HANDHELD FTIR – BEST ON-SITE CHEMISTRY

ANALYSIS SOLUTION

Presented by: Dr. Yanqia Wang

Outline

Background of FTIR Spectrometry and Agilent Handheld

FTIR - TopScan 4300

Versatile sampling interfaces (Diamond/Ge ATR, Specular

Reflection, Grazing Angle Reflection and Diffuse

Reflection) to satisfy different applications.

Powerful and user-friendly software to assist easy data

collection and analysis qualitatively and quantitatively.

Excellent outcome from real applications.

Potential Applications

Infrared Light

Heat Motion of atoms and molecules IR radiation/absorption

Principles of IR Spectroscopy

• Most organic molecules absorb light in the infrared region to yield IR absorption spectra

• Absorption at certain frequencies or wavenumbers corresponds specifically to certain vibrations of functional groups

• Absorbance of the spectral features is associated with the concentration of the certain components

• Qualitative and Quantitative Characterization

FTIR Spectrometer

Moving

Mirror

Fixed Mirror

Reference

Laser IR Source

Laser

Detector

Sample

Cell

IR Detector

Key components of an FTIR spectrometer.

Smaller is Better

Computer Evolution

FTIR Evolution

1998 – Mini

Size:10 ¼” x 12” x 4 ½”

Weight: 10 lbs.

2002 – Midget

Size:4 ¼” x 2 ½” x 5 ¾”

Weight: 3.6 lbs

2007 – Micro Size:2 ½” x 2 ¾” x 4 ¼”

Weight: 1.9 lbs

Mobile FTIR (Thanks to Smaller Interferometer)

2013

Nano

Comparison Research vs Field FTIR Spectrometer

8

Source: Multiple vs Single

Laser: Gas Phase vs Solid State

Beam Splitter: Interchangeable vs Fixed

Alignment: Multi-adjustments vs Pin in place

Detector: Multiple vs Single

~4x scale

Trading Rules Number of Adjustments versus Alignment Tolerance

9

Perf

orm

ance

0

Alignment

•Maximum Adjustments

•Optimum Performance

•“Research” system

Perf

orm

ance

0

Alignment

•Optimum adjustments

•Stable Performance

•“Field” system

Agilent portable systems are designed to have stable performance. Small

changes in alignment have a minimal effect on performance.

Common Specifications Multiple Instruments from the same engine

Frequency range

– 5100 – 650 cm-1 (ZnSe)

– 7000 – 350 cm-1 (KBr)

Maximum Resolution

– 2 cm-1

Non-hygroscopic optics

– ZnSe beam splitter

Power

– AC or Onboard Lithium Ion Battery

Operating temperature

– 0⁰ to 50⁰ C

Humidity

– 95% non-condensing

RELIABLE: “From White Coats to Work Boots”

Where to find a Handheld FTIR?

• Parking lots, Mine pits, Workshops, Warehouses, wild field …

Anywhere and even a regular lab

Agilent Confidential

Moving Measurements From the Lab to the Field

Analysis on Location

Too big for lab / object can not be moved

Faster Time to Answer

Lab is too far / samples need to be sent away

Deployment of Routine Analysis Program

Non technical user can used field systems

Increase QBD (quality by design) effort

Cost savings

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Requirements for Field and Routine Use

Effective Performance

• Achieve required measurement limits

• Analytical performance still matters

Form Factor – Compact, Rugged, Portable, Versatile

• System needs to go where the sample is

• Frequent travel/inexperienced users - subjects it to shock and vibration

Correct Sampling Interfaces

• Little or no sample prep

• Versatility: Multiple uses and matrices

Ease of Use and Provide Answers

• Easy to understand, meaningful results

14

Handheld Opto-Chemical Instrumentation

Smart Phone

UV-Vis

Raman XRF LIBS

NIR QCL-MIR

Sci-Fi do-it-all

Light-absorption Based

Light-interaction (e.g. Scattering ,Emission) Based

FTIR

Advantages of Handheld FTIR over other Handheld

Systems

• FTIR can be used for both chemical qualification and quantitation

• Non-destructive

• Works for a wide variety of samples with versatile sampling

interfaces

• Abundant spectral database and method support.

• Less sample restriction (e.g. fluorescence interference for Raman)

• Safety (Laser, X-Ray)

Advantages of TopScan 4300 over Other Handheld

FTIR

• Really “Handheld”

• Truly Rugged

– Same optics that are used in our bench systems – not a

WATERED DOWN VERSION

– Can be used in any direction

– Permanently aligned optics (No “dynamic alignment” is

necessary)

• High Flexibility

• Optics/Sealed Desiccated Compartments

–No need to worry about KBr beam-splitters and desiccant

–No need to purge your system

Competitive

14 lbs

8.6” x 11.8”

Evolution of Handheld FTIR 4300

March 17, 2016

Confidentiality Label

18

Award Winning Design (TopScan 4300)

