Mass-spectrometric on-line gas analysis ensures better process understanding, simplifies monitoring and reduces drying times

The PAT Initiative of the American Food and Drug Administration (FDA) requires that manufacturers of pharmaceuticals incorporate and maintain systems for the continuous monitoring and control of production processes.

The mass spectrometric determination of solvent concentrations or solvent partial pressures in the gaseous atmosphere of a drying apparatus provides data sets that are very suitable for optimising drying processes.

The drying curve may be tracked and documented online with the mass spectrometer. As soon as the correlation to the Loss-On-Drying (LOD) values has been determined, the end of the drying process can be immediately identified through the mass spectrometric data. The resulting time savings allows for an improved plant utilisation and reduces energy costs. The redundance of unnecessary offline analyses also contributes to cost reduction.

The mass spectrometric data gives important information for optimisation of the temperature, pressure and carrier gas parameters in process development, particularly with regard to influencing the sequence of individual drying steps if these involve several solvents. It is also easy to detect critical dryer conditions (leakages, starting disintegration of the product, etc.).

Flyer Dryer - MS

White Paper - Dryer Application

By deploying the GAM 3000 at various points it is possible to precisely determine the composition of gases thereby provide important information for monitoring and controlling blast furnace processes. The acquired data can for example be used to monitor the hydrogen content and secure ideal process control.

The GAM 3000 process gas mass spectrometer is most successfully deployed in the analysis of converter gas. By continuously monitoring converter waste gases it is possible to identify the current process status at any given time. The data provided by the GAM 3000 can be used to model the entire process. Hence the blowing cycle can be shortened and process disruptions prevented.
Converter gas analysis can substantially reduce energy consumption and optimize steel quality. Compared with traditional converter control methods the GAM 3000 is the economical alternative.

Converter gas analysis

The large-scale production of ketene from acetic acid can be optimised with the help of mass spectrometers. This requires the online analysis of the reactant and product composition.
Samples of the product composition are extracted from the reactor under low-pressure and continuously analysed by a GAM300. This is essential for the adjustment of the reaction process to improve the quality and yield.
The crutial calibration of about 20 components in this complex reaction mix is elaborate and was part of the entire development of this method. The excellent long-term stability of the GAM300 made it first possible to successfully deploy this technique.
The optimisation of the process parameters with the help of the data provided by GAM300 increase the yield by 13 percent. At the same time by reducing impurities it was possible to substantially increase the quality of the ketene.

Ketene production

Separation of Helium and Deuterium

Experiments with nuclear fusion require exact knowledge of the helium-deuterium ratio. The mass of both elements (about 4 amu) varies only by approximately 0.025 amu. Only high-quality quadrupole analysers can reliably perform this demanding analytical task.

He/D₂ separation with GAM 400

Use of Quadrupole Mass Spectrometers for the Automatic Online Determination of Isotope Ratios of the Stable Isotopes ¹³Carbon and ¹⁵Nitrogen

Quadrupole mass spectrometers are highly efficient mass spectrometers with a wide dynamic measuring range. They are robust and compact in design and are relatively simple to use and maintain. In addition they are also comparatively inexpensive. Hence quadrupole mass spectrometers are the clever alternative to standard magnetic mass spectrometers when it comes to the online determination of isotope abundance of light elements in isotopically enriched samples in a continuous flow environment.

Isotope ratio analysis with QMS

SPINMAS - Instrument and Method for Automatic and Sensitive Determination of ¹⁵N-Abundance in Inorganic Compounds of Aqueous Samples

The mass spectrometers GAM 400 and ESD 100 in conjunction with our new sample preparation device SPIN (Sample Preparation for Inorganic ¹⁵Nitrogen) enables the sensitive and selective determination of ¹⁵N abundance in ammonia, nitrite and nitrate in aqueous samples. The minimum amount of nitrogen is 0,1 µg and a simple test takes approx. 8 minutes.

SPINMAS

The usage of hydrogen in energy technologies has huge potential. Unlike fossil fuels it can be generated from renewable energy sources. It is also non-polluting and forms water as a post-combustion product. The storage of hydrogen still remains a problem so that the distribution and utilisation of this fuel has been limited.

Measurement of hydrogen release from metal hydrides

Characterising Polymer Electrolyte Membranes for Direct Methanol Fuel Cells with Online Mass Spectrometry

The development and characterisation of polymer electrolyte membranes (PEM), which are to be used in direct methanol fuel cells (DMFC), requires a variety of properties such as low methanol permeability. Methanol diffusing through the membrane leads to a loss in fuel cell performance.
Online mass spectrometry is perfectly suited to quickly and precisely determine the membrane quality.
A membrane test cell developed by Fraunhofer Institute for Chemical Technology (ICT) allows the determination of the transport parameters of proton-conducting membranes using an online mass spectrometer.
In addtion to methanol diffusion, methanol permeation and electroosmotic drag, the test determines the proton conductivity of the membrane.
The test can determine all four parameters in correlation with temperature.

Reprint (German) "Permeation through membranes"

Ultrapure and customized blended gases are becoming increasingly important in the development of modern technologies. The demands placed on ultrapure gases and the variety of gas blends present manufacturers and users with new challenges in production, quality control as well as in the deployment and use of these gases and gas blends.

The analytics required is becoming increasingly complex and requires the combination and deployment of various methods. Mass spectrometry is a valuable supplement to the standard methods (GC, IR, UV etc.) and a number of gas-specific methods. It is perfectly qualified for handling the broadest range of process challenges.

Reprint (German) "Quality assurance for special gas mixtures"