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Erich Heiden Sales Manager UV/Vis; µ-UV NMR Everything is possible to analyze with a UV/Vis systems
Erich Heiden
Sales Manager UV/Vis; µ-UV NMR
Everything is possible
to analyze with a UV/Vis systems
All kind of samples
•Liquid down to 0,5 µl
•Solid nearly all size
•Gases
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UV / Vis range 2014
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UV-Vis/µ-UV Product Portfolio - Focus Markets
Education
• SPEC 200
• Genesys
10/20
• NanoDrop lite
Research
• Evolution
200/300
• NanoDrop
8000
Analytical
• Evolution
200/300
• NanoDrop
2000
QA/QC
• Evolution
200/300
• Genesys
10/20
• SPEC200
• NanoDrop
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Spectronic 200
• Spectronic 200 visible spectrophotometer offers outstanding features and bold new styling.
• Four user selectable modes make it ideal for teaching, routine %T/A monitoring, concentration measurements or tailored applications.
• A CCD detector allows instant collection of sample spectra.
• The instrument supports USB data storage and PC connectivity.
NEW
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• Movie spectronic 200
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Xenon Light Source
• Xenon light source, on all UV-Vis models, is one of the most critical and unique features of this whole UV family
• 2 x 108 pulses - equivalent to 11,000 hours of operation, or five years typical life
• Produces no heat
• Xenon source peaks are used for calibration
• Why it makes a difference? • Convenience and cost savings
• No downtime during lamp changes
• Low temperature operation with no fan required – minimizes dust and fumes around the optics.
• Working I a glove box without heathing
• Higher intensity in UV – good for life science applications.
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Xenon Light Source – Cost of Ownership
In addition to technology and performance advantages, xenon offers a better
value.
Above calculations do not include down time and other difficult to measure
losses related to analytical equipment being down
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Genesys 10s UV/Vis spectrophotometers
• Dual beam
• 190 – 1100 nm
• Xenon lamp
• 5 + 1 automatic cell changer as standard
• 1.8 nm Resolution
• USB stick memory
• Internal or USB printer
• Additional Windows 7 64-bit software
• A lot of accessories
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• All GENESYS 10S UV-Visible instruments feature 1.8 nm SBW
• Offers better peak resolution
• Meets perceived international Pharmacopeia requirements
• Better Resolution and better sensitivity
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0.5
1
1.5
2
2.5
3
425 430 435 440 445 450 455 460 465 470 475
Wavelength
Ab
so
rba
nc
e
2nm
5nm
8nm
Spectra offset
for clarity
1.8nm Resolution in a low cost instrument UNIQUE
Effects of Spectral
Bandwidth (SBW) on
the ability of the
spectrophotometer to
resolve peaks (see
sample absorbance
nuances)
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A lot of Accessories and Software Options
Available PC Software:
VISIONlite, EnzLab, ColorCalc, MaterialsCalc
Liquid thermostatted
cell holders
Long path cell
holder
Solid sample
cell holder
Long path cylindrical
cell holder Test tube cell
holder
nanoCell Fiber optic probe Sipper Single cell Peltier Many cuvettes
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Evolution 200 New area in UV/Vis
• real double beam system
• 190 – 1100 nm wavelength range
• fast scanner 1.2000 nm/min with 0.2nm data rate
• Local and PC control with the same Software
• Xenon lamp
• Application Focused Beam Geometry
• 8x 80µl cells in the cell changer can be used
NEW
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Whole Range of Accessories
8-position, precision
linear cell changer for
use with 80µl cells
Sipper
8-Position, Peltier
controlled Cell Changer
Single Peltier
Mercury Calibration
Lamp
EP / USP Compliant
Validation Carousel
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• See movie evolution 200
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Evolution 300
• High performance in both -- sensitivity and reliability --
• A wide range of advanced applications
• Dual cell changer configuration
• Auto sampler connectivity with flexible rack geometry for all kind of test-tubes
• Largest sample compartment in the market
updated
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Optical Design of Evolution 300
Optics Quartz coated
optics for long
lasting
reflectivity
and cleaning without
damaging the
optical surface
Mercury Lamp Primary reference
standard, allows
seamless validation
and calibration of
the instrument
Light Source Xenon flash lamp
is only on when
taking measurements
extending its lifetime Slit Mechanism Photo-etched slits
for greater accuracy.
