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Ed Cahill
National Director Asbestos Lab Services
ecahill@emsl.com

                       EMSL Analytical, Inc.
            200 Route 130 North, Cinnaminson, NJ 08108
                856-303-2565         www.emsl.com
Asbestos in Soil
Soil is a Great Hiding Place
                                       3
   1% Unconsolidated                       1% Consolidated
      Chrysotile                            Chrysotile




Copyright 2011 EMSL Analytical, Inc.
Soil is a Great Hiding Place for
  Asbestos                             4




                                           1% asbestos
Copyright 2011 EMSL Analytical, Inc.
Sources of Asbestos
           in Soil
                                            5



      Asbestos
      Contamination
                                       Natural Occurrences
                                       of Asbestos (NOA)
Copyright 2011 EMSL Analytical, Inc.
Asbestos Contamination
                                       6




Copyright 2011 EMSL Analytical, Inc.
7




Copyright 2011 EMSL Analytical, Inc.
8




Copyright 2011 EMSL Analytical, Inc.
9




Copyright 2011 EMSL Analytical, Inc.
Natural Occurrences
         of Asbestos (NOA)
                                       10




Copyright 2011 EMSL Analytical, Inc.
Staten Island Serpentinite
      I 278 road cut. Up to 50% Chrysotile




Copyright 2011 EMSL Analytical, Inc.         Picture and info: Brooklyn CUNY.edu
Why is Soil so Hard
       to Analyze?
                                       12




Copyright 2011 EMSL Analytical, Inc.
Why is Soil so Hard
       to Analyze?
                                       13




         Non-
      Homogeneity
                                            Grain size

Copyright 2011 EMSL Analytical, Inc.
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.
Scales on Non-Homogeneity
                                       15


 The Medium
  Picture
  How deep to go?
  What layers to
     include?



Copyright 2011 EMSL Analytical, Inc.
Scales on Non-Homogeneity
                                       16




  The Fine Picture
  Obtaining a
  representative sub-
  sample in the lab is
  important.



Copyright 2011 EMSL Analytical, Inc.
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.
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.
Analytical Choices
              What Method to Choose?
                                       19




Copyright 2011 EMSL Analytical, Inc.
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.
Two Approaches to Soil
                   Sieving             Milling




Copyright 2011 EMSL Analytical, Inc.
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.
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.
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.
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



      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
                                       ASTM Sieve Method



 The fine fraction is
 fine enough and
 homogenous enough
 for a PLM slide prep
 and analysis



Copyright 2011 EMSL Analytical, Inc.
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.
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.
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.
Coarse, Medium and Fine Fractions
                                soil clods fail to make it
                                                31

                                through the 2mm sieve




Copyright 2011 EMSL Analytical, Inc.
Wet Sieving of Same Sample
                                       32


              Sieve Stack                   Coarse, Medium




Copyright 2011 EMSL Analytical, Inc.
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.
Dry vs. Wet Sieving
                                       34

  100.00

    90.00

    80.00
                                        DRY     WET
    70.00

    60.00

    50.00

    40.00

    30.00

    20.00

    10.00

     0.00
                             >2mm      >106µm     <106µm
Copyright 2011 EMSL Analytical, Inc.
Visual and Stereomicroscopic
 Analysis
                                       35




  HAND PICKING
   SUSPECT ACM
  OUT OF COARSE
   AND MEDIUM
    FRACTIONS.



Copyright 2011 EMSL Analytical, Inc.
ASTM Analysis
                                       36




Copyright 2011 EMSL Analytical, Inc.
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.
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.
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?
Copyright 2011 EMSL Analytical, Inc.
Two Approaches to Soil
                   Sieving             Milling




Copyright 2011 EMSL Analytical, Inc.
The MILLING Approach




 Disk pulverizer/plate grinder
 Cross Beater Mill
 Freezer mill
 Ball mill, etc.…….

