Download presentation
Presentation is loading. Please wait.
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 Systems
IV 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 . Head Office: Surface Measurement Systems, Ltd. 5 Wharfside, Rosemont Road London HA0 4PE, UK Tel: +44 (0) Fax: +44 (0) United States Office: Surface Measurement Systems, Ltd, NA th Street SW, Suite 1 Allentown PA, 18103 Tel: Fax:
Similar presentations
© 2025 SlidePlayer.com Inc.
All rights reserved.