10. Natural Occurrences
of Asbestos (NOA)
10
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11. Staten Island Serpentinite
I 278 road cut. Up to 50% Chrysotile
Copyright 2011 EMSL Analytical, Inc. Picture and info: Brooklyn CUNY.edu
12. Why is Soil so Hard
to Analyze?
12
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13. Why is Soil so Hard
to Analyze?
13
Non-
Homogeneity
Grain size
Copyright 2011 EMSL Analytical, Inc.
14. Scales of Non-Homogeneity
14
The Big Picture
Obtaining
representative samples
in the field can be
difficult.
Samples tend to be
very non-homogeneous
especially over the
large areas that are
typical on outdoor sites.
How many samples for
a baseball field or 100
miles of road or rail
bed?
Copyright 2011 EMSL Analytical, Inc.
15. Scales on Non-Homogeneity
15
The Medium
Picture
How deep to go?
What layers to
include?
Copyright 2011 EMSL Analytical, Inc.
16. Scales on Non-Homogeneity
16
The Fine Picture
Obtaining a
representative sub-
sample in the lab is
important.
Copyright 2011 EMSL Analytical, Inc.
17. Scales on Non-Homogeneity
17
The Very Fine Picture
stereoscopic view of play sand
The presence of even sand sized quartz crystals are a problem.
Copyright 2011 EMSL Analytical, Inc.
18. In Summary
18
Soil is a problem matrix for field and lab
personnel alike.
Careful sampling plans are needed to
reduce inconsistencies, and help to
carefully define …… “What is the sample?”
The Analytical method used needs to
address potential non homogeneity and
grain size
Copyright 2011 EMSL Analytical, Inc.
19. Analytical Choices
What Method to Choose?
19
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20. Limitations of “Standard” PLM
20
EPA PLM Method (EPA/600/R-93/116)
Method for the Determination of Asbestos in Bulk Building Materials
• As the title suggests and the method explains, this
is a method for relatively homogenous bulk
building materials, not soil.
• The final version of this method is quite
flexible though and matrix
modification prior to analysis is
described
Copyright 2011 EMSL Analytical, Inc.
21. Two Approaches to Soil
Sieving Milling
Copyright 2011 EMSL Analytical, Inc.
22. Scenario 1 - Contamination of Soil with ACM
The Main Sieve Methods Available
Some of the sieving Methods available
• EPA Region 1 Screening Protocol
“Protocol for Screening Soil and Sediment Samples for
Asbestos Content” used by the EPA Region 1 Lab
- low tech screening method, semi-quantitative at best.
- been around since 1994, revised ’97 and ’99
- stereoscopic (20X mag) estimate of % Asbestos
• ASTM Sieve Method for Soil
Best option yet for sieving protocol for soil, yet to be
published
Copyright 2010 EMSL Analytical, Inc.
23. Scenario 1 - Contamination of Soil with ACM
EPA Region 1 Protocol
EPA Region 1 Screening Protocol
The soil is sub-sampled (only particles < 16mm)
Wet sieved through a 60 mesh (250 micron) sieve
Only the >250 micron fraction is analyzed
Stereoscope (20-40X) used to quantify, and PLM
used to identify
Note: This is a screening method.
Qualitative or Semi-Quantitative at best
Copyright 2011 EMSL Analytical, Inc.
24. DRAFT ASTM Sieve Method
24
Sample Size 250 cc or less
Sieve Stack
• 19 mm (3/4”)
• 2 mm
• 106 micron
Anything larger than 19 mm is not considered part
of the sample
Copyright 2011 EMSL Analytical, Inc.
25. ASTM Sieve Method
25
1) Sample is dried
2) Weighed
3) Dry Sieved
(wet sieving is
optional) on
sieve shaker
for 5 minutes
Copyright 2011 EMSL Analytical, Inc.
26. 26
ASTM Sieve Method
This is a common
4) Weigh each fraction type of sample
(mini clods))
5) Analyze each fraction
Coarse and Medium Fractions still too large for straight PLM
Copyright 2011 EMSL Analytical, Inc.
27. 27
ASTM Sieve Method
The fine fraction is
fine enough and
homogenous enough
for a PLM slide prep
and analysis
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28. Wet or Dry?
28
Pros
• Washes the suspect
ACM making for
easier detection
• Breaks down matrix
to its smallest
components
Copyright 2011 EMSL Analytical, Inc.
29. Wet Sieving Can Be Better
for Some Soils
29
Cons
• More labor intensive
• More time (drying)
• Even more time and possible
fiber loss as fine fraction
needs to be sedimented
• Water disposal an issue
Copyright 2011 EMSL Analytical, Inc.
