Material characterisation

aqueous-gel-permeation-chromatography-system-aqueous-gpcAqueous gel permeation chromatography system (GPC)

Aqueous size exclusion chromatography (SEC) is widely used for the determination of molecular weight distributions of a variety of synthetic and naturally occurring water soluble polymers, and separations of oligomers and small molecules. Gel permeation chromatography (GPC) is a form of SEC. The requirement to eliminate ionic and hydrophobic effects makes aqueous GPC very demanding. GPC uses specialised columns for the separation. The PL aqua gel-OH columns provide a chemically and physically stable matrix for reliable aqueous GPC separations. The columns are packed with macro porous copolymer beads with an extremely hydrophilic poly-hydroxyl functionality. The neutral surface and the capability to operate across a wide range of eluent conditions provide for high performance analyses of compounds.

GPC is used as a polymer characterisation tool. The molecular weight can greatly change the properties of a polymer, from a low molecular weight sample that is quite flexible to a high molecular weight sample that is more rigid.

ANFF-Q has been equipped with an Agilent Technologies Aqueous GPC 1260 Infinity system with RI, UV, viscosity and light scattering detectors, which allows both the measurement of molecular weights compared to reference standards and the measurement of absolute molecular weights.

Examples of use

The Aqueous GPC 1260 Infinity system can be used for the determination of molecular weights of low to very high molecular weights of many biomaterials, PEG, poly-acrylates, PVA, cellulose derivatives, starch etc.

Purpose:

Gel permeation chromatography that separates on size exclusion and the measurement of the molecular weight of water-soluble polymeric samples.

Material systems:

Polymers/bio-materials.

Scale/volume:

2 mL sample vials, 100 µL injection syringe and a 1.5 mL sample loop.

Specifications/resolution:

Measures molecular weight using either RI, UV, viscometer and light scattering detectors (15 and 90 degree) in the (range of 500 to 1 200 000 daltons), an isocratic pump 0.1 to 1.0 mL/min, a 2 port column heater 30 to 60 degrees Celsius and an auto injector capable of holding either 48 x 2 mL vials.

Model:

Agilent Technologies Aqueous GPC 1260 Infinity system

Site:

The University of Queensland

Location:

PC2 Laboratory, Level 2E, AIBN (Bldg #75), St Lucia

Instrument contact:

Javaid Khan


gel-permeation-chromatography-system-gpcGel permeation chromatography system (GPC)

The gel permeation chromatography (GPC) system is a variation of high performance liquid chromatography (HPLC) using specialised columns that separate on the basis of size exclusion. GPC is specifically used for the measurement of the molecular weight of polymeric samples and is a polymer characterisation tool.

The molecular weight of a polymer can greatly change the properties that it will have, from a low molecular weight sample that is quite flexible and has high gas permeability to a high molecular weight sample that is more rigid and has reduced gas permeation.

ANFF-Q has a Waters system with an RI, UV and a Shimadzu MALS detectors, which allows not only the measurement of molecular weights compared to reference standards but the measurement of absolute molecular weights.

Examples of use

Kinetic determination of rates in polymerisation systems with transfer agents such as di-thioesters. Theoretical models of polymerisation have these rates being dependent on both the molecular weight and transfer agent concentrations. RAFT is a currently used method to obtain polymers with a specific and narrow molecular weight distribution.

Degradation of polymers by UV can be monitored over time for changes that will relate to product failure.

Purpose:

Gel permeation chromatography that separates on size exclusion and measure molecular weight of polymeric samples.

Material systems:

Polymers/biomaterials.

Scale/volume:

1 mL sample vials, 50 µL injection syringe and a 1.0 mL sample loop.

Specifications/resolution:

Measures molecular weight using either RI detection only (range 1 300 to 1 200 000 Da) or MALS (500 to 1 500 000 Da), a isocratic pump 0.1 – 1.0 mL/min, a 4 port column heater 20 – 60 °C and an auto injector capable of holding  96 x 1 mL vials.

