Syracuse University Radiogenic Isotope Laboratory

The main components of the Scott Samson’s radiogenic isotope laboratory include a VG Sector 54 thermal ionization mass spectrometer equipped with seven Faraday detectors and an ion-counting Daly photomultiplier detector system, a custom-modified degas bench, a large class 100 clean laboratory, full mineral separation facilities, and most recently, a high pressure microwave digestion system, the Milestone Ethos plus. A

variety of different studies are pursued in the radiogenic isotope laboratory, but the current emphasis is on studies combining high precision U-Pb dating of accessory minerals (zircon, monazite, titanite, and xenotime) with Sm-Nd, Rb-Sr, and common Pb isotopic measurements. Lu-Hf isotopic studies are also being pursued now that chemical techniques to isolate Hf have been developed as standard part of our traditional U and Pb separation procedures of dissolved zircon. Each of the major components of the laboratory are described below.

Custom modified filament degas bench

The originally purchased VG degas bench, employing a Balzers turbo pump and Edwards roughing pumps, has undergone a series of dramatic modifications. The system now incorporates a custom fabricated all stainless housing (replacing the older bell jar system) equipped with a liquid nitrogen cold finger and with a combined ceramic and stainless steel filament black design that can be completely dismantled and cleaned with

nitric acid. As a result ultra-low Pb loading blanks can be consistently obtained (~ 0.1 picograms). This bench will continue to be used with the new TIMS.

Class 100 Clean Laboratory

The clean lab, originally constructed in 1990, has also undergone a series of significant upgrades. The primary upgrades include he installation of series of large class 10 laminar flow benches where all chemical separations occur. In addition, specially designed ‘clean boxes’ were constructed allowing samples to be dried down under continuous flow of HEPA-filtered air with Teflon beakers exposed to only Plexiglas and

Teflon material (i.e. all metal components are shielded). This simple, but elegant, design has been copied by a number of research s who have visited the SU radiogenic isotope laboratory.

The most recent upgrades include a new large, custom-made HEPA-filtered exhaust hood allowing for both class 10 chemistry and the exhausting of acid fumes, a new Millipore water purification system (replacing the previous aging Millipore system), and an overhaul of the electrical system feeding the clean laboratory. It is partly thanks to this

excellently designed clean laboratory that we are able to obtained full Pb procedural blanks of < 1 picogram.

Milestone Ethos Plus High pressure Microwave Digestion system

Scott Samson has been working with microwave digestion companies for the past decade to help develop a microwave system capable of reaching and maintaining very high (~ 280 °C) temperatures for several hours. Recently, the Milestone company developed a proto-type instrument designed to hold vessels at 270 – 280 °C for a minimum of two

hours with the goal of being able to completely dissolve zircon. Scott Samson worked with Milestone engineers and finally they were able to produce an instrument capable of digesting typical zircon within two hours. The normal current dissolution times for zircon at the SU laboratory (using a conventional oven and Parr metal jacket system) is between 48-60 hours. As a result of the successful demonstration a system was purchased. This is the only such ultra high-pressure microwave system in the USA. Its substantial advantage is a dramatic increase in sample throughput for digestion, the lowering of blanks due to

the reduced time of solutions in contact with vessels, and the ability to rapidly clean beakers at very high temperatures.

Petrographic Microscopes

Petrographic microscopes are used in the study of minerals and rocks in thin section. The Department owns several older Leitz student microscopes and research microscopes. Individual faculty members also have a number of research microscopes for use in their own labs. We also have a number of Universal stages and other peripheral devices for the older generation of Leitz scopes as well as a number of dedicated reflected light Leitz microscopes. The Department recently acquired 9 student and 1 teaching petrographic microscopes with funding generously donated by alumni. These Leica microscopes are used in laboratory sections of several graduate and undergraduate courses. They are also used for undergraduate and graduate research.

Electron Microscopy Laboratory

The Department’s 2 Scanning Electron Microscopes (JEOL JXA8600 and JSM733) provide excellent microbeam analytical capabilities. The JXA8600 is used for imaging and elemental analysis of minerals, fossils, and rocks. Image modes include secondary electron and backscattered electron modes. Upgrade of this instrument to include full electron probe X-ray microanalysis and cathode luminescence imaging capabilities was made possible with funding from NSF's Instrumentation & Facilities Program, and cost-shared by Syracuse University. This instrument is used regularly by undergraduate and graduate researchers as well as in various graduate and undergraduate courses.

Sample Preparation Facilities

The thin section laboratory is used in student and faculty research and has

recently been substantially upgraded. The Department has invested in two new Hilquist rock saws including a 24” slab saw, and a 7” trim saw. These saws complement a Buehler 3 phase 12” precision cut-off saw as well as a Buehler Dual-Belt sander acquired from Texaco/Chevron in 2003. We have refurbished an Ingram Thin Section Cutoff saw as

well as an Ingram thin section cup grinder. In June of 2007 we acquired two Buehler 8” Ecomet polisher/grinder units. In late 2008, Dr. Jeff Karson purchased a Struers 12” automated polisher/grinder for thick section, thin section, and 1” round mineral mounts. Rock crushing facilities consist of a jaw crusher and Bico disk mill. Samples are

washed and initially separated on a Rodgers Gemini Table The mineral separation and sample preparation facilities have recently been upgraded in order to increase the efficiency and quality of sample processing.

Mineral separation facilities consist of heavy liquid set-ups within several fume hoods, Frantz LB-1 Barrier magnetic separators, shaker table, sieves etc.