Stepper-motor
driven slit drive
with intelligent
optimization
Grating 1200 lines/mm,
240 nm blazed,
holographic grating,
for exceptional
stray light
performance
Micrometer Monochromator
Drive with Sliding Coupling Provides excellent accuracy,
reproducibility and minimizes
temperature effects
Chassis Rigid, cast-aluminum base with
optical mounts bolted directly onto
the base provides superior system
stability and reliable results
Detectors Silicon photodiodes for
extended wavelength
range to 1100 nm
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Accessories for all evolution 200/300
Research
• Rapid mix Kinetics
• Solids measurement – transmittance and reflectance
• DNA melting
• Routine
• Multi-cell changers
• Linear 8 Peltier
• Rotary 7 incl. 7x7
• Peltier heat/cool
• Recirculator heat/cool
• Sipper
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Evolution 300 specials
Evolution 300
fastest double beam
system for fast kinetics
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Dual Cell Changer Configuration
• 7 x 7 is perfect for kinetics studies where each sample must be compared to a unique blank
• The 7 x 7 sample-to-reference configuration is unique to the Evolution 300 spectrophotometers
• This 7 x 7 sampling configuration is also useful for highly variable samples; including allergy testing and human and plant tissue analyses
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NanoDrop
The Thermo Scientific NanoDrop 2000/2000c
Two models – NanoDrop 2000 & NanoDrop 2000c
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NanoDrop Family of Products
Small, simple, robust
Patented sample retention technology
All of the applications customers expect
Responsive, knowledgeable customer support
New
Improved lower wavelength monitoring capability
Expanded concentration ranges (>15,000 ng/ul dsDNA)
Smaller sample size capability for concentrated samples
Custom methods capability
Oligo Calculator, Units flexibility
Cuvette capability (Model 2000c)
NanoDrop 2000/2000c
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NanoDrop 2000c – Unique Built in Cuvette Capability
Pathlengths – 10,5,2,1 mm
Kinetics/time-based
measurements
Volatile samples
Cell Cultures (OD 600)
Lower concentration ranges
(0.4ng/ul dsDNA)
Heating (37 deg C)
Stirring
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Key Specifications
NanoDrop 2000/2000c
Min Sample Size: 0.5 uL
Measurement Time: < 5 seconds
Wavelength range: 190 – 840 nm
Path length: 1 mm (auto-ranging to .05 mm)
Absorbance Range: 0.002 – 300 (10 mm equivalent)
Concentration Range: 2 - 15,000 ng/ul (dsDNA)
Footprint: 14 x 20 cm
Weight: 2.0 kg
NanoDrop 2000c
Beam height: 8.5 mm
Heating: 37 ± 0.5°C
Stirring: 150 – 850 rpm
Lower detection limit: 0.4 ng/ul (dsDNA)
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• See movie NanoDrop 2000
Measuring of solid samples
in Reflexion / Transmission mode
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How do you use UV-Vis with solid samples?
• Anything that’s not totally black reflects some visible light
• Even if it is totally black, it may reflect in the UV or NIR.
• Traditional UV-Vis experiment – transmittance
• Shine light through sample
• some is absorbed, some is transmitted
• transmitted light determines the color seen
• Materials UV-Vis experiment - reflectance
• Bounce light off the sample
• some is absorbed, some is reflected
• reflected light determines the color seen
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Two Types of Transmittance
• Unscattered “Normal” transmittance
• Clear solutions
• Clear glasses
• Scattered/diffuse transmittance
• Suspensions
• Colloids
• Roughened or translucent
glass or plastic
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Two Types of Reflectance
• Specular Reflectance
• Mirror or gloss like reflectance
• Shiny surfaces
• Reflected angle = incident angle
• Diffuse/Lambertian Reflectance
• Reflected light goes everywhere
• Matte or rough surfaces
• Hemispherical reflectance
θ θIncident Reflected
Normal
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More Realistic…………..
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Markets – Normal Transmission – Optics
• Absorptive coatings/dopants for eye protection
• Sun glasses
• Ski goggles
• Pilot helmet visors
• Optical components
• Colored glasses & plastics for lighting
• Architectural glass
• Industrial glass
• Lighting gels
• Vehicle turn and brake signals
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Transmission measurement accessories
• Filter holder
• Solid sample holder
• Universal sample holder
• Variable angle transmission accessory (VATA)
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Testing for Sunglass Safety
• Europe & Australia/New Zealand Standards (EN 1836:2007 & AS/NZS 1067:2003 )
• Label for Protection Level
• 0 means 80 – 100% transmitting
• 1 means 43 – 80% transmitting (everyday sunglasses)
• 2 means 18 – 43% transmitting (dark sunglasses)
• 3 means 8 – 18% transmitting (glacier or desert goggles)
• 4 means 3 – 8% transmitting (welding goggles)
• Label for UV-A protection (315 – 380nm)
• Label for UV-B protection (280 – 315nm)
• Signal light recognition testing
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Thermo Scientific Sunglass Testing
• Evolution UV-vis
spectrophotometer
• VISIONlite MaterialsCalc
software
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Transmittance Calculation in VL MaterialsCalc
+Red Iridium is a Trademark of Oakley, Inc.
