Professional Documents
Culture Documents
An introduction to stable
isotope mass spectroscopy
Stable Isotope analysis
Sample preparation
Chemically convert sample material (ie rocks, water, biological materials)
into gas
Quantitative
Normalization of results
Laboratory references
International standards
Stable Isotope mass specs are
gas-source
D/H H2
18O/16O CO2, CO, O2
C/12C
13 CO2, CO
15N/14N N2
34S/32S SO2, SO, SF6
Cl/35Cl
37 CH3Cl
Combust:
(C6H10O5)n + O2 CO2 + H20
(C6H10O5)n + C CO + H2
Reduce:
H20 + Zn H2 + ZnO
React:
SiO2 + BrF5 O2 + SiF2
O2 + C CO2
Equilibrate:
C16O2 + 2H218O C16O18O + 2H216O18O
Purification
Vacuum lines
Cryogenic (LN2) traps for
separation of gasses
He
TCD detectors
Combustion/Reduction
Automation Mass
Spec
On-Line
Mass spectrometers
JJ Thomspon 1910 parabola
spectrograph
Discovered first stable isotopes (Ne mass 20-22)
Discovered the electron
Awarded nobel prize 1906
Source of ions
M+ Pumping system
Diffusion or turbo
pumps
Analyser =
Magnetic sector
Detectors
-Faraday cups
-electronic ion
counting
Ion Source
Electron Impact source: M + e- M+ + 2e-
Problems:
-Linearity current const
measured ratios
-memory
-stability
Burn marks
Extraction
Fine-tuning
Generally
empirically tuned
Problem areas of source design
1. Deviations from linear behavior discrimination
ion-molecule interactions forming isobaric interferences
ie H3+
collimating magnetic field can lead to non-linear
response
changes in number of ions affects space charge of
ion-source therefore extraction conditions
careful source design
more important in CF instruments.
Problem areas of source design
2. Gas exchange
Minimize gas exchange in ion source
Pumping efficiency of source region
Avoidance of dead volumes
Chemical inertness of source materials
Filament chemical inertness and
conditioning
Problem areas in ion sources
3. High stability over time
electrostatic potentials need to be
Error sources
-Secondary electrons
Circuit where charged ions are
-backscattering
the charge carriers in vacuum
N/t = I/e
N/t= #of ions/sec, I= current,
e= elementary
charge(1.6x10-19 C)
GC techniques coupled to MS
No change over or dual inlet
Viscous flow in GC stream
Smaller sample sizes
Completely taken over most modern
analyses
Well suited for automated analyses
3. Valve mixing
-mixing of reference and sample
gasses in the changeover valve
by cross seat leakage
- new changeovers minimize
this
Computation of values
HDO
H2O
Absorption spectrometry is a
direct measure of concentration