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Ed Cahill National Director Asbestos Lab Services [email protected] EMSL Analytical, Inc. 200 Route 130 North, Cinnaminson, NJ 08108 856-303-2565 www.emsl.com
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Soil method performance asbestos eia annapolis 2011 09 16

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Page 1: Soil method performance asbestos  eia annapolis 2011 09 16

Ed Cahill

National Director Asbestos Lab Services

[email protected]

EMSL Analytical, Inc.

200 Route 130 North, Cinnaminson, NJ 08108

856-303-2565 www.emsl.com

Page 2: Soil method performance asbestos  eia annapolis 2011 09 16

Asbestos in Soil

Page 3: Soil method performance asbestos  eia annapolis 2011 09 16

Soil is a Great Hiding Place

1% Unconsolidated Chrysotile

1% Consolidated Chrysotile

3

Copyright 2011 EMSL Analytical, Inc.

Page 4: Soil method performance asbestos  eia annapolis 2011 09 16

Soil is a Great Hiding Place for Asbestos

1% asbestos

4

Copyright 2011 EMSL Analytical, Inc.

Page 5: Soil method performance asbestos  eia annapolis 2011 09 16

Asbestos

Contamination

Sources of Asbestos in Soil

Natural Occurrences

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

5

Page 6: Soil method performance asbestos  eia annapolis 2011 09 16

Asbestos Contamination

Copyright 2011 EMSL Analytical, Inc.

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Page 7: Soil method performance asbestos  eia annapolis 2011 09 16

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Copyright 2011 EMSL Analytical, Inc.

Page 8: Soil method performance asbestos  eia annapolis 2011 09 16

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Copyright 2011 EMSL Analytical, Inc.

Page 9: Soil method performance asbestos  eia annapolis 2011 09 16

9

Copyright 2011 EMSL Analytical, Inc.

Page 10: Soil method performance asbestos  eia annapolis 2011 09 16

Natural Occurrences of Asbestos (NOA)

Copyright 2011 EMSL Analytical, Inc.

10

Page 11: Soil method performance asbestos  eia annapolis 2011 09 16

Staten Island Serpentinite

Copyright 2011 EMSL Analytical, Inc.

I 278 road cut. Up to 50% Chrysotile

Picture and info: Brooklyn CUNY.edu

Page 12: Soil method performance asbestos  eia annapolis 2011 09 16

Why is Soil so Hard to Analyze?

Copyright 2011 EMSL Analytical, Inc.

12

Page 13: Soil method performance asbestos  eia annapolis 2011 09 16

Why is Soil so Hard to Analyze?

Non-Homogeneity

Grain size

Copyright 2011 EMSL Analytical, Inc.

13

Page 14: Soil method performance asbestos  eia annapolis 2011 09 16

Scales of Non-Homogeneity

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.

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Page 15: Soil method performance asbestos  eia annapolis 2011 09 16

Scales on Non-Homogeneity

The Medium

Picture

How deep to go?

What layers to

include?

Copyright 2011 EMSL Analytical, Inc.

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Page 16: Soil method performance asbestos  eia annapolis 2011 09 16

Scales on Non-Homogeneity

The Fine Picture

Obtaining a

representative sub-

sample in the lab is

important.

Copyright 2011 EMSL Analytical, Inc.

16

Page 17: Soil method performance asbestos  eia annapolis 2011 09 16

Scales on Non-Homogeneity

The presence of even sand sized quartz crystals are a problem.

The Very Fine Picture

stereoscopic view of play sand

Copyright 2011 EMSL Analytical, Inc.

17

Page 18: Soil method performance asbestos  eia annapolis 2011 09 16

In Summary

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.

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Page 19: Soil method performance asbestos  eia annapolis 2011 09 16

Analytical Choices What Method to Choose?

Copyright 2011 EMSL Analytical, Inc.

19

Page 20: Soil method performance asbestos  eia annapolis 2011 09 16

Limitations of “Standard” PLM

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.

