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PATLAB succeeded to establish a laboratory with special modern high quality equipment with excellent technical performance as required by international and European Union norms. The laboratory with thi instrumentation is open for cooperation and collaboration with institutes, universities and economic agents for approach of technical and scientific research and development programs. Furthermore Master- and PhD-students from universities (with their supervisors) should feel welcome to use the well-equipped facilities in PATLAB with our expertise as basis for their studies. Currently PATLAB is equipped with the following instrumentation.

 

PATLAB has 5 high level advanced modern research FloPro process analyzer systems suitable for real-time monitoring and PID control. These FloPro instruments are the most versatile commercially available and can be used for advanced research and development projects and method development. As flow-based systems they are ideally suited for the activity domain of PATLAB which is based on research and development of process systems for intelligence interactive monitoring and control and small scale synthesis with advantages of the technology and applications in informatics, industries (oil, gas, petroleum, chemical, mining, pharmaceutical, food, beverages, textile e.g. clothes, surfactants, cosmetics, etc.), water, pollution, energy, environment, health, agriculture (fertilizers, animal feedstuffs, soil, herbicides, insecticides, farm products etc.), quality of food and beverages, biotechnologies, innovative products and processes, construction materials (bricks, cement, tiles, wooden materials, paints etc.), household appliances and consumer products, entertainment (ink, paper, polymer films, liquid crystals, electronic chemicals etc.), transport, space and security. They can also be used for routine, on-line, and field analyses applications.  With their modular design, based on state-of-the-art panel-mounted components, the instruments can easily and quickly be configured to perform essentially any flow-based methodology; or re-configured to change methodologies. A powerful, full-feature FlowZF software was designed specifically for flow-based systems by an expert in the field.

 

PATLAB is equipped with 1 FloPro and 4 mini FloPro research analyzer systems.

   

1. FLOPRO-FLOW PROCESS ANALYZER.

 

The picture gives a global view of the FloPro research analyzer system in PATLAB.

 

 

 

The FlowPro process analyzer is configured with two milliGAT pumps, 2 multiposition selection valves, a LED-based photometer, heated reactor, process robust computer and software

 

Below is a close-up view of the sampling part and process PID controller of PATLAB.

 

 

  

 

 

The picture below gives a view of the 4 flowpro mini-zone fluidic process analyzers in operation.

 

 

2. FLOPRO-MINI-ZONE FLUIDICS PROCESS ANALYZER. UV/Vis DETECTION.

 

This mini-FloPro is equipped with a milliGAT pump, 2 selection valves, heated reactor and plumbed for zone fluidics equipped to study a variety of chemistries. An Ocean Optics multi wavelength spectrometer is used for UV/vis detection. The system is controlled by a Laptop PC and FlowZF process development software.

 

The following picture shows the mini FloPro zone fluidics research process analyzer system with UV/Vis detection in operation in PATLAB.

 

 

3. FLOWPRO-MINI-ZONE FLUIDICS PROCESS ANALYZER. POTENTIOSTAT

     FOR AMPEROMETRIC DETECTION

 

This mini-FloPro is equipped with a milliGAT pump, 2 selection valves, a heated reactor and plumbed for zone fluidics and equipped to study a variety of chemistries. A bioanalytical Petit Ampere potentiostat is used for amperometric detection. The system is controlled by a Laptop PC and FlowZF process development software.

 

The following picture shows the mini FloPro zone fluidics research process analyzer system with amperometric detection in operation in PATLAB.

 

 

4. FLOWPRO-MINI-ZONE FLUIDICS PROCESS ANALYZER. FLUORESCENCE DETECTION.

 

This mini-FloPro is equipped with a milliGAT pump, 2 selection valves, a heated reactor and plumbed for zone fluidics equipped to study a variety of chemistries. An Ocean Optics detector is used for fluorescence detection. Laptop PC and process development software. The system is controlled by a Laptop PC and FlowZF process development software.

  

The following picture shows the mini FloPro zone fluidics research process analyzer system with fluorescence detection in operation in PATLAB.

 

 

5. FLOWPRO-MINI-ZONE FLUIDICS PROCESS ANALYZER.

    CHEMILUMINESCENCE DETECTION.

