1. Dynamic Vapor Sorption (DVS)
SMS Application Science Team
Surface Measurement Systems

2. Overview Dynamic Vapour Sorption Technique
Comparison with other techniques
Basic information obtained through DVS
DVS Instruments by SMS
Applications/Markets
Unique Sales points
Competition
Conclusions

3. I How the Dynamic Vapour Sorption (DVS) Technique works

4. How the DVS Technique works
Balance
Temperature controlled environment
Sample on one side of balance

5. How the DVS Technique works
Sample sorbs water  weight changes
Controlled inflow of water vapour (humidity)
Balance

6. How the DVS Technique works
Sample sorbs water  weight changes
Controlled inflow of water vapour (humidity)
Balance
Time
Relative Humidity
Weight

7. How the DVS Technique works
Sample sorbs water  weight changes
Controlled inflow of water vapour (humidity)
Balance
Time
Relative Humidity
Weight

8. How the DVS Technique works
Sample sorbs water  weight changes
Controlled inflow of water vapour (humidity)
Balance
Time
Temperature
Weight

9. II How do Dynamic Vapour Sorption (DVS) compares to the Static Gravimetric Techniques

10. How DVS compares to Static Gravimetric Technique
ASTM E96: “Standard Test Method for Water Vapor Transmission of Materials“
ASTM D3201 / D3201M – 13
ASTM C1104/C1104M-13a
...and several others

11. Regulatory Requirement:
DVS technique recognised standard for characterising water-solid sorption interactions under Chapter 1241 of the American USP and the European Pharmacopoeia (Ph. Eur. Draft)
DVS technique soon to be ‘Japanese Standard’ for characterising water-solid interactions

12. Other (but old) Methods
Majority are for measuring moisture content and not full isotherm
Loss on Drying (LOD)
Sample is weighed, heated and reweighed
Risk of contamination, sample loss and human error
Karl Fischer titration
Classic titration method
Determines water only and not the volatile substances
Water has to be accessible and easily brought into methanol solution
Many substances, e.g. foods release water slowly and with difficulty
Destructive method i.e. samples can not be used for further analysis
Jar Method (Static gravimetric method)
Different jars for different %RH levels
Slow experiments, labour intensive
Large amount of sample is required
High errors

13. Jar Method (static method)
Need many of them: each one for a different relative humidity (RH) level
DVS (dynamic sorption)
Just one instrument can cope with all relative humidity levels

14. DVS (dynamic sorption)
Jar Method (static sorption)
DVS (dynamic sorption)
Needs 1 to 10 milligrams of sample: thanks to high sensivity microbalance (0.1 µg)
Needs 1 to 10 grams of sample

15. DVS (dynamic sorption)
Jar Method (static sorption)
DVS (dynamic sorption)
Very slow achievement of equilibrium: only brownian motion transports gases
Fast equilibrium due to optimized flow of gas + vapours (up to 200 ml/min)

16. DVS (dynamic sorption)
Jar Method (static sorption)
DVS (dynamic sorption)
Start DVS experiment
Finish DVS experiment
Can take weeks or months for a single data point
Can take less than a day for the whole experiment

17. Jar Method (static sorption) DVS (dynamic sorption)
6000 minutes =
4.2 days for full cycle
300 days for a single equilibrium data point
minutes
Need to remove sample from desiccator for weighting every time: risk of contamination or sample loss
Sample is constantly weighted throughout the experiment: no contamination or loss of sample

18. DVS (dynamic sorption)
Jar Method (static sorption)
DVS (dynamic sorption)
Mass uptake
Mass uptake
Relative humidity (RH)
Relative humidity (RH)
Usually only the sorption curve is measured, not registering the desorption curve nor any possible hysteresis involved
Can register sorption and desorption, obtaining more information in less time: eg fast kinetics or morphology changes

19. Basic Information Provided by the DVS:
III
Basic Information Provided by the DVS:
Kinetics & Isotherm

20. DVS – Kinetics of Moisture Sorption of Rice Starch
Drying
Sorption
Desorption
First cycle
Second cycle

21. DVS- Rice Starch Isotherms
Back to 0  reversible
Hysteresis
Point: from last 3-5 datapoints of each humidity step
Desorption
Sorption

