Protecting Workers Exposed to Lead-based Paint Hazards
A Report to Congress

 

DHHS (NIOSH) PUBLICATION NO. 98-112
JANUARY 1997


Chapter 5
METHODS TO SAMPLE AND ANALYZE ENVIRONMENTAL LEAD

Introduction
Sample collection

Sample preparation
Analysis
Screening methods
Additional Methods
Recommendations for performance evaluation
Recommendations
References


INTRODUCTION

Numerous studies conducted by NIOSH and others have found that workplace air and surface dust are the primary sources of occupational lead exposures. Paint and soil are environmental lead sources in residential and commercial environments. These environmental lead sources may become occupational lead hazards when work activities generate airborne dust from lead-contaminated paint, soil, or surface dust.

In order to control worker lead exposures during LBP activities, it is necessary to be able to accurately measure environmental lead. This chapter discusses laboratory-based sampling and analytical methods, on-site lead screening methods, and evaluation of laboratories and field testing methods.

NIOSH bases its recommendations on NIOSH and EPA protocols, and consensus standards developed by the American Society for Testing and Materials (ASTM). All of the sample preparation and analytical methods recommended here meet the performance criteria specified by NIOSH and EPA.1 - 7

The environmental action level for the health risk of interest should be considered when selecting a method, to ensure accuracy and quality of analytical results. The detection limit for the method selected should be at least an order of magnitude below the action level of concern. The range of measured concentrations should extend at least to twice the action level.

SAMPLE COLLECTION

Samples collected must be representative of the environmental matrix (e.g., workplace air, paint, soil, and surface dust). Samples should be collected, using consistent techniques, to assure comparability of samples among sites and among different areas at a site. Recommended methods for sample collection are listed in Table 5.1.

Lead in Airborne Particulate

Sampling methods for measuring worker exposure use a two-piece filter holder cassette with a 0.8-micrometer (µm) cellulose ester membrane filter. Personal air samples are collected in the worker's personal breathing zone, usually for the duration of the full-work shift. However, shorter periods may be important to assess exposures by task (task-based exposure assessment), or to prevent overloading of sample filters in very dusty environments (e.g., during abrasive blasting).

NIOSH investigators have found that personal air sampling may be inaccurate during abrasive blasting in confined areas on steel structures.8,9 A large percentage of the personal samples may be torn off the workers as they move about in confined areas.10 These environments are usually extremely dusty, and large particles (> 100 µm diameter) of paint or abrasive grit rebounding directly from the substrates may enter sample filter cassettes, biasing the results. Locating the sample at the back of the worker's neck will reduce entry of grit rebound in all but the most confined areas.

Lead in Surface Dust

Lead in workplace surface dust can be collected by wipe sampling and vacuum sampling techniques. Most of these methods were originally developed to measure lead poisoning risks to children in homes.11 Wipe sampling, which determines surface lead loading (microgram [µg] lead per unit area), is the method currently preferred by HUD for determining surface lead concentrations as part of residential lead risk assessments.12 Wipe sampling requires systematically wiping a measured surface area (or the area within a sampling template) with a pre- wetted wipe. Some widely available commercial hand wipes are suitable for this purpose. Wipes used should have low background lead contamination and be of constituents that can be readily processed in the laboratory.13 Wipe sampling is also used for assessing dermal lead exposures, especially lead dust on hands.14

Vacuum sampling requires systematically vacuuming a measured area. A commonly used portable dust vacuum method is convenient because it uses the same equipment that is routinely used by industrial hygienists for personal air sampling.15 This method is useful for sampling dust on soft surfaces, and it can determine both lead loading and lead concentration (ppm or percent by weight) in the dust when pre-weighed filters or filter cassettes are used.


Table 5.1 Recommended Sample Collection, Preparation, and Analysis Methods for Lead in Paint, Surface Dust, Soil, and Workplace Air

Matrix Collection Preparation * Analysis # (all matrices)
Air NIOSH 7082, 7105,& 7300
ASTM E1553
Field:
EPA Field SOP
Lab:
NIOSH 7082 &7105
ASTM E1741
Field:
Portable ASV**
EPA Field SOP