 

This mini-FloPro is equipped with a milliGAT pump, 2 selection valves, a heated reactor and plumbed for zone fluidics equipped to study a variety of chemistries.  Global FIA FireFly detector for chemiluminescence detection is used. The system is controlled by a Laptop PC and FlowZF process development software.

 

The following picture shows the mini FloPro zone fluidics research process analyzer system with fluorescence detection in operation in PATLAB.

 

 

  

 

6. QE65000 SCIENTIFIC-GRADE SPECTROMETER FOR FLUORESCENCE DETECTION.

 

 

 

PATLAB is equipped with a QE65000 Scientific-grade spectrometric setup for fluorescence detection as outlined above. The different components in PATLAB is illustrated and discussed below.

 

The HPX-2000 Xenon Light Source is a high-power, high-intensity source that is especially useful for fluorescence applications and for other applications where a high-intensity lamp is necessary. The 35-watt, short-arc lamp supplies a continuous spectrum from the UV through the NIR (185-2200 nm). The HPX-2000 features an integrated shutter that can be controlled via switch or TTL signal. Below is the spectral output of the HPX-2000 Xenon Light source.

 

 

The double LVF-UV linear variable filters inside the UV In-Line Filter Holder (shown above) is optimized by the researchers in PATLAB in such a way by shaping the excitation energy from the single broadband HPX-2000 Xenon Light Source. Only the excitation energy necessary to excite the specific fluorescent sample is allowed to pass through and unnecessary energy is blocked. This is reflected by a spectral band with Spectra Suite at a certain wavelength for the fluorescent sample.

 

 

The temperature-controlled cuvette holder outlined above with temperature control water bath and temperature control box is especially useful for fluorescence measurements that require stringent control of the samples temperature. Typical applications include protein and DNA thermodynamics, fluorophore characterization, enzyme kinetics and on-line thermocycling of biological particles.

 

 

The QE65000 Scientific-grade Spectrometer is a very sensitive spectrometer. The Hamamatsu FFT-CCD detector used in the QE65000 provides 90% quantum efficiency (defined as how efficiently a photon is converted to a photo-electron) has a detector range 200-1100 nm, and full scans to memory every 7 ms with USB 2.0 port as data transfer rate.

Technical Characteristics:-

Detector

Detector:

Hamamatsu S7031-1006

Detector range:

200-1100 nm

Pixels:

1024 x 58 (1044 x 64 total pixels); 24.6 m square size

Pixel size:

24.576 μm square size

Pixel well depth:

300,000 electrons/well; ~ 1.5 million electrons/column

Sensitivity:

22 electrons/count for all wavelengths; 250 nm: 26 photons/count

Quantum efficiency:

90% peak

Optical Bench

Design:

f/4, Symmetrical crossed Czerny-Turner

Focal length:

101.6 mm input and output

Entrance aperture:

5, 10, 25, 50, 100 or 200 m wide slits or fiber (no slit)

Grating options:

14 different grating options, UV through Shortwave NIR

HC-1 grating option:

provides 200-950 nm range

Detector collection lens option:

None

OFLV filter options:

OFLV-QE

Other bench filter options:

Longpass OF-1 filters

Collimating and focusing mirrors:

Standard only

UV enhanced window:

No

Fiber optic connector:

SMA 905 to 0.22 numerical aperture single-strand optical fiber

Spectroscopic

Wavelength range:

Grating dependent

Optical resolution:

~0.14-7.7 nm FWHM

Signal-to-noise ratio:

1000:1 (at full signal)

A/D resolution:

16 bit

Dark noise:

3 RMS counts

Dynamic range:

7.5 x 109 (system), 25000:1 for a single acquisition

Integration time:

8 ms to 15 minutes

Stray light:

<0.08% at 600 nm; 0.4% at 435 nm

Corrected linearity:

>99.8%

Electronics

Power consumption:

500 mA @ 5 VDC (no TE cooling); 3.5 A @ 5 VDC (with TE cooling)

Data transfer speed:

Full scans to memory every 7 ms with USB 2.0 port

Inputs/Outputs:

10 onboard digital user-programmable GPIOs (general purpose inputs/outputs)

Analog channels:

No

Auto nulling:

Yes

Breakout box compatibility:

Yes, the BREAKOUT BOX is a passive module that allows multiple interfaces to a spectrometer such as: external triggering, GPIO, light sources, RS-232 interface and analog input/output.