Copyright 2011 EMSL Analytical, Inc.
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.
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




Copyright 2011 EMSL Analytical, Inc.
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.
TEM CARB Method

                                       Analyzed by TEM at
                                            20,000X




Copyright 2011 EMSL Analytical, Inc.
How Do They
                    Compare?
                                       46




Copyright 2011 EMSL Analytical, Inc.
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.
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.
The Big Plan
                                            49

          Phase 1                                      Phase 2
  Unconsolidated Asbestos                    Consolidated (ACM) Asbestos




Copyright 2011 EMSL Analytical, Inc.
Asbestos Characterization
                                       50




Copyright 2011 EMSL Analytical, Inc.
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.
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.
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.
Phase 1 Samples
                                       54




Copyright 2011 EMSL Analytical, Inc.
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.
56




  Phase 1
  EPA 600
  Method Results




Copyright 2011 EMSL Analytical, Inc.
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.
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.
EPA 600 Results at 1%
       Phase I     30                               59

                   25


                   20
Percent Asbestos




                   15


                   10


                   5


                   0
    Sample               1            2       3          4        5   6   7

                        Overall Percent Recovery:         835 %
                        Overall (Pooled) RSD:            0.56
   Copyright 2011 EMSL Analytical, Inc.
EPA 600 Summary
              Phase I
                                       60



   Overall (Pooled) Percent Recovery :             1574 %


    Overall (Pooled) RSD :                  0.54



Copyright 2011 EMSL Analytical, Inc.
ASTM Sieve Method
         Results
                                       61




Copyright 2011 EMSL Analytical, Inc.
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.
Analyst 1
                   63
                                                  PLM Results                        TEM Results

                                                                                Drop Mount Detect/Non
                                        Label #    Analyst 1           True %          Detect
                                       ASTM 02       0.00                0.0             ND
                                       ASTM 05       0.50                0.0             ND
                                       ASTM 09       0.00                0.0             ND


 TEM
                                       ASTM 14       0.00                0.0             ND
                                       ASTM 15       0.00                0.0             ND
                                       ASTM 16       0.00                0.0             ND


 Drop
                                       ASTM 18       0.00                0.0             ND
                                       ASTM 01       2.46                0.1           Detect
                                       ASTM 03       2.75                0.1           Detect


 Mount
                                       ASTM 04       1.67                0.1           Detect
                                       ASTM 07       2.44                0.1           Detect
                                       ASTM 13       2.25                0.1           Detect
                                       ASTM 17       4.74                0.1           Detect
                                       ASTM 18       3.96                0.1           Detect
                                       ASTM 06       8.65                1.0           Detect
                                       ASTM 07       7.52                1.0           Detect
                                       ASTM 11       7.57                1.0           Detect
                                       ASTM 12       4.30                1.0           Detect
                                       ASTM 19       7.45                1.0           Detect
                                       ASTM 20       8.61                1.0           Detect
                                       ASTM 21       6.20                1.0           Detect
Copyright 2011 EMSL Analytical, Inc.
ASTM Results at 0.1% Phase I
                   4.50                                       64
                   4.00

                   3.50

                   3.00

                   2.50
Percent Asbestos




                   2.00

                   1.50

                   1.00

                   0.50

                   0.00
  Sample                       1          2            3            4   5   6   7



                          Overall Percent Recovery :       1432 %
                          Overall (Pooled) RSD :           0.39
   Copyright 2011 EMSL Analytical, Inc.
ASTM Results at 1% Phase I
                   16.0                                  65

                   14.0


                   12.0


                   10.0
Percent Asbestos




                    8.0


                    6.0


                    4.0


                    2.0
             Sample
                    0.0
                              1           2        3          4   5   6   7


                          Overall Percent Recovery :    569 %
                          Overall (Pooled) RSD :       0.23
   Copyright 2011 EMSL Analytical, Inc.
Summary of ASTM
                Results - Phase I
                                       66




