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An electron microscopy based method for the detection and quantification of nanomaterial number concentration in environmentally relevant media
Improved detection and characterization of nanomaterials (NMs) in complex environmental media requires the development of novel sampling approaches to improve the detection limit to be close to environmentally realistic concentrations. Transmission electron microscopy (TEM) is an indispensable metro...
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| Published in: | The Science of the total environment 2015-12, Vol.537, p.479-486 |
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| container_title | The Science of the total environment |
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| creator | Prasad, A. Lead, J.R. Baalousha, M. |
| description | Improved detection and characterization of nanomaterials (NMs) in complex environmental media requires the development of novel sampling approaches to improve the detection limit to be close to environmentally realistic concentrations. Transmission electron microscopy (TEM) is an indispensable metrological tool in nanotechnology and environmental nanoscience due to its high spatial resolution and analytical capabilities when coupled to spectroscopic techniques. However, these capabilities are hampered by the conventional sample preparation methods, which suffer from low NM recovery. The current work presents a validated, fully quantitative sampling technique for TEM that overcomes conventional sample preparation shortcomings, and thus enables the use of TEM for measurement of particle number concentration and their detection in complex media at environmentally realistic concentrations. This sampling method is based on ultracentrifugation of NMs from suspension onto a poly-l-lysine (PLL) functionalized TEM grid, using active deposition (by ultracentrifugation) and retention (by PLL interactions with NM surface) of NMs on the substrate, enabling fully quantitative analysis. Similar analysis with AFM was satisfactory in simple media but the lack of chemical-selectivity of AFM limits its applicability for the detection of NMs in complex environmental samples. The sampling approach was validated using both citrate- and PVP-coated AuNMs in pure water, which demonstrated an even distribution of NM on the TEM grid and high NM recovery (80–100%) at environmentally relevant NM concentrations (ca. 0.20–100μgL−1). The applicability of the sampling method to complex environmental samples was demonstrated by the quantification of particle number concentration of AuNMs in EPA soft water (with and without Suwannee River fulvic acid) and lake water. This sample preparation approach is also applicable to other types of NMs with some modifications (e.g. centrifugation force and time) to insure full sample recovery. This TEM sampling method is key to the accurate quantification of NM number concentration, and therefore to improving our understanding of environmental fate, behavior, effects and dose of NMs.
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•Fully quantitative sampling method for analysis of NMs by TEM is presented•The method combines ultracentrifugation and TEM grid functionalization•Initial validation has been performed using AuNMs in pure and synthetic EA waters•The TEM sampling method ena |
| doi_str_mv | 10.1016/j.scitotenv.2015.07.117 |
| format | article |
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[Display omitted]
•Fully quantitative sampling method for analysis of NMs by TEM is presented•The method combines ultracentrifugation and TEM grid functionalization•Initial validation has been performed using AuNMs in pure and synthetic EA waters•The TEM sampling method enables direct measurement of NM number concentration•The TEM sampling method enables detection of NMs in complex natural samples</description><identifier>ISSN: 0048-9697</identifier><identifier>EISSN: 1879-1026</identifier><identifier>DOI: 10.1016/j.scitotenv.2015.07.117</identifier><identifier>PMID: 26322596</identifier><language>eng</language><publisher>Netherlands: Elsevier B.V</publisher><subject>Atomic force microscopy ; Electron microscopy ; Environmental media ; Environmental Monitoring - methods ; Environmental Pollutants - analysis ; Media ; Microscopy, Electron - methods ; Nanomaterials ; Nanostructure ; Nanostructures - analysis ; Particles number concentration ; Quantitative analysis ; Recovery ; Sample preparation ; Sampling ; Sampling methods ; Transmission electron microscopy</subject><ispartof>The Science of the total environment, 2015-12, Vol.537, p.479-486</ispartof><rights>2015 Elsevier B.V.</rights><rights>Copyright © 2015 Elsevier B.V. All rights reserved.</rights><lds50>peer_reviewed</lds50><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c486t-13013b482776d016801309d97a7fb5e408067453e1b0a86f1eb1f356dfa5d4cf3</citedby><cites>FETCH-LOGICAL-c486t-13013b482776d016801309d97a7fb5e408067453e1b0a86f1eb1f356dfa5d4cf3</cites><orcidid>0000-0001-7491-4954</orcidid></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><link.rule.ids>315,786,790,27957,27958</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/26322596$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Prasad, A.</creatorcontrib><creatorcontrib>Lead, J.R.</creatorcontrib><creatorcontrib>Baalousha, M.