Trigger modes:

4 modes

Strobe functions:

No

Gated delay feature:

Yes

Connector:

30-pin connector

Power-up time:

<5 seconds

Dark current:

4000 e-/pixel/sec @ 25 C; 200 e-/pixel/sec @ 0 C

Computer

Operating systems:

Windows 2000/XP with USB port

Computer interfaces:

USB 2.0 @ 480 Mbps

Peripheral interfaces:

SPI (3-wire); I2C inter-integrated circuit

Temperature and Thermoelectric (TE) Cooling

Temperature limits:

-15 C to 50.0 C; no condensation

Set point:

Software controlled; lowest set point is 40 C below ambient, to -15 C

Stability

+/-0.1 C of set temperature in <2 minutes

The following Figure is an COMPUTER SCREEN illustration of experimental results obtained in PATLAB

with the SPECTRA SUITE software program. 

 

 

7. HR4000 HIGH-RESOLUTION SPECTROMETER.

 

There is a HR4000 high-resolution spectrometer in PATLAB. The setup of the instrument is given above and the different components illustrated and discussed below.

  

 

The DH-2000-BAL Deuterium Tungsten Halogen Light Source combines the continuous spectrum of deuterium and tungsten halogen light sources in a single optical path, producing a powerful, stable output from 215-2000 nm. The innovative DH-2000-BAL is the world's only balanced UV-NIR deuterium tungsten halogen source. The saturation and signal-to-noise problems associated with the D-alpha line in the deuterium source are eliminated by patterned dichroic filters as an innovation in light source technology to create the only combined-spectrum illumination source available. The DH-2000-BAL balances the intensity of the deuterium and tungsten halogen sources, producing a "smoother" spectrum across the entire wavelength range and eliminating problems associated with saturation.

  

The CUV-ALL-UV 4-way Cuvette Holder for 1-cm path length cuvettes is equipped with fiber optic couplings at each of four quartz f/2 collimating lenses, which couple to optical fibers to either read or illuminate the sample. When used with Ocean Optics modular spectrometers and light sources, CUV-ALL-UV Cuvette Holders can measure absorbance, fluorescence, scattering or any combination of these optical phenomena.

 

The HR4000 high resolution spectrometer has a 3648-element CCD-array detector from Toshiba that enables optical resolution as precise as 0.02 nm (FWHM). The HR4000 is responsive from 200-1100 nm, but the specific range and resolution depend on the grating and entrance slit choices. The detector has full scans to memory every 4 ms with a USB port as data transfer rate.

 

Technical Characteristics:-

Detector

Detector:

Toshiba TCD1304AP linear CCD array

Detector range:

200-1100 nm

Pixels:

3648 pixels

Pixel size:

8 μm x 200 μm

Pixel well depth:

~100,000 electrons

Sensitivity:

130 photons/count at 400 nm; 60 photons/count at 600 nm

Optical Bench

Design:

f/4, Symmetrical crossed Czerny-Turner

Focal length:

101.6 mm input and output

Entrance aperture:

5, 10, 25, 50, 100 or 200 m wide slits or fiber (no slit)

Grating options:

14 different gratings, UV through Shortwave NIR

HC-1 grating option:

provides 200-1050 nm range (best efficiency)

Detector collection lens option:

Yes, L4

OFLV filter options:

OFLV-200-1100

Other bench filter options:

Long pass OF-1 filters

Collimating and focusing mirrors:

Standard or SAG+UPG-HR

UV enhanced window:

Yes, UV4

Fiber optic connector:

SMA 905 to 0.22 numerical aperture single-strand optical fiber

Spectroscopic

Wavelength range:

Grating dependent

Optical resolution:

~0.02-8.4 nm FWHM

Signal-to-noise ratio:

300:1 (at full signal)

A/D resolution:

14 bit

Dark noise:

12 RMS counts

Dynamic range:

2 x 10^8 (system); 1300:1 for a single acquisition

Integration time:

3.8 ms to 10 seconds

Stray light:

<0.05% at 600 nm; <0.10% at 435 nm

Corrected linearity:

>99.8%

Electronics

Power consumption:

450 mA @ 5 VDC

Data transfer speed:

Full scans to memory every 4 ms with USB 2.0 port

Inputs/Outputs:

Yes, 10 onboard digital user-programmable GPIOs

Analog channels:

One 13-bit analog input; one 9-bit analog output

Auto nulling:

No

Breakout box compatibility:

Yes, the BREAKOUT BOX is a passive module that allows multiple interfaces to a spectrometer such as: external triggering, GPIO, light sources, RS-232 interface and analog input/output.

