Complex thermal analysis laboratory

System for complex thermal analysis STA (TG/DSC) - FTIR – GCMS

The system for complex thermal analysis consists of a thermal analysis instrument STA 449 C F3 from Netzsch, which allows performing thermogravimetric analysis, in the temperature range -100 oC - 1000oC (by cooling with liquid nitrogen). The heating C rate of the sample can be varied in the range of 0.1-100 K / min. The analyzes can be performed in an inert or oxidizing atmosphere (synthetic air). Solid or liquid samples with a mass between 10-50 mg can be analyzed. Loss/increase of mass, thermal effects accompanying chemical reactions (decomposition, oxidation, etc.), or physical processes (melting, boiling, solidification, other phase transitions) are determined.

The gases released during the thermal analysis can be afterward analyzed by coupling with the Bruker FTIR Tensor 27 spectrometer and the JAS GC-MS system.

Thermal analysis for two magnetite samples. One sample is pristine, and one sample is encapsulated in silica. The silica coating protects the magnetite from oxidation reactions.

3D diagram obtained from the sum of the FTIR spectra of the eliminated gases depending on the oven temperature. We can see the bands characteristic of organic compounds at low temperature (up to 200 oC) and then the presence of CO2 obtainedofrom the oxidation2 of organic compounds.

The eliminated gases can be analyzed by FTIR or GC-MS and a profile of the generation of the species of interest can be constructed (the burning of the polyurethane foam generates toxic gases CO and HCN - the „Collective„ case).2


Equipment for elemental analysis CHNOS

Knowing the composition of the organic elements helps analysts to determine the structure of the sample substance. The chemical characterization of organic compounds is used in research as well as for quality control. It is a reliable and cost-effective technique used to evaluate the purity and chemical composition of compounds and can be used on a wide range of samples. 

The most common elementary analysis technique CHNS-O is based on sample combustion. Upon combustion, the sample generates composite gases of elements C, H, N, and S. These combustion products (eg CO2, H2O, NO2 etc.) are measured using gas chromatography and thus the ratio of the elements in the original sample is determined. Elements C, H, N, and S can be analyzed simultaneously, while O can be analyzed in a second stage by pyrolysis. As the final quantities of each item are usually given as a percentage of the weight of the original sample, the sample must be accurately weighed. Due to the very small sample size, a very accurate microbalance is recommended.

The FLASH 2000 elemental analyzer (Thermo Scientific ™) is equipped with:

The tool is completely controlled by the computer through the dedicated software, Eager Xperience, used both for the acquisition and for the processing and interpretation of the obtained results.

The elemental analyzer can be used to determine the concentrations of sulfur, oxygen, nitrogen, hydrogen, and carbon in solid samples, such as food or biological samples.