30. Comparison of Dry vs. Wet Sieving
30
“Typical” soil sample DRY Sieving on an
on sieve stack Automatic sieve shaker
Copyright 2011 EMSL Analytical, Inc.
31. Coarse, Medium and Fine Fractions
soil clods fail to make it
31
through the 2mm sieve
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32. Wet Sieving of Same Sample
32
Sieve Stack Coarse, Medium
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33. The Same Sample !
33
Dry Sieving Wet Sieving
Fine
1%
Medium Fine Coarse
12% 40% 34%
Coarse
86% Medium
26%
Copyright 2011 EMSL Analytical, Inc.
35. Visual and Stereomicroscopic
Analysis
35
HAND PICKING
SUSPECT ACM
OUT OF COARSE
AND MEDIUM
FRACTIONS.
Copyright 2011 EMSL Analytical, Inc.
36. ASTM Analysis
36
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37. THE ASBESTOS % FOR EACH TYPE OF
ACM IS DETERMINED. THE PERCENT
ASBESTOS IS EXTRAPOLATED TO
THAT FRACTION, AND THEN TO THE
ENTIRE SAMPLE.
37
Copyright 2011 EMSL Analytical, Inc.
38. ASTM Sieve Method
38
If all three fractions are non detect by PLM then a
TEM analysis is performed.
Optional drop mount Qualitative only (detect/non
detect). This enable us to find asbestos that is not
visible by light microscopy
If drop mount is positive then
grav reduction followed by
Quantitative TEM analysis
Structures/µg
Copyright 2011 EMSL Analytical, Inc.
39. TEM Quantitative Analysis
39
100 to 250 mg of the material from the fine
fraction is gravimetrically reduced via muffle
furnace and acid treatment.
Filtered onto a 0.2µm PC or 0.22µm MCE
filter
TEM examination using a direct method
consistent with Test Method D6281.
Results reported in Structures per microgram
Is that a useful number?
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40. Two Approaches to Soil
Sieving Milling
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41. The MILLING Approach
Disk pulverizer/plate grinder
Cross Beater Mill
Freezer mill
Ball mill, etc.…….
Copyright 2011 EMSL Analytical, Inc.
42. CA Air Resources Board
(CARB) Method 435
Determination of Asbestos Content of Serpentine Aggregate
42
This is the current de facto standard for
milling methods.
1. One pint (473cc) sample
2. milled to 200 mesh (74 microns)
3. PLM
Copyright 2011 EMSL Analytical, Inc.
43. CARB 435 Method
43
The sample is dried in a drying Milled to reduce the nominal
oven and material >3/8” is
removed by sieving particle size to 75 microns
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44. CARB 435
After milling, the sample is
analyzed by a PLM
400 or 1000
point count
(0.25% or 0.1%)
Copyright 2011 EMSL Analytical, Inc.
45. TEM CARB Method
Analyzed by TEM at
20,000X
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46. How Do They
Compare?
46
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47. Study Design
47
Test the performance of three common
methods for asbestos analysis of soil.
• Soil spiked at 0.1% and 1% by weight
• Analysis by
1. “standard” EPA 600 R-93/116
2. ASTM Sieve Method
3. CARB Method 435
Copyright 2011 EMSL Analytical, Inc.
48. Phase I
48
Spiking with Unconsolidated Asbestos
Two chrysotile sources were used
1. The majority was chrysotile asbestos
(Plastibest-20) from the Jeffrey mine in
Canada. It was left over from an old
ingestion study performed by NIEHS.
Thanks Jim Millette!
2. Chrysotile from Salt River Canyon in
Arizona (just south of Chrysotile, Arizona).
Copyright 2011 EMSL Analytical, Inc.
49. The Big Plan
49
Phase 1 Phase 2
Unconsolidated Asbestos Consolidated (ACM) Asbestos
Copyright 2011 EMSL Analytical, Inc.
51. Asbestos Characterization
51
Fiber Size Data for Data Plastibest-20 – 100 fibers by TEM at 20K Mag
18
16
Approx. 20% of fibers are optically visible (> 0.2 microns in width)
14
12
10
8
6
4
2
0
Fiber Length (microns)
Copyright 2011 EMSL Analytical, Inc.
52. Asbestos Characterization
52
Fiber Size Data for Arizona Chrysotile – 100 fibers by TEM at 20K Mag
30
25
Approx. 13% of fibers are optically visible (> 0.2 microns in width)
20
15
10
5
0
Fiber Length (microns)
Copyright 2011 EMSL Analytical, Inc.
