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| The
picture above shows the lab after its first month of service, in 2002.
It is equipped with three fume hoods,
twin
solvent purification system, state-of-the art Schlenk lines and glove
boxes, in addition to all the basic
instrumentation
and glassware required by a synthetic lab.
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| The syntheses are normally performed using top of the line, mercury-free four port, double manifold Schlenk lines operating with prepurified argon. For the non-specialist, the vacuum is provided by an Edwards pump (bottom right) connected to the line through two traps cooled with liquid nitrogen (middle/top right). The ports (upper middle) have grease-free teflon valves. The vacuum (5 x 10-6 torr) is monitored continuously with a digital Pirani pressure gage (upper left). The argon circuit is equipped with an overpressure release oil valve (top left). | ||
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| Two glove-boxes operating with
argon facilitate the manipulation of sensitive
compounds under complete exclusion of air and moisture. One of them is
fitted with solid-state moisture
and oxygen detectors for the continuous monitoring of the atmosphere,
as well
as -35 ºC freezers for crystal growth and storage of thermally
sensitive
compounds. |
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The
third glove-box,
fitted with solid-state moisture and oxygen detectors and -35 ºC
freezer, is connected
with a Parstat 2273 potentiostat / galvanostat for conducting
electrochemical
measurements under strict exclusion of air and moisture. |
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| The
most powerful separation technique available to the synthetic chemist
is
chromatography. Separation of air sensitive compounds by column
chromatography
(left, Hanh mastering the ceremony) is certainly not a trivial
technique.
One fraction was collected, other four still on the column (right). |
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| A Varian 4000 ion trap GC-MS (gas chromatograph - mass spectrometer) equipped with direct insertion probe for MS measurements by-passing the separation column, as well as FID and MS detectors enables qualitative and quantitative analysis of complex samples. It has capability to run EI and +/-CI in internal and external modes, as well as MS/MS. | ||
| A three solvent double-column purification system
is expected to arrive at the end of February 2006 and extend the
capability of the existing two-solvent system. Its purpose is to
deliver safely high-purity dry and deoxygenated solvents for the daily
use. |
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| The routine 1H, 13C, 11B and 31P NMR spectra are collected on the two departmental 300 MHz Brucker instruments, while for more advanced measurements 300 and 400 MHz Brucker NMR spectrometers are used on a weekly basis. All NMR instruments are operated by graduate students. |