Instrumentation Lab | Department of Chemistry

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Instrumentation Lab

The Chemistry Departmental Instrumentation Laboratory is located in Room 152 Chemistry Building.

UNT Department of Chemistry - Instrumentation Lab
Hours of operation are from 8:00 AM till 5:00 PM.
Director: Dr. Teresa Golden tgolden@unt.edu
Lab Manager: Dr. Jose Calderon josec@unt.edu

Services provided by the Departmental Instrumentation Lab:

The facility provides the Chemistry Department with modern instruments for the chemical analyses using the following techniques: Gas chromatography (FID and TCD detectors), Gas Chromatography-Mass Spectroscopy, HPLC, Fourier Transform Infrared Spectroscopy, UV-Visible Spectroscopy, Fluorescence Spectroscopy, and both Flame and Graphite Furnace Atomic Absorption Spectroscopy.

The lab manager, Jose Calderon, provides training and assistance in the use of the facility equipment.

Facilities and Equipment:

Cary Eclipse Fluorescence Spectrophotometer (located in room 152)

The Cary Eclipse is equipped with both standard single cell base holder and microplate reader accessory. The Cary Eclipse fluorescence spectrophotometer uses xenon flash lamp technology, plug-and-identify electronics and featured-packed, intuitive software. The Cary Eclipse is controlled by the Cary Eclipse Bio Pack software.

Features of the Cary Eclipse Fluorimeter include:

  • Collection mode can be fluorescence, phosphorescence or chemi/bio luminescence.
  • Detector collects 80 points/second and gets all the steady-state fluorescence kinetic data.
  • A phosphorescence data point is captured every microsecond.
  • The Eclipse's performance can be validated using the built-in instrument test software.

PerkinElmer Spectrum One FT-IR Spectrophotometer (located in room 152)

The FT-IR spectrophotometer is equipped with both transmission and ATR modes. It is configured to run in single-beam, ratio, or interferogram modes. FTIR Spectrometer is capable of data collection over a wavenumber range of 370-7800 cm-1 using a fast recovery deuterated triglycine sulfate detector with KBr splitting. The FT-IR spectrophotometer is controlled by Spectrum One HP software, which allows the user obtain qualitative and quantitative data from the method and generate custom reports.

Optical Performance:

  • Wavelength range 7,800-350 cm-1 Optimized KBr beamsplitter
  • Signal-to-noise 35,000:1 RMS 1.2 x 10-5 Abs
  • 7,000:1 peak-peak 6.2 x 10-5 Abs
  • (4 cm-1 spectral resolution, 5 second data collection time, room temperature, KBr optics, DTGS detector)
  • Wavelength accuracy Better than 0.1 cm-1 at 1,600 cm-1
  • (1 scan accumulation, 4 cm-1 spectral resolution, measured peak maxima deviation from peak position @ 3060.02 cm-1)

MIDAC FT/IR Spectrometer (located in room 152)

The spectrometer provides a full range of resolution, from 2cm-1 for routine analysis up to 0.5cm-1 for high resolution work such as gas analysis. All models are step selectable down to 32cm-1. The sample compartment is accessible from front side. The wavelength range is from 7,800 to 350 cm-1.

The instrument is controlled via the GRAMS/AI software which allows for standard data processing such as baseline correction (multi-point, polynomial fit), Peak fitting (Gaussian, Lorentzian, Voigt and other functions), Smoothing, Derivatives, Automatic spectral subtraction, and Spectral unit conversion.


8453 UV-Vis (located in room 152A)

Specifications 8453 UV-Visible Spectrophotometer:

  • Wavelength range - 190-1100 nm
  • Slit width - 1 nm
  • EP resolution test - >1.6 toluene in hexane, ratio abs. at 269 nm/266 nm
  • Stray light - <0.03 % at 340 nm (NaN02, ASTM)
    <0.05 % at 220 nm (Nal, ASTM)
    <1 % at 200 nm (KCI, EP)
  • Wavelength accuracy - <±0.5 nm - 0.5-second scan
    |<±0.2 nm (at 486.0 and 656.1 nm)
  • Wavelength reproducibility - <±0.02 nm - ten consecutive scans
  • Photometric noise - <0.0002 A - sixty 0.5-second scans at 0 A, 500 nm, r m s
  • Photometric stability - <0.001 A -at 0 A, 340 nm after 1-hour warm up, measured over 1 hour, every 5 seconds, constant ambient temperature.