Trigger modes:

4 modes

Strobe functions:

Yes

Gated delay feature:

No

Connector:

30-pin connector

The following Figure is a COMPUTER SCREEN illustration of experimental results obtained in PATLAB with the SPECTRA SUITE software program.

  

8.  UNISCAN PG580 MINI-POTENTIOSTATS (2 UNITS)

 

 

PG580 setup in PATLAB

 

  

                                                              

              PG580 plus docking station                                Screen with some electrochemistry techniques

 

                                           

             Screen-printed sensor experiment                           Results of experiment in PATLAB

                                in PATLAB

 

There are  2 very well-equipped Uniscan mini-Potentiostats-Galvanostats in PATLAB. The PG580 is a high quality digital scanning potentiostat with excellent and very stable research laboratory performance. The response of the potentiostat is very fast making it an ideally suited device for real-time monitoring and control as required by PATLAB. The instrument has a friendly user configuration for advanced research innovative studies with remote control by a PC (labtop or benchtop) in a laboratory, as well as in-field on-site without PC control using an internal rechargeable battery. The research program of PATLAB with the PG580 includes various basic and applied research electrochemistry studies, surface electrochemistry studies with AFM/STM, flow-based real-time studies with PAT and NPAT, corrosion studies, studies on sensors, fuel cells research, electroanalytical and biomedical research.

 

Technical Characteristics:-

   ●  Battery Life: approximately 5 hours. Rechargeable NiMH cell.

   ●  PC Interface: Serial/USB

   ●  Display: Graphic LCD 160x100 pixels. Back light: Blue LED.

   ●  Processor: Dual 16 bit H8S@18MHz.

   ●  Data Acquisition: 16 Bits, > 100KHz.

   ●  Rise Time: 1V/sec. Into 1kΩ.

   ●  Maximum current: 20mA.

   ●  Maximum Measurable Current: 20mA.

   ●  Current Ranges: 1nA to 10mA in 8 decade ranges.

   ●  Current Measurement Resolution 16 bits.

   ●  Current Measurement Accuracy < 0.5%.

   ●  I/E Input Bias: < 10pA.

   ●  Applied Potential Range: 2Volts.

   ●  Applied Potential Accuracy: 0.2%.

   ●  Applied Potential Resolution: 16 bits (61V).

   ●  Compliance Voltage: 8Volts.

   ●  RE Input: >1011 Ohms║ 5pF

 

In PATLAB the experimental parameters and data display are implemented on a Labtop computer in powerful WindowsTM Software with full suite of electrochemical and corrosion techniques which provides full, detailed graphs, and filing of data objects. 

 

The UiEChemTM suite of electrochemical techniques includes:-

   ●  Cyclic and linear voltammetry.

   ●  Square wave voltammetry.

   ●  Normal and differential pulse voltammetry.

   ●  Chronoamperometry and chronopotentiometry

   ●  User definable experiments via macro programming.

 

The UiECorrTM suite of corrosion techniques includes:-

   ●  ECorr vs Time.

   ●  Potentiostatic polarization.

   ●  Galvanostatic polarization.

   ●  Potentiodynamic polarization.

   ●  Linear Polarization Resistance (LPR).

   ●  Zero Resistance Ammetry (ZRA).

   ●  Tafel.

 

  

9. AGILENT 5500 SERIES ATOMIC FORCE MICROSCOPY (AFM)/SCANNING

     PROBE MICROSCOPY (SPM)

 

PATLAB is equipped with an Agilent 5500 ideal multiple-user research system for atomic force microscopy (AFM) and scanning probe microscopy (SPM) with an electrochemical scanning microprobe microscopy (EC-SPM) to study the behaviour and kinetics of electrochemical micro- and nanoprobes in real time, Pico-TREC for simultaneous topography and recognition imaging with SPM for mapping target molecules on a sampling surface ideally suited for nanoelectrode sensor structuring and modifying, lithography and nanomanipulation with micro machining through force variations, nano patterning via probe bias and electrochemical etching, nano writing and nano modification via surface potential controlled deposition. The system is engineered for advanced research in electrochemistry, material science, polymer science, health and life sciences and biotechnology.