20

Page 21: Soil method performance asbestos  eia annapolis 2011 09 16

Sieving Milling

Copyright 2011 EMSL Analytical, Inc.

Two Approaches to Soil

Page 22: Soil method performance asbestos  eia annapolis 2011 09 16

Scenario 1 - Contamination of Soil with ACM

The Main Sieve Methods Available

Copyright 2010 EMSL Analytical, Inc.

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

Page 23: Soil method performance asbestos  eia annapolis 2011 09 16

Copyright 2011 EMSL Analytical, Inc.

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

EPA Region 1 Screening Protocol

Scenario 1 - Contamination of Soil with ACM

EPA Region 1 Protocol

Page 24: Soil method performance asbestos  eia annapolis 2011 09 16

Sample Size 250 cc or less

Sieve Stack

• 19 mm (3/4”)

• 2 mm

• 106 micron

DRAFT ASTM Sieve Method

Copyright 2011 EMSL Analytical, Inc.

24

Anything larger than 19 mm is not considered part of the sample

Page 25: Soil method performance asbestos  eia annapolis 2011 09 16

1) Sample is dried

2) Weighed

3) Dry Sieved (wet sieving is optional) on sieve shaker for 5 minutes

ASTM Sieve Method

Copyright 2011 EMSL Analytical, Inc.

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Page 26: Soil method performance asbestos  eia annapolis 2011 09 16

ASTM Sieve Method

Coarse and Medium Fractions still too large for straight PLM

4) Weigh each fraction 5) Analyze each fraction

Copyright 2011 EMSL Analytical, Inc.

26

This is a common type of sample (mini clods))

Page 27: Soil method performance asbestos  eia annapolis 2011 09 16

ASTM Sieve Method

The fine fraction is

fine enough and

homogenous enough

for a PLM slide prep

and analysis

Copyright 2011 EMSL Analytical, Inc.

27

Page 28: Soil method performance asbestos  eia annapolis 2011 09 16

Wet or Dry? 28

Copyright 2011 EMSL Analytical, Inc.

Pros • Washes the suspect

ACM making for easier detection

• Breaks down matrix to its smallest components

Page 29: Soil method performance asbestos  eia annapolis 2011 09 16

Wet Sieving Can Be Better for Some Soils

29

Copyright 2011 EMSL Analytical, Inc.

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

Page 30: Soil method performance asbestos  eia annapolis 2011 09 16

“Typical” soil sample

on sieve stack

DRY Sieving on an Automatic sieve shaker

30

Copyright 2011 EMSL Analytical, Inc.

Comparison of Dry vs. Wet Sieving

Page 31: Soil method performance asbestos  eia annapolis 2011 09 16

Coarse, Medium and Fine Fractions 31

Copyright 2011 EMSL Analytical, Inc.

soil clods fail to make it through the 2mm sieve

Page 32: Soil method performance asbestos  eia annapolis 2011 09 16

Sieve Stack Coarse, Medium

32

Copyright 2011 EMSL Analytical, Inc.

Wet Sieving of Same Sample

Page 33: Soil method performance asbestos  eia annapolis 2011 09 16

The Same Sample ! 33

Copyright 2011 EMSL Analytical, Inc.

Coarse 86%

Medium 12%

Fine 1%

Dry Sieving

Coarse 34%

Medium 26%

Fine 40%

Wet Sieving

Page 34: Soil method performance asbestos  eia annapolis 2011 09 16

Dry vs. Wet Sieving 34

Copyright 2011 EMSL Analytical, Inc.

0.00

10.00

20.00

30.00

40.00

50.00

60.00

70.00

80.00

90.00

100.00

>2mm >106µm <106µm

DRY WET

Page 35: Soil method performance asbestos  eia annapolis 2011 09 16

HAND PICKING SUSPECT ACM

OUT OF COARSE AND MEDIUM FRACTIONS.

35

Copyright 2011 EMSL Analytical, Inc.

Visual and Stereomicroscopic Analysis

Page 36: Soil method performance asbestos  eia annapolis 2011 09 16

ASTM Analysis 36

Copyright 2011 EMSL Analytical, Inc.