Agilent Confidential

http://www.brettcapron.com/agilent-4300-ftir/

Ergonomic Design

2KG, balanced Multi Functional

RFID Embedded Accessory

Battery or AC

Mobile and PC

Control

Robust and Graceful

4300 Handheld FTIR Overview The most powerful handheld FTIR ever developed

OVERVIEW

• Ergonomics

– ~4.5 lbs, balanced

• Engine + electronics ~60 in3

• Performance Optimized

• Great scan speed (5.6

scans/second@ 4 cm-1)

• Fast software response

MARKETS

•Expand existing markets

•Materials

•Energy

•Food

WHY WE WILL BE

SUCCESSFUL

Proven applications

Better ergonomics

Increased usability

Defend current market

position

Agilent Confidential

Handheld Models

Features 4300MCT 4300DTGS ExoScan 4100

Lightweight 2 kg 3.2 kg

Measurement Speed 5.6 scans/sec 2.3 scans/second

Software Response Every 0.3 sec Every 1 sec

Smart Sampling RFID None

Sample Interface Interchangeable Interchangeable

Docking Station Yes Yes

Battery Life 2+ hours 3 hours

SNR >4000:1 >3500:1

Resolution 4 cm-1 4 cm-1

Interferometer Nano Micro

Detector MCT DTGS

Battery Pair, Hot-swap Single

Agilent Confidential

Frequency Range 5500 – 1100 cm-1 5000 – 650 cm-1 5100 – 650 cm-1

DTGS

2.3 scans/sec

>3000:1

TopScan 4300 Advantages

for Field Measurement

Lighter weight, Balanced, Ergonomic

– 2 kg

Compact size

– Access to difficult sample locations

High performance

– Meets the needs of challenging applications

Integrated Computer

– Fast response for real time answers

Ease of use

– Straightforward application-specific software

– Microlab

March 17, 2016

Agilent Confidential

22

IR Sampling Techniques

Specular

Reflectance

Diffuse

Reflectance

Sample

Reflectance

(External) • Diffuse reflectance

accessory

• Specular reflectance

accessory

• Grazing angle

reflectance accessory

Sample

ATR Crystal

Reflectance

(Internal) • ATR

accessory

Other Types of

Accessories • Fiber optics

probe

• Photo-acoustic

spectroscopy

(PAS)

Path length

Io I1

Sample

Transmittance • Liquid cell

• Gas cell

• KBr pellet

technique

Bulk Surface Surface

Attenuated Total Reflectance (ATR)

Diamond/Ge ATR

• Surface contact required

• Solids or liquids

• Consistent path length

• Little or No sample Prep

Evanescent Wave ~ 2 um

Infrared Energy Path

Sample

Reflectance

Diffuse Reflectance Specular Reflectance

Handheld FTIR with Multiple Sample Interfaces

Spherical ATR

• ID of Solids or liquids

• Gross surface contamination

• Thick coating identification - paints

External Reflectance (45⁰)

• Metal and composite surfaces

• Surface oxidation, coating thickness and chemistry

• ID of thin coatings

Grazing Angle (~82⁰)

• Used for smooth metal surfaces

• Cleaning validation

• Trace contaminant identification

• Bonding applications

Diffuse Reflectance

• Rough samples

• Geology applications

• Heat damage applications

4300 Handheld FTIR - Sampling Flexibility

RFID:

• Easily change I/F’s in the

field

• RFID Identifier

• Auto-sets Gain in the

Field when changed

• Allows user to lock

methods according to

sampling interface

Sampling interfaces available:

• Diffuse reflectance

• External Reflectance

• Diamond ATR

• Ge ATR

• Grazing Angle Reflectance

Downward Looking Position

Diffuse Reflectance for Powders,

soils, and other complex sample

media

Upward Looking Position

Stages for External Ref, Grazing

Angle, D-ATR and Ge-ATR

sample interfaces

4300 Handheld FTIR - Instrument Stand

5500 Series FTIR

• Dedicated sampling interfaces

• Optimized for performance

• No alignment

• ZnSe Optics Only

How do I choose the right system for me?

March 17, 2016 29

Laboratory

or field

deployable

system?

Dedicated

analysis

or

flexibility? Flexibility Dedicated

Choice A:

Lab based system

Cary 630

• Interchangeable

sampling interfaces

• Auto Recognition

• No alignment

• KBr or ZnSe Optics

4500 Series FTIR

• Dedicated sampling interfaces

• Optimized for performance

• Battery or Mains line

• ZnSe Optics for portability

How do I choose the right system for me?

March 17, 2016 30

Laboratory

or field

deployable

system?

Sample

type:

NDT or

Liquids/

Powders NDT

Choice B:

Combined Use

System

4300 TopScan FTIR

• Interchangeable sampling interfaces

• ZnSe Optics

• Battery Operated

• Docking Station for Laboratory

Development work

How do I choose the right system for me?

31

Laboratory

or field

deployable

system?

How often

is it in the

field?