  Overall (Pooled) Percent Recovery:               1090 %

  Overall (Pooled) RSD:                     0.32


Copyright 2011 EMSL Analytical, Inc.
ASTM Round Robin Results
                                   Soil spiked with 0.2% Asbestos
                                                  67
        950% recovery
                                       Lab A   Lab B   Lab C    Lab D      Mean
    % asbestos in                       0.5     0.75    0.72        2.0    0.99
    >2mm fraction *
    % asbestos in 2mm                   2.0     2.5     0.87        3.7     2.3
    – 100um fraction *
    % asbestos in                       0.5     0.5      0          0.25   0.31
    <100um fraction *
    Total percent                       1.7     2.15    0.73        3.1     1.9
    asbestos *
    % asbestos by                       0.5     0.5     0.25        0.25   0.375
    point-count
    Drop mount                         Trace   <0.1     1%      Trace      <1%
    estimate
    Structures per                     5,700    520    15,000   7,700      7,200
    microgram

Copyright 2011 EMSL Analytical, Inc.
CARB Method 435 Results
                                       68




Copyright 2011 EMSL Analytical, Inc.
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.
CARB 435 Results at 0.1%
 4
      Phase I                               70


3.5

 3

2.5

 2

1.5

 1

0.5

 0 Sample
              1                  2     3         4         5          6   7

          Overall Percent Recovery: 787 % Excluding False Negatives
          Overall (Pooled) RSD:     0.73
Copyright 2011 EMSL Analytical, Inc.
CARB 435 Results at 1%
                   Phase I
                   18                            71

                   16

                   14

                   12

                   10
Percent Asbestos




                    8

                    6

                    4

                    2

                    0
                            1            2   3        4      5        6        7
                   Sample

        Overall Percent Recovery:                  475 % excluding false negatives
        Overall (Pooled) RSD:                     0.52
  Copyright 2011 EMSL Analytical, Inc.
CARB 435 Performance
        Phase I
                                       72




 Overall (Pooled) Percent Recovery:                650 %
 Overall (Pooled) RSD:                      0.64


Copyright 2011 EMSL Analytical, Inc.
Method Performance Phase I
   Accuracy                                                          73


                     0.1% Spiked Sample                                                        1% Spiked sample

                   2500
                                                                                         900

                               Excluding false negatives
                                                                                         800
                   2000
                                                                                         700
Percent Recovery




                                                                                         600




                                                                      Percent Recovery
                   1500
                                                                                         500

                                                                                         400
                   1000
                                                                                         300

                                                                                         200
                   500
                                                                                         100

                                                                                          0
                     0
                                                                                                EPA   ASTM   CARB   Target
                          EPA         ASTM       CARB       Target

   Copyright 2011 EMSL Analytical, Inc.
Method Performance Phase I
Precision                                     74


        0.1% Spiked Sample                               1% Spiked sample
 Relative Standard Deviation                       Relative Standard Deviation
  0.8                                              7


  0.7                                              6

  0.6
                                                   5

  0.5
                                                   4
  0.4
                                                   3
  0.3

                                                   2
  0.2


  0.1                                              1


   0                                               0
              EPA               ASTM   CARB                EPA           ASTM    CARB

Copyright 2011 EMSL Analytical, Inc.
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.
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.
Phase II
                                          77



  Spiking with Consolidated
   Asbestos (ACM)
  - Transite supplied by RTI
  - Estimated Chrysotile
    percentage = 14%


Copyright 2011 EMSL Analytical, Inc.
78




  Phase II
  EPA 600
  Method Results




Copyright 2011 EMSL Analytical, Inc.
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.
EPA 600 - 0.1% - Phase II
                                           80
 3.5

    3

 2.5

    2

 1.5

    1

 0.5

    0
                 1                 2   3        4   5        6   7
          Overall Percent Recovery :                 726 %
          Overall (Pooled) RSD:                     0.43
Copyright 2011 EMSL Analytical, Inc.
EPA 600 - 1% - Phase II
                                               81

