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NAA using Kayzero: from peak areas to element concentration. R. van Sluijs , k 0 -ware, Heerlen, the Netherlands D. Bossus, DSM Geleen, the Netherlands F. De Corte, RUG, Ghent, Belgium. Element concentration, ρ. Peak area, A. k 0 -method. Problem? No problem!?. - PowerPoint PPT Presentation
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19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
1
NAA using Kayzero: from peak areas to element concentration
NAA using Kayzero:from peak areas to element
concentration
R. van Sluijs, k0-ware, Heerlen, the Netherlands
D. Bossus, DSM Geleen, the NetherlandsF. De Corte, RUG, Ghent, Belgium
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
2
NAA using Kayzero: from peak areas to element concentration
Problem? No problem!?
k0-methodPeak area, A
Element concentration, ρ
Simple? Perhaps not, but very well documented! nowadays there are many programs to help!
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
3
NAA using Kayzero: from peak areas to element concentration
No problem,but ..... (1)
How to get the correct peak area?
Use a perfect gamma spectrometry system and keep it in the best possible condition!
Use the perfect gamma spectrum deconvolution program!
However: who has this perfect set-up?
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
4
NAA using Kayzero: from peak areas to element concentration
No problem, but......... (2)
How to select the analytical line K0-library has data for 68 elements, 144 nuclides and
more than 700 gamma-lines For a panoramic analysis you use preferably 2
irradiations (short and long) each followed by 2-3 measurements
A single element will give data for several nuclides and probably tens of gamma lines.
All we want one single list:Containing the all elements with their concentrations and/or limits of detection.
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
5
NAA using Kayzero: from peak areas to element concentration
DSM’s/Kayzero’s method
Optimise the peak table! Peak Table: Area’s and Energies from gamma
spectrum deconvolution program
Calculation Concentrations for all lines in the k0- library
EvaluationIdentify the nuclides in the sample Correct for gamma interferencesCalculate averages per nuclide and per element Average over all measurements
Refine the results
User Input
Automatic
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
6
NAA using Kayzero: from peak areas to element concentration
Optimise the peak table!
Peak Areas: Broadened peaks (due to count rate effects, bad
pile-up correction, etc..) can be split by the gammaspectrum deconvolution program into two separate peaks.
Sum the false/artificial peaks for a correct result Peak locations:
Linear energy calibration, non-linear is often better
Re-do the energy calibrationHypermet shifts data 1 channel to the left Shift back
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
7
NAA using Kayzero: from peak areas to element concentration
Measurement Input screen
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
8
NAA using Kayzero: from peak areas to element concentration
Peak summation screen
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
9
NAA using Kayzero: from peak areas to element concentration
Re-do energy calibration
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
10
NAA using Kayzero: from peak areas to element concentration
k0-calculations
Calculate concentrations for all library linesIncluding Corrections for:
background, dead-time, gamma-absorption, burn-up, neutron self absorption, True-coincidence correction
No matching peak: the LD concentration is calculated using the spectrum base line.
No result if calculated concentration >100%
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
11
NAA using Kayzero: from peak areas to element concentration
Evaluation of the results: Check the presence of a nuclide
0
20
40
60
80
100
1 2 3 4
Energy
Con
cent
ratio
n
Limit of Detection
positive
negative
positive neutral
4 energies of nuclide X
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
12
NAA using Kayzero: from peak areas to element concentration
Evaluation of the results:Check the presence of an
element
0
20
40
60
80
100
Nucl. A/Meas.1
Nucl. A/Meas.2
Nucl. B/Meas.1
Nucl. B/Meas.2
Nuclide data from 2 measurements
Co
nce
ntr
atio
n
Limit of Detection
positive
negative
positive neutral
Nuclide data of Element X
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
13
NAA using Kayzero: from peak areas to element concentration
Evaluation of the resultsCorrect for gamma interferences
0
20
40
1 E 2 3Energy
Co
nce
ntr
atio
n
Average this nuclide is producing 50% of the area in line E =Cn, aver./Cn,E
)1(1 ,
.,,,,
N
n En
avernEacorrectedEa C
CCC N=number of interfering
nuclides on line E
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
14
NAA using Kayzero: from peak areas to element concentration
Evaluation of all results Calculate averages and standard
deviations • over the lines of a nuclide
• weighing factor wi= 1/σ2i
• σobserved should be approx. equal to σexpected
w1)-(n
)-(w=
i
2ii
obs
)w(
)w(= 2i
2ii
exp
w
w=
i
ii
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
15
NAA using Kayzero: from peak areas to element concentration
Refine the resultsselect the analytical lines
Select by hand:gamma’s to be used correct for threshold, fission,
second-order reaction interferences,
blank correction,
Alarm for high epi-thermal self shielding
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
16
NAA using Kayzero: from peak areas to element concentration
Ba-131: large observed SD
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
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NAA using Kayzero: from peak areas to element concentration
Deselect Ba-131 line
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
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NAA using Kayzero: from peak areas to element concentration
Fission Correction for La-140
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
19
NAA using Kayzero: from peak areas to element concentration
Fission Correction
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
20
NAA using Kayzero: from peak areas to element concentration
Blank subtraction
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
21
NAA using Kayzero: from peak areas to element concentration
The goal of all our work:a (digital) list of concentrations
19/04/23www.kayzero.com
NAMLS-8, Rio de Janeiro, April 17th-22nd 2005
22
NAA using Kayzero: from peak areas to element concentration
Conclusion
k0-method (DeCorte/Simonits) is a very complete method, all
aspects of INAA are taken into account, elaborate calculations are needed but this is no problem nowadays
The method presented to handle k0-data is based on almost
20 years of experience, analysing all kinds of samples
Evaluation of the data of a panoramic elemental analysis of an unknown sample takes less than half an hour
Although very much automated: the analyst is in control
The competition in our lab is though, NAA is the most expensive technique so quality and reliability is a prerequisite