Abstract
Environmental risk assessments of engineered nanoparticles require thorough characterization of nanoparticles and their aggregates. Furthermore, quantitative analytical methods are required to determine environmental concentrations and enable both effect and exposure assessments. Many methods still need optimization and development, especially for new types of nanoparticles in water, but extensive experience can be gained from the fields of environmental chemistry of natural nanomaterials and from fundamental colloid chemistry. This review briefly describes most methods that are being exploited in nanoecotoxicology for analysis and characterization of nanomaterials. Methodological aspects are discussed in relation to the fields of nanometrology, particle size analysis and analytical chemistry. Differences in both the type of size measures (length, radius, aspect ratio, etc.), and the type of average or distributions afforded by the specific measures are compared. The strengths of single particle methods, such as electron microscopy and atomic force microscopy, with respect to imaging, shape determinations and application to particle process studies are discussed, together with their limitations in terms of counting statistics and sample preparation. Methods based on the measurement of particle populations are discussed in terms of their quantitative analyses, but the necessity of knowing their limitations in size range and concentration range is also considered. The advantage of combining complementary methods is highlighted.
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References
Aitken RJ, Chaudhry MQ, Boxall ABA, Hull M (2006) Manufacture and use of nanomaterials: current status in the UK and global trends. Occup Med 56:300–306
Aitken RJ, Hankin SM, Tran CL, Donaldson K, Stone V, Cumpson P, Johnstone J, Chaudhry Q, Cash S (2007) REFNANO: reference materials for engineered nanoparticle toxicology and metrology. DEFRA, UK. http://www.iom-world.org/pubs/REFNANOReport.pdf
Andrievsky GV, Klochkov VK, Bordyuh AB, Dovbeshko GI (2002) Comparative analysis of two aqueous-colloidal solutions of C-60 fullerene with help of FTIR reflectance and UV–vis spectroscopy. Chem Phys Lett 364:8–17
Aryal S, Bahadur KCR, Bhattard N, Kim CK, Kim HY (2006) Study of electrolyte induced aggregation of gold nanoparticles capped by amino acids. J Colloid Interface Sci 299:191–197
Bailey RE, Smith AM, Nie S (2004) Quantum dots in biology and medicine. Physica E 25:1–12
Balnois E, Wilkinson KJ (2002) Sample preparation techniques for the observation of environmental biopolymers by atomic force microscopy. Colloids Surf Physicochem Eng Aspects 207:229–242
Balnois E, Papastavrou G, Wilkinson KJ (2007) Force microscopy and force measurements of environmental colloids. In: Wilkinson KJ, Lead JR (eds) Environmental colloids and particles: behaviour, structure and characterization. IUPAC series on analytical and physical chemistry of environmental systems. John Wiley and Sons, Chichester, pp 405–468
Banfield JF, Navrotsky A (eds) (2001) Nanoparticles and the environment. Reviews in Mineralogy & Geochemistry, vol 44. The Mineralogy Society of America, Washington, DC, p 349
Barth HG, Boyes BE (1992) Size exclusion chromatography. Anal Chem 64:428R–442R
Barth HG, Flippen RB (1995) Particle size analysis. Anal Chem 67:257R–272R
Becker L, Bada JL, Winans RE, Hunt JE, Bunch TE, French BM (1994) Fullerenes in the 1.85-billion-year-old Sudbury impact structure. Science 265:642–645
Bogner A, Thollet G, Basset D, Jouneau PH, Gauthier C (2005) Wet STEM: a new development in environmental SEM for imaging nano-objects included in a liquid phase. Ultramicroscopy 104:290–301