Choice C:

Field Use system

4100 Exoscan 4300 - DTGS 4300 - MCT

• Visually instruct users through collection

• User Levels

Administrator, Certification, Operator

• Methods

Data collection

Library search

Quantitative

• Results

Green, yellow, red display based on limits

• PC and Mobile

Full collection/ prediction on mobile

Sync. Between mobile and PC

Microlab PC – Method Driven Software

Microlab PC - Fast Data Collection

• The latest Microlab PC has

embedded a Quant module,

a Simple, guided methods

development package for

quantitative applications.

• Different Quant Algorithms

allows single/multiple-

component quantitations

– Simple Beer’s Law

– Classical Least Squares

– Inverse Least Squares

(Also known as Inverse

Beer’s Law, or Multiple

Linear Regression)

Microlab PC – Quant Module

• MicrolabPC component

formatting

• Microsoft Word Add-on

enables easy report

formatting

• Multiple template

function

• PDF generation

Microlab PC – Easy Report Generation

Infield Applications for Handheld 4300 • Materials

– Coatings

• Coating Identification

• Surface cleanliness and preparation

• Coating wear and weathering

– Composites

• Heat and UV Damage on Composites

• Composite Cure

– Polymers

• UV resistance and weathering

• Polymer ID.

• Energy

• Wind

– Heat damage, coating wear and composite

cure of wind blades

• Solar

– Coating performance, UV damage, Material ID

• Geology

• Ground Truth-ing

• Mineralogy

• Soil Science

• Food

• Incoming ID, Product Quality

Agilent Confidential

Handheld Application – Heat Damage Oxidation of Carbon Composite

Aircraft and other structures will increasingly be constructed from composite material

Composites are susceptible to heat and oxidative damage Heat or UV Damage In service or mfg damage

Chemical damage of the epoxy resin Prior to delamination

Infrared provides an effective non-destructive testing to detect heat damage

787-8

Composites Serve as Primary

Structural Material

Carbon sandwich

Carbon laminate

Other composites

Aluminum

Titanium

Carbon sandwich

Carbon laminate

Other composites

Aluminum

Titanium

CFRP

43%

Misc.

9%

Composites

50%

Aluminum

20%

Titanium

15%

Steel

10%

Other

5%

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0

0.02

0.04

0.06

0.08

0.1

0.12

0.14

Wavenumber

Ab

so

rba

nc

eNo damage

High damage

5990-7792EN_AppNote

Hand Held FTIR Surface Contamination Diffuse Reflectance and Grazing Angle

FTIR well suited to surface

contamination

Hydrocarbon and Silicone are strong

absorbers

Unique signal = positive ID of

contaminant

Different Sample Interfaces for

Aluminum and Carbon Fiber

Aluminum highly reflective

-> Grazing angle interface

Carbon fiber low reflectivity

-> Diffuse Reflectance

38

Soil Analysis by Handheld FTIR

- Soil Mid-IR signal can be correlated to key parameters (pH/Hydrogen, Electrical Conductivity, Extractable Al, Ca, Mg and Total Carbon and Nitrogen)

- Massive amount samples: time consuming and expensive

- Comparison between benchtop and mobile FTIR (PLS-Cross Validation predictions and comparisons)

39

Hand Held FTIR in Art Conservation Measurement of oxalates on paint

Beigan’s Chao-Tian Temple in Taiwan Vibrant red painted doors

Stained black

Soot? Algae growth?

Diffuse Reflection (Non-destructive)

Black covering most of door

Red spots where black wore off

Oxalates found on black areas Oxalates formed as a by-product of biological

growth

Oxalate formation and removal is a growing

area of art conservation

40

FTIR has been used for years in art

conservation

Typically microscopy

Small samples removed from

paintings for analysis

Potential Application: Ground-Zero Chemical ID

41

In 2015, a series of massive explosions

rocked Tian Jin, a harbor city in China.

Hundreds tons of different hazardous

chemicals on ground zero need to be

identified ASAP. Handheld FTIR is

believed to be the best solution

NaNO3

KNO3

NH4NO3

NaCN

Potential Application: Melamine/Urea Formaldehyde

Dinnerware ID

42

Plastic shatter-proof dinnerware has become

very popular in people’s life. Melamine

Formaldehyde dinnerware is widely used due

to its strength and heat-resistance.

While someone thinks cheaper Urea

Formaldehyde can do the “same” thing.

Melamine Formaldehyde

Fine for hot soup

Nothing hot

Summary

• Agilent Handheld FTIR provided a valid way to bring

spectrometers to the samples, enable fast and accurate

on-site or in-field FTIR analysis.

• Wide selection of sampling interfaces can meet the

challenges of different applications.

• Easy-using software ensure customer’s need for fast

data collection and qualification/quantitation

characterization

• The value of the handheld FTIR has been approved by

many successful applications.

March 17, 2016

Confidentiality Label

44

4300 Handheld FTIR Demonstration

https://www.youtube.com/watch?v=OVKg3s4GswU