Model:

Waters 1515 Isocratice HPLC Pump, 717plus Autosampler, 2414 Refractive Index Detector, 2489 UV/Visible Detector.

Site:

The University of Queensland

Location:

Room 441, Level 4E, AIBN (Bldg #75), St Lucia

Instrument contact:

Javaid Khan


laser-light-scattering-spectrometry-system-surfscan-7700mLaser light scattering spectrometry system

The Surfscan 7700M is a laser light scattering spectrometer for full front side wafer inspection. It can be used for analysing wafer pattern defects and defect analysis of non-patterned wafers.

System handling is set for 150 mm wafers, 675 µm thick.

For more detailed specifications and capabilities see information and pdf files at Queensland Microtechnology Facility.

Examples of use:

Wafer level defect detection.

Purpose:

  • Quantification of defectivity issues in films for optimisation of deposition processes.
  • Routine assessment of particle contamination for equipment within the QMF to maximise yield

Material systems:

Standard Si wafers and deposited films including SiC.

Scale/volume:

Auto handling from cassette.

Specifications/resolution:

100 mm, 150 mm and 200 mm wafer size compatibility. Particle and defect quantification down to 0.15 µm for non-patterned wafers.

Model:

Surfscan 7700M

Site

Griffith University

Location:

QMF (Bldg N74), Nathan Campus

Instrument Contact:

Alan Iacopi


laser-scannerLaser scanner

The Tecan LS Reloaded laser scanner is a micron-resolved optical scanning device that has the option of either use with fluorescence or reflectance imaging. Applications for the laser scanner range from material science in the imaging of fluorescent polymers and fluorescent dye-treated polymeric materials to microfluidic devices and biological-based samples such as protein arrays and biological specimens.

The Tecan LS Reloaded laser scanner has two lasers: a 635 nm laser and a 532 nm laser suitable for imaging samples treated with far red dyes (e.g. Cy5, Alexa 633) and green and red dyes (e.g. DsRed, Cy3, Cy2, FITC, DiO) respectively. The resolution of imaging on this device is in the region of 4 – 60 µm.

Examples of use:

For microfluidic devices the entire device can be scanned within minutes to check on tube structure and uniformity. A 2D image can be created and static images of the device can be taken during operation of the device.

For arrays and microarrays the scanner can be used as a tool for quick analysis. The laser scanner has in-built software that can set up controls and carry out an automated quality control.

Fluorescent-treated polymeric images created by lithography processes can be imaged within minutes.

Fluorescent-treated biological samples can be imaged using the laser scanner. Fluorescent tagging of organs or proteins in a section of a mouse can be imaged.

Purpose:

It is a micron resolved optical scanning device using either fluorescence or reflectance imaging with two lasers: 635 nm and 532 nm.

Material systems:

Organic, inorganic, polymers and biological.

Scale/volume:

Microscope slide or micro well plates up to a size of 15 x 85 x 127 mm.

Specifications/resolution:

Contains 633 nm and 532 nm lasers suitable for Cy 3 and Cy 5 dyes; has 620/20 nm, 575/50 nm, 635/35 nm, 535/25 nm and 692/40 nm filters; spot from 70 µm to 300 µm; resolution from 4 µm to 40 µm per pixel; and has array analysis software.

Model:

Tecan LS Reloaded laser scanner

Site:

The University of Queensland

Location:

PC2 Lab, Level 2E, AIBN (Bldg #75), St Lucia

Instrument contact:

Lien Chau


liquid-chromatography-mass-spectrometryLiquid chromatography mass spectrometry (LC-MS)

Liquid chromatography mass spectrometry (LC-MS) is used as a complimentary technique for the synthesis of organic and biological compounds such as proteins and peptides. This technique can be used qualitatively for the identification of unknown compounds or quantitatively for analysing the purity of a sample. The versatility of columns available for this technique means that samples can be separated in an ionic, aqueous or even organic based environment.