Breil R, Fries T, Garnaes J, Haycocks J, Huser D, Joergensen J, Kautek W, Koenders L, Kofod N, Koops KR, Korntner R, Lindner B, Mirande W, Neubauer A, Peltonen J, Picotto GB, Pisani M, Rothe H, Sahre M, Stedman M, Wilkening G (2002) Intercomparison of scanning probe microscopes. Precis Eng-J Int Soc Precis Eng Nanotechnol 26:296–305
Brunauer S, Emmet PH, Teller E (1938) Adsoprtion of gases in multimolecular layers. J Am Chem Soc 60:309–319
Buffle J, Perret J, Newman J (1992) The use of filtration and ultrafiltration for size fractionation of aquatic particles, colloids and macromolecules. In: Buffle J, van Leeuwen HP (eds) Environmental particles I. Lewis, Chelsea, pp 171–230
Colvin VL (2003) The potential environmental impact of engineered nanomaterials. Nat Biotechnol 21:1166–1170
Crane M, Handy RD (2007) An assessment of regulatory testing strategies and methods for characterizing the ecotoxicological hazards of nanomaterials, Report for Defra, London, UK. Available at: http://randd.defra.gov.uk/Document.aspx?DocumentID=2270
Doucet FJ, Lead JR, Maguire L, Achterberg EP, Millward GE (2005) Visualisation of natural aquatic colloids and particles—a comparison of conventional high vacuum and environmental scanning electron microscopy. J Environ Monit 7:115–121
Duesberg GS, Burghard M, Muster J, Philipp G, Roth S (1998) Separation of carbon nanotubes by size exclusion chromatography. Chem Commun 3:435–436
Ebdon L, Foulkes M, Sutton K (1997) Slurry nebulization in plasmas. J Anal Atom Spectrom 12:213–229
EPA (2007) Nanotechnology white paper, U.S. Environmental Protection Agency, Washington, DC. http://es.epa.gov/ncer/nano/publications/whitepaper12022005.pdf
Federici G, Shaw BJ, Handy RD (2007) Toxicity of titanium dioxide nanoparticles to rainbow trout (Oncorhynchus mykiss): gill injury, oxidative stress, and other physiological effects. Aquat Toxicol 84:415–430
Filella M (2007) Colloidal properties of submicron particles in natural waters. In: Wilkinson KJ, Lead JR (eds) Environmental colloids and particles: behaviour, structure and characterization. IUPAC series on analytical and physical chemistry of environmental systems. John Wiley and Sons, Chichester, pp 17–93
Filella M, Zhang J, Newman ME, Buffle J (1997) Analytical applications of photon correlation spectroscopy for size distribution measurements of natural colloidal suspensions. Colloids Surf A 120:27–46
Finsy R (1994) Particle sizing by quasi-elastic light-scattering. Adv Colloid Interface Sci 52:79–143
Fortner JD, Lyon DY, Sayes CM, Boyd AM, Falkner JC, Hotze EM, Alemany LB, Tao YJ, Guo W, Ausman KD, Colvin VL, Hughes JB (2005) C60 in water: nanocrystal formation and microbial response. Environ Sci Technol 39:4307–4316
Franklin NM, Rogers NJ, Apte SC, Batley GE, Gadd GE, Casey PS (2007) Comparative toxicity of nanoparticulate ZnO, bulk ZnO, and ZnCl2 to a freshwater microalga (Pseudokirchneriella subcapitata): the importance of particle solubility. Environ Sci Technol 41:8484–8490
Gee GW, Bauder JW (1986) Particle size analysis, methods of soil analysis. Part 1. Physical and mineralogical methods. Agronomy monograph no. 9, 2nd edn. SSSA, Madison, Wisconsin, pp 383–411
Giddings JC (1993) Field-flow fractionation: analysis of macromolecular, colloidal, and particulate matter. Science 260:1456–1465
Gimbert LJ, Haygarth PM, Beckett R, Worsfold PJ (2005) Comparison of centrifugation and filtration techniques for the size fractionation of colloidal material in soil suspensions using sedimentation field-flow fractionation. Environ Sci Technol 39:1731–1735
Gimbert LJ, Haygarth PM, Beckett R, Worsfold PJ (2006) The influence of sample preparation on observed particle size distributions for contrasting soil suspensions using flow field-flow fractionation. Environ Chem 3:184–191
