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in > Training > Overview > Practical Training Courses |
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Practical Training Courses
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Practical LC-MS
Practical HPLC Troubleshooting & Maintenance
Practical GC Troubleshooting & Maintenance
HPLC Method Development
Practical GC-MS
Practical GC Method Development
Practical 'Fast' HPLC |
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Run at our laboratory facilities in Manchester, these hands-on courses are designed to introduce both theory and practical concepts of instrumental analysis. Modern equipment is used in conjunction with interactive teaching techniques and well established practical exercises to ensure maximum return on your training investment.
These courses are invaluable for anyone wishing to have the most comprehensive grounding in instrumental analysis techniques or those wishing to increase their knowledge and practical ability with our advanced training programs.
There are only SIX places on each of these courses to allow maximum training impact – very early booking is advised as these courses are very popular indeed.
More information – click here
Register – click here
Practical LC/MS |
(practical exercises and experiments in italics)
Day 1
- Overview of Atmospheric Pressure Ionisation Techniques
- HPLC Considerations for LC-MS
- Flow Rate and Flow Splitting Considerations
- Eluent Design for LC-MS
- Modern Column Chemistry for LC-MS
- Design an HPLC method suitable for MS Analysis
- Electrospray Ionisation Theory & Instrumentation
- Atmospheric Pressure Ionisation Theory & Instrumentation
- Calibrating and Tuning the LC-MS
- Tuning and Optimising the Electrospray Interface Parameters
- Tune, calibrate and optimise the MS system
- Choosing API Mode, Alternative Sources and Multi-mode sources
Day 2
- Designing Spectral Experiments – Scan v’s SIM Acquisition for Qualitative or Quantitative Operation
- Quantitative Analysis using the MS Detector (Calibration / External vs Internal Standard / Isotopically Labeled Standards / Limit of Detection etc.)
- Design and Implement a Quantitative LC-MS Analysis to quantify an unknown at low concentration
- Qualitative Analysis using the MS Detector (In-house libraries / Peak ID & Library Searching)
- In-Source Collsion Induced Dissociation (CID)
- Introduction to Spectral Interpretation
- Design and Implement a Qualitative LC-MS Analysis to identify a suspected contaminant
- LC-MS Diagnostics and Introduction to LC-MS Routine Maintenance
- Carry out Routine LC-MS Maintenance exercise
Course Duration: 2 days
Course Hours: 9:00am – 5:00pm
Course Pre-requisites: A basic working knowledge of mass spec operation is helpful but this course can be also undertaken by complete novices with no prior hands-on experience
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Practical HPLC Troubleshooting & Maintenance |
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(practical exercises and experiments in italics)
- Instrument problems – identifying the issue
- Common Maintenance Schedule Operations
- Maintenance of Pumps - pistons, mixers etc.
- Maintenance of Autosamplers – Rheodyne valves, seals, metering devices, syringes etc.
- Maintenance of detectors – Flow cell clean, Lamp replacement
- Common Calibration and Investigative Operations
- Log-keeping
- Calibrating Pump Flow
- Calibrating Autosampler volume
- Calibrating detector wavelength and response
- Testing Lamp Intensity
- Testing Flow Cell Cleanliness
- Calibrating Column Temperature
- Chromatographic Problem Solving
- Baseline problems
- Peak Shape Problems
- Retention Time Drift
- Peak Area Irreproducibility
- Putting it all together
- Commissioning an HPLC system from storage to tackle a particularly tricky separation!!
Course Duration: 2 days
Course Hours: 9:00am – 5:00pm
Course Pre-requisites: Experience with working with HPLC equipment is advantageous but not essential
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Practical GC Troubleshooting & Maintenance |
(practical exercises and experiments in italics)
- Instrument problems – identifying the issue
- Common Maintenance Schedule Operations
- Importance of good quality gas supply
- GC Inlet Maintenance ( Split / Splitless) – including liners
- GC Detector Maintenance (FID practical) – also consider TCD / ECD / NPD
- Column Installation Conditioning and Storage
- Common Calibration and Investigative Operations
- Log-keeping
- Testing the inlet for leaks
- Establishing proper split flows - differences between split and splitless injection
- Establishing the hold-up time and calibrating the pressure control system and carrier gas flow
- Optimising detector settings
- Chromatographic Problem Solving
- Baseline problems
- Peak Shape Problems
- Retention Time Drift
- Peak Area Irreproducibility
- Putting it all together
- Commissioning a GC system from storage to tackle a particularly tricky separation!!
Course Duration: 2 days
Course Hours: 9:00am – 5:00pm
Course Pre-requisites: Experience with working with GC equipment is advantageous but not essential
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HPLC Method Development |
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(practical exercises and experiments in italics use a mixture of HPLC experiments and simulations using LC optimisation software)
- Choosing columns – column dimensions, particle size, selectivity differences
- Optimising throughput using reduced column dimensions and particle size
- Optimising separation selectivity through stationary phase choice
- Using software to predict suitable columns
- Sample concentration, injection solvent, injection solvents
- Reverse phase HPLC:
- Solvent Choice
- Quick ways to optimise %B
- Analyte pH – influence of pKa and eluent pH on analyte retention
- Altering eluent pH to optimise separations
- Predicting and optimising separation robustness
- Choosing appropriate buffers and influence of buffer concentration
- Ion Pair Chromatography
- Influence of ion pair reagent type and concentration
- Gradient HPLC
- Characterising your system (dwell volume, re-equilibration volume etc.)