 10
   8
   6
   4
   2
   0
                  1                    2   3        4   5     6      7
     Overall Percent Recovery for this Sample:               214 %
     Overall (Pooled) RSD for this Sample:                  0.32
Copyright 2011 EMSL Analytical, Inc.
EPA 600 Summary
              Phase II
                                       82




   Overall (Pooled) Percent Recovery 535 %

         Overall (Pooled) RSD :             0.38


Copyright 2011 EMSL Analytical, Inc.
Phase II ASTM Sieve
         Method Results
                                       83




Copyright 2011 EMSL Analytical, Inc.
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.
ASTM - 0.1% - Phase II
                                           85
 4.00

 3.50

 3.00

 2.50

 2.00

 1.50

 1.00

 0.50

 0.00
                 1                 2   3        4   5     6     7

    Overall Percent Recovery:                           519 %
    Overall (Pooled) RSD for this Sample:               0.6
Copyright 2011 EMSL Analytical, Inc.
ASTM - 1% - Phase II
                                           86
10.00

 9.00

 8.00

 7.00

 6.00

 5.00

 4.00

 3.00

 2.00

 1.00

 0.00
               1                  2    3        4   5      6    7


  Overall Percent Recovery :                            188 %
  Overall (Pooled) RSD:                                 0.4
Copyright 2011 EMSL Analytical, Inc.
ASTM Summary
                        Phase II
                                       87




 Overall (Pooled) Percent Recovery:         391 %
   Overall (pooled) RSD:                    0.5



Copyright 2011 EMSL Analytical, Inc.
Phase II
   CARB Method 435 Results
                                       88




Copyright 2011 EMSL Analytical, Inc.
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.
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.
Phase II – CARB - 1%
                                           91
  3


2.5


  2


1.5


  1


0.5


  0
              1                  2     3        4   5   6        7

 Overall Percent Recovery :                               91 %
 Overall (Pooled) RSD:                                  0.46
Copyright 2011 EMSL Analytical, Inc.
Phase II CARB
                      Summary
                                       92



     Overall (Pooled) Percent Recovery :           167 %

     Overall (Pooled) RSD:                  0.57



Copyright 2011 EMSL Analytical, Inc.
Final Score Card
                                            93

Phase I                           EPA600    ASTM Sieve   CARB 435
 % Recovery                        1540        1090        650
    RSD                            0.55        0.32        0.64




Phase II
                                   EPA600   ASTM Sieve   CARB 435
  % Recovery                         535       391         167
     RSD                            0.38       0.5         .57

Copyright 2011 EMSL Analytical, Inc.
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.
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.
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.
• CARB 435 mentioned
  • 1% is not an appropriate action level for asbestos in soil
                                       97




Copyright 2011 EMSL Analytical, Inc.
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.
Real World Test Drive
            of the Methods
                                       99




Copyright 2011 EMSL Analytical, Inc.
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.
Savage Arms
                                            10
                                            1




Copyright 2011 EMSL Analytical, Inc.
Charlestown Mall
                                       10
                                       2




Copyright 2011 EMSL Analytical, Inc.
Photo Taken by NY DOL on
            First Walk Through of Site 103




Copyright 2011 EMSL Analytical, Inc.
Charlestown Mall
                                       104




Copyright 2011 EMSL Analytical, Inc.
Charlestown Mall
                                       105




                                             Utica NY
Copyright 2011 EMSL Analytical, Inc.
Charlestown Mall
                                       106




Copyright 2011 EMSL Analytical, Inc.
107




Copyright 2011 EMSL Analytical, Inc.
Perimeter Air Samples
                                       108




Copyright 2011 EMSL Analytical, Inc.
Controlled Demo
                                       109




Copyright 2011 EMSL Analytical, Inc.
School Across the Street
                                       110




Copyright 2011 EMSL Analytical, Inc.
111




Copyright 2011 EMSL Analytical, Inc.
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.
One way to
 help
 homogenize
 the samples
 either in the
 field or after
 submittal to
 the lab

                                       Riffle Splitting
Copyright 2011 EMSL Analytical, Inc.
Charlestown Nuggets
                                       114