LC-MS has the capability of separating and detecting a variety of compounds in a mixture. The ANFF-Q LC-MS equipment contains a Waters separations module 2695 combined with a Quattro-micro unit. The separations module can be used in unison with the mass spectrometry unit or as a stand-alone mass spectrometry unit.

Examples of use

Pharmaceutical and biopharmaceutical samples can be analysed for amino acids, intact proteins, oligonucleotides and peptides. This can give a guide for purity and quality control. Drug testing is a common application in this area.

Environmental testing of pollutants and contaminants such as dioxins and furans in samples such as ground water, soils and waste water.

Purpose:

For separation, characterisation and analysis of organic aqueous, volatile, and bio-polymer materials.

Material systems:

Organic, inorganic, polymers and biological.

Scale/volume:

Individual sample/system analysis.

Specifications/resolution:

  1. LC-MS mass range 20 – 2 000 Da, column 35 °C; 90 position auto-sampler.
  2. HPLC 2 mL/4 mL vial holder, 2 mL sample loop for preparative C18 column, 20 µL sample loop for analytical column, 4 line pump for gradient elution, UV detector.

Model:

Waters Alliance 2695 Separations Module and Micromass Quattro micro API.

Site:

The University of Queensland

Location:

Room 444, Level 4E, AIBN (Bldg #75), St Lucia

Instrument contact:

Javaid Khan


Thermal analysis characterisation suite (DMA, DSC, TGA)

The examination of the thermal properties of both organic and inorganic based samples gives an idea of the possible applications that a material can be used for. ANFF-Q has access to three different thermal analysis techniques: dynamic mechanical analysis (DMA), differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA).

DMA is a technique where the viscoelastic properties of a sample are tested. A sample undergoes an oscillation motion and the resulting displacement is measured. This technique is typically used to measure properties of polymer samples. DMA can be used to obtain a very precise glass transition temperature as well as the storage modulus.

DSC is a technique where the heat flow of a sample cell is measured in comparison to a reference cell as a function of temperature. Thermal transitions such as melting points, glass transition temperatures or exothermic decompositions can be analysed. DSC is particularly useful in the analysis of polymers as it can give information vital for the suitability of a polymer for a particular application. DSC allows you to detect endothermic and exothermic effects, measure peak areas (transition and reaction enthalpies), determine temperatures that characterise a peak or other effects, and measure specific heat capacity.

TGA measures the weight and hence the mass of a sample as a function of temperature. Sample features such as decomposition temperatures, moisture content, and the amount of volatile organics can be determined. The environment in which the measurement is taken can be modified, e.g. whether it is an oxidative environment (air) or an inert environment (Argon), to analyse different thermal features of a sample. TGA allows you to detect changes in the mass of a sample (gain or loss), evaluate stepwise changes in mass (usually as a percentage of the initial sample mass), and determine temperatures that characterise a step in the mass loss or mass gain curve.

Examples of use:

Measurement of the glass transition temperature of polymers
Above the glass transition temperature a polymer is soft, rubbery and tacky, e.g. low density polyethylene. Below the glass transition temperature a polymer is hard, stiff and brittle, e.g. poly methyl methacrylate (PMMA) or Perspex. The glass transition temperature can be measured by using either DMA or DSC. DMA is more accurate but the set sample geometry for testing and lengthy analysis makes DSC a much easier technique.

Sample purity
The purity of a sample can be analysed using TGA. Measurement of the decomposition and amount of water present in a zinc carbonate can indicate the purity of the sample and in some cases the phase structure such as hydrozincite.

Thermal properties
Thermal properties such as the thermal expansion coefficient can be obtained from DMA. It is important to know how much a polymer will expand and contract with temperature during application so that the correct design of a system can be obtained. PMMA can be analysed to make sure that it can be used correctly in exterior applications where temperatures can range from -20 °C to 50 °C.


thermal-analysis-characterisation-suite-dynamic-mechanical-analysis-dmaDynamic mechanical analysis

Purpose:

To detect the dynamic mechanical behaviour of a material sample as a function of frequency and temperature.