Single cell holders:

  • Long path cell holder - rectangular and cylindrical cells with path lengths up to 100 mm and additional stops at 10, 20 and 50 mm.
  • Thermostatable cell holder - for operation in combination with a circulating-water bath, optional accessory for water-driven stirring with magnetic stirring bar for 10-mm cells.
  • Peltier thermostated cell holder - Fully controlled through software using GPIB interfacing, optional sample sensor for precise sample temperature, stirring with magnetic stirring bar for 10-mm cells (stirrer speed of 40 - 1000 rpm). Temperature range: 10 - 100 ° C (-10 to 80 °C relative to ambient), temperature accuracy: ± 0.2 °C (20 - 40 °C), ± 0.3 °C (0 - 20 °C, 40 - 60 °C), ± 0.5 °C (60 - 100 °C), temperature reproducibility: ± 0.1 °C at 0 - 60 °C, ± 0.2 °C at 60 °C. Build-in heat exchanger (stainless steel) for use with flow system to achieve thermal equilibrium faster
  • Standard cell holder - Quick and precise cell positioning of standard rectangular cells (12.5 mm quadratic base, 15 mm center height ); standard with all Agilent spectrophotometers

UV-VIS Spectrophotometer MultiSpec-1501 (located in room 152A)

The MultiSpec-1501 acquires spectra from 190 to 800 nm wavelength range.
Hyper-UV software, running under Windows® 98, controls the spectrometer. The user can obtain an array of different quantitative analyses including multiple linear regression, calibration curves, custom equations, color, and kinetics. Time course data can be displayed in 2-dimensional or 3-dimensional plots.

Hyper-UV Basic Functions:

  • Acquire Modes - Spectral measurement, Time Course measurement, and Photometric measurement.
  • Application Measurement Modes - Quantitative Analysis, Color, PLS, Kinetics, 2-D/3-D analysis.
  • Data Processing - Constant addition, subtraction, multiplication and division, absorbance/transmittance conversion, normalization, logarithm conversion, baseline correction, absorbance shift, index smoothing, smoothing, 1st and 2nd derivatives, data separation, data subtraction and addition, wave number/wavelength conversion, peak detection, peak area, differential spectrum, spectral division, spectral wavelength matching, spectral wavelength shifting, degree of spectrum matching, Kubelka Munk transformation.
  • Quantitative Analysis functions - Intensity reading, single-point calibration curve, multipoint calibration curve, peak height ratio/area ratio, enzyme activity, Michaelis-Menten Calculations, multiple linear regression analysis, PLS, custom equations and pass/fail indicators.

Specifications:

  • Measurement Wavelength Range 190.0nm - 800.0nm
  • Wavelength accuracy ± 1.0nm
  • Wavelength repeatability ± .01nm
  • Wavelength Scanning Time Minimum 0.1 sec (full wavelength range) Time Course mode
  • Measurement Time Approx. 1 sec (measurement start display, depends on PC)
  • Resolution < 3nm
  • Detector 512 element photodiode array
  • Element Resolution 1.5nm
  • Photometric Mode Single beam, multi-channel mode
  • Photometric Range Absorbance: -0.500 - 2.000 Abs Transmittance: 0.0 - 300.0%
  • Photometric Accuracy ± 0.005 Abs (at 1 Abs)
  • Photometric Repeatability ± 0.002 Abs (at 1 Abs)
  • Baseline Stability Within 0.001 Abs/h
  • Baseline Flatness ± 0.001 Abs
  • Noise Level 0.002 Abs
  • Light Source 20W halogen lamp, deuterium lamp
  • Sample Chamber 11.0 cm (l) x 23.0cm (w) x 10.5 cm (h) Open type, Coverless
  • Ambient Temperature Room temperature 15°C - 35°C
  • Basic Measurement Modes Spectral measurement, Time Course measurement
  • Application Measurement Modes Quantitative Analysis
  • Main Data Processing 4 arithmetic operations, smoothing, derivative, (1st, 2nd order),area calculation, peak detection, normalization, best fit

Thermo Scientific Finnigan HPLC SpectraSystem (located in room 152)

The system is equipped with a P2000 binary gradient pump, which allows for real-time pressure feedback control. The two solvent gradient solvent is provided with a two channel solvent input. The detection system uses the UV2000 detector equipped with a variable dual wavelength detector. The mobile phase is degassed via the SCM1000 degasser which continually removes dissolved gases.

The column is a THERMO ODS Hypersyl 15.0cm long x 4.6mm i.d. x 5micron particle size.

The HPLC system is controlled with the ChromQuest chromatography work station software, version 4.2.

Injections are made manually and injection loops of 10, 20, 50 and 100-microliter volumes are available.

Column can be thermally controlled from 5 °C above ambient to 85 °C.


Shimadzu HPLC System (located in room 152)

The HPLC system is equipped with a LPM 600 degasser, the CL-600 dual pump can receive up to 4 solvents for elution gradients, the SPD-6A UV spectrophotometric detector uses a single variable wavelength detector.

The column is a Discovery C18 5.0cm long x 4.6mm i.d. x 5micron particle size.

Injections are made manually using a 20-microliter injection loop.

Data is recorded via the Shimadzu CR501 Chromatopac integrator.


THERMO Finnigan Gas Chromatogram/Mass Spectrometer (located in room 152)

DSQ II Mass Spectrometer Specifications:

Electron Impact Ionization

  • 1 μL of a 1 pg/μL (OFN) in iso-octane produces the following minimum signal to noise for m/z 272 when scanning from 200 - 300 amu: 75:1 (70 L/s pump); 100:1 (250 L/s pump); 100:1 (200/200 L/s pump).

Positive Chemical Ionization

  • 1 μL of a 10 pg/μL benzophenone produces the following minimum signal to noise for m/z 183 when scanning from 200 - 300 amu: 10:1 (250 L/s pump); 10:1 (200/200 L/s pump).