Copyright 2011 EMSL Analytical, Inc.
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.
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.
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.
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.
Risk Assessment Methods

     The Elutriator Method

   Tumbler
   apparatus
   filled with
   soil



Copyright 2011 EMSL Analytical, Inc.
Risk Assessment Methods

     The Elutriator Method
                Tumbler inside enclosed humidity chamber




Copyright 2011 EMSL Analytical, Inc.
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.
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.
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.
RAF Unit




Copyright 2011 EMSL Analytical, Inc.
RAF Unit




Copyright 2011 EMSL Analytical, Inc.
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.
Fluidized Bed




Copyright 2011 EMSL Analytical, Inc.
Fluidized
                                          Bed



Copyright 2011 EMSL Analytical, Inc.
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.

Más contenido relacionado

Soil method performance asbestos eia annapolis 2011 09 16

  • 1. Ed Cahill National Director Asbestos Lab Services ecahill@emsl.com EMSL Analytical, Inc. 200 Route 130 North, Cinnaminson, NJ 08108 856-303-2565 www.emsl.com
  • 3. Soil is a Great Hiding Place 3  1% Unconsolidated  1% Consolidated Chrysotile Chrysotile Copyright 2011 EMSL Analytical, Inc.
  • 4. Soil is a Great Hiding Place for Asbestos 4 1% asbestos Copyright 2011 EMSL Analytical, Inc.
  • 5. Sources of Asbestos in Soil 5 Asbestos Contamination Natural Occurrences of Asbestos (NOA) Copyright 2011 EMSL Analytical, Inc.
  • 6. Asbestos Contamination 6 Copyright 2011 EMSL Analytical, Inc.
  • 7. 7 Copyright 2011 EMSL Analytical, Inc.
  • 8. 8 Copyright 2011 EMSL Analytical, Inc.
  • 9. 9 Copyright 2011 EMSL Analytical, Inc.
  • 10. Natural Occurrences of Asbestos (NOA) 10 Copyright 2011 EMSL Analytical, Inc.
  • 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 Copyright 2011 EMSL Analytical, Inc.
  • 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 Copyright 2011 EMSL Analytical, Inc.
  • 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 Copyright 2011 EMSL Analytical, Inc.
  • 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 Copyright 2011 EMSL Analytical, Inc.
  • 32. Wet Sieving of Same Sample 32 Sieve Stack Coarse, Medium Copyright 2011 EMSL Analytical, Inc.
  • 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.
  • 34. Dry vs. Wet Sieving 34 100.00 90.00 80.00 DRY WET 70.00 60.00 50.00 40.00 30.00 20.00 10.00 0.00 >2mm >106µm <106µm 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 Copyright 2011 EMSL Analytical, Inc.
  • 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? Copyright 2011 EMSL Analytical, Inc.
  • 40. Two Approaches to Soil Sieving Milling Copyright 2011 EMSL Analytical, Inc.
  • 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 Copyright 2011 EMSL Analytical, Inc.
  • 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 Copyright 2011 EMSL Analytical, Inc.
  • 46. How Do They Compare? 46 Copyright 2011 EMSL Analytical, Inc.
