Nuts and Bolts of Mass Spectrometry

The short course is designed to develop understanding and key practical skills for early stage researchers in Earth Science who use sector-field, isotope ratio mass-spectrometry (i.e. multi-collector plasma, and thermal ionisation instruments). 

The course will be consist of lectures, discussion sessions and some paper-data handling exercises. Participants will be expected to share their own experiences in measurements and gain insight not only from the taught components but also by discussion with other users with a wide range of experience. Each day will deal with different main topics: Day 1, hardware, Day 2, sample preparation and calibration, Day 3 data handling and uncertainties.

This course was held January 2012 at the School of Earth Sciences, Bristol University.

More information about this course can be found here.

Day One:  Hardware

Introduction

  • Ion sources
  • Mass analysers
  • Detectors
  • Examples of instruments

Ion optics

  • Current and charge
  • Electrostatic and Magnetic Fields
  • Motion of charged particles
  • Mass calibration and magnet control
  • Geometric optics
  • Focusing by electrostatic and magnetic sectors
  • Energy (double) focusing

Measurement

  • Peak shape
  • Mass resolving power
  • Nuclear mass defect
  • Abundance sensitivity
  • Faraday cups
  • Ion counting

Day Two:  Calibration and Sample Preparation

Lecture 1: Introduction
Lecture 2: Reference Materials part I
Lecture 3: Reference Materials part II
Lecture 4. Methods for measuring U isotopic using TIMS and UF6 Mass spectrometry
Lecture 5. Isotope dilution and tracer calibration (mixed elemental and/or isotopic)
Lecture 6. Principles of sample analyses by microbeam methods (mainly LA-ICP-MS)
Lecture 7. Sample purification by ion exchange

Day Three:   Data reduction and Uncertainties

Lecture 1: the language of uncertainty, error, bias, precision, accuracy.  What do they all mean?
Lecture 2:  Measurement uncertainty-some basics
Lecture 3:  Limits of detection, background evaluation and assessing performance
Lecture 4: Uncertainty/error propagation
Lecture 5: Over-determined systems

 

Some light reading...

There are lots of great things to read in the Royal Society of Chemistry’s Analytical Methods Committee (AMC) Technical Briefs series:
#15 Is my uncertainty estimate realistic?
#13 Terminology - the key to understanding analytical science: Part 1: Accuracy, precision and uncertainty

Some not so light reading...

H.E. Duckworth, R.C. Barber, and V.S. Venkatasubramanian. Mass Spectrometry 2nd ed. Cambridge (1990).

A. Septier. Focusing of Charged Particles. Vols I and II. Academic Press (1967).

M.E. Wieser and J.B. Schwieters. The development of multiple collector mass spectrometry for isotope ratio measurements. Int J. Mass Spectrom. (2005) 242, 97-115

J.M. Hayes and D.A. Schoeller. High precision pulse counting: liminations and optimal conditions. Anal. Chem. (1977), 49(2), 306-311.

A. Montaser. Inductively coupled plasma mass spectrometry. Wiley-VCH (1998).

John F. Rudge, Ben C. Reynolds, and Bernard Bourdon, The Double-Spike Toolbox, Chemical Geology (2009), 265, 420–431