Malvern Macromolecular Solutions. Innovative Solutions in Material Characterization

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1 Malvern Macromolecular Solutions Innovative Solutions in Material Characterization

2 MALVERN HEADQUARTERS

3 Malvern Instruments is a Spectris company. Innovative Solutions in Material Characterization Particle size Particle morphology Zeta potential Rheological properties Our understanding delivers your comprehensive advantage Chemical imaging Molecular weight Thermal analysis

4 Application Solutions

5 200 employees in the Americas 800+ Malvern employees worldwide Northampton 17 dedicated applications laboratories 220 employees in Asia 28 offices in 15 countries 4 manufacturing operations across 3 continents

6 Malvern macromolecular solution characterisation Molecular weight and distribution Intrinsic viscosity and distribution Molecular size and distribution Branching and distribution Copolymer or blend composition Solution viscosity, rheology and microrheology Molecular, colloid and particle size Zeta-potential Thermodynamics

7 Malvern technologies for macromolecular solution characterisation Viscotek GPC/SEC systems and detectors Viscotek TDA & 270 Viscotek HT-GPC Viscotek SEC-MALS 20 Zetasizer DLS, SLS and ELS (zeta potential) Zetasizer Nano Zetasizer MicroV Malvern Rheology solutions Rosand capillary rheometer Kinexus rotational rheometers RheoSense mvroci Zetasizer DLS microrheology

8 Malvern Products covered today TDAmax system SEC-MALS 20 Zetasizer µv OmniSEC software Rheology solutions MicroCal Calorimetry instruments

9 VISCOTEK GPC/SEC

10 Viscotek Detectors & Systems A Viscotek detector or system is available for any experimental setup Modular and integrated detectors and systems are available for advanced GPC measurements The TDA is an integrated multi-detector system with RI, UV, Light Scattering and Viscometer detectors The 270 is a modular light scattering and viscometer detector The SEC-MALS 20 is a modular MALS detector with 20 measurement angles for molecular weight measurements The Zetasizer µv is a modular RALS detector capable of molecular weight and molecular size (DLS) measurements. It can also be used in batch mode

11 TDAmax Software and hardware from a single company, designed from the ground up for multi-detector GPC/SEC, fully controlled by one software TDA + GPCmax + OmniSEC

12 Hardware Schematic Tetra Detection Vacuum Degasser GPC Pump Autosampler Solvent Column Oven and Columns Injection Loop GPCmax Waste UV or PDA Detector LS Detector RI Detector Viscometer Detector

13 Maltodextrin Maltodextrin is a polysaccharide derived from starch for use in food products Purchasing is based on bulk viscosity but leads to variation Compare these 3 samples

14 Polycarbonate branching Polycarbonate branching affects its properties Two samples with different MWD The MH-plot shows a small shift between the samples (red & blue) Compare with the significant difference with polystyrene Branching level and frequency can then be calculated Wf / [dlog MW] 1,40 1,20 1,00 0,80 0,60 0,40 0,20 Molecular Weight Distribution PC 1 PC 2 0,00 3,00 3,40 3,80 4,20 4,60 5,00 5,40 5,80 Log(Molecular Weight)

15 SEC-MALS 20 In 2013 Malvern launched the SEC-MALS 20 detector This instrument has proved to be extremely successful High specification (20 angles, working low angles to 12 ) High sensitivity Robust design Easy to use OmniSEC software

16 Why is the SEC-MALS 20 so successful? Vertical flow cell with radial optics gives three big benefits: It minimizes background noise as all light entering and exiting the cell does so at a perpendicular angle Angles are known and fixed. A single cell covers all eluents. It reduces contaminant noise by avoiding laser intersection with flow dead volumes

17 PMMA measured using MALS SEC-MALS accurately measures the molecular weight independent of column retention volume PMMA95k Peak RV (ml) Mn (kda) Mw (kda) Mz (kda) Mw / Mn Rg(w) (nm) 10.2 Additionally, Rg can be measured across (most of) the peak

18 Pepsin aggregation In this sample, Pepsin aggregates are so large they scatter light anisotropically Aggregates Monomer Degradation products Peak RV (ml) Mn (kda) Mw (kda) Mw / Mn Rg(w) (nm) 69.9 N/C N/C Wt Fr (Peak) These aggregates have been measured to have a measured Rg of approximately 70 nm

19 MALVERN ZETASIZER

20 Zetasizer µv features & specs Dynamic light scattering to measure size Static light scattering to measure molecular weight Seconds to switch between batch and flowmodes Simply switch the cell

21 Zetasizer μv optical setup High power laser focussed into measurement volume increases scattered light intensity 90º measurement angle minimises flare from the cell wall to achieve highest signal to noise ratio Avalanche photodiode 90º measurement angle also minimises the measurement volume 2 µl batch 8 µl flow