Guo L, Wen L-S, Tang D, Santschi PH (2000) Re-examination of cross-flow ultrafiltration for sampling marine colloids: evidence from molecular probes. Mar Chem 69:75–90
Guzman KAD, Finnegan MP, Banfield JF (2006) Influence of surface potential on aggregation and transport of titania nanoparticles. Environ Sci Technol 40:7688–7693
Hall GEM (1998) Relative contamination levels observed in different types of bottles used to collect water samples. Explorer 101:1–7
Handy RD, von der Kammer F, Lead JR, Hassellöv M, Owen R, Crane M (2008) The ecotoxicology and chemistry of manufactured nanoparticles. Ecotoxicology 17:287–314
Hansen SF, Larsen BH, Olsen SI, Baun A (2007) Categorization framework to aid hazard identification of nanomaterials. Nanotoxicology 1:243–250
Hassellöv M, Lyven B, Haraldsson C, Sirinawin W (1999) Determination of continuous size and trace element distribution of colloidal material in natural water by on-line coupling of flow field-flow fractionation with ICPMS. Anal Chem 71:3497–3502
Hassellöv M, Lyven B, Bengtsson H, Jansen R, Turner DR, Beckett R (2001) Particle size distributions of clay-rich sediments and pure clay minerals: a comparison of grain size analysis with sedimentation field-flow fractionation. Aquat Geochem 7:155–171
Hassellöv M, von der Kammer F, Beckett R (2007) Characterisation of aquatic colloids and macromolecules by field-flow fractionation. In: Wilkinson KJ, Lead JR (eds) Environmental colloids and particles: behaviour, structure and characterization. John Wiley and Sons, Chichester, pp 223–276
Hochella MF, Madden AS (2005) Earth’s nano-compartment for toxic metals. Elements 1:199–203
Holt MS, Fox K, Griebach E, Johnsen S, Kinnunen J, Lecloux A, Murray-Smith R, Peterson DR, Schröder R, Silvani M, ten Berge WFJ, Toy RJ, Feijtel TCM (2000) Monitoring, modelling and environmental exposure assessment of industrial chemicals in the aquatic environment. Chemosphere 41:1799–1808
Hunter KA, Liss PS (1979) The surface charge of suspended particles in estuarine and coastal water. Nature 282:823–825
Hyung H, Fortner JD, Hughes JB, Kim JH (2007) Natural organic matter stabilizes carbon nanotubes in the aqueous phase. Environ Sci Technol 41:179–184
Isaacson CW, Usenko CY, Tanguay RL, Field JA (2007) Quantification of fullerenes by LC/ESI-MS and its application to in vivo toxicity assays. Anal Chem 79:9091–9097
Jackson BP, Ranville JF, Bertsch PM, Sowder A (2005) Characterization of colloidal and humic-bound Ni and U in the “dissolved” fraction of contaminated sediment extracts. Environ Sci Technol 39:2478–2485
Jiang L, Gao L, Sun J (2003) Production of aqueous colloidal dispersions of carbon nanotubes. J Colloid Interface Sci 260:89–94
Kim JI, Walther C (2007) Laser induced breakdown detection (LIBD). In: Wilkinson KJ, Lead JR (eds) Environmental colloids and particles: behaviour, structure and characterization. IUPAC series on analytical and physical chemistry of environmental systems. John Wiley and Sons, Chichester, pp 555–612
Larsson J, Gustafsson O, Ingri J (2002) Evaluation and optimization of two complementary cross-flow ultrafiltration systems toward isolation of coastal surface water colloids. Environ Sci Technol 36:2236–2241
Lead JR, Wilkinson KJ (2006) Aquatic colloids and nanoparticles: current knowledge and future trends. Environ Chem 3:159–171
Lead JR, Wilkinson KJ, Balnois E, Cutak BJ, Larive CK, Assemi S, Beckett R (2000a) Diffusion coefficients and polydispersities of the Suwannee River fulvic acid: comparison of fluorescence correlation spectroscopy, pulsed-field gradient nuclear magnetic resonance, and flow field-flow fractionation. Environ Sci Technol 34:3508–3513
Lead JR, Wilkinson KJ, Starchev K, Canonica S, Buffle J (2000b) Determination of diffusion coefficients of humic substances by fluorescence correlation spectroscopy: role of solution conditions. Environ Sci Technol 34:1365–1369
