TA-QMS Coupling
16Pages

Proven Excellence. Thermal Analysis -Mass Spectrometer Capillary Coupling Analyzing & Testing Evolved Gas Analysis Method, Techniques and Applications

Thermal Analysis and Evolved Gas Analysis Thermoanalytical Techniques Thermoanalytical techniques are universal tools for characterizing solids and liquids with respect to their thermal behavior. Especially Thermogravimetry and Simultaneous Thermal Analysis (STA, TGA-DTA/DSC) find broad application in testing the weight changes of a sample during a programmed heat treatment. This yields a multitude of information on material properties, composition and stability. However, chemical and analytical information about the products causing the weight changes to the sample is often lacking....

Complementary Information Mass changes detected by thermal analysis can be explained by gas analysis in the mass spectrometer; coupling thus creates a workstation for analytical chemistry. Evolved species are detected down to the ppm level in mass spectrometry, which exceeds the standard sensitivity of thermal analysis methods. The coupling of the two therefore allows for top-notch material research and characterization. Quadrupole Mass Spectrometry (QMS) A quadrupole mass spectrometer's sensitivity, selectivity, speed and capacity for continuous operation make the system ideally suited for...

HYPHENATION OF THERMAL ANALYSIS AND EVOLVED GAS ANALYSIS STA 449 F1 Jupiter coupled to QMS 403 Aëolos Quadro; other thermal analyzers can also be coupled to MS, such as the TG 209 F1 Libra

Ideal Gas Flow Conditions Ensure Transport of All Relevant Gases The aim of coupling is to have all relevant gases and vapors transported from the sample area into the ion source of the mass spectrometer for precise qualitative and quantitative analysis. This is only achieved through perfect gas flow conditions in the thermal analyzer, the coupling interface and the gas inlet of the mass spectrometer. As only a small amount of gas is required for the analysis, a bypass is used at the gas outlet on the thermobalance for the excess purge gas flow; i.e., for the flow not passing through the...

TA-QMS 403 Aëolos Quadro Coupling Top-Notch Capillary Coupling – Heating Throughout and Single-Step Pressure Reduction The QMS 403 Aëolos Quadro quadrupole mass spectrometer features a fleshed-out design for capillary coupling to NETZSCH thermal analyzers (e.g., simultaneous TGA-DSC or STA). Volatile sample materials under controlled temperature treatment are directly transferred into the electron impact ion source of the MS via a fused silica capillary (optionally capillary made of stainless steel). The Capillary Coupling Is Designed for Optimum Gas Flow Conditions and Flexibility...

Insulated inert quartz glass capillary with controlled heating to 300°C (optionally 350°C) for loss-free gas transfer to the QMS Heated chamber for easy handling and precise adjustment of the capillary inlet to the QMS Capillary Coupling Possibilities for the QMS 403 Aëolos Quadro TGA-DSC/DTA Systems STA 449 F1 Jupiter: -150°C to 2000°C STA 449 F3 Jupiter: -150°C to 2400°C STA 449 F5 Jupiter: RT to 1600°C Quadrupole MS Capillary guiding device Hyperbolic quadrupole TGA Systems TG 209 F1 Libra: RT to 1100°C Dilatometer/Thermomechanical Analyzer DIL 402 Expedis Supreme*: RT to 1600°C DIL 402...

High Detection Sensitivity from Low to Hydrogen and Xenon Detected by the QMS 403 Aëolos Quadro Detection Sensitivity for Hydrogen For demonstration of the detection sensitivity in the low mass range, argon purge gas was treated with pulses of hydrogen by using the NETZSCH PulseTA. The volume of the pulses was equivalent to 1 μg, 5 μg and 10 μg hydrogen. For m/z 2, an integration time of 1 s was used. Due to high performance of the MS, low hydrogen quantities can be detected with high precision. Excellent linearity enables quantification over a large concentration range. Detection...

High Mass Range Continuous heating of the entire gas transfer line reduces the risk of condensation so that even larger molecules can be detected. High Detection Sensitivity Even for High Mass Numbers This TGA-QMS Aëolos Quadro measurement on polystyrene (PS, granulates) shows one mass-loss step between 300°C and 560°C. The plot indicates styrene (m/z 104) and its dimer detected at m/z 208. The high detection sensitivity of the QMS Aëolos Quadro is substantiated with detection of the trimer at m/z 312 (see red circle).

Proteus The Software for Performing Simultaneous Measurements Using Thermal Analysis Coupled with the QMS 403 Aëolos Quadro Measurements using STA/TGA/DSC/DIL instruments coupled to the QMS 403 Aëolos Quadro can be controlled entirely via Proteus software, which combines the measurement and analysis software of the two coupled methods into a single software application for both control and data acquisition. Proteus allows for the individual definition of any parameters relevant to thermal analysis (e.g., temperature program, heating rate, etc.) as well as any parameters relevant to the mass...

Excellent correlation between the area of the MS signal and decreasing sample mass Several TGA measurements on baking soda with decreasing sample mass (plot on top, solid lines), when compared with the evolving CO2 shown as MID curves (m/z 44, dashed lines), exhibit a linear relationship between the sample mass and CO2 (see plot below). This behavior demonstrates the very good linearity of the Aëolos Quadro mass spectrometer. Direct Correlation Between Mass Loss and Evolved Gas via MID Curves Evolution of CO2 from baking soda (NaHCo3)

Key Software Features Measurement ■ Complete integration of thermal analysis and QMS software into Proteus ■ Method-based measurement and evaluation ■ Simultaneous start/stop of the coupled measurements ■ Three different scan modes: scan analog, scan bargraph, MID ■ Selection of different scan bargraph ranges at the same time ■ Selection of scan bargraph or scan analog with optimized rate and sensitivity in different channels ■ Individual MS parameters for each position of the automatic sample changer Analysis ■ Evaluation of MS results within Proteus ■ Evaluation of results precisely...