 

 

 

 

The full AFM/SPM setup is outlined above. Below is a close-up viewpoint of the AFM/SPM scanning part of the setup.

 

 

 

 

 

MAC (magnetic AC) Mode AFM

 

In atomic force microscopy (AFM), a sharp tip is scanned over a sample while maintaining a constant interatomic force between atoms on the end of the tip and atoms on the surface of interest. Early implementation of AFM employed the contact mode of operation in which the repulsive force experienced by the tip was measured by recording the cantilever deflection. Under ambient conditions, these repulsive forces range from a few to hundreds of nanonewtons. The forces between the AFM tip and the sample cause pressures large enough to induce distortion, remove portions of the sample from the substrate, and even damage the tip. By scanning in a liquid, capillary forces are reduced, which decreases the forces between the tip and sample by orders of magnitude. Other forces such as contact pressures, however, can still lead to dulling of the AFM tip and deformation of soft biological samples.

 

An effective method to reduce destructive lateral forces and to enhance sensitivity and reproducibility involves dynamic oscillation of the AFM tip while imaging. MAC mode AFM was developed [1] to reduce damage-causing vertical interactions between the sample and the AFM tip. In MAC mode, a cantilever coated with a paramagnetic film is oscillated directly by a solenoid located underneath or above the sample. The oscillation amplitude that is utilized to drive the cantilever in MAC mode is better controlled and can be much smaller than that used in other dynamic-force AFM modes (acoustic AC mode, tapping mode) [2]. Due to its high resolution and ability to image in fluid, MAC mode with AFM has gained acceptance in the fields of biophysics, structural biology and molecular biology. MAC mode AFM gives detailed structural information about DNA, RNA, proteins, lipids, live cells and sub-cellular structures in native environments.

 

[1] Han et al, APL 69 (1996), 4111 - 4114.

[2] Hansma et al, APL 64 (1994), 1738 - 1740.

 

 

TREC (Topography and Recognition Imaging)

 

PicoTREC is a relatively new technique which offers fast binding site mapping as well as topographic imaging across a surface with nanometer resolution. It has been successfully applied to several model receptor-ligand pairs and some live cell surfaces. PicoTREC has been used to simultaneously record two separate images, one that provides the topography of target molecules on a surface and another that displays a map of specifically recognized target molecules on a surface [3]. Using MAC mode, PicoTREC, and optimized AFM cantilevers, a ligand can be kept in close proximity to the surface, allowing efficient recognition and gentle interaction between tip and sample during scanning. PicoTREC resolves molecular recognition during the lateral scan by processing the asymmetric reduction of the oscillation amplitude. In this way, the locations of target molecules are easily determined from their coordinates on the recognition image. This method eliminates requirements for secondary reporter systems. For example, no fluorescence, radioactivity, or enzyme-linked detection schemes are needed when using PicoTREC. Furthermore, the system is extremely sensitive, since single molecule interactions are readily detected. PicoTREC can be used for nanometer-scale epitope mapping of biomolecules, to localize receptor sites during biological processes, or to expedite force spectroscopy studies on areas of interest [4].

 

[3] Stroh et al, PNAS 101 (2004), 12503 - 12507.

[4] Kada et al, Nanotoday 3 (2008), 12 - 19.

 

10. RESEARCH UV-VIS-NIR SPECTROPHOTOMETER

 

 

PATLAB has a Shimadzu 3600 UV-VIS-NIR spectrometer. The spectrophotometer is equipped with 3 detectors: a PMT detector (photomultiplier tube) for the ultraviolet and visible regions, and InGaAs and PbS detectors for near infrared region. The InGaAs detector bridges the gap between the PMT - PbS switching wavelength where sensitivity is typically low to ensure high sensitivity over the entire measurement wavelength range with <0.00003 Abs noise at 1500 nm.