53. Spiking
53
To eliminate the variability of possible non-homogeneity, no
sub-sampling was performed. 63 individual samples were
prepared.
EPA 600 ASTM Sieve Method CARB Method 435
• Seven Blanks
• Seven samples at 0.1%
• Seven samples at 1%
Copyright 2011 EMSL Analytical, Inc.
55. Analyst Credentials
55
Samples submitted blindly to 6 separate
analysts at separate locations including
external labs.
• minimum 10 years experience PLM
• 2 have over 30 years exp.
• 2 attended McCrone PLM course
• 2 have BS Geology
• 1 MS Analytical mineralogy
Copyright 2011 EMSL Analytical, Inc.
57. EPA 600 Results for Blanks
Phase I 57
Analyst 1 Analyst 2 Analyst 3 Analyst 4 Analyst 5 Analyst 6
Sample Asbestos % % % % % %
Number % Actual Result Recovery Result Recovery Result Recovery Result Recovery Result Recovery Result Recovery
EPA 600
2 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
EPA 600
3 0.00 0 NA 0 NA 0 NA 0 NA trace NA 0 NA
EPA 600
9 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
EPA 600
13 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
EPA 600
16 0.00 0 NA 0 NA 0 NA 0 NA trace NA 0 NA
EPA 600
17 0.00 trace NA 0 NA 0 NA 0 NA 0 NA 0 NA
EPA 600
19 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
Copyright 2011 EMSL Analytical, Inc.
58. EPA 600 Results at 0.1%
Phase I 58
8
7
Each color represents an analyst
6
Percent Asbestos
5
4
3
2
1
0
Sample 1 2 3 4 5 6 7
Overall Percent Recovery: 2063 %
Overall (pooled) RSD: 0.51
Copyright 2011 EMSL Analytical, Inc.
62. ASTM Results for Blanks Phase I
62
Analyst 1 Analyst 2 Analyst3 Analyst 4 Analyst 5 Analyst 6
Sample Asbestos % % % % % % %
Number Actual Result Recovery Result Recovery Result Recovery Result Recovery Result Recovery Result Recovery
ASTM
02 0.00 0.0 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA
ASTM
05 0.00 0.5 NA 0.2 NA 0.0 NA 0.0 NA 0.0 NA 0.27 NA
ASTM
09 0.00 0.0 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA
ASTM
14 0.00 0.0 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA
ASTM
15 0.00 0.0 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA
ASTM
16 0.00 0.0 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA
ASTM
18 0.00 0.0 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA
Copyright 2011 EMSL Analytical, Inc.
69. CARB 435 Results on Blanks
Phase I 69
Analyst 1 Analyst 2 Analyst 3 Analyst 4 Analyst 5 Analyst 6
Sample Asbestos % % % % % %
Number % Actual Result Recovery Result Recovery Result Recovery Result Recovery Result Recovery Result Recovery
CARB 3 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
CARB 7 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
CARB 8 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
CARB 10 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
CARB 11 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
CARB 14 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
CARB 18 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
Copyright 2011 EMSL Analytical, Inc.
75. Score Card Phase I
Pooled Data for the Round
75
EPA600 ASTM Sieve CARB 435
%
Recovery 1540 1090 650
RSD 0.55 0.32 0.64
False Negatives for CARB 435 are a concern
Copyright 2011 EMSL Analytical, Inc.
76. Phase II
Everything up to this point
has compared how the
methods perform at
detecting and quantifying
unconsolidated milled
asbestos in soil
Now let’s see what
happens when we spike
with ACM.
Copyright 2011 EMSL Analytical, Inc.
77. Phase II
77
Spiking with Consolidated
Asbestos (ACM)
- Transite supplied by RTI
- Estimated Chrysotile
percentage = 14%
Copyright 2011 EMSL Analytical, Inc.
78. 78
Phase II
EPA 600
Method Results
Copyright 2011 EMSL Analytical, Inc.
79. EPA 600 - Blanks - Phase II
79
Analyst 1 Analyst 2 Analyst 3 Analyst 4 Analyst 5 Analyst 6
Sample Asbestos % % % % % %
Number % Actual Result Recovery Result Recovery Result Recovery Result Recovery Result Recovery Result Recovery
EPA 600 1 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
EPA 600 8 0.00 0 NA 0.5 NA 0 NA 0 NA 0 NA 0 NA
EPA 600 9 0.00 0.5 NA 0 NA 0 NA 0 NA 0 NA 0 NA
EPA 600
14 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
EPA 600
15 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
EPA 600
19 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
EPA 600
21 0.00 0 NA 0 NA 0.5 NA 0 NA 0 NA 0.5 NA
Copyright 2011 EMSL Analytical, Inc.