Lead JR, Muirhead D, Gibson CT (2005) Characterization of freshwater natural aquatic colloids by atomic force microscopy (AFM). Environ Sci Technol 39:6930–6936
Ledin A, Karlsson S, Duker A, Allard B (1994) Measurements in situ of concentration and size distribution of colloidal matter in deep groundwaters by photon-correlation spectroscopy. Water Res 28:1539–1545
Link S, El-Sayed MA (1999) Spectral properties and relaxation dynamics of surface plasmon electronic oscillations in gold and silver nanodots and nanorods. J Phys Chem B 103:8410–8426
Liu R, Lead JR (2006) Partial validation of cross flow ultrafiltration by atomic force microscopy. Anal Chem 78:8105–8112
Madden AS, Hochella MF (2005) A test of geochemical reactivity as a function of mineral size: manganese oxidation promoted by hematite nanoparticles. Geochim Cosmochim Acta 69:389–398
Mavrocordatos D, Pronk W, Boller M (2004) Analysis of environmental particles by atomic force microscopy, scanning and transmission electron microscopy. Water Sci Technol 50:9–18
Mavrocordatos D, Perret D, Leppard GG (2007) Strategies and advances in the characterization of environmental colloids by electron microscopy. In: Wilkinson KJ, Lead JR (eds) Environmental colloids and particles: behaviour, structure and characterization. IUPAC series on analytical and physical chemistry of environmental systems. John Wiley and Sons, Chichester, pp 345–404
Maynard AD, Aitken RJ, Butz T, Colvin V, Donaldson K, Oberdörster G, Philbert MA, Ryan J, Seaton A, Stone V, Tinkle SS, Tran L, Walker NJ and Warheit DB (2006) Safe handling of nanotechnology. Nature 444:267–269
Morrison MA, Benoit G (2001) Filtration artifacts caused by overloading membrane filters. Environ Sci Technol 35:3774–3779
Murr LE, Esquivel EV, Bang JJ, de la Rosa G, Gardea-Torresdey JL (2004) Chemistry and nanoparticulate compositions of a 10,000 year-old ice core melt water. Water Res 38:4282–4296
Nowack B, Bucheli TD (2007) Occurrence, behavior and effects of nanoparticles in the environment. Environ Pollut 150:5–22
Pal S, Tak YK, Song JM (2007) Does the antibacterial activity of silver nanoparticles depend on the shape of the nanoparticle? A study of the gram-negative bacterium Escherichia coli. Appl Environ Microbiol 73:1712–1720
Perminova IV, Frimmel FH, Kudryavtsev AV, Kulikova NA, Abbt-Braun G, Hesse S, Petrosyan VS (2003) Molecular weight characteristics of humic substances from different environments as determined by size exclusion chromatography and their statistical evaluation. Environ Sci Technol 37:2477–2485
Ranville JF, Chittleborough DJ, Doss F, Harris T, Morrison R, Beckett R (1999) Development of sedimentation field-flow fractionation-inductively coupled plasma-mass spectrometry for the characterization of environmental colloids. Anal Chim Acta 381:315–329
Roco MC (2005) International perspective on government nanotechnology funding in 2005. J Nanopart Res 7:707–712
Santos MC, Nobrega JA (2006) Slurry nebulization in plasmas for analysis of inorganic materials. Appl Spectroscop Rev 41:427–448
SCENIHR (2005) Opinion on the appropriateness of existing methodologies to assess the potential risks associated with engineered and adventitious products of nanotechnology. Scientific Committee on Emerging and Newly Identified Health Risks, European Commission. http://ec.europa.eu/health/ph_risk/committees/04_scenihr/docs/scenihr_o_003b.pdf
Schimpf M, Caldwell K, Giddings JC (eds) (2000) Field-flow fractionation handbook. John Wiley & Sons Inc., New York, p 616
Schurtenberger P, Newman ME (1993) Characterization of biological and environmental particles using static and dynamic light scattering. In: Buffle J, van Leeuwen HP (eds) Environmental particles. Lewis Publishers, Boca Raton, Florida, pp 37–115
