The NIOSH 7500

The NIOSH 7500
Analytical Method
and OSHA PELs for Crystalline Silica
PALMS II Advanced Environmental Workshop at MTA

2 Broadway, NYC
December 2, 2014
Shannon Arlauckas
What is Silica?
Family of materials consisting of silicon dioxide (SiO2)
crystalline or amorphous material
Crystalline Silica
a solid formed by a repeating framework of (Si and O) atoms in 3
dimensions, which have fixed distances between them (d-spacing)
Crystalline Silica Polymorphs Regulated by OSHA
Quartz Cristobalite Tridymite
RJ Lee Group 2
Exposure to Crystalline Silica
Rock an aggregate of minerals

Igneous granite, other felsic igneous rocks
Sedimentary sandstone, shale, carbonates
Metamorphic schist, gneiss, quartzite, etc.
Many industries exposed
Mining
Construction
Railroads
Delayed health effects:
Silicosis
Lung cancer
Chronic obstructive pulmonary disease (COPD)
Kidney disease
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How Do We Monitor Crystalline Silica?
Gravimetric Analyses
NIOSH 0500, Total Dust
NIOSH 0600, Respirable Dust
NIOSH 7500, Crystalline Silica by XRD

Analytes: respirable quartz, cristobalite, tridymite
Instruments: Microbalance, X-ray Diffractometer
Sampling: cyclone + cassette
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Cassette Assembly Performed by the lab
Filters Used:
5 m pore size
37 mm diameter
Polyvinyl chloride (PVC)
Filters are conditioned
Pre-weights:
Weighed in sets of 10
Every 10th weight is re-
weighed to ensure that the
balance did not drift during
weighing of the set
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Pre-weighed filters are

placed into cassette
housing on top of a
backing pad that has
been stamped with a
unique tracking number
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Cassettes capped,
closed and taped
Labeled again with the
unique tracking number
Shipped to clients for air
sampling
Cassettes can be 2 piece

or 3 piece
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Sampling Performed by the Client
Cyclone Flow Rate
10-mm nylon cyclone (Dorr-Oliver) 1.7 5 % L/min Sample for an
Higgins-Dewell (HD) cyclone 2.2 5 % L/min 8 hour shift
(480 min, ~ 816 L)
Aluminum cyclone + 5 m PVC filter 2.5 5 % L/min
Tubing
Tips from the lab: Outlet
Ensure the cassette is loaded

into the cyclone properly
Do not invert sampler
assembly while using the
Outlet-side of Cassette
cyclone Air Flow (connect tubing here)
Direction
Grit pot
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Sample Preparation preformed in the lab
Samples received
Dried in a desiccator
Cassettes are carefully
opened to remove
filters
Filters are post-
weighed, recorded
Gravimetric Analysis
Total respirable dust NIOSH 0600
mass is calculated
Reporting Limit: 0.100 mg
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Removal of the filter

Low temperature plasma
ashing (beaker)
1 hr
Muffle furnace ashing
(crucible)
2hr @ 600C
Filter dissolution
Tetrahydrofuran (THF)
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15 mL of 2-Proponal is
added to each beaker
Cover and sonicate
Obtain a silver
membrane filter
25 mm
0.45 m
Attach funnel
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Pour suspension into

the funnel
Walls of beaker are
rinsed well
Apply vacuum
Remove the silver filter
with the sample
deposited on it
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Mount into XRD holder

Place in tray
Ready for analysis
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X-Ray Diffractometer
X-ray Detector
Source
Sample
Goniometer
PANalytical Cubix3 Diffractometer

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XRD Basics
n=2dsin
= 1.54 , CuKa
Incident X-ray Diffracted beam
beam
Atomic Planes d
q
Bombardment of X-rays results in scattering of the