83. Phase II ASTM Sieve
Method Results
83
Copyright 2011 EMSL Analytical, Inc.
84. ASTM – Blanks - Phase II
84
Analyst 1 Analyst 2 Analyst 3 Analyst 4 Analyst 5 Analyst 6
Sample Asbestos % % % % % % %
Number Actual Result Recovery Result Recovery Result Recovery Result Recovery Result Recovery Result Recovery
ASTM 4 0.00 0.0 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA
ASTM 8 0.00 0.0 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA 0.00 NA
ASTM 9 0.00 0.0 NA 0.2 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA
ASTM
11 0.00 0.0 NA 0.4 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA
ASTM
12 0.00 0.0 NA 0.0012 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA
ASTM
17 0.00 0.0 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA
ASTM
19 0.00 0.0 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA 0.0 NA
Copyright 2011 EMSL Analytical, Inc.
88. Phase II
CARB Method 435 Results
88
Copyright 2011 EMSL Analytical, Inc.
89. Phase II - CARB - Blanks
89
Analyst 1 Analyst 2 Analyst 3 Analyst 4 Analyst 5 Analyst 6
Sample Asbestos % % % % % %
Number % Actual Result Recovery Result Recovery Result Recovery Result Recovery Result Recovery Result Recovery
CARB 1 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
CARB 2 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
CARB 9 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
CARB 11 0.00 0 NA 0.125 NA 0 NA 0 NA 0 NA 0 NA
CARB 16 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
CARB 17 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
CARB 20 0.00 0 NA 0 NA 0 NA 0 NA 0 NA 0 NA
Copyright 2011 EMSL Analytical, Inc.
90. Phase II - CARB - 0.1%
90
1.6
1.4
1.2
1
0.8
0.6
0.4
0.2
0
1 2 3 4 5 6 7
Overall Percent Recovery for this Sample: 218 %
Overall (Pooled) RSD for this Sample: 0.65
Copyright 2011 EMSL Analytical, Inc.
94. Summing Up
94
Pros Straight EPA 600 Cons
• Well known • Gross over estimation,
esp. at low percentages
• fast / cost effective
• Since method not
• pretty good at finding the designed for this matrix
asbestos not legally defensible?
Copyright 2011 EMSL Analytical, Inc.
95. Summing Up
95
Pros ASTM Sieve Method Cons
• Once published it will be
• Most time consuming
defensible (“fit for use”)
• potential cross
• Allows for a forensic analysis as
contamination due to sieves
it does not alter the asbestos or
(difficult to clean)
ACM as it exists in the sample
• cost
• TEM follow up on NAD
circumvents to some extent the •Course and medium fraction
0.25 micron width limitation still not amenable to PLM
Copyright 2011 EMSL Analytical, Inc.
96. Summing Up
96
Pros CARB 435 Cons
• Homogenizes the entire sample
• Potential to create fibers (cleavage
prior to analysis. fragments with large aspect ratios)
from non asbestiform minerals.
• Reduces grain size of entire sample
• Alters fiber sizes dimensions
• Less labor intensive than sieving
• Potentially better quantification
• mentioned in the EPA framework
document
• options for better DL 0.25 , 0.1 or even
lower
• Milled sample is also amenable to
TEM
Copyright 2011 EMSL Analytical, Inc.
97. • CARB 435 mentioned
• 1% is not an appropriate action level for asbestos in soil
97
Copyright 2011 EMSL Analytical, Inc.
98. Thanks!
98
• Jim Millette of MVA
• Owen Crankshaw and Todd Ennis at
RTI
• Alan Segrave and BV
• Howard Varner and EHS
Copyright 2011 EMSL Analytical, Inc.
99. Real World Test Drive
of the Methods
99
Copyright 2011 EMSL Analytical, Inc.
100. CharlesTown Timeline
10
0
Early 1900s:Constructed by gun manufacturer Savage Arms Corporation,
which continued to use the site through World Wars I and II.
1950s: Sperry Univac makes the complex the center of its manufacturing
operations in the Mohawk Valley. Employment peaks in the thousands, then
gradually declines.
1977: Charles A. Gaetano buys the property and announces plans for a
factory-outlet complex, which becomes a reality and is successful for several
years until it declines in the late 1980s.
1991: The CharlesTown Factory Outlet Center officially becomes the
CharlesTown Business Complex, with only three retail stores remaining.
