Techniques for Monitoring Asbestos Fiber Concentration in Ambient and Indoor Air using SEM

 
APC GmbH 2011
 
Asbestos measurement techniques,
monitoring ambient and indoor air using
SEM, methods and results of a first
international PT scheme.
Authors/presenter: R. Koenig, APC GmbH, Eschborn, Germany;
 L. Davies, HSL, Buxton, Great Britain;
 N. Hoefert, VDI, Düsseldorf, Germany;
 Jan Tempelman, TNO, Utrecht, Netherlands
 
 
APC GmbH 2011
 
 
The above mentioned guidelines (with
some modifications) using Scanning
Electron Microscope (SEM) based
measurement methods are widely used
for the determination
of the asbestos fibre concentration in
indoor and ambient air in Germany and
to some extent in some of its
neighboured European countries
 
ISO 14966 / VDI 3492
 
APC GmbH 2011
 
 
The results of measurements of the
asbestos fibre concentration are used to
make decisions, which may result in
financial and economical consequences,
in addition to the health effects of
workers and others.
 
PT Schemes
 
 APC GmbH 2011
 
 
As a result it is critical, that laboratories
operating in this field are giving
comparable results. It is therefore
surprising, that -with the exception of
two round robins in Germany during the
1990’s - no regular PT scheme is
available for this technique.
 
PT Schemes
 
APC GmbH 2011
 
 
The main reason for this is the technical
difficulty of producing large numbers of
filters each with equivalent fibre
densities, in a suitable concentration
range and at a reasonable cost.
 
PT Schemes
 
APC GmbH 2011
 
 
To address this problem a small
consortium of interested parties was
formed (namely APC and VDI in
Germany, TNO in the Netherlands and
HSL in the UK), with the remit of
developing a suitable SEM PT scheme.
 
PT Schemes
 
APC GmbH 2011
 
 
From the beginning we were aiming for
an international acceptable scheme,
therefore the basis was ISO 14966,
being also very similar to VDI 3492 and
other SEM methods
 
ISO 14966 PT Scheme
 
APC GmbH 2011
 
 
The intention was to produce a larger
number of equally loaded filter cassettes
with fibre concentrations up to
 50 fibres / mm² filter area.
 
The sample set for the participants shall
include at least three filter cassettes
having different qualities both in fibre
number and  asbestos type on the filter.
 
ISO 14966 PT Scheme
 
APC GmbH 2011
 
 
 
ISO 14966 PT Scheme
(
steps included)
 
APC GmbH 2011
 
 
 
ISO 14966 PT Scheme
(
production of loaded filter cassettes)
 
Sample production is achieved by HSL
using a combination of a modified
dustiness tester to generate airborne
fibre concentrations and a multi-port
sampling device – the “Sputnik”.
 
A combination of commercial asbestos
containing materials and specially
prepared spiked materials was the
source for generating the dust for the
filter loading
APC GmbH 2011
 
 
ISO 14966 PT Scheme
(
production of loaded filter cassettes)
 
Using a critical orifice and a sampling
flow rate of around 1.8 litres per
minute, the “sputnik” has the capability
to collect up to 114 equally loaded
filters (mounted in cassettes), in one
batch.
 
In the first pilot PT scheme two
differently loaded filters were used
together with an ambient air filter
generated by parallel sampling at the
same location.
 
APC GmbH 2011
 
 
 
ISO 14966 PT Scheme
(
production of loaded filter cassettes)
 
APC GmbH 2011
 
 
 
 
 
APC GmbH 2011
 
 
 
ISO 14966 PT Scheme
Additional Information Package
 
An additional information package
was sent together with the samples, to
ensure with other things, that the
counting rules are well understood.
Most people use WHO counting rules in
their every day business, which are
different in some cases from ISO
counting rules
 
APC GmbH 2011
 
 
 
Pilot PT Scheme ISO 14966
 
During this first trial the number of
participants was limited to 15
laboratories, representing five European
countries (Austria, Germany, Great
Britain, Netherlands and Switzerland).
 
APC GmbH 2011
 
 
 
APC GmbH 2011
 
 
 
APC GmbH 2011
 
 
 
Pilot PT Scheme ISO 14966
 
Asbestos varieties in the sample:
50 % crocidolite
45% amosite
5% chrysotile
 
 
APC GmbH 2011
 
 
 
Pilot PT Scheme ISO 14966
Results
 
Observed Deviations:
 
In a simple estimation the deviation S
R
resulting from the evaluation by the
participants extending the unavoidable
poissonian random variation S
P
 can be
calculated:
 
 
 
where S
N
 is the standard deviation of the
counting results for one filter type
 
 
 
 
 
APC GmbH 2011
 
 
 
Pilot PT Scheme ISO 14966
Results
 
Observed deviations in between-laboratory
comparison:
 
For the ambient air filters no deviation extending
the poissonian uncertainty detectable
 
For the filter type R 24 the variation S
R
, which
results from the between-laboratory comparison of
the fibre counts is:  appr. 10% relative
 
For R 25 the variation S
R
 is appr. 30% relative
 
 
 
 
 
 
APC GmbH 2011
 
 
 