X-rays off of atomic planes
X-Ray diffraction produces patterns that are
indicative of the atomic planes in a material, which
serve as a fingerprint for individual minerals
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XRD Data
Counts
360000
160000
40000
0
10 20 30
Position [2Theta] (Copper (Cu))
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XRD Data
Counts
Quartz Primary
Silver Silver
Silver Chloride Peak
360000
Primary Quartz Peak

160000
Secondary Quartz Peak

40000
0
10 20 30
Position [2Theta] (Copper (Cu))
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NIOSH 7500 - External Standard Method
Create a Calibration Curve

Create a set of standards using a pure mineral of
various concentrations
Compare unknown sample data to results from
known standards to determine silica mineral
concentrations
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Pure Mineral Standards Used in Calibration
5 g Qtz Quartz Detection Limit (0.005mg)

10 g Qtz
20 g Qtz
50 g Qtz
100 g Qtz
500 g Qtz
Blank
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Calibration Curves External Standard Method
Calibration Curve for Calibration Curve for

Quartz 26.6 2 Quartz 20.8 2
250 250
Actual Quartz Concentration (ug)

Actual Quartz Concentration (ug)
200 200
150 150
100 100
y = 0.0007x - 0.4596 y = 0.0032x + 3.6198
R = 0.9995 R = 0.9952
50 50
0 0
0 100000 200000 300000 400000 0 20000 40000 60000 80000
Area Under the Curve (counts) Area Under the Curve (counts)
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Quality Assurance Practices in the Lab
Balance
Calibration daily
Gravimetric test samples
Calibration Curve
Reanalyze and re-measure standards (every 3 mos.)
CCV Continuing Calibration Verification Set of standards run after every 10th sample
To ensure the calibration curves remain accurate
RL Reporting limit Set of standards run daily
To ensure that tube intensity is strong enough to see the RL (0.5g)
Sample Preparation
Blanks every day
To check for cross contamination between samples during preparation
Analysis
10% of unknown samples are re-measured by a second analyst
10% of CCVs and RLs are re-measured by a second analyst
Audits
AIHA audit every 2 years
Internal audits annually
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Common Mineral Interferences
Mica*
Potash
Feldspars*
Zircon
Graphite
Aluminosilicates
Best way to determine interferences: collect a bulk settled dust

sample or send the bulk material in question for XRD analysis for
phase identification.
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Standard Report
RJ Lee Group, Inc.
350 Hochberg Roa d, Monroevi l l e, PA 15146
Tel : (724) 325-1776 | Fa x: (724) 733-1799
LABORATORY REPORT
ABC Company
1 Industrial Way
Pittsburgh, PA 15200 REPORT DATE June 4, 2014
ATTENTION: Crystal N. Silica SAMPLES RECEIVED May 30, 2014
TELEPHONE: 724-XXX-XXX RJ LEE GROUP JOB NO. PA30052014001
CLIENT JOB NO. N/A
ANALYSIS: Respirable Dust and Crystalline Free Silica Dust on 5 m PVC Air Filters PURCHASE ORDER NO: N/A
METHODS: Gravimetry, NIOSH 0600 and X-Ray Diffraction, NIOSH 7500
LOD: 0.005 mg Quartz , Cristobalite, and Tridymite 0.100 mg Respirable Dust
Air* Respirable Masses of Free Weight Percentages of Airborne Dust