22 Zetasizer μv for batch and SEC measurements Combined solution for batch DLS and SEC-LS Batch measurements of size by DLS at 90º Size Thermal trends Add LS to an existing SEC system with: 1 concentration detector for molecular weight 2 concentration detectors for conjugate analysis Intensity (%) Size (nm) 1472,0 36,0 1394,0 34,0 1312,0 32,0 1230,0 Refractive Index Response (mv) 1148,0 1066,0 984,0 902,0 820,0 738,0 656,0 574,0 Viscometer DP Response (mv) 30,0 28,0 26,0 24,0 22,0 20,0 18,0 16,0 14,0 492,0 12,0 410,0 10,0 328,0 8,0 246,0 6,0 164,0 4,0 82,0 2,0 0,0 0,0 High MW Aggregates (Mw > 1 Mio D) Trimer Trimer Dimer Dimer Monomer Monomer 5,30 5,6 5,8 6,0 6,2 6,4 6,6 6,8 7,0 7,2 7,4 7,6 7,8 8,0 8,2 8,4 8,6 8,8 9,0 9,2 9,4 9,6 10,00 Retention Volume (ml) 239,0 7, ,0 6, ,0 6, ,0 6, ,0 6, ,0 6, ,0 5, ,0 98,0 Right Angle Light Scattering Response (mv) Log Molecular Weight 126,0 5, ,0 5,400 5,200 84,0 5,000 70,0 4,800 56,0 4,600 42,0 4,400 28,0 14,0 4,200 0,0 4,000

23 OmniSEC so far OmniSEC the most powerful and easy to use software in the market. Two clicks from raw data to results! The only GPC software that doesn t force the user to compromise their data by fitting Handles all 6 channels of data RI, Visc (DP+IP), UV, LS (90º+7º) required for multi-detector GPC Online DLS and 3D PDA results Compliant with 21CFR part 11 Special features include: Copolymer analysis, determination of dn/dc and A2, variable dn/dc etc.

24 OmniSEC 5.1 Includes Waters Empower integration Share sequences New OmniSEC Bio interface More protein specific features MALS detector integration and calculations 3D angle plot

25 MALVERN RHEOLOGY SOLUTIONS

26 Rheological Properties Rotational rheometer Kinexus range Viscosity and viscoelastic profiling Flow curves vs (shear rate dependent) Yield stress Thixotropy (time dependent) Linear viscoelastic moduli G', G'' vs and Wide variety of sample types Low viscosity fluid to high modulus solid-like Flow instabilities limit access to very high shear rates Inertial considerations limit access to high frequency (short timescale) measurements h u

27 Rheological Properties Rheometer on a Chip - hybrid microfluidic flow/mems sensors m-vroci Partnership with RheoSense Inc., CA Viscosity profiling Flow curves vs (shear rate dependent) Full non-newtonian data corrections (Assessment of extensional viscosity) Lower viscosity materials Colloidal dispersions Extend flow curves to ultra high shear rates process-relevant conditions Volatile solvent matrices

28 Rheological Properties Capillary rheometer Rosand range Viscosity profiling Flow curves vs (shear rate dependent) Full non-newtonian data corrections Assessment of extensional viscosity High viscosity materials Polymer melts, pastes and slurries Extrusion process industrially-relevant Extend flow curves to high shear rates process-relevant conditions

29 Rheological Properties DLS Microrheology Zetasizer Nano ZS/ZSP Viscoelastic profiling Linear viscoelastic moduli G', G'' vs Can use Cox-Merz approximation for * vs Low viscosity, weakly-structured materials Polymer and surfactant solutions ideal must be viable for DLS measurements Track motion of dispersed tracer particles Extend viscoelastic spectrum to very high frequencies characterise short timescale material response Sample preparation important

30 Malvern rheology - complementary techniques

31 MicroCal instruments Isothermal Titration Calorimetry (ITC) The instrument measures exothermic and endothermic reactions during mixing of two fluid components. Data Analysis uses Thermal Data(DP) and concentration information to directly calculate N (Stoichiometry ), Ka (binding constant), H (Enthalpy), calculated S (Entropy) Differential Scanning Calorimetry (DSC) is a powerful analytical tool which directly measures the stability and unfolding of a protein, lipid, or nucleic acid. It measures the heat changes that occur during a linear increase (or decrease) in temperature. Transition midpoint T m, Enthalpy ( H) and heat capacity change ( Cp) associated with unfolding

32 Thank you for listening! Need more additional information? Useful links: Malvern GPC instruments: Light scattering explained: Molecular weight: Microrheology