Beckman Spectrospan V Direct Current Plasma Spectrometer

The Beckman DCP, purchased in 1984, has the capability to analyze samples of water for concentrations of most metals from about 20 ug/L to over thousands of mg/L. This equipment is used by the Hydrology research group. The DCP, although one of the oldest pieces of equipment in the Department, still produces outstanding data and is maintained because analyses with it are unaffected by most spectral interferences associated with other plasma spectrometers, and the cost of operation is minimal. Waters analyzed in the lab range from rainwater to brines, and the DCP still offers the broadest capabilities for routine analyses at high quality.

Dionex ICS-2000 Ion Chromatograph

The ion chromatograph is used for analysis of major (and some minor) ions in environmental water samples (i.e. groundwater, soil water, stream water, precipitation, etc). For example, it can be used to measure Ca, Na, Mg, K, Cl, SO4, NO3, PO4, F, Br and a few others simultaneously. It has a detection limit on the order of 10-100 ppb, depending on the ion.

Merchantek MicroMill

The MicroMill is a microsampling device designed for high resolution milling to recover sample powder for chemical and isotopic analysis. The combination of submicron stage resolution and positional accuracy, real-time video observation and a custom designed software system allows for sampling of complex accretionary structures in skeletal and crystalline materials.

Fission Track Laboratory

The Fission Track Laboratory comprises two Nikon Optiphot2 scopes, one with a computer controlled Kinetek automated stage and Calcomp digitizing tablet used for fission track thermochronology and the other for petrography. 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 G4 desktop computer.

Micromass 5400 mass spectrometer and noble gas extraction line

The Micromass 5400 mass spectrometer and extraction line is used to determine the isotopic composition of noble gases extracted from minerals and rocks (e.g., 40Ar/39Ar analysis to determine the temperature-time evolution of minerals, and noble gas diffusion studies). The laboratory employs a custom furnace system, and an ultrahigh vacuum extraction line connected to a Micromass 5400 noble gas mass spectrometer. The mass

spectrometer has both faraday cup and ion-counting electron multiplier capabilities.

Quadrupole and He extraction line

Helium determinations for (U-Th)/He analyses and for He diffusion studies are made using a quadrupole mass spectrometer and gas handling system. A Balzers quadrupole mass spectrometer, fitted with electron multiplier detectors, is used to determine the 4He concentration. A double vacuum resistance-heated furnace can be used for outgassing minerals. Reservoirs containing a 3He spike and a 4He standard are attached to the line behind all metal, calibrated pipettes.

A 25 watt CO2 laser equipped with two-color IR probe is also available for outgassing minerals in the noble gas lab on both the 5400 and quadrupole mass spectrometers.

A custom built ArF excimer laser ablation system is used for in situ

outgassing of minerals in oriented thick sections and for in situ noble gas diffusion experiments. A Janis high-temperature, closed cycle cryogenic cold trap system is available for applications involving separation of noble gases.

HP Plotter

The HP large-format plotter was purchased by Scholz in 2000, with minor

research fund contributions from G. Seltzer and K.D. Nelson. Scholz now provides for 50% of cost of the service contract and supplies for the plotter, and other faculty members in the Department provide the remaining funds. This plotter is housed in the seismic facility space, although for many years has been used as a defacto Department facility.

Sedimentology Equipment

Dr. Chris Scholz has a complete sedimentology lab equipped for granulometry/textural/compositional studies, smear slide analysis, and coulometry studies. In addition there are Beckman-Coulter automated grain size analyzer: Model LS230, sediment X-radiography imaging and core epoxy impregnation systems and 3 walk-in refrigerated core storage facilities.

Major Seismic Laboratory Equipment

For the processing and analysis of seismic reflection data, Dr. Scholz’s lab

includes a complete seismic processing and interpretation facility. This consists of LINUX/PROMAX processing workstations, LANDMARK SEISWORKS/CAEX interpretation workstations, HP DesignJet Plotter; desktop mapping/GIS workstations with 18 kW UPS back-up power, assorted tape drives including AIT, 3480, 8 mm, and 4 mm tape drives. There is also a Chesapeake Technologies Sidescan Sonar Mosaic Workstation and assorted ARCGIS workstations.

Major Field Geophysical and Sediment Sampling Equipment and Vessels

Dr. Scholz also has an array of field geophysical and sediment sampling gear as well as boats for use in lacustrine studies. Most of this equipment is stored off-site. These items include the following:

48 Ch 1200 m Digital Hydroscience Technologies MCS streamer & acquisition system

48 Ch. 600 m Analog ITI Stealth array seismic streamer

OYO DAS-1 48-channel, Digital Seismic acquisition system

Chesapeak high-resolution seismic acquisition system

ELICS Delph2 high-res seismic/side-scan sonar acquisition system

Assorted airgun arrays, including BOLT, I/O sleeve guns

Two diesel-powered seismic air compressors (65 SCFM total)

ITI ST-5 single channel streamer

Teledyne 24 channel hi-res streamer (150 m, 300 m active sections)

Rossfelder deepwater electric vibracoring system (1200 m working depth)

Portable diesel generators

2 Trimble AG132 Differential GPS systems

Assorted portable GPS receivers

Assorted field communications equipment including two Iridium satellite phones with

data link, assorted VHF radios etc

40' modular research catamaran with VHF radios, radar, 11' rigid-body inflatable boat

24’ Zodiac Hurricane RIB Offshore Inflatable w/ 2x 130 HP engines

Edgetech CHIRP high resolution seismic system

Geopulse 1 kHz Boomer Seismic System

Knudsen 28 kHz Portable Digital Echosounder

Knudsen 200/200kHz Portable Sidescan Sonar System

Portable Seamac hydraulic-powered coring winch

Assorted grab samplers, and lightweight coring systems