Sample Identification Volume Dust Mass Silica Minerals (mg/filter) Crystalline Silica Minerals Concentrations (mg/m3)
Client I.D. RJ Lee Group (liters) (mg/filter) Quartz Cristobalite Tridymite Quartz Cristobalite Tridymite Respirable Quartz Cristobalite Tridymite
Sample A 001 1200. 0.500 0.500 < 0.005 < 0.005 100.0 < 1.0 < 1.0 0.417 0.417 < 0.004 < 0.004
Sample B 002 1200. 0.500 0.250 < 0.005 < 0.005 50.0 < 1.0 < 1.0 0.417 0.208 < 0.004 < 0.004
Sample C 003 1200. 0.500 0.150 < 0.005 < 0.005 30.0 < 1.0 < 1.0 0.417 0.125 < 0.004 < 0.004
Sample D 004 1200. 0.500 0.100 < 0.005 < 0.005 20.0 < 1.0 < 1.0 0.417 0.083 < 0.004 < 0.004
Sample E 005 1200. 0.500 0.050 < 0.005 < 0.005 10.0 < 1.0 < 1.0 0.417 0.042 < 0.004 < 0.004
Blank 006 N/A < 0.100 1.050 < 0.010 < 0.010 N/A N/A N/A N/A N/A N/A N/A
* Supplied by the client.
N/A Not Applicable
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Standard Report
RJ Lee Group, Inc.
Tel : (724) 325-1776 | Fa x: (724) 733-1799
LABORATORY REPORT
ABC Company
1 Industrial Way
CLIENT JOB NO. N/A

Sample A 001 1200. 0.500 0.500 < 0.005 < 0.005 100.0 < 1.0 < 1.0 0.417 0.417 < 0.004 < 0.004
Sample B 002 1200. 0.500 0.250 < 0.005 < 0.005 50.0 < 1.0 < 1.0 0.417 0.208 < 0.004 < 0.004
Sample C 003 1200. 0.500 0.150 < 0.005 < 0.005 30.0 < 1.0 < 1.0 0.417 0.125 < 0.004 < 0.004
Sample D 004 1200. 0.500 0.100 < 0.005 < 0.005 20.0 < 1.0 < 1.0 0.417 0.083 < 0.004 < 0.004
Sample E 005 1200. 0.500 0.050 < 0.005 < 0.005 10.0 < 1.0 < 1.0 0.417 0.042 < 0.004 < 0.004
N/A Not Applicable
Air
volume
during a
workers
shift
RJ Lee Group 24
Standard Report
RJ Lee Group, Inc.
Tel : (724) 325-1776 | Fa x: (724) 733-1799
LABORATORY REPORT
ABC Company
1 Industrial Way
CLIENT JOB NO. N/A

Sample A 001 1200. 0.500 0.500 < 0.005 < 0.005 100.0 < 1.0 < 1.0 0.417 0.417 < 0.004 < 0.004
Sample B 002 1200. 0.500 0.250 < 0.005 < 0.005 50.0 < 1.0 < 1.0 0.417 0.208 < 0.004 < 0.004
Sample C 003 1200. 0.500 0.150 < 0.005 < 0.005 30.0 < 1.0 < 1.0 0.417 0.125 < 0.004 < 0.004
Sample D 004 1200. 0.500 0.100 < 0.005 < 0.005 20.0 < 1.0 < 1.0 0.417 0.083 < 0.004 < 0.004
Sample E 005 1200. 0.500 0.050 < 0.005 < 0.005 10.0 < 1.0 < 1.0 0.417 0.042 < 0.004 < 0.004
N/A Not Applicable
Air Mass of
volume material on
during a filter from
workers micro-
shift balance
RJ Lee Group 25
Standard Report
RJ Lee Group, Inc.
Tel : (724) 325-1776 | Fa x: (724) 733-1799
LABORATORY REPORT
ABC Company
1 Industrial Way
CLIENT JOB NO. N/A

Sample A 001 1200. 0.500 0.500 < 0.005 < 0.005 100.0 < 1.0 < 1.0 0.417 0.417 < 0.004 < 0.004
Sample B 002 1200. 0.500 0.250 < 0.005 < 0.005 50.0 < 1.0 < 1.0 0.417 0.208 < 0.004 < 0.004
Sample C 003 1200. 0.500 0.150 < 0.005 < 0.005 30.0 < 1.0 < 1.0 0.417 0.125 < 0.004 < 0.004
Sample D 004 1200. 0.500 0.100 < 0.005 < 0.005 20.0 < 1.0 < 1.0 0.417 0.083 < 0.004 < 0.004
Sample E 005 1200. 0.500 0.050 < 0.005 < 0.005 10.0 < 1.0 < 1.0 0.417 0.042 < 0.004 < 0.004
N/A Not Applicable
Air Mass of Mass of each mineral

volume material on determined by XRD
during a filter from measurements using the
workers micro- calibration curves derived
shift balance from standards
RJ Lee Group 26
Standard Report
RJ Lee Group, Inc.
Tel : (724) 325-1776 | Fa x: (724) 733-1799
LABORATORY REPORT
ABC Company
1 Industrial Way
CLIENT JOB NO. N/A