 

Ultra-low stray light (0.00005% or less at 340 nm) is achieved at high resolution (highest resolution 0.1 nm)

with the high performance double monochromator,. The instrument has a measurement wavelength range of 185 - 3300 nm allowing measurement over a wide range including the ultraviolet, visible and near infrared regions. This allows spectroscopic analysis in a wide variety of fields.

 

Technical Characteristics:-

Wavelength range 185nm - 3300nm
Spectral Bandwidth 8 steps in ultraviolet/visible region 0.1, 0.2, 0.5, 1, 2, 3, 5, 8 nm
10 steps in near-infrared region 0.2, 0.5, 1, 2, 3, 5, 8, 12, 20, 32 nm
Resolution 0.1 nm
Sampling Pitch 0.01 - 5 nm
Wavelength accuracy UV/VIS region: 0.2 nm NIR region: 0. 8 nm
Wavelength repeatability UV/VIS region: less than 0.08 nm NIR region: less than 0.32 nm
Stray light < 0.00008% (220 nm, NaI)
< 0.00005% (340 nm, NaNO2)
< 0.0005% (1420 nm, H2O)
< 0.005% (2365 nm, CHCl3)
Photometric range -6 to 6 Abs
Noise 0.00005 Abs or less (500 nm), 0.00008 Abs or less (900 nm), 0.00003 Abs or less (1500 nm)
Slit width 2nm, RMS value at 1 sec. response
Photometric System Double beam

 

11. CYBERSCAN PCD 6500 pH/ION/CONDUCTIVITY/DO MULTIMETER.

 

                                                     

                   A Cyberscan multimeter setup                                        Cyberscan in PATLAB

 

 

                                          

A 5 Analyte multimeter setup in Patlab.                               The back panel of the multimeter with

The 5 green points on top of the Figure                                                  some connections.

                give the active sites.

 

The Cyberscan PCD 6500 pH/Ion/Conductivity/Dissolved Oxygen (DO) multimeter in PATLAB measures and views up to four parameters at the same time with no cross-channel reference. It is a CE-Driven Full-Colour Touchscreen 21 CFR Part 11-compliant Bench meter with a real-time on-screen multichannel, single channel or graphical analysis functions to give quick, convenient analysis of data with advanced, extensive communication capabilities with USB. The Cyberscan multimeter features very well into the research program of PATLAB on research projects for water quality testing, sewage treatment, waste water management, food processing, industrial process control, pharmaceutical production, health care, paper and pulp processing and chemical industries.

 

Technical Characteristics:-

Product Specification

Description

pH Range

-2.000 to 20.000 pH

Resolution & Accuracy

0.1/0.01/0.001 pH & 0.002 pH

mV Range

-1800 to +1800 mV

Resolution & Accuracy

0.1 mV & 0.1 mV

Ion Concentration Range

1 x 10-7 to 9.99 x 1010

Resolution & Accuracy

4 sig. figures & 0.17n%

DO Range

0 to 60 ppm, 0 to 600%

Resolution & Accuracy

0.01/0.10% & 0.1% + 1 LSD

Conductivity Range

0 to 500 mS/cm

Resistivity Range

3 ohm cm to 100 megohm cm

Salinity Range

0 to 90 ppt

Accuracy

0.5% full scale + 1 LSD

Cell Constant

0.1, 1.0, 10.0

Temperature Range

-5.0 to 105.0 C (Meter)

Resolution & Accuracy

0.1 C & 0.2 C

No. of pH Calibration Points

Up to 5

pH Buffer Options

USA: 2, 4, 7, 10, 12
NIST: 1.68, 4.01. 6.86, 9.18, 12.45
Euro: 1, 3, 6, 8, 10, 12 

No. of Ion Calibration Points 

5

Incremental methods

KA, KS, AA, AS

Temperature Compensation

Automatic / Manual (0 to 100 C)

DO Testing

5-day BOD, OUR and SOUR testing

Automatic Barometric Pressure Compensation

450 to 825 mmHg

Memory

10,000 Data Sets with Date/Time stamping

Programmable data storage/output

On stable, time and manual

Output

USB, IRDA, RS232C

Print Interval

3 to 86400 sec

Electrode Input

FET (solid-state non-glass) or Glass pH electrode

Display

640x480 digit LCD

Power

9VDC, 3.3A center negative