Oakley® +Red Iridium™ Sunglasses
Manufacturer Data
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Markets – Diffuse Transmission – Haze
• Plastic windows
• Plexiglass/Lucite/Perspex, etc.
• Vehicle lamp lenses
• Plastic (and glass) bottles
• Pharmaceutical bottles (highly regulated)
• Opaque bottles
• Milk bottles
• Soft drink bottles
• Storage containers
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Haze (ASTM D 1003-00)
• Haze is the percentage of transmitted light which, when passing through a sample, deviates from the incident beam by forward scattering. Lower haze values imply greater transparency.
• Haze is an important property when designing for a transparent application in which observers must be able to see inside or through a part easily and clearly. If a material has a high haze value, it will have decreased transparency – making it more difficult to see inside or behind the sample. A sample with a high haze value will still transmit light, but images may appear foggy or blurred.
• Typically, polycarbonate resins have a haze value of about 0.5 to 2.0%. Haze value ranges for other transparent materials are:
• Polystyrene: 0.1 to 3.0%
• Styrene acrylonitrile: 0.6 to 3.0%
• Polymethylmethacrylate: 1.0 to 3.0%
• Cellulose acetate: 0.5 to 5.0%
• Glass: 0 to 0.17%
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Haze Measurements on Plastic Film
Scattering effect
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UV Protection Fabrics
• What is UV Protection Factor?
• The Ultraviolet Protection Factor (or UPF) rating system measures the UV
protection provided by fabric
• It is very similar to the SPF rating system used for sunscreens
• For example: A garment with a UPF of 50 only allows 1/50th of the UV
radiation falling on the surface of the garment to pass through it.
In other words, it blocks 49/50ths or 98% of the UV radiation
• Who makes UPF measurements?
• Manufacturers of Sun Protection Fabric
• Manufacturers of Sun Protection Garments
• Independent testing facilities
• Government Regulatory Agencies (ASTM, ARPANSA, etc.)
• Target ALL fabric and clothing manufacturers
http://www.coolibar.com/upf-ratings.html
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UPF Regulations
• Australian/New Zealand Standard 4399
• Enforced by ARPANSA
• Uses raw fabric – easy to comply with.
• ASTM D 6544 - Voluntary
• ASTM D 6603 - Voluntary
• AATCC Method 183 – Voluntary
• Used for “Outdoor Research” brand products sold at REI.
• Requires 40 washes and wet as well as dry testing – more effort to comply with.
• In the US, while the FDA regulates sunscreens, there is presently no Federal program for sun protective garments
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Factors Affecting UPF Measurements
• Addition of chemicals such as UV absorbers or UV diffusers during the
manufacturing process
• weave -- tighter is better
• color -- darker is better
• weight -- heavier is better
• stretch -- less stretch is better
• wetness -- dry is better
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UPF Calculations
• Baseline measured with fluorescence filter
(UG-11) in place
• Fabric measured in taut but not stretched
condition
• Areas of different color are measured
independently
• Measurements taken with and against the
weave and averaged together
• Variation must be within specified statistical
limits in standard
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Diffuse Reflectance
• An ideal diffuse reflectance surface reflects and scatters light in all directions.
• Examples of excellent diffuse reflectors include
• matte paint
• unglazed ceramics
• packed powders
• etched metal surfaces
• Any surface that is made up of stabilized or compacted particles is likely to be a diffuse reflector
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Diffuse Reflectance Applications
• Analyze powders or crystals by
reflectance
• Paint or ink color
• Surface gloss or texture
• Electronic properties of solids
• Electronic properties of surface films
• Eliminates possible solvent effects
• E.g., Inorganic metal complexes subject to
solvent substitution for ligands in solution
• Analyze optical or microelectronic
materials by transmission or reflectance
• Quality control measurements to
determine product quality
• R&D for developing new materials
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Solid Sample Measurement – Diffuse Reflectance
• Integrating Spheres
• Turbid solutions
• Color
• Diffuse reflectance
• Praying Mantis
• Diffuse reflectance accessory
• Small samples, heating/cooling,
• Catalyst research
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External reflexion accessories for evolution 200 / 300
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Diffuse Reflectance Applications
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Comparison of Different Sunscreens
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Calculation in VL MaterialsCalc
SPF 50 Sunscreen with Broad Spectrum Protection
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Praying Mantis
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Praying Mantis Diffuse Reflectance Accessory
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Praying Mantis Diffuse Reflectance Accessory
• Diffuse Reflectance of powders and small samples
• Beam image at sample position ~ 3 mm diameter
• Optics are MgF2 coated mirrors
• Wavelength range ~ 190-1100 nm
• Rejects specula component of reflection
• Ideal for Inorganic chemists and solid state physics
researchers
• Works in Evolution 200/300 (190-1100 nm)
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Praying Mantis Diffuse Reflectance Accessory
• Sample mounts in special cup inside the accessory
• Small slices or flat faced chunks of sample can be laid
on top of the large cup
Large cup
Depth = 0.125 inch = 3.2 mm
Diameter = 0.42 inch = 10.5 mm
Volume = 0.277 cm3
Extra/spare - PN 268-828200 $310 (2007)
Small cup
Depth = 0.125 inch = 3.2 mm
Diameter = 0.125 inch = 3.2 mm
Volume = 0.026 cm3
Extra/spare - PN 268-828300 $310 (2007)
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Temp. and Atmosphere Controlled Reaction Chambers
• High Temperature Reaction Chamber
• Operates from high vacuum (10-6 torr) to 2-3 atmospheres
• Temperatures up to 600°C (under vacuum).
