Mass Spectrometry for Chemists: Direct Analysis of TLC Plates, Solids and Gases

TLC/CMS, the atmospheric liquids and solids probe (ASAP), and the volatile APCI source provide direct analysis without sample preparation – even for air-sensitive compounds.

With the daily need to analyze a variety of samples, these techniques are indispensable in a busy lab.

Learn how a single instrument can be adapted to each of these sample requirements and rapidly changed to accommodate back-to-back assays. Listen to users in the field speak about the innovative sample inlets that have cut down on sample prep and streamlined their everyday work flow.

During this webinar you will:

  • Learn how the CMS offers real-time results and decision making right at the bench. This allows chemists to optimize reactions, know when to quench, and know when they have failed and to move on
  • Learn several novel sample techniques that can streamline workflow in your lab
  • Find fast analysis methods for liquids, solids and vapor-phase compounds

Hear from leaders in mass spectrometry including:

  • Dr. Jack Henion, Advion Scientific Founder
  • Matthew Turner, Experimental Officer in Mass Spectrometry, Department of Chemistry, Loughborough University
  • Tao Yongfeng, Post Doctorate, The Romo Group, Baylor University
  • Sean M. Kerwin, PhD, Associate Professor, Department of Chemistry & Biochemistry, Texas State University

Synthesis and full characterization of an iridium B–H activation intermediate of the monocarba-closo-dodecaborate anion

The preparation and full characterization of an iridium complex of the monocarba-closo-dodecaborate anion is reported. It was prepared by B–H bond activation using a tosyl amide directing group.

Analysis by spectroscopic methods and X-ray crystallography revealed the presence a direct B–Ir interaction. The carborane acts as aB,N chelating ligand towards the Ir(Cp*)(solvent) fragment, resulting in a monomeric complex that is inert in solution and the solid state.

Treatment with N-chlorosuccinimide resulted in selective monochlorination of the B–Ir position. In addition, its structure, spectroscopic features and reactivity were investigated by DFT calculations.

University of Cambridge, Ley Group

Q: WHAT IS THE FOCUS OF YOUR LAB’S RESEARCH?
A: One of the focus points for Ley Group research is the development of continuous flow synthesis methods. We aim to include new enabling techniques into our work to facilitate the collection of data relevant to the reactions we conduct. We work across the early synthesis spectrum – from discovery to scale-up and process development.

Q: WHAT WAS YOUR PREVIOUS WORKFLOW AND EXPERIENCED CHALLENGES? 

A: Standard detectors we use in our work can be problematic when trying to discern what is in a product mixture leaving a flow reactor. For example, UV detectors are useful only in very restricted flow-based situations and don’t give compositional information. IR is a step up from this, but suffers from issues when peaks in starting materials, products and by-products overlap. Some transformations may also lead to undetectable changes in an IR spectrum. While flow-based NMR can be good when it’s usable, its expense and lack of resolution at a bench-top level hinder its utility.

Q: WHY DID YOU INCORPORATE THE EXPRESSION® CMS INTO YOUR LABORATORY? 

A: The expression® CMS struck the perfect balance between cost, ease-of-use and detection capabilities that we needed for our research. We’re able to get large amounts of relevant information about reaction mixtures, in real-time, without worrying in most cases about overlapping peaks or detection signals. This information is used by our control systems to make decisions about product stream composition, allowing us to automate procedures such as reaction telescoping, process start up and self-optimization. The expression® CMS software is fantastic also – everything is recorded, letting us go back over the raw data to gain even more insights into how product compositions change over time in our processes.

Q: TO WHOM WOULD YOU RECOMMEND THE EXPRESSION® CMS? 

A: I would recommend the system to any group that works with continuous flow chemistry, especially those that need real-time analysis of stream compositions. The ease at which the unit can be integrated into any process makes it an extremely attractive unit to use. It’s also very easy to switch the expression® CMS into a standalone MS unit for independent sample analysis, making it versatile in any organic chemistry laboratory.

Q: HAVE YOU CONTRIBUTED TO ANY PUBLICATIONS USING THE EXPRESSION® CMS?

A: Org. Process Res. Dev., 2016, 20, 386–394

vAPCI: How it Works

Direct sample analysis of liquids, solids and powders without chromatography is as easy as it sounds, and provides mass spectral information within seconds. The video demonstrates analysis of a reaction mixture.

iASAP: How it Works

The inert Atmospheric Solids Analysis Probe (iASAP) allows easy sampling of air-sensitive compounds, such as metal catalysts and organometallics, from reactions that are carried out in a glovebox or Schlenk line.

Peak Express™ Software: For the Analytical Chemist

Introducing a new type of mass spectrum, available exclusively in the Advion Peak Express™ software suite: the Delta Spectrum (ΔS). The ΔS is available with the expression compact mass spectrometer (CMS) to look beyond chemical noise and automatically detect even the smallest peaks without knowing the m/z in advance.

With the Peak Express™ software, you can:

  • Find minor components and impurities you would otherwise miss
  • Find unknowns in complex samples like natural products
  • Acquire XIC-quality data while scanning the entire mass range, allowing Peak Express™ to tell you the m/z
  • Perform real-time, mass-directed purification without knowing the mass Realize automatic ‘expert’ data processing

TAMI Molecular Identification Software Suite for expression® CMS

Turn your expression® CMS into a high resolution, exact mass instrument in its ability to provide elemental formulae. TAMI uses accurate centroiding and mass correction algorithms to provide a more accurate mass assignment.  In combination with isotope abundance analysis and careful consideration of chemical valence rules this provision of elemental formulae with a high level of confidence.

TAMI includes a post-run mass calibration tool that further increases the mass accuracy of your data. TAMI software is accessed directly from Data Express as you process your data.