- Scouting Gradients
- Estimating Isocratic Conditions
- Calculating gradient conditions (starting and ending composition and gradient time)
- Bringing it all together
- Developing a method from scratch using all of the tools and tricks learnt on the course
Course Duration: 2 days
Course Hours: 9:00am – 5:00pm
Course Pre-requisites: Some experience of operating HPLC equipment and analysing HPLC data is required in order to fully participate in this course
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Practical GC-MS
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(practical exercises and experiments in italics)
- GC Considerations for GC-MS
- Appropriate carrier gas and flow rate Column choices GC method parameters
- Ionisation in GC-MS – Electron Impact (EI) and Chemical (CI) Ionisation
- Ion Sources and Transfer Lines
- Ion source components and operating parameters Cleaning Ion Source Components
- Auto-tuning and manual tuning
- Interpreting tune reports Optimising the MS detector through manual tuning
- Quadrupole Mass Analysers - principles
- Experiment parameters – optimising SCAN and SIM experiment variables
- Ion Trap Mass Analysers – principles and typical data
- MS n – advantages and uses Data dependant scanning
- Detectors in GC-MS
- GC-MS Vacuum Systems
- Monitoring vacuum Establishing and breaking vacuum correctly Maintaining the vacuum system
- Bringing it all together
- Developing a GC-MS method for a particularly challenging determination
Course Duration: 2 days
Course Hours: 9:00am – 5:00pm
Course Pre-requisites: Some experience of operating GC-MS equipment and analysing GC-MS data is required in order to fully participate in this course
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Practical GC Method Development
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- Establishing Method Objectives
- Existing Information - what is known, what should be known
- Chromatographic Theory Overview
- Mechanisms of Separation
- Equilibrium and the Distribution Constant
- Solute - Stationary Phase Interaction
- Sample Preparation Protocols
- Injection System Choice - spilt / splitless, on-column, direct, PTV, headspace. (Each of the above will be considered with reference to the physical properties of the analyte / matrix / solvent which govern choice)
- Carrier Gas Choice
- Column Choice (stationary phase chemistry choice as governed by the analyte/s)
- Detector System Choice / Operation, including FID, ECD, TCD, MS etc. (Once again, each of the above will be considered with reference to the physical properties of the analyte/matrix/solvent which govern choice)
- Measuring and Optimising Chromatographic Parameters
- Capacity Factor (k), Efficiency (N), Selectivity ( a ) and Resolution (R)
- Temperature Effects
- Appropriate Methods of Quantitation
Course Duration: 2 days
Course Hours: 9:00am – 5:00pm
Course Pre-requisites: Some experience of operating GC-MS equipment and analysing GC-MS data is required in order to fully participate in this course
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Practical ‘Fast’ HPLC
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This course is designed as a comprehensive introduction to the principles and practice of Fast and Ultra-Fast HPLC.
The course is a mix of theory, computer simulation and lab sessions that allow the student to quickly gaink nowledge on the theory, practice and limitations of the common approaches to speeding up HPLC analysis.
The main factors in speeding up analysis – reduced column dimension, sub 2ım particles, superficially porous silica all combined with elevated temperature and pressure - are discussed in detail and method conversions are attempted practically.
Instrumentation is also taken into account and the various approaches to Fast HPLC using conventional pressure as well as Ultra High Pressure system hardware and the importance of extra column volume and hysteresis effects are also discussed and demonstrated.
The overall aim of the training is to ‘enable’ clients to speed up existing separations or to develop novel ‘Fast’ HPLC separations.
- Introduction
- Acronyms and Nomenclature
Theory of Fast & Ultra Fast HPLC
- Why Fast HPLC – separation speed as a limiting factor in analysis
- Resolution / Selectivity / Efficiency (Chemistry and Physics!)
- Broad Choices for Optimising Efficiency
- Optimising Plate Number – different theories and approaches
- Superficially Porous Silica
- Sub 2um Silica
- Monolithic Silica
- Effectively measuring plate number / reduced plate heights / Poppe Plots
- So what happened to selectivity?
- Effects of high pressure on Solvent and Column Properties
- The influence of column geometry
- Importance of temperature control
- Temperature and flow rate interdependence (the cost / bar!)
- Instrument requirements (delay volume, extra column volume, acquisition rates)
- Simple Software tools for scaling separations
- Transferring & Developing Methods:
- Sub 2 μm method transfer and optimisation
- Superficially Porous Silica meth transfer and optimisation
- Client method student optimisation / test sample optimisation
- Review and close
Course Duration: 1 day
Course Hours: 9:00am – 5:00pm
Course Pre-requisites: Some experience of operating HPLC equipment and analysing HPLC data is required in order to fully participate in this course
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