</creatorcontrib><title>An electron microscopy based method for the detection and quantification of nanomaterial number concentration in environmentally relevant media</title><title>The Science of the total environment</title><addtitle>Sci Total Environ</addtitle><description>Improved detection and characterization of nanomaterials (NMs) in complex environmental media requires the development of novel sampling approaches to improve the detection limit to be close to environmentally realistic concentrations. Transmission electron microscopy (TEM) is an indispensable metrological tool in nanotechnology and environmental nanoscience due to its high spatial resolution and analytical capabilities when coupled to spectroscopic techniques. However, these capabilities are hampered by the conventional sample preparation methods, which suffer from low NM recovery. The current work presents a validated, fully quantitative sampling technique for TEM that overcomes conventional sample preparation shortcomings, and thus enables the use of TEM for measurement of particle number concentration and their detection in complex media at environmentally realistic concentrations. This sampling method is based on ultracentrifugation of NMs from suspension onto a poly-l-lysine (PLL) functionalized TEM grid, using active deposition (by ultracentrifugation) and retention (by PLL interactions with NM surface) of NMs on the substrate, enabling fully quantitative analysis. Similar analysis with AFM was satisfactory in simple media but the lack of chemical-selectivity of AFM limits its applicability for the detection of NMs in complex environmental samples. The sampling approach was validated using both citrate- and PVP-coated AuNMs in pure water, which demonstrated an even distribution of NM on the TEM grid and high NM recovery (80–100%) at environmentally relevant NM concentrations (ca. 0.20–100μgL−1). The applicability of the sampling method to complex environmental samples was demonstrated by the quantification of particle number concentration of AuNMs in EPA soft water (with and without Suwannee River fulvic acid) and lake water. This sample preparation approach is also applicable to other types of NMs with some modifications (e.g. centrifugation force and time) to insure full sample recovery. This TEM sampling method is key to the accurate quantification of NM number concentration, and therefore to improving our understanding of environmental fate, behavior, effects and dose of NMs.
[Display omitted]
•Fully quantitative sampling method for analysis of NMs by TEM is presented•The method combines ultracentrifugation and TEM grid functionalization•Initial validation has been performed using AuNMs in pure and synthetic EA waters•The TEM sampling method enables direct measurement of NM number concentration•The TEM sampling method enables detection of NMs in complex natural samples</description><subject>Atomic force microscopy</subject><subject>Electron microscopy</subject><subject>Environmental media</subject><subject>Environmental Monitoring - methods</subject><subject>Environmental Pollutants - analysis</subject><subject>Media</subject><subject>Microscopy, Electron - methods</subject><subject>Nanomaterials</subject><subject>Nanostructure</subject><subject>Nanostructures - analysis</subject><subject>Particles number concentration</subject><subject>Quantitative analysis</subject><subject>Recovery</subject><subject>Sample preparation</subject><subject>Sampling</subject><subject>Sampling methods</subject><subject>Transmission electron microscopy</subject><issn>0048-9697</issn><issn>1879-1026</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2015</creationdate><recordtype>article</recordtype><recordid>eNqNkc1u3CAURlHVqJmkfYWUZTd2wdiAl6Oof1KkbJo1wnBRGNkwATzSPEVfuUwnybZhg7g63E_6DkKfKWkpofzrrs3Gl1ggHNqO0KEloqVUvEMbKsXYUNLx92hDSC-bkY_iEl3lvCP1CEk_oMuOs64bRr5Bf7YBwwympBjw4k2K2cT9EU86g8ULlMdosYsJl0fAFkolfSV1sPhp1aF4543-N4oOBx3iogskr2cc1mWChE0MBkJJZ8jXtHDwNWypQz3PR5xq_KFuqmHW64_owuk5w6fn-xo9fP_2-_Znc3f_49ft9q4xveSloYxQNvWyE4LbWoisTzLaUWjhpgF6IgkX_cCATkRL7ihM1LGBW6cH2xvHrtGX8959ik8r5KIWnw3Msw4Q16yoEJIMPWPyDWjP5UhGyd6AUjYOlElSUXFGT5XnBE7tk190OipK1Mmx2qlXx-rkWBGhquP68-Y5ZJ1qZ6__XqRWYHsGoBZ48JBOi6BqsD5Vf8pG_9-Qv8gVvzY</recordid><startdate>20151215</startdate><enddate>20151215</enddate><creator>Prasad, A.</creator><creator>Lead, J.R.</creator><creator>Baalousha, M.</creator><general>Elsevier B.V</general><scope>CGR</scope><scope>CUY</scope><scope>CVF</scope><scope>ECM</scope><scope>EIF</scope><scope>NPM</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>7X8</scope><scope>7ST</scope><scope>C1K</scope><scope>SOI</scope><scope>8FD</scope><scope>FR3</scope><scope>KR7</scope><orcidid>https://orcid.org/0000-0001-7491-4954</orcidid></search><sort><creationdate>20151215</creationdate><title>An electron microscopy based method for the detection and quantification of nanomaterial number concentration in environmentally relevant media</title><author>Prasad, A. ; Lead, J.R. ; Baalousha, M.