2007: Property is purchased by local developer Michael Cancilla, who plans
to work with two Massachusetts developers to obtain grant money and
redevelop the site into a mix of residential and retail.
2010: Lack of grant money and environmental problems have stalled the site,
and the EPA is preparing to clean up and demolish dilapidated buildings.
Copyright 2011 EMSL Analytical, Inc.
101. Savage Arms
10
1
Copyright 2011 EMSL Analytical, Inc.
112. Non-Scientific Study
112
4 grab samples collected from various areas
No careful sampling pan :o(
Unlike the formal study these samples need
to be riffle split (remember non
homogeneity issue) into 3 separate sub-
samples for
EPA 600
CARB 435
ASTM Sieve Method
Copyright 2011 EMSL Analytical, Inc.
113. One way to
help
homogenize
the samples
either in the
field or after
submittal to
the lab
Riffle Splitting
Copyright 2011 EMSL Analytical, Inc.
115. Conclusions?
115
All conclusions need to be taken with a grain (block?) of salt.
Remember that each sample was split into 3 sub-samples.
Each sample is therefore a unique sample unto itself.
• CARB seemed to miss 6
asbestos at low percentages EPA 600
5
• Generally good agreement CARB 435
between EPA 600 and ASTM 4
ASTM Sieve
3
2
1
0
1CN 1GV 2CN 2GV 3CN 3GV 4CN 4GV
Copyright 2011 EMSL Analytical, Inc.
116. Another Approach
Fiber Releasability
• Determining the percentage of asbestos in
soil is useful for knowing that there is a
potential for exposure.
• But it does not give us a clue as to what the
risk actually is.
• 1% is not an acceptable action level to use
for asbestos in soil
Copyright 2011 EMSL Analytical, Inc.
117. Fiber Releasability
Risk Assessment
• If we can determine the amount of
respirable asbestos fibers that are
released from a soil upon agitation
then we have an insight into risk
• The EPA is all about minimizing risk to
the population.
Copyright 2011 EMSL Analytical, Inc.
118. Risk Assessment Methods
The Elutriator Method
The Elutriator Method
Superfund EPA 540-R-97-028
With this method a soil sample is gravimetrically
tracked through sieving into course and fine fractions
The fine fraction is then tumbled in a closed chamber and
any respirable dust generated is collected on air cassettes
Analysis is performed by ISO 10312 counting rules
This method is peer reviewed and (arguably)
acceptable for risk assessment studies
Copyright 2011 EMSL Analytical, Inc.
119. Risk Assessment Methods
The Elutriator Method
Tumbler
apparatus
filled with
soil
Copyright 2011 EMSL Analytical, Inc.
120. Risk Assessment Methods
The Elutriator Method
Tumbler inside enclosed humidity chamber
Copyright 2011 EMSL Analytical, Inc.
121. Risk Assessment Methods
The Elutriator Method
Isokinetic sampling at
top of elutriator stack to
catch only the
respirable fraction of
fibers released from
the soil.
ISO 10312 Analysis
Results in structures/g
Copyright 2011 EMSL Analytical, Inc.
122. Field Alternatives
to the Elutriator
The EPA uses other techniques in the field
that also collect and measure releasable
fibers from soil.
• Activity Based air Sampling (ABS)
• Releasable Asbestos Field (RAF) Unit
• Fluidized Bed Asbestos Segregator(FBAS)
Copyright 2011 EMSL Analytical, Inc.
123. Activity Based Air Sampling
Activity Based Air Sampling
Personnel (and sometimes area) monitoring
is performed while samplers mimic likely
activity for that location.
Copyright 2011 EMSL Analytical, Inc.
126. Fluidized Bed
Air is injected at a precise flow rate to get the soil
sample behaving like a fluid.
Then air samples are collected from above.
Copyright 2011 EMSL Analytical, Inc.
128. Fluidized
Bed
Copyright 2011 EMSL Analytical, Inc.
129. Summing Up
The answer depends on the question…
“I see building material debris in the soil. Does it have asbestos and if
so how much? Do I need to dispose of it as hazardous waste?”
ASTM Sieving Method
“I don’t necessarily see suspect asbestos but I think it might be there
either from contamination (ex brake shops) or from NOA.”
PLM CARB 435 (down to 0.25% or 0.1%)
TEM CARB 435 (EPA 600 Mass Analysis)
ASTM Sieving Method with TEM
Does the Soil Contain Respirable / Releasable Fibers?
EPA 540-R-97-028 Superfund Method (Elutriator)
Activity based air sampling
RAFS / FBAS
Copyright 2011 EMSL Analytical, Inc.