Sample A 001 1200. 0.500 0.500 < 0.005 < 0.005 100.0 < 1.0 < 1.0 0.417 0.417 < 0.004 < 0.004
Sample B 002 1200. 0.500 0.250 < 0.005 < 0.005 50.0 < 1.0 < 1.0 0.417 0.208 < 0.004 < 0.004
Sample C 003 1200. 0.500 0.150 < 0.005 < 0.005 30.0 < 1.0 < 1.0 0.417 0.125 < 0.004 < 0.004
Sample D 004 1200. 0.500 0.100 < 0.005 < 0.005 20.0 < 1.0 < 1.0 0.417 0.083 < 0.004 < 0.004
Sample E 005 1200. 0.500 0.050 < 0.005 < 0.005 10.0 < 1.0 < 1.0 0.417 0.042 < 0.004 < 0.004
N/A Not Applicable

volume material on determined by XRD Mass of mineral
during a filter from measurements using the 100
Mass of total dust
RJ Lee Group 27
Standard Report
RJ Lee Group, Inc.
Tel : (724) 325-1776 | Fa x: (724) 733-1799
LABORATORY REPORT
ABC Company
1 Industrial Way
CLIENT JOB NO. N/A

Sample A 001 1200. 0.500 0.500 < 0.005 < 0.005 100.0 < 1.0 < 1.0 0.417 0.417 < 0.004 < 0.004
Sample B 002 1200. 0.500 0.250 < 0.005 < 0.005 50.0 < 1.0 < 1.0 0.417 0.208 < 0.004 < 0.004
Sample C 003 1200. 0.500 0.150 < 0.005 < 0.005 30.0 < 1.0 < 1.0 0.417 0.125 < 0.004 < 0.004
Sample D 004 1200. 0.500 0.100 < 0.005 < 0.005 20.0 < 1.0 < 1.0 0.417 0.083 < 0.004 < 0.004
Sample E 005 1200. 0.500 0.050 < 0.005 < 0.005 10.0 < 1.0 < 1.0 0.417 0.042 < 0.004 < 0.004
N/A Not Applicable

volume material on determined by XRD Mass of mineral Mass
during a filter from 100 1000
measurements using the Mass of total dust Air Volume
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Current OSHA Personal Exposure Limits (PEL)
5.0

4.5

=
4.0 % +
Respirable Dust PEL mg/m3
3.5
3.0
2.5
2.0
The OSHA PEL for Respirable Dust is not a
1.5 number, but a function that is dependent on
1.0
the percentage of crystalline silica in the dust
0.5
0.0
0 10 20 30 40 50 60 70 80 90 100
Quartz Concentration (wt. %)
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5.0

4.5

=
4.0 Dust containing no quartz: % +
PEL = 5 mg/m3
3.5 or
5000 g/m3
3.0
2.5
Dust containing all quartz:

2.0
PEL = 0.1 mg/m3
1.5
or
100 g/m3
1.0
0.5
0.0
0 10 20 30 40 50 60 70 80 90 100
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Sample A 001 1200. 0.500 0.500 < 0.005 < 0.005 100.0 < 1.0 < 1.0 0.417 0.417 < 0.004 < 0.004
Sample B 002 1200. 0.500 0.250 < 0.005 < 0.005 50.0 < 1.0 < 1.0 0.417 0.208 < 0.004 < 0.004
Sample C 003 1200. 0.500 0.150 < 0.005 < 0.005 30.0 < 1.0 < 1.0 0.417 0.125 < 0.004 < 0.004
Sample D 004 1200. 0.500 0.100 < 0.005 < 0.005 20.0 < 1.0 < 1.0 0.417 0.083 < 0.004 < 0.004
Sample E 005 1200. 0.500 0.050 < 0.005 < 0.005 10.0 < 1.0 < 1.0 0.417 0.042 < 0.004 < 0.004
5.0
4.5
4.0

3.5
=
3.0 % +
2.5
2.0
1.5
1.0
0.5
0.0
*Based on an 8 hour shift
0 20 40 60 80 100
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Sample A 001 1200. 0.500 0.500 < 0.005 < 0.005 100.0 < 1.0 < 1.0 0.417 0.417 < 0.004 < 0.004
Sample B 002 1200. 0.500 0.250 < 0.005 < 0.005 50.0 < 1.0 < 1.0 0.417 0.208 < 0.004 < 0.004
Sample C 003 1200. 0.500 0.150 < 0.005 < 0.005 30.0 < 1.0 < 1.0 0.417 0.125 < 0.004 < 0.004
Sample D 004 1200. 0.500 0.100 < 0.005 < 0.005 20.0 < 1.0 < 1.0 0.417 0.083 < 0.004 < 0.004
Sample E 005 1200. 0.500 0.050 < 0.005 < 0.005 10.0 < 1.0 < 1.0 0.417 0.042 < 0.004 < 0.004
5.00
4.50
4.00

3.50
=
3.00 % +
2.50
2.00
1.50
1.00
0.50
0.00
0 20 40 60 80 100
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Sample A 001 1200. 0.500 0.500 < 0.005 < 0.005 100.0 < 1.0 < 1.0 0.417 0.417 < 0.004 < 0.004
Sample B 002 1200. 0.500 0.250 < 0.005 < 0.005 50.0 < 1.0 < 1.0 0.417 0.208 < 0.004 < 0.004
Sample C 003 1200. 0.500 0.150 < 0.005 < 0.005 30.0 < 1.0 < 1.0 0.417 0.125 < 0.004 < 0.004
Sample D 004 1200. 0.500 0.100 < 0.005 < 0.005 20.0 < 1.0 < 1.0 0.417 0.083 < 0.004 < 0.004
Sample E 005 1200. 0.500 0.050 < 0.005 < 0.005 10.0 < 1.0 < 1.0 0.417 0.042 < 0.004 < 0.004
5.00
4.50
4.00
Compare this
3.50
=
3.00 % + value to the
2.50 calculated PEL
2.00
PELE =
1.50 0.83 mg/m3 PEL =
D
1.00 0.45 mg/m3 PELC =
PELB = PELA=
0.50 0.31 mg/m3 0.19 mg/m3 0.10 mg/m3
0.00
0 20 40 60 80 100
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Sample A 001 1200. 0.500 0.500 < 0.005 < 0.005 100.0 < 1.0 < 1.0 0.417 0.417 < 0.004 < 0.004
Sample B 002 1200. 0.500 0.250 < 0.005 < 0.005 50.0 < 1.0 < 1.0 0.417 0.208 < 0.004 < 0.004
Sample C 003 1200. 0.500 0.150 < 0.005 < 0.005 30.0 < 1.0 < 1.0 0.417 0.125 < 0.004 < 0.004
Sample D 004 1200. 0.500 0.100 < 0.005 < 0.005 20.0 < 1.0 < 1.0 0.417 0.083 < 0.004 < 0.004
Sample E 005 1200. 0.500 0.050 < 0.005 < 0.005 10.0 < 1.0 < 1.0 0.417 0.042 < 0.004 < 0.004
5.00
4.50
4.00
Samples A, B and C have
3.50
=
3.00 % + Airborne Dust Concentrations
2.50 OVER the calculated PEL
2.00
PELE =
1.50 0.83 mg/m3 PEL =
D
1.00 0.45 mg/m3 PELC =
PELB = PELA=
0.50 0.31 mg/m3 0.19 mg/m3 0.10 mg/m3
0.00
0 20 40 60 80 100
RJ Lee Group 34
New Proposed OSHA
Personal Exposure Limits (PEL)
Sample A 001 1200. 0.500 0.500 < 0.005 < 0.005 100.0 < 1.0 < 1.0 0.417 0.417 < 0.004 < 0.004
Sample B 002 1200. 0.500 0.250 < 0.005 < 0.005 50.0 < 1.0 < 1.0 0.417 0.208 < 0.004 < 0.004
Sample C 003 1200. 0.500 0.150 < 0.005 < 0.005 30.0 < 1.0 < 1.0 0.417 0.125 < 0.004 < 0.004
Sample D 004 1200. 0.500 0.100 < 0.005 < 0.005 20.0 < 1.0 < 1.0 0.417 0.083 < 0.004 < 0.004
Sample E 005 1200. 0.500 0.050 < 0.005 < 0.005 10.0 < 1.0 < 1.0 0.417 0.042 < 0.004 < 0.004
New Proposed OSHA PEL for quartz:

0.05 mg/m3
or Compare this
50 g/m3 value to the new
proposed OSHA
New Proposed OSHA Action level for quartz:
PEL
0.025 mg/m3
or
25 g/m3
RJ Lee Group 35
New Proposed OSHA
Personal Exposure Limits (PEL)
Sample A 001 1200. 0.500 0.500 < 0.005 < 0.005 100.0 < 1.0 < 1.0 0.417 0.417 < 0.004 < 0.004
Sample B 002 1200. 0.500 0.250 < 0.005 < 0.005 50.0 < 1.0 < 1.0 0.417 0.208 < 0.004 < 0.004
Sample C 003 1200. 0.500 0.150 < 0.005 < 0.005 30.0 < 1.0 < 1.0 0.417 0.125 < 0.004 < 0.004
Sample D 004 1200. 0.500 0.100 < 0.005 < 0.005 20.0 < 1.0 < 1.0 0.417 0.083 < 0.004 < 0.004
Sample E 005 1200. 0.500 0.050 < 0.005 < 0.005 10.0 < 1.0 < 1.0 0.417 0.042 < 0.004 < 0.004
New Proposed OSHA PEL for quartz: Samples A, B, C and D

0.05 mg/m3 are now OVER the new
or proposed PEL for quartz
50 g/m3
New Proposed OSHA Action level for quartz:

0.025 mg/m3
or
25 g/m3
RJ Lee Group 36
New Proposed OSHA
Personal Exposure Limit (PEL)
Sample A 001 1200. 0.500 0.500 < 0.005 < 0.005 100.0 < 1.0 < 1.0 0.417 0.417 < 0.004 < 0.004
Sample B 002 1200. 0.500 0.250 < 0.005 < 0.005 50.0 < 1.0 < 1.0 0.417 0.208 < 0.004 < 0.004
Sample C 003 1200. 0.500 0.150 < 0.005 < 0.005 30.0 < 1.0 < 1.0 0.417 0.125 < 0.004 < 0.004
Sample D 004 1200. 0.500 0.100 < 0.005 < 0.005 20.0 < 1.0 < 1.0 0.417 0.083 < 0.004 < 0.004
Sample E 005 1200. 0.500 0.050 < 0.005 < 0.005 10.0 < 1.0 < 1.0 0.417 0.042 < 0.004 < 0.004
New Proposed OSHA PEL for quartz: Samples A, B, C and D

0.05 mg/m3 are now OVER the new
or proposed PEL for quartz
50 g/m3
New Proposed OSHA Action level for quartz: Sample E is at the