  • 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.
  • 50. Asbestos Characterization 50 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.
  • 54. Phase 1 Samples 54 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.
  • 56. 56 Phase 1 EPA 600 Method Results 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.
  • 59. EPA 600 Results at 1% Phase I 30 59 25 20 Percent Asbestos 15 10 5 0 Sample 1 2 3 4 5 6 7 Overall Percent Recovery: 835 % Overall (Pooled) RSD: 0.56 Copyright 2011 EMSL Analytical, Inc.
  • 60. EPA 600 Summary Phase I 60 Overall (Pooled) Percent Recovery : 1574 % Overall (Pooled) RSD : 0.54 Copyright 2011 EMSL Analytical, Inc.
  • 61. ASTM Sieve Method Results 61 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.
  • 63. Analyst 1 63 PLM Results TEM Results Drop Mount Detect/Non Label # Analyst 1 True % Detect ASTM 02 0.00 0.0 ND ASTM 05 0.50 0.0 ND ASTM 09 0.00 0.0 ND TEM ASTM 14 0.00 0.0 ND ASTM 15 0.00 0.0 ND ASTM 16 0.00 0.0 ND Drop ASTM 18 0.00 0.0 ND ASTM 01 2.46 0.1 Detect ASTM 03 2.75 0.1 Detect Mount ASTM 04 1.67 0.1 Detect ASTM 07 2.44 0.1 Detect ASTM 13 2.25 0.1 Detect ASTM 17 4.74 0.1 Detect ASTM 18 3.96 0.1 Detect ASTM 06 8.65 1.0 Detect ASTM 07 7.52 1.0 Detect ASTM 11 7.57 1.0 Detect ASTM 12 4.30 1.0 Detect ASTM 19 7.45 1.0 Detect ASTM 20 8.61 1.0 Detect ASTM 21 6.20 1.0 Detect Copyright 2011 EMSL Analytical, Inc.
  • 64. ASTM Results at 0.1% Phase I 4.50 64 4.00 3.50 3.00 2.50 Percent Asbestos 2.00 1.50 1.00 0.50 0.00 Sample 1 2 3 4 5 6 7 Overall Percent Recovery : 1432 % Overall (Pooled) RSD : 0.39 Copyright 2011 EMSL Analytical, Inc.
  • 65. ASTM Results at 1% Phase I 16.0 65 14.0 12.0 10.0 Percent Asbestos 8.0 6.0 4.0 2.0 Sample 0.0 1 2 3 4 5 6 7 Overall Percent Recovery : 569 % Overall (Pooled) RSD : 0.23 Copyright 2011 EMSL Analytical, Inc.
  • 66. Summary of ASTM Results - Phase I 66 Overall (Pooled) Percent Recovery: 1090 % Overall (Pooled) RSD: 0.32 Copyright 2011 EMSL Analytical, Inc.
  • 67. ASTM Round Robin Results Soil spiked with 0.2% Asbestos 67 950% recovery Lab A Lab B Lab C Lab D Mean % asbestos in 0.5 0.75 0.72 2.0 0.99 >2mm fraction * % asbestos in 2mm 2.0 2.5 0.87 3.7 2.3 – 100um fraction * % asbestos in 0.5 0.5 0 0.25 0.31 <100um fraction * Total percent 1.7 2.15 0.73 3.1 1.9 asbestos * % asbestos by 0.5 0.5 0.25 0.25 0.375 point-count Drop mount Trace <0.1 1% Trace <1% estimate Structures per 5,700 520 15,000 7,700 7,200 microgram Copyright 2011 EMSL Analytical, Inc.
  • 68. CARB Method 435 Results 68 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.
  • 70. CARB 435 Results at 0.1% 4 Phase I 70 3.5 3 2.5 2 1.5 1 0.5 0 Sample 1 2 3 4 5 6 7 Overall Percent Recovery: 787 % Excluding False Negatives Overall (Pooled) RSD: 0.73 Copyright 2011 EMSL Analytical, Inc.
  • 71. CARB 435 Results at 1% Phase I 18 71 16 14 12 10 Percent Asbestos 8 6 4 2 0 1 2 3 4 5 6 7 Sample Overall Percent Recovery: 475 % excluding false negatives Overall (Pooled) RSD: 0.52 Copyright 2011 EMSL Analytical, Inc.
  • 72. CARB 435 Performance Phase I 72 Overall (Pooled) Percent Recovery: 650 % Overall (Pooled) RSD: 0.64 Copyright 2011 EMSL Analytical, Inc.