Material systems:

Organic, inorganic and polymers.

Scale/volume:

Individual sample/system analysis.

Specifications/resolution:

Temperature range -150–500 °C; technical resolution 0.003 K; accuracy 0.5 K; peak force 12 N, 18 N or 40 N; minimal force 0.005 N; frequency range 0.001–1000 Hz.

Model:

METTLER TOLEDO DMA/SDTA861e STARe System

Site:

The University of Queensland

Location:

Level 4E, AIBN (Bldg #75), St Lucia

Instrument Contact:

Wael Al Abdulla


thermal-analysis-characterisation-suite-differential-scanning-calorimetry-dscDifferential scanning calorimetry

Purpose:

For testing, analysis and characterisation of the thermal properties of polymers such as glass transition, enthalpy of melting (fusion), heat capacity and thermal degradation.

Material systems:

Organic, inorganic and polymers.

Scale/volume:

Individual sample/system analysis.

Specifications/resolution:

Temperature range room temperature to 550 °C, 34 position auto sampler, nitrogen purge (-100 °C to 500 °C), temperature precision ±0.02 K.

Model:

METTLER TOLEDO DSC 1 STARe System

Site:

The University of Queensland

Location:

Level 4E, AIBN (Bldg #75), St Lucia

Instrument Contact:

Javaid Khan


thermal-analysis-characterisation-suite-thermal-gravimetric-analysis-tgaThermal gravimetric analysis

Purpose:

  • Determines temperature and weight change of decomposition reactions.
  • Determines water content or the residual solvents in a material.
  • Allows analysis of reactions with air (oxygen).
  • Used to measure the weight of fiberglass and inorganic fill materials in plastics, laminates, paints, primers, and composite materials by burning off the polymer resin.
  • Measures the fill materials added to some foods, such as silica gels, cellulose, calcium carbonate, and titanium dioxide.
  • Determines the purity of a mineral, inorganic compound, or organic material.
  • Distinguishes different mineral compositions from broad mineral types, such as borax, boric acid, and silica gels.

Material systems:

Organic, inorganic and polymers.

Scale/volume:

Individual sample/system analysis.

Specifications/resolution:

Temperature range room temperature to 500 °C, 34 position auto sampler.

Model:

METTLER TOLEDO TGA/DSC 1 STAR e System

Site:

The University of Queensland

Location:

Level 4E, AIBN (Bldg #75), St Lucia

Instrument Contact:

Javaid Khan


uv-plate-readerUV plate reader

The Tecan Infinite 200 is a multifunctional microplate reader which provides high performance for the vast majority of today’s microplate applications and research.

It is designed as a general purpose laboratory instrument for professional use, supporting common 6 to 384-well microplates conforming to the ANSI/SBS standards. In addition it offers high flexibility in wavelength selection for fluorescence intensity and absorbance measurements.

Examples of use

The Infinite 200 PRO offers unlimited flexibility for a wide range of biological assays and measurements including:

  • DNA/RNA
  • Protein quantification
  • Ion channel studies
  • Ion flux studies
  • Calcium ion detection
  • Reporter gene and gene expression assays
  • Cell viability and toxicity assays
  • Cell-based assays
  • Fluorescence and absorbance applications
  • TR-FRET/HTRF applications
  • AlphaScreen assays

Purpose:

UV plate reader.

Material systems:

Organic, inorganic, polymeric and biological.

Scale/volume:

Microscope slide or micro well plates up to the size of 15 x 85 x 127 mm.

Specifications/resolution:

Capable of single wavelength UV Vis measurement or a scan from 230 nm to 1000 nm. Capable of single wavelength, fluorescence measurement or a scan from ex 230/600 nm and em 330/600 nm.

