Everything is possible to analyze with a UV/Vis systems · 7 Xenon Light Source •Xenon light...

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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

0

0.5

1

1.5

2

2.5

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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

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• Thanks for your interest!

•Questions ?

• More info from

• Erich.Heiden@thermofisher.com