  • 73. Method Performance Phase I Accuracy 73 0.1% Spiked Sample 1% Spiked sample 2500 900  Excluding false negatives 800 2000 700 Percent Recovery 600 Percent Recovery 1500 500 400 1000 300 200 500 100 0 0 EPA ASTM CARB Target EPA ASTM CARB Target Copyright 2011 EMSL Analytical, Inc.
  • 74. Method Performance Phase I Precision 74 0.1% Spiked Sample 1% Spiked sample Relative Standard Deviation Relative Standard Deviation 0.8 7 0.7 6 0.6 5 0.5 4 0.4 3 0.3 2 0.2 0.1 1 0 0 EPA ASTM CARB EPA ASTM CARB 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.
  • 80. EPA 600 - 0.1% - Phase II 80 3.5 3 2.5 2 1.5 1 0.5 0 1 2 3 4 5 6 7 Overall Percent Recovery : 726 % Overall (Pooled) RSD: 0.43 Copyright 2011 EMSL Analytical, Inc.
  • 81. EPA 600 - 1% - Phase II 81 10 8 6 4 2 0 1 2 3 4 5 6 7 Overall Percent Recovery for this Sample: 214 % Overall (Pooled) RSD for this Sample: 0.32 Copyright 2011 EMSL Analytical, Inc.
  • 82. EPA 600 Summary Phase II 82 Overall (Pooled) Percent Recovery 535 % Overall (Pooled) RSD : 0.38 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.
  • 85. ASTM - 0.1% - Phase II 85 4.00 3.50 3.00 2.50 2.00 1.50 1.00 0.50 0.00 1 2 3 4 5 6 7 Overall Percent Recovery: 519 % Overall (Pooled) RSD for this Sample: 0.6 Copyright 2011 EMSL Analytical, Inc.
  • 86. ASTM - 1% - Phase II 86 10.00 9.00 8.00 7.00 6.00 5.00 4.00 3.00 2.00 1.00 0.00 1 2 3 4 5 6 7 Overall Percent Recovery : 188 % Overall (Pooled) RSD: 0.4 Copyright 2011 EMSL Analytical, Inc.
  • 87. ASTM Summary Phase II 87 Overall (Pooled) Percent Recovery: 391 % Overall (pooled) RSD: 0.5 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.
  • 91. Phase II – CARB - 1% 91 3 2.5 2 1.5 1 0.5 0 1 2 3 4 5 6 7 Overall Percent Recovery : 91 % Overall (Pooled) RSD: 0.46 Copyright 2011 EMSL Analytical, Inc.
  • 92. Phase II CARB Summary 92 Overall (Pooled) Percent Recovery : 167 % Overall (Pooled) RSD: 0.57 Copyright 2011 EMSL Analytical, Inc.
  • 93. Final Score Card 93 Phase I EPA600 ASTM Sieve CARB 435 % Recovery 1540 1090 650 RSD 0.55 0.32 0.64 Phase II EPA600 ASTM Sieve CARB 435 % Recovery 535 391 167 RSD 0.38 0.5 .57 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.
  • 102. Charlestown Mall 10 2 Copyright 2011 EMSL Analytical, Inc.
  • 103. Photo Taken by NY DOL on First Walk Through of Site 103 Copyright 2011 EMSL Analytical, Inc.
  • 104. Charlestown Mall 104 Copyright 2011 EMSL Analytical, Inc.
  • 105. Charlestown Mall 105 Utica NY Copyright 2011 EMSL Analytical, Inc.
  • 106. Charlestown Mall 106 Copyright 2011 EMSL Analytical, Inc.
  • 107. 107 Copyright 2011 EMSL Analytical, Inc.
  • 108. Perimeter Air Samples 108 Copyright 2011 EMSL Analytical, Inc.
  • 109. Controlled Demo 109 Copyright 2011 EMSL Analytical, Inc.
  • 110. School Across the Street 110 Copyright 2011 EMSL Analytical, Inc.
  • 111. 111 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.
  • 114. Charlestown Nuggets 114 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.
  • 124. RAF Unit Copyright 2011 EMSL Analytical, Inc.
  • 125. RAF Unit 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.
  • 127. Fluidized Bed 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.