</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c486t-13013b482776d016801309d97a7fb5e408067453e1b0a86f1eb1f356dfa5d4cf3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2015</creationdate><topic>Atomic force microscopy</topic><topic>Electron microscopy</topic><topic>Environmental media</topic><topic>Environmental Monitoring - methods</topic><topic>Environmental Pollutants - analysis</topic><topic>Media</topic><topic>Microscopy, Electron - methods</topic><topic>Nanomaterials</topic><topic>Nanostructure</topic><topic>Nanostructures - analysis</topic><topic>Particles number concentration</topic><topic>Quantitative analysis</topic><topic>Recovery</topic><topic>Sample preparation</topic><topic>Sampling</topic><topic>Sampling methods</topic><topic>Transmission electron microscopy</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Prasad, A.</creatorcontrib><creatorcontrib>Lead, J.R.</creatorcontrib><creatorcontrib>Baalousha, M.</creatorcontrib><collection>Medline</collection><collection>MEDLINE</collection><collection>MEDLINE (Ovid)</collection><collection>MEDLINE</collection><collection>MEDLINE</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>MEDLINE - Academic</collection><collection>Environment Abstracts</collection><collection>Environmental Sciences and Pollution Management</collection><collection>Environment Abstracts</collection><collection>Technology Research Database</collection><collection>Engineering Research Database</collection><collection>Civil Engineering Abstracts</collection><jtitle>The Science of the total environment</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Prasad, A.</au><au>Lead, J.R.</au><au>Baalousha, M.</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>An electron microscopy based method for the detection and quantification of nanomaterial number concentration in environmentally relevant media</atitle><jtitle>The Science of the total environment</jtitle><addtitle>Sci Total Environ</addtitle><date>2015-12-15</date><risdate>2015</risdate><volume>537</volume><spage>479</spage><epage>486</epage><pages>479-486</pages><issn>0048-9697</issn><eissn>1879-1026</eissn><notes>ObjectType-Article-1</notes><notes>SourceType-Scholarly Journals-1</notes><notes>ObjectType-Feature-2</notes><notes>content type line 23</notes><abstract>Improved detection and characterization of nanomaterials (NMs) in complex environmental media requires the development of novel sampling approaches to improve the detection limit to be close to environmentally realistic concentrations. Transmission electron microscopy (TEM) is an indispensable metrological tool in nanotechnology and environmental nanoscience due to its high spatial resolution and analytical capabilities when coupled to spectroscopic techniques. However, these capabilities are hampered by the conventional sample preparation methods, which suffer from low NM recovery. The current work presents a validated, fully quantitative sampling technique for TEM that overcomes conventional sample preparation shortcomings, and thus enables the use of TEM for measurement of particle number concentration and their detection in complex media at environmentally realistic concentrations. This sampling method is based on ultracentrifugation of NMs from suspension onto a poly-l-lysine (PLL) functionalized TEM grid, using active deposition (by ultracentrifugation) and retention (by PLL interactions with NM surface) of NMs on the substrate, enabling fully quantitative analysis. Similar analysis with AFM was satisfactory in simple media but the lack of chemical-selectivity of AFM limits its applicability for the detection of NMs in complex environmental samples. The sampling approach was validated using both citrate- and PVP-coated AuNMs in pure water, which demonstrated an even distribution of NM on the TEM grid and high NM recovery (80–100%) at environmentally relevant NM concentrations (ca. 0.20–100μgL−1). The applicability of the sampling method to complex environmental samples was demonstrated by the quantification of particle number concentration of AuNMs in EPA soft water (with and without Suwannee River fulvic acid) and lake water. This sample preparation approach is also applicable to other types of NMs with some modifications (e.g. centrifugation force and time) to insure full sample recovery. This TEM sampling method is key to the accurate quantification of NM number concentration, and therefore to improving our understanding of environmental fate, behavior, effects and dose of NMs.
[Display omitted]
•Fully quantitative sampling method for analysis of NMs by TEM is presented•The method combines ultracentrifugation and TEM grid functionalization•Initial validation has been performed using AuNMs in pure and synthetic EA waters•The TEM sampling method enables direct measurement of NM number concentration•The TEM sampling method enables detection of NMs in complex natural samples</abstract><cop>Netherlands</cop><pub>Elsevier B.V</pub><pmid>26322596</pmid><doi>10.1016/j.scitotenv.2015.07.117</doi><tpages>8</tpages><orcidid>https://orcid.org/0000-0001-7491-4954</orcidid><oa>free_for_read</oa></addata></record> |
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| subjects | Atomic force microscopy Electron microscopy Environmental media Environmental Monitoring - methods Environmental Pollutants - analysis Media Microscopy, Electron - methods Nanomaterials Nanostructure Nanostructures - analysis Particles number concentration Quantitative analysis Recovery Sample preparation Sampling Sampling methods Transmission electron microscopy |
| title | An electron microscopy based method for the detection and quantification of nanomaterial number concentration in environmentally relevant media |
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