Lab:
NIOSH 7082
NIOSH 7105
NIOSH 7300
EPA Lab SOP
EPA SW-846 6010A
EPA SW-846 7420
EPA SW-846 7421
ASTM E1613
Dust Wipe NIOSH 9100
ASTM E1728
NIOSH 7082 & 7105
ASTM E1644
EPA SW-846 3050A
DustVacuum ASTM D5438
ASTM PS46
NIOSH 7082 & 7105
ASTM E1644
EPA SW-846 3050A
EPA SW-846 3051
EPA Lab SOPf
Paint ASTM E1729 Field:
EPA Field SOP
Lab:
NIOSH 7082 & 7105
ASTM E1645
EPA SW-846 3050A
EPA SW-846 3051
Soil ASTM E1727 NIOSH 7082 & 7105 ASTM E1726
EPA Lab SOP
EPA SW-846 3050A
EPA SW-846 3051
NOTES:
NIOSH methods include protocols for sample collection, preparation, and analysis. The EPA and ASTM methods listed are specific for one of these three elements.

* Hotplate digestion: NIOSH 7082, NIOSH 7105, ASTM E1741, ASTM E 644, ASTM E1645, EPA SW-846 3050A, EPA Lab SOP. Microwave digestion: ASTM E1741, ASTM E1645, EPA Lab SOP, EPA SW-846 3051. Ultrasonic extraction: EPA Field SOP.

# Flame atomic absorption spectrophotometry: NIOSH 7082, ASTM E1613, EPA Lab SOP, EPA SW-846 7420. Graphite furnace atomic absorption spectrophotometry: NIOSH 7105, ASTM ES 35, EPA SW-846 7421. Inductively coupled plasma atomic emission spectrophotometry: NIOSH 7300, ASTM E 1613, EPA Lab SOP, EPA SW-846 6010A.

SOP = standard operating procedure.
ASV = anodic stripping voltammetry.


Lead in Paint and Soil

A sensitive method is needed to assess worker exposures to lead in paint and soil. Hazardous occupational exposures have been found to occur even when average paint concentrations are well below the Title X definition of LBP (0.5%) or the Consumer Product Safety Commission (CPSC) definition of lead-containing paint (0.06%).16,17 To measure these levels accurately the sample usually must be analyzed in a laboratory. The recommended method for paint sample collection is ASTM E1729, which requires removing all of the existing paint layers. Field screening methods for testing for lead in paint in-place (in-situ) are mentioned later in this chapter.

The recommended practice for collection of soil samples is ASTM E1727, which involves scooping or coring methods.

Compositing Samples

Compositing of wipe, vacuum, paint, and soil samples has been suggested to reduce analytical costs. Compositing is generally not recommended by NIOSH for lead risk assessments because it results in a loss of information about environmental variability with relatively little reduction in total project cost. Additionally, compositing of wipe samples can cause serious problems in the sample preparation because the entire sample, including all of the wipes, must be digested.

SAMPLE PREPARATION

The recommended sample preparation methods for lead in workplace air, dust, paint, and soil are listed in Table 5.1. Air samples (filters) can be prepared in the laboratory or in the field. Laboratory preparation is done by hotplate- or microwave-based digestion in strong acid, and field preparation is done by ultrasonic extraction in dilute acid. Paint samples are ground to a powder to maximize lead recoveries, then prepared like air samples. Surface dust (wipe) samples are prepared in the laboratory by hotplate digestion in strong acid. Soil samples are sieved to remove stones and other objects, then prepared in the laboratory by hotplate- or microwave-based digestion in strong acid.

ANALYSIS

Recommended laboratory and field analytical methods for lead in workplace air, dust, paint, and soil are listed in Table 5.1. Analysis methods in the laboratory include graphite furnace atomic absorption spectrometry, flame atomic absorption spectrometry, and inductively coupled plasma atomic emission spectrometry. In contrast to these laboratory methods which use spectrometry, field methods for lead are based on colorimetric or electroanalytical techniques.18,19,20 Higher airflow rates (2 to 4 liters per minute) and a highly sensitive method, such as graphite furnace atomic absorption spectrometry, should be used when performing short-term (<30 minutes) air sampling.

SCREENING METHODS

Screening and semi-quantitative methods are used to estimate the lead content of paints and other environmental matrices. Field screening techniques include portable x-ray fluorescence (XRF) and chemical spot test kits.