22. DVS Instruments by Surface Measurement SystemsIV
DVS Instruments by Surface Measurement Systems

23. DVS Introduction Fully automatic sorption instrument
Dynamic gravimetric Vapor Sorption (DVS)
Fully automatic sorption instrument
Fast equilibrium: significantly improved kinetics over static sorption systems
SMS pioneer in vapor sorption technology
SMS UltraBalance
Up to 0.1 µg sensitivity
Allows use of small samples 1-10 mg
Unrivaled long-term baseline stability
‘Real-world’ conditions
Wide range of temperatures: measurement and preheat conditions
Wide range of measurement pressures: atmospheric down to 10-6 Torr (DVS-vacuum)
Wide range of vapors: water and organic vapors

24. DVS Models Summary Water vapor only 20-40 °C Small footprint
Water + Organic Vapors
5-60 °C
Camera and Raman Options
Sample preheat to 150 °C
10-6 Torr to Atmospheric
20-70 °C
Water + Organic Vapors
Gases
Competitive sorption
Sample preheat to 400 °C
Same as Advantage
20 – 85 °C

25. DVS in brief Dynamic Flowing Gas System (200 ml/min)
Fast Equilibrium due to optimised mass transport
High sensitivity Ultra-Microbalance (0.1 µg)
Allows small sample to be used (1 to 10 mg)
Fast equilibrium – 10 point isotherm in ~ 24 hours
Electronic Mass Flow Controllers - Mix Saturated (100%RH) and Dry (0%RH) Carrier Gas Flows.
Single Temperature Zone – Ensures Stable Humidities Throughout the System.
Symmetrical Design – Excellent Baseline and Minimal Gas Buoyancy Effects.
Mini RH Probe (5mm dia.) - Humidity Measured Next to Sample.
No PID Control on RH Probe – Excellent Long Term Reproducibility (Better than 1%RH over many years)

26. DVS – Water Sorption
Water-solid interactions important for wide range of industries:
Food
Pharma
Proteins
Fuel cells
Accurately determining water sorption isotherms critical for proper development and storage of these materials
Packaging
High energy materials
Personal care
Textiles
Building materials
Agriculture

27. V
DVS Applications

28. DVS Analysis Suite Standard Advanced Isotherm Suite
The widest range of isotherm models available in a single suite.
Automatic best fit selection.
Chart and plot options.
Automatic report summary generation.
Standard
Plot Manager
Isotherm
Baseline Correction
Vapor Content Offset
Salt validation calibration
Partial pressure check
Drift noise check
Method report
Configurations
Advanced
Spreading pressure
BET isotherm
Heat of sorption
Diffusion
Activation energy of diffusion
Knudsen vapor pressure
Iso activity plot
Amorphous content
Permeability
Database
Isotherm Suite
BET
Guggenheim Anderson DeBoer
Double Freundlich
Dubinin Radushkevich
Micropore distribution
Mesopore distribution
Reference
Langmuir
Alternative
Young & Nelson

29. DVS Applications Pharmaceutical
Applications/Examples
DVS Applications Pharmaceutical
Important areas of interest include:
Preformulation - Stability Testing of Active Salt Complexes.
Hydrate/Solvate formation
Formulation - Excipients / Formulations.
Characterization of Amorphous Content in Pharmaceutical Powders.
Moisture Induced Morphology Changes.
Packaging – coating. Tablet moisture, barriers, Blister packs/desiccants

30. Pharmaceutical target groups
#1 market for SMS DVS instruments (~50%)
SMS DVS instruments used in every major pharmaceutical company world-wide
Formulation or preformulation groups
Materials characterization groups
Contract Research Organizations (CRO’s)
Pharma excipient suppliers
Drug delivery companies
Strong university sales potential: physical pharmacy groups
Animal health divisions

31. DVS Applications Personal Care
Applications/Examples
DVS Applications Personal Care
Important areas of interest include:
Hair: moisture retention with different treatments (i.e. shampoo, conditioner)
Skin: moisture retention/drying with different treatments
Contact Lens: drying of films
Super Absorbent Polymers (i.e. diapers)

32. Personal Care Market/Applications
Large, multi-national personal care companies
Personal care divisions of pharma companies
Personal care Tier 1 suppliers
Research Institutes
Cosmetics

