Abstract

Laser-induced breakdown spectroscopy (LIBS) was evaluated to determine elements collected on swipes as surface contamination. A series of long laser plasmas formed along the swipe surface (Post-it paper) interrogated the collected contamination. LIBS detection limits, determined for the elements Ag, As, Ba, Be, Cd, Cr, Cu, Hg, Mn, Ni, Pb, Sr, and Zn on swipes (2cm2 area), ranged from 0.002μg (Be) to 1.46μg (Pb). The elements were introduced as constituents of synthetic silicate particles serving as a contaminant dust stimulant. The average predicted mass was within 16% of the actual mass on the swipe. The efficiency of collecting particles from surfaces including plastic, Formica, and Al metal was also evaluated. The ability to detect and differentiate two amino acids on a swipe from each other and from the swipe using chemometric modeling techniques was also demonstrated.

© 2010 Optical Society of America

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References

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    [CrossRef]
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    [CrossRef]
  17. S. Dyment “(OSRTI/TIFSD) XRF Web Seminar, Module 2,” a series of web-based seminars sponsored by Superfund's Technology Innovation & Field Services Division (2008).
  18. Innov-X-Systems “(Innovative XRF technologies) website under detection limits,” http://www.innovx.com/products/detect?applications=30#details.
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2009 (1)

K. Ashley, “Field-portable methods for monitoring occupational exposures to metals,” J. Chem. Health Safety doi:10.1016/j.jchas.2009.07.002 (2009).
[CrossRef]

2008 (1)

2006 (1)

S. K. Dufay and M. Archuleta, “Comparison of collection efficiencies of sampling methods for removable beryllium surface contamination,” J. Environ. Monit. 8, 630-633 (2006).
[CrossRef] [PubMed]

2002 (1)

D. L. Donohue, “Key tools for nuclear inspections advances in environmental sample strengthen safeguards,” IAEA Bull. 44, 17-23 (2002).

2001 (2)

M. P. Buttner, P. Cruz-Perez, and L. D. Stetzenbach, “Enhanced detection of surface-associated bacteria in indoor environments by quantitative PCR,” Appl. Environ. Microbiol. 67, 2564-2570 (2001).
[CrossRef] [PubMed]

U. Panne, R. E. Neuhauser, M. Theisen, H. Fink, and R. Niessner, “Analysis of heavy metal aerosols on filters by laser-induced plasma spectroscopy,” Spectrochim. Acta Part B 56, 839-850 (2001).
[CrossRef]

1996 (1)

A. A. Dost, “Monitoring Surface and Airborne Inorganic Contamination in the Workplace by a Field Portable X-Ray Fluorescence Spectrometer,” Am. Occup. Hyg. 40, 589-610(1996).

1995 (1)

S. D. Arnold and D. A. Cremers, “Rapid-determination of metal particles on air sampling using laser-induced breakdown spectroscopy,” AIHA 56, 1180-1186 (1995).
[CrossRef]

1985 (1)

Archuleta, M.

S. K. Dufay and M. Archuleta, “Comparison of collection efficiencies of sampling methods for removable beryllium surface contamination,” J. Environ. Monit. 8, 630-633 (2006).
[CrossRef] [PubMed]

Arnold, S. D.

S. D. Arnold and D. A. Cremers, “Rapid-determination of metal particles on air sampling using laser-induced breakdown spectroscopy,” AIHA 56, 1180-1186 (1995).
[CrossRef]

Ashley, K.

K. Ashley, “Field-portable methods for monitoring occupational exposures to metals,” J. Chem. Health Safety doi:10.1016/j.jchas.2009.07.002 (2009).
[CrossRef]

Buttner, M. P.

M. P. Buttner, P. Cruz-Perez, and L. D. Stetzenbach, “Enhanced detection of surface-associated bacteria in indoor environments by quantitative PCR,” Appl. Environ. Microbiol. 67, 2564-2570 (2001).
[CrossRef] [PubMed]

Cremers, D. A.

S. D. Arnold and D. A. Cremers, “Rapid-determination of metal particles on air sampling using laser-induced breakdown spectroscopy,” AIHA 56, 1180-1186 (1995).
[CrossRef]

D. A. Cremers and L. J. Radziemski, “Direct detection of beryllium on filters using the laser spark,” Appl. Spectrosc. 39, 57-63 (1985).
[CrossRef]

Crouch, S. R.

J. D. Engel and S. R. Crouch, Spectrochemical Analysis (Prentice-Hall, 1988).

Cruz-Perez, P.

M. P. Buttner, P. Cruz-Perez, and L. D. Stetzenbach, “Enhanced detection of surface-associated bacteria in indoor environments by quantitative PCR,” Appl. Environ. Microbiol. 67, 2564-2570 (2001).
[CrossRef] [PubMed]

De Lucia, F. C.

Donohue, D. L.

D. L. Donohue, “Key tools for nuclear inspections advances in environmental sample strengthen safeguards,” IAEA Bull. 44, 17-23 (2002).