Portable XRF is the most commonly used method for screening for LBP in residences and is the method recommended by HUD and EPA. NIOSH does not recommend portable XRF instruments for occupational exposure assessment until they have been shown to meet established performance criteria for quantitative analyses.21,22 A method for the determination of lead in workplace air samples using a portable XRF instrument (with cadmium 109 source) is under development.23

Some chemical spot test kits are able to detect very low lead levels in a variety of environmental matrices and, therefore, may prove to be useful for screening for potentially hazardous levels of lead in the workplace.24 A rhodizonate-based chemical spot test kit has been evaluated for screening of lead in workplace air samples.25 ASTM standard E1753 describes the use of qualitative chemical spot test kits for screening of lead in paint, and ASTM E1828 covers the evaluation of test kits for lead in paint.

ADDITIONAL METHODS

Additional laboratory and field sample preparation and analytical methods for lead in a variety of sample matrices are under development or evaluation by federal agencies. ASTM is continuing to develop a series of standards dealing with lead hazard identification and mitigation.26

RECOMMENDATIONS FOR PERFORMANCE EVALUATION

Laboratory Testing for Lead

NIOSH recommends, and the HUD guidelines require, the use of laboratories recognized by EPA's National Lead Laboratory Accreditation Program (NLLAP) to ensure the consistency and quality of measurement results. The Environmental Lead Proficiency Analytical Testing program (ELPAT) is part of NLLAP and is administered by the American Industrial Hygiene Association (AIHA) in cooperation with NIOSH and the EPA. ELPAT performance criteria are similar to those of the well-established Proficiency Analytical Testing (PAT) program for workplace air samples administered by AIHA and NIOSH. On a quarterly basis, NIOSH evaluates the performance of approximately 400 laboratories located throughout the United States and Canada and publishes the results in the American Industrial Hygiene Association Journal and Applied Occupational and Environmental Hygiene. Over the past three years, the ELPAT laboratories have demonstrated good agreement in lead measurements among the recommended methods for sample preparation and analysis of lead in paint, dust, and soil samples.27

Field–Based Testing for Lead

With the advent of new field-portable methods for environmental lead analysis, it is anticipated that more on-site lead determinations will be performed in the future. NIOSH recommends that ASTM E1775 be used for performance evaluation of on-site extraction and analytical methods. ASTM E1583 should be used to evaluate organizations involved in field-based assessments of lead hazards. A system similar to NLLAP is needed to evaluate the quality of analyses of lead in paint, dust, and soil done in-place (in-situ) with portable instruments (e.g., by portable x-ray fluorescence).

RECOMMENDATIONS

Further research is needed to evaluate the utility of chemical spot test kits for assessing worker lead exposures and to develop a sampling method to reliably measure lead exposures in confined abrasive blasting environments.

REFERENCES

  1. NIOSH [1991]. SOP 018 Limits of detection and quantitation. Quality Assurance & Laboratory operation procedures of the Measurements Research Support Branch, Methods Research Branch. Cincinnati, OH: U.S. Department of Health and Human Services, Public Health Service, Centers for Disease Control, National Institute for Occupational Safety and Health, Division of Physical Sciences and Engineering. Revision 6, December 1991 (unpublished).

  2. EPA [1992]. Laboratory accreditation program guidelines—measurement of lead in paint, dust, and soil. Washington, DC: U.S. Environmental Protection Agency. Publication No. EPA 747/R–92/001.

  3. OMB [1993]. Federal participation in the development and use of voluntary standards. Washington, DC: Office of Management and Budget. Circular No. A–119, revised October 20, 1993.

  4. ASTM [1994]. ASTM standards on lead-based paint abatement in buildings. Philadelphia, PA: American Society for Testing and Materials. ASTM PCN 03–506194–10.

  5. ASTM [1996]. Annual book of ASTM standards. Vol. 04.07. West Conshohocken, PA: American Society for Testing and Materials.

  6. EPA [1990]. Test methods for evaluating solid waste-physical/chemical methods. 3rd ed. Washington, DC: U.S. Environmental Protection Agency.

  7. Eller PM and Cassinelli ME, eds. [1994]. NIOSH manual of analytical methods. 4th ed. Cincinnati, OH: U.S. Department of Health and Human Services, Public Health Service, Centers for Disease Control and Prevention, National Institute for Occupational Safety and Health, DHHS (NIOSH) Publication No. 94–113.

  8. NIOSH [1994]. In-depth survey report: control technology for removing lead-based paint from steel structures: abrasive blasting using steel grit with recycling. Cincinnati, OH: U.S. Department of Health and Human Services, Public Health Service, Centers for Disease Control and Prevention, National Institute for Occupational Safety and Health, DHHS (NIOSH) Report No. ECTB 183–12a.