33. DVS Applications Foods
Applications/Examples
DVS Applications Foods
Moisture induced morphology changes in food ingredients and products.
Stability of Food Ingredients & shelf life – e.g. Unstable amorphous moisture behavior.
Rapid Isotherms for Food Ingredients – e.g. Starches, Celluloses, Sugars
Moisture Adsorption/absorption/expulsion.
Diffusion in Food Packaging Materials.
Caking of powders
Flavor-Fragrance release
Flavor-Matrix interactions
Agriculture, seeds, fertilizers, etc

34. Food-Flavor Market/Applications
Large, multi-national food companies
Gum/Confectionary
Flavor and fragrance companies
University research groups
Pet care/pet food
National government labs

35. DVS Applications Packaging
Applications/Examples
DVS Applications Packaging
Materials applications for packaging films and materials:
Pill Capsules and Blister Packs
Electronics Components
Packaging of Foodstuffs
Type of measurements:
Permeability of Real Packages
Calculation of Diffusion Constants

36. Other Market/Applications
Applications/Examples
Other Market/Applications
Fuel Cell Membranes
Water uptake and diffusion
Gas Diffusion Layer and Proton Exchange Membrane
Filtration
Selective filtration
Zeolite, activated carbons, molecular sieves
Tobacco
Water sorption on raw materials
‘Selective’ filtration of smoke components
Building Materials
Moisture sorption behavior of cements
Moisture sorption/diffusion in wood and wood composites
Preservation – storage and compatibility of historical artifacts

37. Other Market/Applications
Electronics/Adhesives
85 °C/85% RH is standard testing condition
Diffusion in electronic sealants
Defense labs
Storage of ‘high energy’ materials
Sorption of chemical agents on various materials
Personal protection and selective filtration of chemical agents
Polymers
Solvent-solid interactions
Vapor flux and diffusion measurements
Minerals/Fillers
Water sorption on carbon black
Wettability of minerals (i.e. floatation)
Wettability of shale
Adsorption research
Porous materials sorption properties
Catalysts, CO2 capture, Methanol adsorption, water sorption at subtamospheric conditions

38. VI
Unique Selling points

39. Sales Points – DVS Hardware DVS – Key Design Features
SMS UltraBalance – designed and developed by SMS; resolution down to 0.1 μg; masses up to 5g; unrivalled long-term baseline stability
High Resolution Electronic Mass Flow Controllers - Mix Saturated (100%RH) and Dry (0%RH) Carrier Gas Flows; allows for RH steps as low as 0.2% RH.
Single Temperature Vapor Generation and Delivery Zone – Ensures Stable Humidities Throughout the System.
‘True Zero’ RH – ensure 0%RH and complete drying of samples
Measure both water and organic vapor concentrations in real time – competitors only ‘predict’ organic vapor concentration

40. Sales Points - Scientific Support
SMS Leaders in Vapor Sorption Instruments
Making DVS since 1991
First to have organics, video, and Raman options
Dedicated Application Science Group
Lab in Allentown, Pennsylvania and London, UK
8+ PhD Scientists at SMS
Over 90 combined years of experience with vapor sorption instrumentation and applications
Scientific support for lifetime of instrument

41. VIII
Conclusions about DVS

42. Expanding the DVS Technique
Conclusions
Expanding the DVS Technique
The ability to use organic vapours  opens other applications for the DVS technique with building material.
The DVS-Advantage instrument also has the ability to couple in-situ spectroscopy (Raman and/or Near-IR) with the gravimetric sorption measurements. This can elucidate more subtle structural changes in the material (i.e. polymer rearrangement, hydrate formation, polymorph identification or hydrogen bonding).
The DVS-Advantage can also couple an in-situ video microscopy. This allows for the investigation of vapour-induced colour change, swelling or phase changes.

43. Conclusions Conclusions
The DVS Technique is a very fast one compared to older gravimetric methods
The DVS obtains very accurate and reliable results
It is suitable to study many types of materials, not only building materials
Obtains easily sorption and desorption isotherms
Can be used to study other phenomena, like permeability, diffusion and phase transitions,
Can simulate real-world conditions.

44. Summary
SMS offers a series of DVS products to cover a wide range of industries and applications.
SMS are innovators and market leaders in the realm of vapor sorption science.
More information on specific applications can be obtained by ing .
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Surface Measurement Systems, Ltd.
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