Dost, A. A.

A. A. Dost, “Monitoring Surface and Airborne Inorganic Contamination in the Workplace by a Field Portable X-Ray Fluorescence Spectrometer,” Am. Occup. Hyg. 40, 589-610(1996).

Dufay, S. K.

S. K. Dufay and M. Archuleta, “Comparison of collection efficiencies of sampling methods for removable beryllium surface contamination,” J. Environ. Monit. 8, 630-633 (2006).
[CrossRef] [PubMed]

Dyment, S.

S. Dyment “(OSRTI/TIFSD) XRF Web Seminar, Module 2,” a series of web-based seminars sponsored by Superfund's Technology Innovation & Field Services Division (2008).

Engel, J. D.

J. D. Engel and S. R. Crouch, Spectrochemical Analysis (Prentice-Hall, 1988).

Esbensen, K. H.

K. H. Esbensen, Multivariate Data Analysis-In Practice, 5th ed. (Camo, 1994).

Fink, H.

U. Panne, R. E. Neuhauser, M. Theisen, H. Fink, and R. Niessner, “Analysis of heavy metal aerosols on filters by laser-induced plasma spectroscopy,” Spectrochim. Acta Part B 56, 839-850 (2001).
[CrossRef]

Gottfried, J. L.

Gullett, B.

Kerr, K.

K. Kerr, “Beryllium wipe sampling (differing methods--differing exposure potentials),” (National Nuclear Security Administration), http://www.osti.gov/bridge/servlets/purl/837591-M4P95G/native/837591.pdf.

Miziolek, A. W.

Munson, C. A.

Neuhauser, R. E.

U. Panne, R. E. Neuhauser, M. Theisen, H. Fink, and R. Niessner, “Analysis of heavy metal aerosols on filters by laser-induced plasma spectroscopy,” Spectrochim. Acta Part B 56, 839-850 (2001).
[CrossRef]

Niessner, R.

U. Panne, R. E. Neuhauser, M. Theisen, H. Fink, and R. Niessner, “Analysis of heavy metal aerosols on filters by laser-induced plasma spectroscopy,” Spectrochim. Acta Part B 56, 839-850 (2001).
[CrossRef]

Panne, U.

U. Panne, R. E. Neuhauser, M. Theisen, H. Fink, and R. Niessner, “Analysis of heavy metal aerosols on filters by laser-induced plasma spectroscopy,” Spectrochim. Acta Part B 56, 839-850 (2001).
[CrossRef]

Radziemski, L. J.

Snyder, E. G.

Stetzenbach, L. D.

M. P. Buttner, P. Cruz-Perez, and L. D. Stetzenbach, “Enhanced detection of surface-associated bacteria in indoor environments by quantitative PCR,” Appl. Environ. Microbiol. 67, 2564-2570 (2001).
[CrossRef] [PubMed]

Theisen, M.

U. Panne, R. E. Neuhauser, M. Theisen, H. Fink, and R. Niessner, “Analysis of heavy metal aerosols on filters by laser-induced plasma spectroscopy,” Spectrochim. Acta Part B 56, 839-850 (2001).
[CrossRef]

Tyler, G.

G. Tyler, “ICP-OES, ICP-MS and AAS Techniques Compared,” Technical Note 05 (Jobin Yvon Horiba ICP Optical Emission Spectroscopy), http://www.jobinyvon.com/usadivisions/Emission/applications/TN05.pdf.

AIHA (1)

S. D. Arnold and D. A. Cremers, “Rapid-determination of metal particles on air sampling using laser-induced breakdown spectroscopy,” AIHA 56, 1180-1186 (1995).
[CrossRef]

Am. Occup. Hyg. (1)

A. A. Dost, “Monitoring Surface and Airborne Inorganic Contamination in the Workplace by a Field Portable X-Ray Fluorescence Spectrometer,” Am. Occup. Hyg. 40, 589-610(1996).

Appl. Environ. Microbiol. (1)

M. P. Buttner, P. Cruz-Perez, and L. D. Stetzenbach, “Enhanced detection of surface-associated bacteria in indoor environments by quantitative PCR,” Appl. Environ. Microbiol. 67, 2564-2570 (2001).
[CrossRef] [PubMed]

Appl. Opt. (1)

Appl. Spectrosc. (1)

IAEA Bull. (1)

D. L. Donohue, “Key tools for nuclear inspections advances in environmental sample strengthen safeguards,” IAEA Bull. 44, 17-23 (2002).