Smith CJ, Shaw BJ, Handy RD (2007) Toxicity of single walled carbon nanotubes to rainbow trout (Oncorhynchus mykiss): respiratory toxicity, organ pathologies, and other physiological effects. Aquat Toxicol 82:94–109
Suzuki Y, Kelly SD, Kemner KM, Banfield JF (2002) Radionuclide contamination—nanometre-size products of uranium bioreduction. Nature 419:134–134
Taylor R (2006) Addition reactions of fullerenes. C R Chimie 9:982–1000
Taylor R, Parsons JP, Avent AG, Rannard SP, Dennis TJ, Hare JP, Kroto HW and Walton DRM (1991) Degradation of C60 by light. Nature 351
Thiberge S, Nechushtan A, Sprinzak D, Gileadi O, Behar V, Zik O, Chowers Y, Michaeli S, Schlessinger J, Moses E (2004) Scanning electron microscopy of cells and tissues under fully hydrated conditions. Proc Natl Acad Sci USA 101:3346–3351
Treubig JM, Brown PR (2002) Analysis of C60 and C70 fullerenes using high-performance liquid chromatography–Fourier transform infrared spectroscopy. J Chromatogr A 960:135–142
Viguie JR, Sukmanowski J, Nolting B, Royer FX (2007) Study of agglomeration of alumina nanoparticles by atomic force microscopy (AFM) and photon correlation spectroscopy (PCS). Colloids Surf Physicochem Eng Aspects 302:269–275
Vogl J, Heumann KG (1997) Determination of heavy metal complexes with humic substances by HPLC/ICP-MS coupling using on-line isotope dilution technique. Fresenius J Anal Chem 359:438–441
von der Kammer F (2005) Characterization of environmental colloids applying field-flow fractionation—multi detection analysis with emphasis on light scattering techniques. Hamburg University of Technology, Hamburg, p 254
von der Kammer F, Baborowski M, Friese K (2005a) Application of HPLC fluorescence detector as a nephelometric turbidity detector following field-flow fractionation to analyse size distributions of environmental colloids. J Chromatogr A 1100:81–89
von der Kammer F, Baborowski M, Friese K (2005b) Field-flow fractionation coupled to multi-angle laser light scattering detectors: applicability and analytical benefits for the analysis of environmental colloids. Anal Chim Acta 552:166–174
Waychunas GA, Kim CS, Banfield JF (2005) Nanoparticulate iron oxide minerals in soils and sediments: unique properties and contaminant scavenging mechanisms. J Nanopart Res 7:409–433
Wigginton NS, Haus KL, Hochella MF (2007) Aquatic environmental nanoparticles. J Environ Monit 9:1306–1316
Williams A, Varela E, Meehan E, Tribe K (2002) Characterisation of nanoparticulate systems by hydrodynamic chromatography. Int J Pharm 242:295–299
Wyatt PJ (1998) Submicrometer particle sizing by multiangle light scattering following fractionation. J Colloid Interface Sci 197:9–20
Yu WW, Qu L, Guo W, Peng X (2003) Experimental determination of the extinction coefficient of CdTe, CdSe, and CdS nanocrystals. Chem Mater 15:2854–2860
Acknowledgements
Hassellöv thanks the Swedish Environmental Research Council FORMAS and University of Gothenburg Nanoparticle platform for financial support. J. Readman acknowledges partial support of his contribution through the UK Natural Environment Research Council Environmental Nanoscience Initiative (Grant Reference Number: NE/E014321/1). Ranville acknowledges partial support through EPA STAR Grant RD-83332401-0
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Hassellöv, M., Readman, J.W., Ranville, J.F. et al. Nanoparticle analysis and characterization methodologies in environmental risk assessment of engineered nanoparticles. Ecotoxicology 17, 344–361 (2008). https://doi.org/10.1007/s10646-008-0225-x
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DOI: https://doi.org/10.1007/s10646-008-0225-x
Keywords
- Nanoparticles
- Nanoaggregates
- Nanometrology
- Analytical chemistry
- Particle size analysis