Page 37: Soil method performance asbestos  eia annapolis 2011 09 16

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.

Page 38: Soil method performance asbestos  eia annapolis 2011 09 16

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

ASTM Sieve Method

Copyright 2011 EMSL Analytical, Inc.

38

Page 39: Soil method performance asbestos  eia annapolis 2011 09 16

TEM Quantitative Analysis

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?

39

Copyright 2011 EMSL Analytical, Inc.

Page 40: Soil method performance asbestos  eia annapolis 2011 09 16

Sieving Milling

Copyright 2011 EMSL Analytical, Inc.

Two Approaches to Soil

Page 41: Soil method performance asbestos  eia annapolis 2011 09 16

Copyright 2011 EMSL Analytical, Inc.

The MILLING Approach

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

Page 42: Soil method performance asbestos  eia annapolis 2011 09 16

Determination of Asbestos Content of Serpentine Aggregate

This is the current de facto standard for milling methods.

1. One pint (473cc) sample

2. milled to 200 mesh (74 microns)

3. PLM

CA Air Resources Board (CARB) Method 435

Copyright 2011 EMSL Analytical, Inc.

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Page 43: Soil method performance asbestos  eia annapolis 2011 09 16

Milled to reduce the nominal particle size to 75 microns

The sample is dried in a drying oven and material >3/8” is removed by sieving

CARB 435 Method

Copyright 2011 EMSL Analytical, Inc.

43

Page 44: Soil method performance asbestos  eia annapolis 2011 09 16

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.

Page 45: Soil method performance asbestos  eia annapolis 2011 09 16

Copyright 2011 EMSL Analytical, Inc.

Analyzed by TEM at 20,000X

TEM CARB Method

Page 46: Soil method performance asbestos  eia annapolis 2011 09 16

How Do They Compare?

Copyright 2011 EMSL Analytical, Inc.

46

Page 47: Soil method performance asbestos  eia annapolis 2011 09 16

Study Design

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.

47

Page 48: Soil method performance asbestos  eia annapolis 2011 09 16

Phase I

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.

48

Page 49: Soil method performance asbestos  eia annapolis 2011 09 16

Phase 1

Unconsolidated Asbestos

Phase 2

Consolidated (ACM) Asbestos

49

Copyright 2011 EMSL Analytical, Inc.

The Big Plan

Page 50: Soil method performance asbestos  eia annapolis 2011 09 16

Asbestos Characterization

Copyright 2011 EMSL Analytical, Inc.

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Page 51: Soil method performance asbestos  eia annapolis 2011 09 16

Asbestos Characterization

Copyright 2011 EMSL Analytical, Inc.

51

Fiber Size Data for Data Plastibest-20 – 100 fibers by TEM at 20K Mag

Fiber Length (microns)

0

2

4

6

8

10

12

14

16

18

Approx. 20% of fibers are optically visible (> 0.2 microns in width)

Page 52: Soil method performance asbestos  eia annapolis 2011 09 16

Asbestos Characterization

Copyright 2011 EMSL Analytical, Inc.

52

0

5

10

15

20

25

30

Fiber Size Data for Arizona Chrysotile – 100 fibers by TEM at 20K Mag

Fiber Length (microns)

Approx. 13% of fibers are optically visible (> 0.2 microns in width)

Page 53: Soil method performance asbestos  eia annapolis 2011 09 16

Spiking

Copyright 2011 EMSL Analytical, Inc.

53

• Seven Blanks

• Seven samples at 0.1%

• Seven samples at 1%

ASTM Sieve Method EPA 600 CARB Method 435

To eliminate the variability of possible non-homogeneity, no

sub-sampling was performed. 63 individual samples were

prepared.

Page 54: Soil method performance asbestos  eia annapolis 2011 09 16

Phase 1 Samples

Copyright 2011 EMSL Analytical, Inc.

54

Page 55: Soil method performance asbestos  eia annapolis 2011 09 16

Analyst Credentials 55

Copyright 2011 EMSL Analytical, Inc.