• Can be adapted for high-pressure operation (up to
500 psi) with a high-pressure dome assembly.
• Low Temperature Reaction Chamber
• Operates from high vacuum to 2-3 atmospheres and at temperatures from -150°C to 600°C (under vacuum).
• Three inlet/outlet ports for evacuating the cell and introducing gases.
• Made of chemically resistant 316 stainless steel.
• Quartz windows for full range UV-Vis spectra
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Praying Mantis Diffuse Reflectance Accessory
• Customer Applications
• Absorption edge calculations – find band gap in semi-
conductors
• Studying Surface plasmon resonance – analytical tool in
nano-science and trace gas/contaminant detector
technology
• In-situ catalysis studies
• Measurements under controlled atmosphere
• UV-Vis of molecules absorbed on a surface
• Measurements at elevated or reduced temperature
• Substituted/intercalated metals in minerals
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Praying Mantis Catalysis Systems
• Reflectance studies
• Cooking
• Build-up of carbon on the
surface
• Reduction of the surface
• Electronic structure of the
surface of the catalyst
Gas flows through or over catalyst bed
• Middle pipe is plumbed to underside of catalyst bed
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Praying Mantis Catalysis Systems
• Accessories
• High Pressure Dome
• VCO to Swagelock adaptor
• Evolution 300
• Especially in UV
• Easy to align
• Highest total energy throughput
• Evolution 600
• Good, but lower energy throughput than Evo300
• Harder to align and more sensitive to positioning changes
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It’s not just silicon wafers
• Many materials are semiconductors
• GaAs, InP, doped Si, GaInP
• Organic molecules and films
• Inorganic films
• Doped inorganic compounds
• Natural minerals (e.g. TiO2)
• Doped minerals
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Band Gap in Semiconductors
• Band Gap refers to the energy difference between two electronic levels
in a material.
• Valence Band
• Lower energy level. Electrons are stuck on individual atoms.
• Conduction Band.
• Higher energy level. Electrons move around the material freely
conduction band
valence band
band gap Energy
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Band Gap in Semiconductors
• Metal
• Band gap = zero
• Conductor
• Semiconductor
• Small band gap
• External influence such as applied
voltage or photon of correct energy can
promote electrons from valence to
conduction band
• Insulator
• Electrons cannot get into
conduction band
conduction band
valence band Energy
conduction band
valence band
Small band gap Energy
conduction band
valence band
Large band gap Energy
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Tauc Plot for Bandgap
Science and Technology of Advanced Materials 6 (2005) 11–17, Sakae Tanemura, Lei Miaoa, Wilfried Wunderlich, Masaki Tanemura,Yukimasa Mori, Shoichi Toh, Kenji Kaneko
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Specular Reflectance
• Specular Reflectance is the reflectance from a “mirror-like” or glossy surface
• Glossy paints have a higher proportion of specular reflection than matte paints
• If you can see a “reflection” in it, it has significant specular reflectance
• Specular reflectance measurements are performed on the Thermo VN Absolute Specular reflectance accessory (10°) and Relative Specular reflectance accessories at 8°, 15°,20°,30°,45°,60° & 85° angles of incidence
Reflected angle = Incident angle
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Solid Sample Measurement -- Specular
• Specular (mirror-like) Reflectance Accessories (SRAs)
• VeeMAX SRA – variable angle 30° – 80°
• Fixed angle SRAs (15°, 20°, 30°, 45°, 60°)
• 8° and grazing angle (85°) on kinematic baseplate