0.025 mg/m3 proposed action level
or
25 g/m3
RJ Lee Group 37
Concerns Raised by Proposed OSHA PELs
Regulatory compliance will be more difficult

There will be increased costs associated with
monitoring and correcting non-compliance
Can crystalline silica can be reliably measured at

these levels?
Flow rate of 1.7 L/min for an 8 hour shift

Current PEL (assume 100% Quartz): 0.1 mg/m3 (100 g/m3) 0.08 mg/filter (80 g/filter)
New Proposed PEL: 0.05 mg/m3 (50 g/m3) 0.04 mg/filter (40 g/filter)
New Proposed Action Limit: 0.025 mg/m3 (25g/m3) 0.02 mg/filter (20 g/filter)
RJ Lee Group 38
OSHA PEL Blind Study Overview
Make sets of 10 samples of known quartz loadings
Quartz
Mixed matrix
50% quartz + 50% kaolinite
50% quartz + 50% feldspar
Blanks
The concentrations correspond to the current PEL,
proposed PEL and proposed action limit
0.08 mg/filter (80 g/filter)
Send samples to labs for NIOSH 7500 analyses (blind)
RJ Lee Group 39
OSHA PEL Blind Study Preparation
PVC filters were pre-weighed

Known quantities of quartz (and mixed minerals) are
deposited onto PVC filters
PVC filters were post-weighed
RJ Lee Group 40
Filters were loaded into cassettes

Taped and labeled to look like sample cassettes
Cassettes were tested to ensure correct preparation
RJ Lee Group 41
OSHA PEL Blind Study Preparation Problems
Depositing respirable particles suspended in liquid media onto
5m pore size PVC filters resulted in a poor recovery of materials
Solution: Switched to using 0.8 m pore size PVC filters
Recoveries after deposition onto 0.8 m filters were lower than
expected due to partial dissolution of the filters
Solution: Selected filters were analyzed by XRD to confirm
recoveries
20 g Loading 40 g Loading
93% Recovery 96% Recovery
RJ Lee Group 42
Filters were loaded into cassettes

Taped and labeled to look like sample cassettes
Cassettes were tested to ensure correct preparation
Sent to five AIHA accredited laboratories for NIOSH
7500 analysis
RJ Lee Group 43
OSHA PEL Blind Study Results
34% (36/105 filters) of the non-blank filters were

reported to be below the detection limit
Loadings were above each laboratorys reported
Limit of Detection (LOD)
These results were excluded from the following

statistical data
RJ Lee Group 44
Silica-only and blank filters having positive reported results
Reference Lab Result Number of Lab Result
Level (g) Means (g) Data Points* Standard Deviation
0 28.85 2 32.74
20 13.36 7 5.21
40 22.93 12 11.22
80 46.91 12 18.31
*non-detects excluded
Silica-only and mixed-matrix filters having positive reported result

Reference Lab Result Number of Lab Result
Level (g) Means (g) Data Points* Standard Deviation
20 13.33 20 5.21
40 25.04 37 11.22
80 46.91 12 18.31
*non-detects excluded
RJ Lee Group 45
Inter- and intra-laboratory variability was high

None of the laboratory means came within 30% of
the reference values
Accuracy was problematic even when non-detects
were excluded
Most labs could not reliably distinguish between the
different reference levels
Why?
RJ Lee Group 46
NIOSH 7500 Sample Preparation
Muffle Furnace vs. Plasma Asher
Crystalline Silica
Ashing
Test Crucible Scraping Standard Average
Device Average Recovery
(g) (g)
19.4 17.3
1 Plasma n/a n/a 48.6 52.3 100.8 4.7%
96.1 101.4
19.4 14.8
2 Muffle New Complete 48.6 43.1 89.8 4.3%
96.1 100.1
19.4 15.0
3 Muffle Used Complete 48.6 41.4 83.0 4.9%
96.1 83.2
19.4 14.8
5 Muffle Used Partial 48.6 37.9 77.4 4.0 %
96.1 74.9
19.4 3.5
4 Muffle Used None 48.6 23.5 49.0 3.8%
96.1 77.4
RJ Lee Group 47
Recommendation to OSHA
Data from blind study presented to OSHA