J. Chem. Health Safety (1)

K. Ashley, “Field-portable methods for monitoring occupational exposures to metals,” J. Chem. Health Safety doi:10.1016/j.jchas.2009.07.002 (2009).
[CrossRef]

J. Environ. Monit. (1)

S. K. Dufay and M. Archuleta, “Comparison of collection efficiencies of sampling methods for removable beryllium surface contamination,” J. Environ. Monit. 8, 630-633 (2006).
[CrossRef] [PubMed]

Spectrochim. Acta Part B (1)

U. Panne, R. E. Neuhauser, M. Theisen, H. Fink, and R. Niessner, “Analysis of heavy metal aerosols on filters by laser-induced plasma spectroscopy,” Spectrochim. Acta Part B 56, 839-850 (2001).
[CrossRef]

Other (11)

S. Dyment “(OSRTI/TIFSD) XRF Web Seminar, Module 2,” a series of web-based seminars sponsored by Superfund's Technology Innovation & Field Services Division (2008).

Innov-X-Systems “(Innovative XRF technologies) website under detection limits,” http://www.innovx.com/products/detect?applications=30#details.

“Surface Swipe Sampling Procedure,” Standard Operating Procedure, IH75190, Final Rev15 (Brookhaven National Laboratory, Safety and Health Division, Industrial Hygiene Group, 2009).

K. H. Esbensen, Multivariate Data Analysis-In Practice, 5th ed. (Camo, 1994).

J. D. Engel and S. R. Crouch, Spectrochemical Analysis (Prentice-Hall, 1988).

G. Tyler, “ICP-OES, ICP-MS and AAS Techniques Compared,” Technical Note 05 (Jobin Yvon Horiba ICP Optical Emission Spectroscopy), http://www.jobinyvon.com/usadivisions/Emission/applications/TN05.pdf.

K. Kerr, “Beryllium wipe sampling (differing methods--differing exposure potentials),” (National Nuclear Security Administration), http://www.osti.gov/bridge/servlets/purl/837591-M4P95G/native/837591.pdf.

“Surface Wipe Sampling Procedure,” IH75190 (Industrial Hygiene Group, Brookhaven National Laboratory, 2009).

“A Literature Review of Wipe Sampling Methods for Chemical Warfare Agents and Toxic Industrial Chemicals,” EPA/600/R-07/004 (EPA, Office of Development and Research, 2007).

“Evaluation Guidelines for Surface Sampling Methods,” T-005-01-0104-M (OSHA, Industrial Hygiene Chemistry Division), http://www.osha.gov/dts/sltc/methods/surfacesampling/surfacesampling.html.

“Sampling, Measurement Methods, and Instruments, OR-OSHA Technical Manual,” http://www.cbs.state.or.us/external/osha/pdf/techman/tecman1.pdf.

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Figures (6)

Fig. 1
Fig. 1

LIBS portable swipe monitor. L = laser , P = air pump , S = spectrograph , D = detector , TS = translation stage , TSC = translation stage controller , DC = detector controller , F = HEPA   air filter , LPS = laser power supply SC = sample chamber , EC = end cap , SH = swipe holder , and CL = cylindrical lens . The procedure for loading the swipe into the instrument is also shown.

Fig. 2
Fig. 2

Comparison of the average of normalized emission lines for a series of elements using a translation stage to move the swipe with synthetic silicate particles over different increments between shots. A single shot analysis was performed on each spot before moving to an adjacent area, and a total of 10 steps were carried out for each increment.

Fig. 3
Fig. 3

Typical calibration curve; the curve shown is for beryllium.

Fig. 4
Fig. 4

Comparison of LIBS detection limit values (μg/swipe from Table 3 with different mass limits collected over a 100 cm 2 area (regulatory and facility specified) for metals used in this study.

Fig. 5
Fig. 5

Comparison of the collection efficiency of the swipe determined using manganese deposited on smooth and rough plastic surfaces. A new swipe was used each time and swiped over the same area. After and including swipe number 6 on the smooth plastic surface and swipe number 9 on the rough plastic surface, wet swipes were used and allowed to air dry before they were analyzed.

Fig. 6
Fig. 6

PLS2 Regression Model built using “best” (highest intensity) 50 LIBS spectra collected from two amino acids on Post-it paper and clean Post-It paper. The model score space for the first three principal components is plotted on the left (a). From the score space, it can be seen that there is overlap between the sample scores, especially for L-leucine on a Post-it paper and a clean Post-it paper. When the model was tested on 20 of the “worst” (lowest count) spectra (b), however, it was found that the samples could be well separated by choosing prediction values of > 0.8 for L-asparagine on a Post-it paper, < 0.35 for a clean Post-it paper, and between 0.35 and 0.8 for L-leucine on a Post-it paper.

Tables (5)

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Table 1 Analytical Emission Lines for Analytes of Interest

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Table 2 Strong Emission Lines (nm) Observed from LIBS Analysis of Three Swipe Materials

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Table 3 Detection Limits ( C L ) from Synthetic Silicate Particles on Post-it Paper (Area ~ 0.64 cm × 3.2 cm ) and Comparison with Portable XRF [11]

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Table 4 Measurement Accuracy Using Swipes (Synthetic Silicate Particles on Post-it Paper)

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Table 5 Collection Efficiency for Synthetic Silicate Samples Swiped from Surface a

Equations (1)

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Release of housekeeping criteria for metal = A / B [ TLV or OSHA PEL for Metal ] .

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