Pilot PT Scheme ISO 14966
Results
 
Detected reasons for the observed variations:
 
Laboratories with  a tendency to be lower than
average (asbestos) show two types of discernable
deviations:
 
Smallest detected fibre diameter is 0,3 µm or
greater according to their fibre counting form.
or
they record a larger amount of fibres with “no
spectra” = 
u
nidenti
f
ied 
o
bjects
 
 
 
 
 
 
 
 
APC GmbH 2011
 
 
 
Pilot PT 
Scheme
 ISO 14966
Results
 
Reasons for the observed variations:
 
Optimization of EDXA instruments
required:
 
Greater channel width (20 eV or even more) gives
maximum P/B in shortest possible measurement
time and is especially important for the analysis of
very thin fibres, to minimize statistical uncertainties
in the spectra and to reduce the adverse effects of
beam drift during analysis.
 
 
 
 
 
 
 
 
APC GmbH 2011
 
 
 
ISO 14966
 
Optimization of EDXA instruments required:
 
 
APC GmbH 2011
 
 
 
 
Optimization of EDXA instruments
 
APC GmbH 2011
 
 
 
 
Optimization of EDXA instruments
 
APC GmbH 2011
 
 
 
Pilot PT Scheme ISO 14966
Summary
 
The pilot PT scheme was running as scheduled
 
For a first PT scheme including both preparation
and analysis of the filter samples
the results can be regarded as good, especially in
the range of the decision limits (clearance levels as
an example) in Germany and some of its
neighbored countries.
 
Based on the experience HSL (Health and Safety
Laboratory) will offer a full scale PT scheme starting
out later this year.
 
 
 
 
 
 
 
 
APC GmbH 2010
 
Thank you for your attention !
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Explore the methods and results of an international proficiency testing (PT) scheme for measuring asbestos fibers in indoor and ambient air. The use of Scanning Electron Microscope (SEM) based techniques, including ISO 14966 and VDI 3492 guidelines, is discussed. The importance of PT schemes in ensuring accurate and comparable results, along with the challenges faced in producing suitable filters, is highlighted. A collaborative effort by APC, VDI, TNO, and HSL led to the development of an SEM PT scheme based on ISO 14966.

  • Asbestos Measurement Techniques
  • SEM
  • Monitoring
  • Indoor Air Quality
  • PT Scheme

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  1. Asbestos measurement techniques, monitoring ambient and indoor air using SEM, methods and results of a first international PT scheme. Authors/presenter: R. Koenig, APC GmbH, Eschborn, Germany; L. Davies, HSL, Buxton, Great Britain; N. Hoefert, VDI, D sseldorf, Germany; Jan Tempelman, TNO, Utrecht, Netherlands APC GmbH 2011 Folie 1

  2. ISO 14966 / VDI 3492 The above mentioned guidelines (with some modifications) using Scanning Electron Microscope (SEM) based measurement methods are widely used for the determination of the asbestos fibre concentration in indoor and ambient air in Germany and to some extent in some of its neighboured European countries APC GmbH 2011 Folie 2

  3. PT Schemes The results of measurements of the asbestos fibre concentration are used to make decisions, which may result in financial and economical consequences, in addition to the health effects of workers and others. APC GmbH 2011 Folie 3

  4. PT Schemes As a result it is critical, that laboratories operating in this field are giving comparable results. It is therefore surprising, that -with the exception of two round robins in Germany during the 1990 s - no regular PT scheme is available for this technique. APC GmbH 2011 Folie 4

  5. PT Schemes The main reason for this is the technical difficulty of producing large numbers of filters each with equivalent fibre densities, in a suitable concentration range and at a reasonable cost. APC GmbH 2011 Folie 5

  6. PT Schemes To address this problem a small consortium of interested parties was formed (namely APC and VDI in Germany, TNO in the Netherlands and HSL in the UK), with the remit of developing a suitable SEM PT scheme. APC GmbH 2011 Folie 6

  7. ISO 14966 PT Scheme From the beginning we were aiming for an international acceptable scheme, therefore the basis was ISO 14966, being also very similar to VDI 3492 and other SEM methods APC GmbH 2011 Folie 7

  8. ISO 14966 PT Scheme The intention was to produce a larger number of equally loaded filter cassettes with fibre concentrations up to 50 fibres / mm filter area. The sample set for the participants shall include at least three filter cassettes having different qualities both in fibre number and asbestos type on the filter. APC GmbH 2011 Folie 8

  9. ISO 14966 PT Scheme (steps included) APC GmbH 2011 Folie 9

  10. ISO 14966 PT Scheme (production of loaded filter cassettes) Sample production is achieved by HSL using a combination of a modified dustiness tester to generate airborne fibre concentrations and a multi-port sampling device the Sputnik . A combination of commercial asbestos containing materials and specially prepared spiked materials was the source for generating the dust for the filter loading APC GmbH 2011 Folie 10

  11. ISO 14966 PT Scheme (production of loaded filter cassettes) Using a critical orifice and a sampling flow rate of around 1.8 litres per minute, the sputnik has the capability to collect up to 114 equally loaded filters (mounted in cassettes), in one batch. In the first pilot PT scheme two differently loaded filters were used together with an ambient air filter generated by parallel sampling at the same location. APC GmbH 2011 Folie 11