It is possible to analyze for crystalline silica at low
levels (proposed PEL)
Preparation methods in some laboratories is a
concern and this should be addressed before PELs
are changed.
A recommendation was made to OSHA that a larger
blinded study be conducted for all laboratories
performing the NIOSH 7500 method before adopting
new PELs that may not be measured reliably using
current technology and preparation methods
RJ Lee Group 48

The NIOSH 7500 - Shannon Arlauckas

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The NIOSH 7500 - Shannon Arlauckas

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PALMS II Advanced Environmental Workshop at MTA

Crystalline Silica Polymorphs Regulated by OSHA

Quartz Cristobalite Tridymite

Rock an aggregate of minerals

NIOSH 7500, Crystalline Silica by XRD

Pre-weighed filters are

Cassettes can be 2 piece

Ensure the cassette is loaded

Removal of the filter

Pour suspension into

Mount into XRD holder

PANalytical Cubix3 Diffractometer

Bombardment of X-rays results in scattering of the

Primary Quartz Peak

Secondary Quartz Peak

Create a Calibration Curve

5 g Qtz Quartz Detection Limit (0.005mg)

Calibration Curve for Calibration Curve for

Actual Quartz Concentration (ug)

Best way to determine interferences: collect a bulk settled dust

Tel : (724) 325-1776 | Fa x: (724) 733-1799

LOD: 0.005 mg Quartz , Cristobalite, and Tridymite 0.100 mg Respirable Dust

Air* Respirable Masses of Free Weight Percentages of Airborne Dust

Tel : (724) 325-1776 | Fa x: (724) 733-1799

LOD: 0.005 mg Quartz , Cristobalite, and Tridymite 0.100 mg Respirable Dust

Air* Respirable Masses of Free Weight Percentages of Airborne Dust

Tel : (724) 325-1776 | Fa x: (724) 733-1799

LOD: 0.005 mg Quartz , Cristobalite, and Tridymite 0.100 mg Respirable Dust

Air* Respirable Masses of Free Weight Percentages of Airborne Dust

Tel : (724) 325-1776 | Fa x: (724) 733-1799

LOD: 0.005 mg Quartz , Cristobalite, and Tridymite 0.100 mg Respirable Dust

Air* Respirable Masses of Free Weight Percentages of Airborne Dust

Air Mass of Mass of each mineral

Tel : (724) 325-1776 | Fa x: (724) 733-1799

LOD: 0.005 mg Quartz , Cristobalite, and Tridymite 0.100 mg Respirable Dust

Air* Respirable Masses of Free Weight Percentages of Airborne Dust

Air Mass of Mass of each mineral

Tel : (724) 325-1776 | Fa x: (724) 733-1799

LOD: 0.005 mg Quartz , Cristobalite, and Tridymite 0.100 mg Respirable Dust

Air* Respirable Masses of Free Weight Percentages of Airborne Dust

Air Mass of Mass of each mineral

Dust containing all quartz:

New Proposed OSHA PEL for quartz:

New Proposed OSHA PEL for quartz: Samples A, B, C and D

New Proposed OSHA Action level for quartz:

New Proposed OSHA PEL for quartz: Samples A, B, C and D

New Proposed OSHA Action level for quartz: Sample E is at the

Regulatory compliance will be more difficult

Can crystalline silica can be reliably measured at

Flow rate of 1.7 L/min for an 8 hour shift

PVC filters were pre-weighed

Filters were loaded into cassettes

Filters were loaded into cassettes

34% (36/105 filters) of the non-blank filters were

These results were excluded from the following

Silica-only and mixed-matrix filters having positive reported result

Inter- and intra-laboratory variability was high

Data from blind study presented to OSHA

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