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

Page 56: Soil method performance asbestos  eia annapolis 2011 09 16

56

Copyright 2011 EMSL Analytical, Inc.

Phase 1 EPA 600 Method Results

Page 57: Soil method performance asbestos  eia annapolis 2011 09 16

EPA 600 Results for Blanks Phase I

Copyright 2011 EMSL Analytical, Inc.

57

Analyst 1 Analyst 2 Analyst 3 Analyst 4 Analyst 5 Analyst 6

Sample Number

Asbestos % 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

Page 58: Soil method performance asbestos  eia annapolis 2011 09 16

0

1

2

3

4

5

6

7

8

1 2 3 4 5 6 7Sample

Perc

ent

Asb

est

os

Copyright 2011 EMSL Analytical, Inc.

58

Each color represents an analyst

Overall Percent Recovery: 2063 % Overall (pooled) RSD: 0.51

EPA 600 Results at 0.1% Phase I

Page 59: Soil method performance asbestos  eia annapolis 2011 09 16

Sample

Perc

ent

Asb

est

os

Copyright 2011 EMSL Analytical, Inc.

59

0

5

10

15

20

25

30

1 2 3 4 5 6 7

Overall Percent Recovery: 835 % Overall (Pooled) RSD: 0.56

EPA 600 Results at 1% Phase I

Page 60: Soil method performance asbestos  eia annapolis 2011 09 16

EPA 600 Summary Phase I

60

Copyright 2011 EMSL Analytical, Inc.

Overall (Pooled) Percent Recovery : 1574 %

Overall (Pooled) RSD : 0.54

Page 61: Soil method performance asbestos  eia annapolis 2011 09 16

ASTM Sieve Method Results

Copyright 2011 EMSL Analytical, Inc.

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Page 62: Soil method performance asbestos  eia annapolis 2011 09 16

ASTM Results for Blanks Phase I

Copyright 2011 EMSL Analytical, Inc.

62

Analyst 1 Analyst 2 Analyst3 Analyst 4 Analyst 5 Analyst 6

Sample Number

Asbestos % 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

Page 63: Soil method performance asbestos  eia annapolis 2011 09 16

63

Copyright 2011 EMSL Analytical, Inc.

TEM Drop

Mount

Analyst 1

PLM Results TEM Results

Label # Analyst 1 True % Drop Mount Detect/Non

Detect

ASTM 02 0.00 0.0 ND

ASTM 05 0.50 0.0 ND

ASTM 09 0.00 0.0 ND

ASTM 14 0.00 0.0 ND

ASTM 15 0.00 0.0 ND

ASTM 16 0.00 0.0 ND

ASTM 18 0.00 0.0 ND

ASTM 01 2.46 0.1 Detect

ASTM 03 2.75 0.1 Detect

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

Page 64: Soil method performance asbestos  eia annapolis 2011 09 16

Sample

Perc

ent

Asb

est

os

Copyright 2011 EMSL Analytical, Inc.

64

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

4.50

1 2 3 4 5 6 7

Overall Percent Recovery : 1432 % Overall (Pooled) RSD : 0.39

ASTM Results at 0.1% Phase I

Page 65: Soil method performance asbestos  eia annapolis 2011 09 16

Sample

Perc

ent

Asb

est

os

Copyright 2011 EMSL Analytical, Inc.

65

0.0

2.0

4.0

6.0

8.0

10.0

12.0

14.0

16.0

1 2 3 4 5 6 7

Overall Percent Recovery : 569 % Overall (Pooled) RSD : 0.23

ASTM Results at 1% Phase I

Page 66: Soil method performance asbestos  eia annapolis 2011 09 16

Summary of ASTM Results - Phase I

66

Copyright 2011 EMSL Analytical, Inc.