TRACE GC Ultra™ Gas Chromatograph

  • Temperature programmable with seven ramps and eight levels, settable from 0.1- 120 °C/min
  • Eight independent, heated zones for injectors, detectors and auxiliary zones
  • Oven cool-down : 450 - 50 °C in under 250 seconds
  • Digital Pressure and Flow Control (DPFC) with gas saver
  • Maximum oven temperature 450 °C

Data System Software: XcaliburTM Data system, NIST library.


HP 5890 Series II Gas Chromatograph (located in room 152)

Split/Splitless Capillary:

  • Range to 400 °C in 1 °C increments
  • Back-pressure design permits independent adjustment of split flow rate without affecting column flow
  • Septum purge built in at 3 ml/min
  • Accepts columns up to 1.2-mm od
  • Multimode design includes split and splitless injection
  • Splitless purge time variable in 0.01-min elements

Flame Ionization Detector:

  • Range to 450 °C
  • Grounded jet and current limited design for operator safety
  • Push-button flame ignition
  • Sensitive:
    > 18 mCoul/gm carbon: nitrogen carrier, 0.018-in. id jet
    > 15 mCoul/gm carbon: helium carrier, 0.018-in. id jet
    > 22mCoul/gm carbon: nitrogen carrier, 0.018-in. id capillary jet
    > 18 mCoul/gm carbon: helium carrier, 0.018-in. id capillary jet
  • Minimum detectable: <5 pg carbon/sec, nitrogen carrier at S/N=2
  • Linear dynamic range: <+/- 10% over a 10 7 range with 0.018-in. id jet

Gas chromatograph data is obtained with the HP 6890 series integrator.


Shimadzu GC-14A Gas Chromatograph equipped with TCD Detector (located in room 152)

The GC system is fully programmable (time & temperature). Multi-linear programming capability can use up to a maximum of five staged increments within no more than time 655 minutes collection run time.

Data is recorded via the Shimadzu CR601 Chromatopac integrator.

The column is a 10% Carbowax 20 micron with 80/100 Chromosorb WAW support 6 ft long 1/8 inch in i.d.


Shimadzu GC-14A Gas Chromatograph equipped with FID Detector (located in room 152)

The GC system is fully programmable (time & temperature). Multi-linear programming capability can use up to a maximum of five staged increments within no more than time 655 minutes collection run time.

Data is recorded via the Shimadzu CR601 Chromatopac integrator.

The column is a 10% Carbowax 20 micron with 80/100 Chromosorb WAW support 6 ft long 1/8 inch in i.d.


S Series Atomic Absorption Spectrometer (located in room 152)

The spectrometer is equipped with GFS97 Graphite Furnace, GFS97 furnace auto-sampler, which can run up to 60 samples continuously using up to 6 standard solutions.

The optical system covers the range 185nm to 760nm as standard, with an optional wide range PMT up to 900nm. The spectrometer uses a standard 6 lamp auto-aligning turret (using data-coded or un-coded lamps, each with its own power supply) and Stockdale double beam system with Quad-Line deuterium background correction.

SOLAAR software controls and optimizes system parameters and control analyses.

Available elements for analyses include: Al, Bi, Ce, Ni, Na, Zn, Ag, Cd, Mg, Hg, As, K, Sn, Fe, Ca, Sb, Pb, Mg, Cu, and Fe.


PerkinElmer - AAnalyst 300 Atomic Flame Absorption Spectrometer (located in room 152)

The spectrophotometer can use either Acetylene-Air or Acetylene-Nitrous Oxide flames. The system is controlled with WinLab software. Analyses of the following metals can be performed at the ppm level; Pt, Pd, Cr, Ni, Zn, Al, Pb, Co, Mg, Mn, Fe, K, and Cu.


Buck Scientific 200A Flame Atomic Absorption Spectrophotometer (located in room 152)

Wavelength range is from 0 900 nm with an accuracy of 0.1 nm. Band pass windows can be adjusted to 0.2, 0.7, or 2.0 nm. Two interchangeable burner heads are available one is for air-acetylene flame and the other for nitrous oxide-acetylene flame. Data collection is obtained from the digital panel meter.

Available elements for analyses include: Al, Bi, Ce, Ni, Na, Zn, Ag, Cd, Mg, Hg, As, K, Sn, Fe, Ca, Sb, Pb, Mg, Cu, and Fe.


Ambient STM Burleigh Metris for Academic Teaching (located in room 152)


Facilities Mode of Operation

The laboratory provides easy access to sophisticated instruments. To request training or running of samples please complete the Instrumentation Lab Usage Request Form. The lab manager, Jose Calderon, provides training and assistance in the use of the facility equipment. In some cases, the Facility Manager will simply run the experiment for the investigator. In any case, the best course of action will be decided upon in consultation with the investigator.

At present, instrument time is offered on a first come first served basis to anyone in the UNT Chemistry Department. In the event that a particular instrument comes under heavy use, it may become necessary to prioritize access. In this event, instructional laboratory classes will have priority over all others.

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