Thermal Analysis – Mass Spectrometer Coupling Evolved Gas Analysis Method, Techniques and Applications Analyzing & Testing

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 an abundance of information on material properties, composition and stability. However, what is often lacking is chemical and analytical information about the course of events causing the mass change to the sample....

Reasons to Couple a Mass Spectrometer to a Thermal Analyzer Complementary Information Gas analysis allows for an explanation of the effects recorded by means of thermal analysis. The gases evolved can be detected down to the ppb range, which exceeds the typical sensitivity of thermoanalytical methods. The combination of the two methods therefore forms the ideal basis for top-notch material characterization. Quadrupole Mass Spectrometry (QMS) A quadrupole mass spectrometer’s sensitivity, selectivity, speed and capacity for continuous operation make the system ideally suited for evolved gas analysis...

HYPHENATION OF THERMAL ANALYSIS AND EVOLVED GAS ANALYSIS NETZSCH offers complete solutions for Thermal Analysis coupled to Mass Spectrometry in terms of both hardware and software. Evaluation and presentation of the results are carried out with the well-proven Proteus® software. Gas flow conditions in all thermal analyzers are ideal for coupling to a mass spectrometer. STA 509 Jupiter® coupled to QMS 505 Aëolos; other thermal analyzers can also be coupled to MS, such as the TG 309 Libra®

The capillary system is designed for universal application. For the special application field of materials with high condensation tendency, such as metals, salts and high-boiling organics, NETZSCH offers a completely integrated coupling solution: The STA 449 F3 Jupiter® with SKIMMER furnace. This combination provides direct and simultaneous coupling of a thermal analyzer with a mass spectrometer, thus enabling gas transfer temperatures of up to 1950°C. Ask your sales representative about upgrading your STA 449 F3 Jupiter®. Withstanding the Test of Time – Capillary and SKIMMER Coupling Techniques...

TA-QMS Coupling Techniques Interface for Pressure Adjustment Mass spectrometers, composed of a mass filter, an electron impact ion source and an ion detector, work only in high vacuum. Therefore, an interface is required for the coupling of a thermobalance – which works with a purge gas flow at atmospheric pressure – to the mass spectrometer. Different versions of pressure reduction interfaces are realized depending on instrumentation and applications. STA 449 F3 Jupiter® with SKIMMER furnace Single-Step Pressure Reduction Double-Step Pressure Reduction A capillary of small internal diameter...

Ideal Gas Flow Conditions Ensure Transport of All Relevant Gases The aim of coupling is to have all relevant gases 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 quantity 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 coupling interface,...

TA-QMS 505 Aëolos Coupling State-of-the-Art Capillary Coupling – Heating Throughout and Single-Step Pressure Reduction The QMS 505 Aëolos quadrupole mass spectrometer features a fleshed-out design for capillary coupling to NETZSCH thermal analyzers (e.g., simultaneous TGA 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). Optimized Capillary Coupling for Maximum Flexibility ∙ ∙ ∙ ∙ ∙ ∙ Hyperbolic Rod System The hyperbolic rod...

Insulated inert quartz glass capillary with controlled heating to 300°C (optionally 350°C) for loss-free gas transfer to the QMS Furnace for easy assembly and adjustment of the capillary inlet at the QMS Capillary Coupling Possibilities for the QMS 505 Aëolos TGA-DSC/DTA Systems STA 509 Jupiter® Supreme*: -150°C to 2000°C STA 509 Jupiter® Select*: -150°C to 2000°C STA 509 Jupiter® Classic: RT to 1600°C TGA Systems TG 309 Libra® Select/Supreme: RT to 1100°C Capillary guide Dilatometer/Thermomechanical Analyzer DIL 402 Expedis Supreme*: RT to 1600°C DIL 402 Expedis Select: RT to 1600°C TMA 402...

Sensitive and Linear Detector System 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. STA-MS measurement of hydrogen pulses at constant temperature Since the pulse area increases linearly with the pulse volume, quantification over a high concentration...

QMS 505 Aëolos Coupling QMS Specifications Mass range* 1 u to 300 u (optionally to 512 u); including auto-tuning using PFTBA to calibrate the mass scale axis Mass filter Quadrupole with hyperbolic rods and pre-filter (patented) Two iridium cathodes with Y2O3 coating Electron energy Emission current Detector Dynamic range (electronic) Detection limit Resolution Vacuum system RF generator Measuring modes Scan rate (electronic) Power Power consumption SEM with discrete dynodes and integrated Faraday cup 9 decades < 100 ppb (gas-dependent) 0.5 u to 1.5 u Turbo molecular pump with 4-stage diaphragm...