Overall (Pooled) Percent Recovery: 1090 %

Overall (Pooled) RSD: 0.32

Page 67: Soil method performance asbestos  eia annapolis 2011 09 16

ASTM Round Robin Results Soil spiked with 0.2% Asbestos

Lab A Lab B Lab C Lab D Mean

% asbestos in

>2mm fraction *

0.5 0.75 0.72 2.0 0.99

% asbestos in 2mm

– 100um fraction *

2.0 2.5 0.87 3.7 2.3

% asbestos in

<100um fraction *

0.5 0.5 0 0.25 0.31

Total percent

asbestos *

1.7 2.15 0.73 3.1 1.9

% asbestos by

point-count

0.5 0.5 0.25 0.25 0.375

Drop mount

estimate

Trace <0.1 1% Trace <1%

Structures per

microgram

5,700 520 15,000 7,700 7,200

950% recovery

Copyright 2011 EMSL Analytical, Inc.

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CARB Method 435 Results

Copyright 2011 EMSL Analytical, Inc.

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Page 69: Soil method performance asbestos  eia annapolis 2011 09 16

CARB 435 Results on Blanks Phase I

Copyright 2011 EMSL Analytical, Inc.

69

Analyst 1 Analyst 2 Analyst 3 Analyst 4 Analyst 5 Analyst 6

Sample Number

Asbestos % 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

Page 70: Soil method performance asbestos  eia annapolis 2011 09 16

Copyright 2011 EMSL Analytical, Inc.

70

Sample 0

0.5

1

1.5

2

2.5

3

3.5

4

1 2 3 4 5 6 7

Overall Percent Recovery: 787 % Excluding False Negatives Overall (Pooled) RSD: 0.73

CARB 435 Results at 0.1% Phase I

Page 71: Soil method performance asbestos  eia annapolis 2011 09 16

Copyright 2011 EMSL Analytical, Inc.

71

Per

cen

t A

sbes

tos

Sample

0

2

4

6

8

10

12

14

16

18

1 2 3 4 5 6 7

Overall Percent Recovery: 475 % excluding false negatives Overall (Pooled) RSD: 0.52

CARB 435 Results at 1% Phase I

Page 72: Soil method performance asbestos  eia annapolis 2011 09 16

CARB 435 Performance Phase I

72

Copyright 2011 EMSL Analytical, Inc.

Overall (Pooled) Percent Recovery: 650 %

Overall (Pooled) RSD: 0.64

Page 73: Soil method performance asbestos  eia annapolis 2011 09 16

0

500

1000

1500

2000

2500

EPA ASTM CARB Target

0.1% Spiked Sample 1% Spiked sample

Excluding false negatives

73

Copyright 2011 EMSL Analytical, Inc.

Method Performance Phase I Accuracy

Perc

ent

Reco

very

Perc

ent

Reco

very

0

100

200

300

400

500

600

700

800

900

EPA ASTM CARB Target

Page 74: Soil method performance asbestos  eia annapolis 2011 09 16

0.1% Spiked Sample 1% Spiked sample

Relative Standard Deviation

74

Copyright 2011 EMSL Analytical, Inc.

Method Performance Phase I Precision

Relative Standard Deviation

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

EPA ASTM CARB

0

1

2

3

4

5

6

7

EPA ASTM CARB

Page 75: Soil method performance asbestos  eia annapolis 2011 09 16

Score Card Phase I Pooled Data for the Round

EPA600 ASTM Sieve CARB 435 %

Recovery 1540 1090 650

RSD 0.55 0.32 0.64

Copyright 2011 EMSL Analytical, Inc.

75

False Negatives for CARB 435 are a concern

Page 76: Soil method performance asbestos  eia annapolis 2011 09 16

Phase II

Copyright 2011 EMSL Analytical, Inc.

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.

Page 77: Soil method performance asbestos  eia annapolis 2011 09 16

Phase II

Spiking with Consolidated Asbestos (ACM)

- Transite supplied by RTI

- Estimated Chrysotile percentage = 14%

Copyright 2011 EMSL Analytical, Inc.

77

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Copyright 2011 EMSL Analytical, Inc.

