results of the 18 and 19 needle/leaf interlaboratory...
TRANSCRIPT
![Page 1: Results of the 18 and 19 Needle/Leaf Interlaboratory ...api.ning.com/files/hcNvTm2sJjUP0Za-P1O31Tv1UgPrcg9... · Alfred FÜRST Forest Foliage Co-ordinating Centre Pallanza/Italy 7.9](https://reader036.vdocuments.us/reader036/viewer/2022062907/5a7c77917f8b9a49588cc809/html5/thumbnails/1.jpg)
Alfred FÜRST
Forest Foliage Co-ordinating Centre
Pallanza/Italy 7.9. – 8.9.2017
ICP-FORESTS - 6th Meeting of the Heads of the Laboratories
Results of the 18th and 19th Needle/Leaf Interlaboratory Comparison Tests
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Overview
General information about both tests
Main results
Common methods
Problematic parameters / laboratories which failed in both tests
Re-qualification 18th and 19th test
Reference samples
Enlarge parameter list (heavy metals)
Ongoing foliage ringtest program
Database update with new parameters
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Needle/Leaf Interlaboratory Comparison tests
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Countries/Laboratories
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Participating labs decreasing
Stop funding of the monitoring program
Participating only in uneven years - paralell to the monitoring
activities (20th, 18th, 16th Test, ….)
Closing and/or merging of labs
Costs of the ringtest…
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240 € are too expensive?
= 7 l nitric acid 65%
= 100 ml multielement standard
= one PTFE vessel for microwave digestion
= 4 working hours of a lab worker
And how expensive are wrong results??
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Comparison between 7th and 19th Test
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Comparison between 7th and 19th Test
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Difficult Samples & Elements
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Percentage of non tolerable results in
Needle/Leaf samples
%
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Labs failed with the same element/s
in both tests
Germany A59 (C)
Germany A79 (Mg)
Germany A80 (Zn)
ICP-Forests lab - Croatia A62 (Ca, Mg)
ICP-Forests lab - Spain F33 (Fe)
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Re-qualification process
Please, ask your colleagues if they have similar problems!
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What influences data quality? Results of the questionaire:
Laboratory accreditation
Higher number of analyzed samples/a
Control charts
Staff trained on the method/matrix
More than one ringtest participations/a
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Pre-treatment methods 2016/17
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Changes in pre-treatment methods
from 2006 till 2017
N: open digestion no digestion (element analyzers)
Dry ashing open digestion (P, K, Ca, Mg, Mn)
or to microwave
Pressured digestion microwave
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Microwave digestion & Temperature
Target temperature should be 200°C for 20 minutes
In reality:
max. temperature:
111-168°C for oneminute!
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Determination methods 2016/17
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Changes in determination methods
from 2006 till 2017
N: „Kjeldahl method“ Element analyzers
Flame-AAS ICP-AES
Flameless AAS ICP-MS
ICP-AES ICP-MS
Training-course needed!
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ICP-AES / plant samples
Use standards with similar concentration like your samples
Use matrix adapted standards with similar acid & element
concentrations
Use enough standards (>3) depending on the selected
correlation function (linear, quadratic, regressed, weighted)
Check the calibration with an seperate prepared independent
sample/standard solution
On dual view systems: use radial view for Ca, (Mg), K - all other
elements can be measured in axial view with higher
sensitivity
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Calibration ICP-AES / plant samples
„Normal conc. range“ of the sample in mg/l
„Check Standard“
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There are more things in heaven
and earth than you are dreamed of…
in ICP measurement too…!
Training-course needed!
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Drying of standard materials for CNS
element analyzers
Reason was a not (enough) dried
coal standard material…
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Compare your results from the last
tests - what happend?N S P Ca Mg K C Zn Mn Fe Cu Pb Cd B
16th Test >
17th Test >> >
18th Test >> > <>> <> <>>
19th Test > << < < < < >>>> < <<<<
C, N („other element analyzer“)
„Pressure digestion / ICP-MS“
Always problems with Fe! What is with B in the last test?
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Compare your results from the last
tests - what happend?N S P Ca Mg K C Zn Mn Fe Cu Pb Cd B
16th Test >
17th Test >> >
18th Test >> > <>> <> <>>
19th Test > << < < < < >>>> < <<<<
„Is no accredited testing laboratory“
„Lab uses a mean, a range and a blank control chart“
and check nothing?
