Mass Spectrometry & Spectroscopy 11
New Reaction Monitoring Solutions for Benchtop NMR Spectrometer Released
Magritek have released new solutions that enable straightforward reaction monitoring on the Spinsolve benchtop NMR spectrometer. This is complemented with a series of applications notes illustrating the multiple uses for the Spinsolve benchtop NMR spectrometer.
With high stability and spectral resolution Magritek’s Spinsolve delivers measurements that are quantitative with only minimal calibration. The signal has a linear response to concentration and it is generally not sensitive to the matrix. Results are representative of the complete sample and the measurement is non-destructive.
To enable the Spinsolve spectrometer for reaction monitoring Magritek have created full solutions with either glass flow cells or PTFE flow tubing that fit through the completely clear bore of the instrument. The glass flow cell option offers a large sample volume in the sampling region of the spectrometer and a narrow internal diameter outside of that zone. This gives the maximum signal to noise output with minimal fluid in the flow system. The hardware kit is completed with a peristaltic pump, appropriate tubing, and a stand to provide access below the spectrometer. Complementing the hardware is the full experiment scripting capability and pump control available in the latest instrument software. Stop-flow or continuous flow monitoring is straightforward to set up.
A range of application notes available on the Magritek website help Spinsolve users solve specific problems. For example, consider fermentation processes. This is a naturally occurring chemical event. One application note describes how easy it is to monitor a simple fermentation process - to follow the conversion of fructose and glucose into ethanol and carbon dioxide - and to easily get chemical conversion rates and to see where the optimal end point has occurred. The note shows that a simple flow loop setup allows on-line reaction monitoring on a lab bench. While shimming was performed at the start of the experiment on the reactant itself, no extra shimming was required during the ten day experiment. Even gas bubbles in the measurement volume did not disrupt subsequent measurements.
Another application note describes the study the hydrolysis of acetic anhydride by water. Rate constants can easily and reliably be obtained by plotting the peak height or integral of a characteristic peak as a function of reaction time. The activation energy of the process can be determined by carrying out the reaction at different temperatures.
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New White Paper Details Advantages of Simultaneous ICP-OES Elemental Analysis for Cost-Effective Condition Monitoring
Spectrometer-based elemental analysis has become a fundamental technique for condition monitoring (CM) in most service laboratories. A new white paper, ‘Cost-Effective Condition Monitoring’, details why a simultaneous ICP-OES instrument is a serious economic alternative to sequential ICP and atomic absorption spectrometry for elemental analysis in condition monitoring.
The paper includes a complete explanation of basic ICP-OES principles and processes, from sample preparation to plasma generator to the optical system and detectors through to the software developed to interpret measurement data. Using the Spectro GENESIS simultaneous ICP-OES spectrometer as a test instrument, the paper references the typical limits of detection for related elements in condition monitoring. The paper also describes advantages of the Spectro GENESIS’ suitability for elemental analysis in condition monitoring and details its cost advantages versus sequential ICP and AAS analysers.
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5916ad@reply-direct.com Flame Joins ‘Trail by Fire’ Expedition
Ocean Optics has sponsored a team of volcanologists on a mission to study volcanoes in the South American Andes, providing Flame miniature spectrometers and accessories. The ‘Trail by Fire’ project, funded by a grant from Land Rover and the Royal Geographical Society, will attempt to quantify the total amount of volatile chemical elements released by volcanoes in Chile and Peru. Ocean Optics’ Flame spectrometers will be flown directly below volcanic plumes on UAVs, taking differential optical absorption spectrometry (DOAS) measurements to quantify sulphur dioxide (SO2
) levels, with the goal of better understanding volcanic effects on climate.
The Flames will be part of world’s first mobile volcano observatory, a specially outfitted Land Rover Defender 110, reaching some of the most remote and hard to study volcanoes on earth. Faced with difficult to navigate terrain and high altitudes, the team chose TurboAce Matrix UAVs to carry the Ocean Optics spectrometers to the volcanic plumes for measurement. Using UAVs allows the researchers to get closer to the plume and collect a full cross section of measurements. This will provide higher accuracy than the ground-based measurements typically used in DOAS. The Flame’s small size and low weight (265 g) were key factors in its selection, as payload weight, always an important consideration for UAVs, is especially critical at high altitude.
More importantly, despite its small size, the Flame offers the high resolution and thermal stability required for DOAS measurement, allowing the team to measure very small fluctuations in SO2
content.
The spectrometers are controlled by the UAV’s onboard microprocessor, integrated with Ocean Optics’ open source SeaBreeze drivers.
Spectra collected by the Flame are saved to the UAV’s onboard memory and wirelessly beamed back to the ground station. This real-time feedback will allow the team to verify operation and make measurement adjustments as the UAV is in flight. The spectrometer’s modular design, with interchangeable slits to adjust resolution and throughput, will enable the team to respond quickly and easily to changing conditions in the field.
“This is truly a great application for our next generation miniature spectrometers,“ explained Ocean Optics Product Manager Henry Langston. “We love the opportunity to partner with our users, helping them take our science to new places. This is why we have a team of applications engineers on staff, to work with customers to solve challenging measurement problems. It’s been so exciting to see the Trail by Fire project come together.”
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Mass spectrometers for vacuum, gas, plasma and surface science QGA CATLAB-PCS
QGA Gas Analysis System
Fast data acquisition 500 measurements/sec Response time to 150 ms Dynamic range PPB to 100%
Microreactor with integrated MS detector
TPD/TPR/TPO and reaction studies 1-20°C/min heating rates Temperature ramps up to 1000°C Close-coupled hotzone for 500 ms response
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