  12. ISO 14966 PT Scheme (production of loaded filter cassettes) APC GmbH 2011 Folie 12

  13. Pilot PT Scheme Organisation Production of filter cassettes HSL Buxton GB Test for homogenity and fibre density APC Eschborn TNO Utrecht NL Coding of filters Assembling the filter sets APC Sending the parcel with the filter set VDI D sseldorf Evaluation of the filters Sending results PARTICIPANT Anonymisation of results VDI Evaluation of data APC Presentation of results to the Participants VDI APC GmbH 2011 Folie 13

  14. ISO 14966 PT Scheme Additional Information Package An additional information package was sent together with the samples, to ensure with other things, that the counting rules are well understood. Most people use WHO counting rules in their every day business, which are different in some cases from ISO counting rules APC GmbH 2011 Folie 14

  15. Pilot PT Scheme ISO 14966 During this first trial the number of participants was limited to 15 laboratories, representing five European countries (Austria, Germany, Great Britain, Netherlands and Switzerland). APC GmbH 2011 Folie 15

  16. P Pilot PT ilot PT Scheme Fibre Scheme ISO 14966 Fibre numbers ISO 14966 Results numbers (L > 5 m) Results (L > 5 m) Ambient air R 24 R 25 Evaluated filter area mm2 Laboratory Other In. Asbestos Other In Asbestos Other In. Asbestos A 22 0 1 6 22 30 1,05 B 0 0 0 10 0 32 1,04 C 8 0 3 6 2 31 1,03 D 5 0 0 7 2 22 1,01 E 3 0 0 11 1 42 1 F 0 0 4 13 11 18 1 G 0 0 0 10 0 18 1 H 1 0 1 3 0 16 1,01 I 7 1 0 9 5 38 1 K 0 0 0 5,3 0 12,9 1,7 L 0 0 0 5 0 24 1,01 N 0 0 0 8 1 14 1,01 O 0 0 0,5 2,7 0 7,7 1,83 P 11 0 3 8 1 36 1 Q 1 0 1 9 0 26 1 green numbers: calculated for 1 mm evaluated filter area APC GmbH 2011 Folie 16

  17. Distribution of fibre diameter (asbestos) as detected by the participants 0.40 0.35 F r e q u e n c y % / m 0.30 0.25 0.20 %/ m 0.15 0.10 0.05 0.00 0 0.5 1 1.5 2 2.5 3 Fibre Diameter [ m] APC GmbH 2011 Folie 17

  18. Pilot PT Scheme ISO 14966 Asbestos varieties in the sample: 50 % crocidolite 45% amosite 5% chrysotile APC GmbH 2011 Folie 18

  19. Pilot PT Scheme ISO 14966 Results Observed Deviations: Observed Deviations: In a simple estimation the deviation SR resulting from the evaluation by the participants extending the unavoidable poissonian random variation SPcan be calculated: ( R S S = ) 2 N 2 P S where SNis the standard deviation of the counting results for one filter type APC GmbH 2011 Folie 19

  20. Pilot PT Scheme ISO 14966 Results Observed deviations in between comparison: Observed deviations in between- -laboratory comparison: laboratory For the ambient air filters no deviation extending the poissonian uncertainty detectable For the filter type R 24 the variation SR, which results from the between-laboratory comparison of the fibre counts is: appr. 10% relative For R 25 the variation SRis appr. 30% relative APC GmbH 2011 Folie 20

  21. Pilot PT Scheme ISO 14966 Results Detected reasons for the observed variations: Detected reasons for the observed variations: Laboratories with a tendency to be lower than average (asbestos) show two types of discernable deviations: Smallest detected fibre diameter is 0,3 m or greater according to their fibre counting form. or they record a larger amount of fibres with no spectra = unidentified objects APC GmbH 2011 Folie 21

  22. Pilot PT Scheme ISO 14966 Results Reasons for the observed variations: Reasons for the observed variations: Optimization of EDXA instruments required: Greater channel width (20 eV or even more) gives maximum P/B in shortest possible measurement time and is especially important for the analysis of very thin fibres, to minimize statistical uncertainties in the spectra and to reduce the adverse effects of beam drift during analysis. APC GmbH 2011 Folie 22

  23. ISO 14966 Optimization of EDXA instruments required: APC GmbH 2011 Folie 23

  24. Optimization of EDXA instruments Optimization of EDXA instruments APC GmbH 2011 Folie 24

  25. Optimization of EDXA instruments Optimization of EDXA instruments APC GmbH 2011 Folie 25

  26. Pilot PT Scheme ISO 14966 Summary The pilot PT scheme was running as scheduled For a first PT scheme including both preparation and analysis of the filter samples the results can be regarded as good, especially in the range of the decision limits (clearance levels as an example) in Germany and some of its neighbored countries. Based on the experience HSL (Health and Safety Laboratory) will offer a full scale PT scheme starting out later this year. APC GmbH 2011 Folie 26

  27. Thank you for your attention ! APC GmbH 2010 Folie 27

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