Model:

Tecan Infinite 200

Site:

The University of Queensland

Location:

PC2 Lab, Level 2E, AIBN (Bldg #75), St Lucia

Instrument contact:

Javaid Khan


vibrational-spectroscopy-suite-ftir-and-ramanVibrational spectroscopy suite (FTIR and Raman)

Fourier transform infrared (FTIR) and Raman spectroscopy are techniques used to examine chemical composition using the infrared (IR) part of the electromagnetic spectrum. Although often referred to as complementary techniques, Raman and FTIR spectroscopy are based on very different fundamental physical phenomena, and thus present different relative advantages and disadvantages, and indeed technical challenges to their clinical implementation.

IR spectroscopy technique works on the basis that specific bonds rotate and bend at a specific frequency and will hence absorb light of that frequency. A spectrum of these bending, stretching and rotating mechanisms can give a characteristic spectrum of a compound that aids in the identification of this compound. This technique is a general identification tool used for the analysis of synthetic organic compounds and polymers.

Raman spectroscopy, a scattering technique, measures the shift of frequency as a result of the exchange of energy between the incident photon and the material vibrations (or rotations). As such, it can occur nonresonantly and can be measured across the spectral range, although it is most commonly measured in the ultraviolet (UV), visible and near infrared (NIR) regions.

IR spectroscopy relies on the direct absorption of light as a result of transitions between vibrational (or rotational) states and thus must be carried out in the (usually mid) IR region of the spectrum. Whereas the IR electric dipole transitions rely on the change in the average dipole moment of the vibration as a result of the transition, Raman scattering relies on a nonzero change in the average polarisability. IR cross sections therefore tend to be strongest in asymmetric polar moieties, whereas Raman cross sections tend to be strong for symmetric, electron rich moieties. Water is therefore a very strong IR absorber but is a relatively weak Raman scatterer, which suggests Raman as the technique of choice for in vivo applications. The fundamental differences also lead to distinct technological considerations in the application of the two techniques. Raman is an inherently weak technique, and profiling large areas by point to point mapping of signals acquired over (often) tens of seconds is time consuming.

ANFF-Q has access to several different FTIR and Raman machines as indicated below. A wide range of sample types from films, liquid samples and aqueous samples can be run over a wide range of wavelengths. The different types of detectors mean that samples can be run with high sensitivity and that features like profiling of a surface can be performed.

Examples of use:

Vibrational spectroscopy techniques are non-destructive, non-invasive tools that provide information about the molecular composition, structure and interactions within a sample. Vibrational spectroscopy is used in research and industry for quality control and quality assurance, dynamic measurement, monitoring applications, identifying polymer degradation, reaction monitoring, and sample identification, characterisation and structure elucidation. 


vibrational-spectroscopy-suite-agilent-cary-630-ftir-spectrometerAgilent CARY 630 FTIR spectrometer

ANFF-Q’s Agilent CARY 630 FTIR has been installed with the following operational modules:

  • Transmission module – the classic infrared sample interface, allows for the measurement of liquids or films
  • Diamond ATR module – the most common sample interface used in infrared spectroscopy, because it is easy to use and provides high-quality spectra with no sample preparation
  • Germanium ATR module – the shallower penetration depth achieved with a Ge crystal results in a shorter path length, allowing simpler characterisation of samples with a high amount of carbon
  • TumblIR module – Agilent’s unique liquid transmission sample interface is ideal for rapid analysis of both highly viscous and volatile liquid samples

Purpose:

Used for testing, analysis and characterisation of the vibronic and spectral properties of organics and polymers for biomedical analysis; characterisation of thin polymer resists on silicon wafers; or measurement of the build-up of water at the polymer–substrate boundary that will eventually lead to the failure of the polymer coating.

Material systems:

Organic, inorganic, liquid, powder and polymers.