„100-500 plant samples/a“
„Good trained staff on the method/analytical equipment“
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Compare your results from the last
tests - what happend?
C is always too low („Element analyzer“) – no improvement
„Open digestion method & ICP-AES“ contamination?
Changes in the laboratory staff? Wrong samples?
N S P Ca Mg K C Zn Mn Fe Cu Pb Cd B
17th Test > >> >> <<< >>> >>> > >>>> >
18th Test < <<<<
19th Test << >>>> >>>> >>>> >>>> >>>> <<<< >>>> >>>> >>>> >>>> >>>>
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Compare your results from the last
tests - what happend?
„No accredited testing laboratory“
„Lab uses a mean chart and blank chart“ and check nothing?
„1000-5000 samples/a“ 50-250 correct analyzed samples!
„Good trained staff on the method/analytical equipment“
N S P Ca Mg K C Zn Mn Fe Cu Pb Cd B
17th Test > >> >> <<< >>> >>> > >>>> >
18th Test < <<<<
19th Test << >>>> >>>> >>>> >>>> >>>> <<<< >>>> >>>> >>>> >>>> >>>>
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What is a good result?
Accuracy of the mean & precision
% Recovery = 97.79 – 99.93% Vi = 0.60-1.17%
% Recovery = 86.22 – 131.2% Vi = 2.97-7.89%
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This is a good result!
% Recovery close to 100% with a small variation between the four
sample results and without influence of the sample concentration
(= your method is under control)
Vi (variation between the four replicates)
o element analyzer (measurement without extra sample preparation) < 3%
o Macro elements (P, K, Ca, Mg, K) < 5%
o Micro elements and heavy metals < 10%
o Trace elements < 20%
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Reasons for Re-Qualification
Technical problem / no servicing of the instrument (6 labs)
Calibration error (3 labs)
Methodical problem / method changed (4 labs)
Missed data submission deadline or got no samples (one lab)
Calculation error ( 2 lab)
No dry matter correction (2 labs)
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FFCC offers reference materials
Maple leaves A
Litterfall (beech leaves)
Pine needles (Pinus nigra)
Spruce needles B (+heavy metals)
http://bfw.ac.at/rz/bfwcms2.web?dok=5146
www.ffcc.at
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Spruce needles B New
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Statistical evaluation for heavy metals
Heavy metals Heavy metals
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Enlarge parameter list
Use of multielement methods (ICP-AES, ICP-MS)
no additional costs/time
Ringtest participation (> 10 laboratories)
Repetitious accuracy
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New parameter up from the 20th Test
Above the element symbol you can see the number of participants in the last test.
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Evaluation limits
Finalized on the EP Meeting Foliage and Litterfall in Zagreb/TFM Luxembourg 2017
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Parameter list / 20th Test
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Ringtest samples / 20th Test
Sample 1 - Birch leaves (Austria)
Sample 2 - Spruce needles (Germany)
Sample 3 - Spruce needles (Austria)
Sample 4 - Pine cones (Austria)
Ringtest material is needed – especially from broadleaves trees
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Database update – FOM/LFM Forms
FOM - Sampling and Analysis of Needles and Leaves
LFM - Sampling and Analysis of Litterfall
Arsenic
Cobalt
Chromium
Mercury
Nickel
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Database update - d_parameter_lfCODE DESCRIPTION FROM_YEAR TO_YEAR UNIT
Al Aluminium 2009 2007 mg/g
B Bor 2009 µg/g
C Carbon 2009 g/100g
Ca Calcium 2009 mg/g
Cd Cadmium 2009 ng/g
Cu Copper 2009 µg/g
Fe Iron 2009 µg/g
K Potassium 2009 mg/g
Mg Magnesium 2009 mg/g
Mn Manganese 2009 µg/g
N Nitrogen 2009 mg/g
Na Sodium 2009 2007 mg/g
P Phophor 2009 mg/g
Pb Lead 2009 µg/g
S Sulphur 2009 mg/g
Zn Zinc 2009 µg/g
As Arsenic 2017 ng/g
Co Cobalt 2017 µg/g
Cr Chromium 2017 µg/g
Hg Mercury 2017 ng/g
Ni Nickel 2017 µg/g
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Thank you for your attention!