Phase II EPA 600 Method Results

Page 79: Soil method performance asbestos  eia annapolis 2011 09 16

EPA 600 - Blanks - Phase II

Analyst 1 Analyst 2 Analyst 3 Analyst 4 Analyst 5 Analyst 6

Sample Number

Asbestos % 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

79

Copyright 2011 EMSL Analytical, Inc.

Page 80: Soil method performance asbestos  eia annapolis 2011 09 16

EPA 600 - 0.1% - Phase II 80

Copyright 2011 EMSL Analytical, Inc.

0

0.5

1

1.5

2

2.5

3

3.5

1 2 3 4 5 6 7

Overall Percent Recovery : 726 % Overall (Pooled) RSD: 0.43

Page 81: Soil method performance asbestos  eia annapolis 2011 09 16

EPA 600 - 1% - Phase II 81

Copyright 2011 EMSL Analytical, Inc.

0

2

4

6

8

10

1 2 3 4 5 6 7

Overall Percent Recovery for this Sample: 214 %

Overall (Pooled) RSD for this Sample: 0.32

Page 82: Soil method performance asbestos  eia annapolis 2011 09 16

EPA 600 Summary Phase II

82

Copyright 2011 EMSL Analytical, Inc.

Overall (Pooled) Percent Recovery 535 %

Overall (Pooled) RSD : 0.38

Page 83: Soil method performance asbestos  eia annapolis 2011 09 16

Phase II ASTM Sieve Method Results

Copyright 2011 EMSL Analytical, Inc.

83

Page 84: Soil method performance asbestos  eia annapolis 2011 09 16

ASTM – Blanks - Phase II 84

Copyright 2011 EMSL Analytical, Inc.

Analyst 1 Analyst 2 Analyst 3 Analyst 4 Analyst 5 Analyst 6

Sample Number

Asbestos % 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

Page 85: Soil method performance asbestos  eia annapolis 2011 09 16

ASTM - 0.1% - Phase II 85

Copyright 2011 EMSL Analytical, Inc.

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50

4.00

1 2 3 4 5 6 7

Overall Percent Recovery: 519 % Overall (Pooled) RSD for this Sample: 0.6

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ASTM - 1% - Phase II 86

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0.00

1.00

2.00

3.00

4.00

5.00

6.00

7.00

8.00

9.00

10.00

1 2 3 4 5 6 7

Overall Percent Recovery : 188 %

Overall (Pooled) RSD: 0.4

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ASTM Summary Phase II

87

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Overall (Pooled) Percent Recovery: 391 %

Overall (pooled) RSD: 0.5

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Phase II CARB Method 435 Results

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Phase II - CARB - Blanks 89

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Analyst 1 Analyst 2 Analyst 3 Analyst 4 Analyst 5 Analyst 6

Sample Number

Asbestos % 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

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Phase II - CARB - 0.1% 90

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0

0.2

0.4

0.6

0.8

1

1.2

1.4

1.6

1 2 3 4 5 6 7

Overall Percent Recovery for this Sample: 218 %

Overall (Pooled) RSD for this Sample: 0.65

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Phase II – CARB - 1% 91

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0

0.5

1

1.5

2

2.5

3

1 2 3 4 5 6 7

Overall Percent Recovery : 91 % Overall (Pooled) RSD: 0.46

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Phase II CARB Summary

92

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Overall (Pooled) Percent Recovery : 167 %

Overall (Pooled) RSD: 0.57

Page 93: Soil method performance asbestos  eia annapolis 2011 09 16

Final Score Card 93

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EPA600 ASTM Sieve CARB 435

% Recovery 1540 1090 650 RSD 0.55 0.32 0.64

EPA600 ASTM Sieve CARB 435

% Recovery 535 391 167

RSD 0.38 0.5 .57

Phase I

Phase II

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Summing Up

• Well known

• fast / cost effective

• pretty good at finding the

asbestos

Straight EPA 600 Pros Cons

94

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• Gross over estimation,

esp. at low percentages

• Since method not

designed for this matrix

not legally defensible?