Scale/volume:

Individual samples/system analysis.

Specifications/resolution:

Fourier Transform Infrared spectrometer with an attenuated total reflectance accessory; collects IR spectra of materials (400 – 4 000 cm-1).

Model:

Agilent CARY 630 FTIR spectrometer

Site:

The University of Queensland

Location:

PC2 Lab, Level 2E, AIBN (Bldg #75), St Lucia

Instrument contact:

Javaid Khan


vibrational-spectroscopy-suite-dispersive-raman-microscopeDispersive Raman microscope

Purpose:

For testing, analysis and characterisation of the vibronic and spectral properties of organics and polymers.

Material systems:

Organic, inorganic and polymers.

Scale/volume:

Individual samples/system analysis.

Specifications/resolution:

Raman confocal microscope: 633 nm and 780 nm lasers, 10x & 50x objectives, automated X Y Z stage, video capture.

Model:

Nicolet Almega XR visible dispersive Raman microscope

Site:

The University of Queensland

Location:

Room 438, Level 4E, AIBN (Bldg #75), St Lucia

Instrument contact:

Wael Al Abdullah


vibrational-spectroscopy-suite-nicolet-5700-atr-ftir-spectrometerNicolet 5700 ATR-FTIR spectrometer

ANFF-Q’s Nicolet 5700 ATR-FTIR has been installed with the following operational modules:

  • Transmission module – the classic infrared sample interface, allows for the measurement of liquids or films
  • Diamond ATR module – the most common sample interface used in infrared spectroscopy, because it is easy to use and provides high-quality spectra with no sample preparation
  • Germanium ATR module – the shallower penetration depth achieved with a Ge crystal results in a shorter path length, allowing simpler characterisation of samples with a high amount of carbon

Purpose:

Used for testing, analysis and characterisation of the vibronic and spectral properties of organics and polymers for biomedical analysis; characterisation of thin polymer resists on silicon wafers; or measurement of the build-up of water at the polymer–substrate boundary that will eventually lead to the failure of the polymer coating.

Material systems:

Organic, inorganic, liquid and polymers.

Scale/volume:

Individual samples/system analysis.

Specifications/resolution:

FTIR spectrometer with an attenuated total reflectance accessory; collects IR spectra of materials (500 – 4 000 cm-1).

Model:

Nicolet 5700 ATR-FTIR spectrometer

Site:

The University of Queensland

Location:

Room 438, Level 4E, AIBN (Bldg #75), St Lucia

Instrument contact:

Javaid Khan


vibrational-spectroscopy-suite-nicolet-5700-nir-ftir-spectrometerNicolet 5700 NIR-FTIR

Purpose:

For testing, analysis and characterisation of the vibronic and spectral properties of organics and polymers. Biomedical analysis.

Material systems:

Organic, inorganic and polymers.

Scale/volume:

Individual samples/system analysis.

Specifications/resolution:

Fourier Transform Infrared spectrometer with an attenuated total reflectance accessory; Collects IR spectra of materials (4 000 – 10 000 cm-1).

Model:

Nicolet 5700 NIR-FTIR

Site:

The University of Queensland

Location:

Room 438, Level 4E, AIBN (Bldg #75), St Lucia

Instrument contact:

Javaid Khan


vibrational-spectroscopy-suite-nicolet-nxr-ft-ramanNicolet NXR FT-Raman

Purpose:

For testing, analysis and characterisation of the vibronic and spectral properties of organics, polymers and biomedical analysis.

Material systems:

Organic, inorganic and polymers.

Scale/volume:

Individual samples/system analysis.

Specifications/resolution:

Fourier Transform Raman spectrometer (1 064 nm laser); collects Raman spectra of materials (400 –4 000 cm-1).

Model:

Nicolet NXR FT-Raman

Site:

The University of Queensland

Location:

Room 438, Level 4E, AIBN (Bldg #75), St Lucia

Instrument contact:

Javaid Khan