  9. NIOSH [1996]. Hazard evaluation and technical assistance interim report: Bath Iron Works Corporation. Cincinnati, OH: U.S. Department of Health and Human Services, Public Health Service, Centers for Disease Control and Prevention, National Institute for Occupational Safety and Health, NIOSH Report No. HETA 94–0122–2578.

  10. NIOSH [1994]. Hazard evaluation and technical assistance interim report: Seaway Painting, Inc. Cincinnati, OH: U.S. Department of Health and Human Services, Public Health Service, Centers for Disease Control and Prevention, National Institute for Occupational Safety and Health, NIOSH Report No. HETA 91–209–2249.

  11. EPA [1995]. Sampling house dust for lead-basic concepts and literature review. Washington, DC: U.S. Environmental Protection Agency, Office of Prevention, Pesticides, and Toxic Substances. Publication No: EPA 747–R–95–007.

  12. HUD [1995]. Guidelines for the evaluation and control of lead-based paint hazards in housing. Washington, DC: U.S. Department of Housing and Urban Development.

  13. Millson M, Eller PM, Ashley K [1994]. Evaluation of wipe sampling materials for lead in surface dust. Am Ind Hyg Assoc J 55:339–342.

  14. McArthur B [1992]. Dermal measurement and wipe sampling methods: a review. Appl Occup Environ Hyg 7(9): 599–606.

  15. ASTM [1996]. Provisional standard practice for collection of surface dust by air sampling pump vacuum technique for subsequent lead determination. West Conshohocken, PA: American Society for Testing and Materials, Publication PS 46–96.

  16. Sussell A, et al. [1995]. An evaluation of airborne and surface lead concentrations from preliminary cleaning of a building contaminated with deteriorated lead-based paint. In: Beard ME, Iske SD, eds. Lead in paint, soil and dust: health risks, exposure studies, control measures, measurement methods, and quality assurance, ASTM STP 1226. Philadelphia, PA: American Society for Testing and Materials, pp. 145–161.

  17. NIOSH [1992]. Hazard evaluation and technical assistance report: HUD Lead-based Paint Abatement Demonstration Project. Cincinnati, OH: U.S. Department of Health and Human Services, Public Health Service, Centers for Disease Control and Prevention, National Institute for Occupational Safety and Health, NIOSH Report No. HETA 90–070–2181.

  18. EPA [1993]. Standard operating procedure for the field analysis of lead in paint, bulk dust, and soil by ultrasonic, acid digestion and colorimetric measurement. Research Triangle Park, NC: U.S. Environmental Protection Agency. Publication No. EPA 600/R–93/200.

  19. Ashley K [1994]. Electroanalytical applications in occupational and environmental health. Electroanalysis 6:805–820.

  20. Ashley K [1995]. Ultrasonic extraction and field portable anodic stripping voltammetry of lead from environmental samples. Electroanalysis 7:1189–1192.

  21. NIOSH [1995]. Guidelines for air sampling and analytical method development and evaluation. Cincinnati, OH: U.S. Department of Health and Human Services, Public Health Service, Centers for Disease Control and Prevention, National Institute for Occupational Safety and Health, DHHS (NIOSH) Publication No. 95–117.

  22. EPA [1995]. A field test of lead-based paint testing technologies: technical report. Washington, DC: U.S. Environmental Protection Agency. Publication No. EPA 747–R–95–002.

  23. Morley JC [1997]. Evaluation of a portable x-ray fluorescence instrument for the determination of lead in workplace air samples [Master's thesis]. Cincinnati, OH: University of Cincinnati, Department of Environmental Health.

  24. EPA [1993]. Investigation of test kits for detection of lead in paint, soil and dust. Research Triangle Park, NC: U.S. Environmental Protection Agency. Publication No. EPA 600/R–93/085.

  25. Ashley K, Fischbach TJ, Song R [1996]. Evaluation of a chemical spot test for the detection of airborne lead in the workplace. Am Ind Hyg Assoc J 57:161–165.

  26. Ashley K [1996]. ASTM standards for lead paint abatement mitigation of lead hazards. Lead Perspectives 1(1):28–29.

  27. Schlecht P, Groff JH, Feng A, Song R [1996]. Laboratory and analytical method performance of lead measurements in paint chips, soils, and dusts. Am Ind Hyg Assoc J 57:1035–1043.


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