfaced with a fully automated Kiel III carbonate device used for the precise and accurate determination of C and O isotopic ratios in carbonates. The Kiel III features a 48 sample carousel, precise temperature control region in which the reservoir for orthophosphoric acid, acid dosing valves, and sample carousel are all contained. The Kiel III also features two independent reaction positions for high sample throughput. The MAT252 is also interfaced to a HDO II CO2/H2/H20 equilibrator device for waters which features a valve block assembly for 24 samples. The MAT252 is also equipped with a ConFlo II interface allowing for the continuous flow operation of the mass spectrometer. The MAT252 and associated interface equipment are all under computer control via Finnigan’s ISODAT software.

The SIRMS lab also features sample preparation equipment including a vacuum extraction line, Denver Instruments microbalance, Lindberg 1400 C muffle furnace, and a custom built Micromill for sub micron milling of carbonate from microfossils, skeletal material, stalagmites, etc. The Micromill features a Newport MM2000 motion control system. The Micromill is fully automated and controlled via National Instruments Labview operating system.

X-ray Analysis

The X-ray analysis laboratory is equipped with an ARL 8410 X-ray fluorescence Wavelength Dispersive Spectrometer (WDS) featuring a Varian OEG 76 Rh X-ray tube of end window design with a 127 micron Be window and Rh target. The x-ray tune is energized using a "Dry Power Supply" featuring high frequency switching, 0-70 kV voltage range, 0-100 mA current range and a maximum 3 kW output power. The spectrometer features a vacuum tank with 1 goniometer with sample handling, vacuum, and temperature control. The goniometer is a primary collimator + flat crystal + secondary collimator type, with mechanically separate crystal and detector drives and electronic control of the theta/ 2 theta relationship using the Moire fringe technique. The goniometer also features a flow proportional detector with P10 gas and a scintillation detector, as well as LiF, PET, GeIII, InSb, ADP, TLAP crystals. The sample handling system includes 8 coded cassettes for samples 45 mm in diameter and up to 30 mm thick. The ARL 8410 is capable of analyzing all elements in the periodic table except H, Li, Be, and all Noble Gases (He, Ne, Ar, Kr, Xe, Rn). The X-ray analysis laboratory is also equipped with a Phillips XRD outfitted with a standard Cu tube and a monochronometer.

Electron Microprobe Laboratory

The Earth Sciences Department recently acquired a JEOL JSM6300 Scanning Electron Microscope. This SEM is equipped with 3 wavelength dispersive detectors (WDS) and a Noran Voyager EDS, making the JSM6300 an electron probe X-ray microanalyzer. Image modes include secondary electron and backscattered electron modes. The JSM6300 has accelerating voltage capabilities between 0.2 to 30 kV, a magnification range up to 300,000x, an infrared chamber scope for continuous viewing. It is also equipped with a Eucentric goniometer specimen stage along for x=50 mm, y=70 mm, and z= 40 mm with a tilt range between —5 to 90 degrees and 360 degrees continuous rotation. We have a pending NSF EAR/IF proposal to upgrade the system and outfit the SEM with CL imaging capabilities.

Additional Facilities

Additional facilities available to SUNGIRL include:

 

Return to the SU Thermochronology homepage

Return to the SUNGIRL homepage