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Summing Up

• Once published it will be

defensible (“fit for use”)

• Allows for a forensic analysis as

it does not alter the asbestos or

ACM as it exists in the sample

• TEM follow up on NAD

circumvents to some extent the

0.25 micron width limitation

ASTM Sieve Method Pros Cons

95

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• Most time consuming

• potential cross

contamination due to sieves

(difficult to clean)

• cost

•Course and medium fraction

still not amenable to PLM

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Summing Up

• Homogenizes the entire sample

prior to analysis.

• Reduces grain size of entire sample

• 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

CARB 435 Pros Cons

96

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• Potential to create fibers (cleavage

fragments with large aspect ratios)

from non asbestiform minerals.

• Alters fiber sizes dimensions

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97

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• CARB 435 mentioned

• 1% is not an appropriate action level for asbestos in soil

Page 98: Soil method performance asbestos  eia annapolis 2011 09 16

Thanks!

• Jim Millette of MVA

• Owen Crankshaw and Todd Ennis at RTI

• Alan Segrave and BV

• Howard Varner and EHS

98

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Page 99: Soil method performance asbestos  eia annapolis 2011 09 16

Real World Test Drive of the Methods

99

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Page 100: Soil method performance asbestos  eia annapolis 2011 09 16

CharlesTown Timeline

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.

100

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Savage Arms 101

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102

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Charlestown Mall

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Photo Taken by NY DOL on First Walk Through of Site

103

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104

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Charlestown Mall

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105

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Utica NY

Charlestown Mall

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106

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Charlestown Mall

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107

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Perimeter Air Samples 108

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Controlled Demo 109

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School Across the Street 110

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111

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Page 112: Soil method performance asbestos  eia annapolis 2011 09 16

Non-Scientific Study

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

112

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Page 113: Soil method performance asbestos  eia annapolis 2011 09 16

Riffle Splitting

One way to

help

homogenize

the samples

either in the

field or after

submittal to

the lab

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Page 114: Soil method performance asbestos  eia annapolis 2011 09 16

Charlestown Nuggets 114

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Conclusions? 115

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0

1

2

3

4

5

6

1CN 1GV 2CN 2GV 3CN 3GV 4CN 4GV

EPA 600

CARB 435

ASTM Sieve

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 asbestos at low percentages

• Generally good agreement between EPA 600 and ASTM

Page 116: Soil method performance asbestos  eia annapolis 2011 09 16

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

Page 117: Soil method performance asbestos  eia annapolis 2011 09 16

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.

Page 118: Soil method performance asbestos  eia annapolis 2011 09 16

Risk Assessment Methods

The Elutriator Method

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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

Page 119: Soil method performance asbestos  eia annapolis 2011 09 16

Copyright 2011 EMSL Analytical, Inc.

Tumbler

apparatus

filled with

soil

Risk Assessment Methods

The Elutriator Method

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Copyright 2011 EMSL Analytical, Inc.

Tumbler inside enclosed humidity chamber

Risk Assessment Methods

The Elutriator Method

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Copyright 2011 EMSL Analytical, Inc.

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

Risk Assessment Methods

The Elutriator Method

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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)

Page 123: Soil method performance asbestos  eia annapolis 2011 09 16

Copyright 2011 EMSL Analytical, Inc.

Activity Based Air Sampling

Personnel (and sometimes area) monitoring

is performed while samplers mimic likely

activity for that location.

Activity Based Air Sampling

Page 124: Soil method performance asbestos  eia annapolis 2011 09 16

RAF Unit

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Copyright 2011 EMSL Analytical, Inc.

RAF Unit

Page 126: Soil method performance asbestos  eia annapolis 2011 09 16

Fluidized Bed

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Air is injected at a precise flow rate to get the soil sample behaving like a fluid.

Then air samples are collected from above.

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Fluidized Bed

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Page 128: Soil method performance asbestos  eia annapolis 2011 09 16

Fluidized Bed

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Page 129: Soil method performance asbestos  eia annapolis 2011 09 16

Summing Up

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“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

The answer depends on the question…