Laboratory services

  • Thermal analysis
  • DSC
  • mDSC
  • TGA
  • mTGA
  • Hi-Res TGA
  • SDT
  • Liquid chromatography
  • HPLC
  • UHPLC
  • GPC/SEC
  • 2D-LC
  • Mass spectrometry
  • Singe Quad
  • Triple Quad
  • In-combine with LC
  • Other analyzes
  • X-ray diffraction (XRD)
  • Elemental analyzes CHNOS
  • BET
  • Karl Fischer titration
Thermal analysis

TGA

In our laboratory, we use the TA Instruments thermogravimetric analyzer TGA5500, which is characterized by exceptional accuracy, highest sensitivity and best data capture reliability. The heart of the instrument is the unique, thermally insulated TruMass ™ ultramount weighing machine that enables:

  • extremely low base line drift and consequently reliable detection of minimal mass changes.
  • The wide working area weighs up to 1 g.
  • The free-hanging sample allows efficient heat transfer and gas flow over the sample.
  • There is no need for post-processing to improve the data captured.

Samples are heated with a special IR oven that works:

  • in the range RT – 1200 ° C.
  • With a heating rate between 0.1 and 500 °C/min.
  • Ballistic heating possible at a speed of > 1500 °C/min.
  • It is lined with quartz tubes inside for optimum interaction with the atmosphere.

 

THERMOGRAVIMETRIC ANALYSIS (TGA)

Thermogravimetric analysis determines the mass change and the rate of change of the sample mass, as well as the function of temperature, time and atmosphere. TGA is most commonly used to study the composition of complex materials and to predict their thermal stability through continuous monitoring of sample mass during controlled changes in temperature and / or atmosphere. Thus, materials whose mass is reduced or can be analyzed increasing due to desorption or sorption of volatile substances, decomposition, oxidation or reduction.

Information on materials that can be obtained from TGA,
include:

  • Thermal stability,
  • oxidative stability,
  • assembly of multi-component systems,
  • moisture content and other volatile components,
  • life expectancy,
  • decay kinetics and
  • influence of reactive or corrosive atmosphere.

 

HIGH-RESOLUTION THERMOGRAVIMETRIC ANALYSIS (HI-RES™ TGA)

In addition to classic TGA analysis, where temperature is an independent parameter, we also perform Hi-Res ™ TGA high resolution measurements.

The Sample Controlled Thermal Analysis (SCTA) approach is used to determine the rate of warming depending on the rate of change of the sample mass. This achieves the separation of broad and overlapping thermogram events.

 

TEMPERATURE MODULATEDTGA (MTGA™)

Process kinetics research enriches knowledge of your materials with additional information that typically comprises: process activation energy (Ea), reaction order (n), and calculation of conversion curves (α), and material lifetime prediction. The classical methods of determining these parameters involve multiple measurements of the same material with different heating rates, such as the Flynn and Wall method. The activation energy calculation thus comprises some (4-6) sample measurements with further processing of the data. MTGA ™ is an innovative approach to the acquisition of process activation energy data, which is continuously calculated throughout the measurement and can be analyzed as a function of temperature, time and conversion. The method is based on the principle of using different sample heating rates, but these are achieved within a single measurement using sinusoidal t. i. A “modulated” temperature change program.

 

DIFFERENTIAL DYNAMIC CALORIMETRY (DSC)

Differential dynamic calorimetry is a method by which the amount of heat absorbed or released by changes in the structure of a material is determined, and the temperature at which this change occurs. Given that the result of any structural change is heat-related, the scope of DSC is truly enormous. The technique is indispensable at both the initial product development stage and the final product quality control stage. Typically, the following material properties are studied by measuring the heat flux on DSC instruments:

  • steklasti prehod,
  • cold crystallization,
  • phase changes in solid,
  • melting,
  • crystallization,
  • stability,
  • network kinetics,
  • oxidative stability.

 

TEMPERATURE MODULATED DSC (MDSC™)

One of the key advantages of our measurements is the use of a unique innovative approach to the measurement – temperature modulation of the heating of the samples by applying a sinusoidal temperature oscillation. This enables the deconvolution of the recorded heat flow curve containing several overlapping effects and their further interpretation. By applying temperature modulation, the total heat flux curve splits into a reversible heat flux curve containing effects related to a change in the sample heat capacity (vitreous transition, melting) and a non-reversible heat flux containing kinetic effects (evaporation, networking, decay) . The advantages of MDSC ™ are therefore: separation and interpretation of overlapping effects; better sensitivity to detect weak effects; better resolution without loss of sensitivity; direct measurement of heat capacity; a more accurate measurement of the crystallinity of a polymeric material.

Liquid chromatography

LIQUID CHROMATOGRAPHY (LC) AND MASS SPECTROMETRY (MS)

Liquid chromatography has long since become the gold standard of analytical chemistry. Its use is the basis for the chemical development of materials and also the control of their quality in various industries.

In our laboratory, we use the universal chromatographic system – ACQUITY Arc with PDA detector, which can function as a regular HPLC or UHPLC system. Arc Multi-flow path ™ technology is an advantage when transferring methods from HPLC to UPLC®. The system is coupled to an ACQUITY QDa® MS detector, which is controlled using Empower® software.

An ACQUITY H-Class system with a series of sequentially coupled detectors (PDA, TUV, MS) is also available. This system is characterized by very low dispersion for excellent resolution and an ultra-low carryover, which is suitable for pairing with a high sensitivity mass spectrometer.

We use the Quattro Premier XE ™ Triple Quadrupole Mass Spectrometer, which enables MS / MS analyzes and reliable determination of the presence of analytes at low concentrations. The system also supports 2D-LC technology, which means separating the same sample into two or more different columns, with the ability to use different mobile phases, column temperatures, flow rates and other chromatographic parameters. The use of 2D-LC-MS opens new horizons, especially in solving complex problems, both for small molecules and for biopharmaceuticals.

Mass spectrometry

LIQUID CHROMATOGRAPHY (LC) AND MASS SPECTROMETRY (MS)

Liquid chromatography has long since become the gold standard of analytical chemistry. Its use is the basis for the chemical development of materials and also the control of their quality in various industries.

In our laboratory, we use the universal chromatographic system – ACQUITY Arc with PDA detector, which can function as a regular HPLC or UHPLC system. Arc Multi-flow path ™ technology is an advantage when transferring methods from HPLC to UPLC®. The system is coupled to an ACQUITY QDa® MS detector, which is controlled using Empower® software.

An ACQUITY H-Class system with a series of sequentially coupled detectors (PDA, TUV, MS) is also available. This system is characterized by very low dispersion for excellent resolution and an ultra-low carryover, which is suitable for pairing with a high sensitivity mass spectrometer.

We use the Quattro Premier XE ™ Triple Quadrupole Mass Spectrometer, which enables MS / MS analyzes and reliable determination of the presence of analytes at low concentrations. The system also supports 2D-LC technology, which means separating the same sample into two or more different columns, with the ability to use different mobile phases, column temperatures, flow rates and other chromatographic parameters. The use of 2D-LC-MS opens new horizons, especially in solving complex problems, both for small molecules and for biopharmaceuticals.

Other analyzes

X-ray diffraction (XRD)
Elemental analyzes CHNOS
BET
Karl Fischer titration