Chemical Characterization of Nanoparticles

Summary

The Chemical Sciences Division is helping to support nanotechnology research being conducted throughout NIST by developing and applying methods for the chemical compositional characterization of nanomaterials. Measurement capabilities being developed include the detection and quantification of nanoparticles by way of elemental signatures (for example gold or silver nanoparticles), quantification of other chemicals present in nanomaterial formulations, and techniques to distinguish between free and complexed nanoparticles or to distinguish metals present as nanoparticles from other chemical forms of the metal. The research also includes studies of the behavior of nanoparticles in analytical measurement systems.

Description

RM 8027 Silicon Nanoparticles (Nominal Diameter 2 nm)

Credit: NIST

NIST has a broad research program spread throughout the major operating units aimed at building the supporting technical capabilities that U.S. industry needs in their quest to develop new nanotech products with desirable new capabilities and bring them safely to market. The Chemical Sciences Division is developing new capabilities to provide chemical compositional characterization of nanomaterials in support of broader NIST nanotechnology research activities including the development of nanomaterial reference materials and the characterization of nanomaterial formulations being developed for cancer treatment. The latter is a collaboration between NIST and the National Cancer Institute's Nanotechnology Characterization Laboratory.

Major Accomplishments

• Neutron activation analysis of a candidate carbon nanotube reference material revealed very high levels of contamination from catalysts used to produce the materials resulting in rejection of the material as a RM.
• Isotope dilution mass spectrometric analysis of a nanoemulsion submitted by the NCI Nanotechnology Characterization Laboratory (NCI-NCL) for gadolinium content.
• Value assignment of gold, chloride, citrate, and sodium mass fractions, pH, and electrolytic conductivity in RMs 8011 through 8013, Gold Nanoparticle Reference Materials.
• Determination of cadmium concentrations in quantum dot-containing samples in collaboration with CSTL's Surface and Microanalysis Science Division.
• Analysis of tissue samples submitted by NCI-NCL for toxicological study of gold nanoparticles and the transfer of this measurement methodology to NCI-NCL for their future use.
• Development of a method based on size-exclusion chromatography with ICP-MS detection to quantitatively distinguish between free and complexed forms of gadolinium in samples submitted by NCI-NCL.

Additional Technical Details

We have been collaborating with other NIST divisions to provide chemical compositional measurements of reference materials or other types of samples under investigation. In some cases this has required the development of new methods of analysis or studies of the behavior of nanomaterials in analytical measurement systems. To provide information about the chemical form of specific nanomaterials we have coupled various chromatographic separation techniques with sensitive element-specific detection systems such as inductively coupled plasma mass spectrometry (ICP-MS). We are also developing a system that couples an ion mobility analyzer with ICP-MS as a means of separating metal-containing nanoparticles by size and as a means of distinguishing metals present as nanoparticles from those present as dissolved ions. This type of chemical information is particularly valuable for toxicological studies.

Related Product(s)

RMs 8011, 8012, and 8013 Gold Nanoparticles 

SRM 1963a, 1964 Polystyrene Spheres 

(To view the certificates for these materials, click on the RM number to be transferred to a page from which they can be accessed.) 

Associated Publications

1. Bustos, A. R. M., Murphy, K. E., and Winchester, M. R., "Evaluation of the Potential of Single Particle ICP-MS for the Accurate Measurement of the Number Concentration of AuNPs of Different Sizes and Coatings," Analytical Chemistry, 94, 3091-3102 (2022). 

2. Minelli, C., Wywijas, M., Bartczak, D., Cuello-Nunez, S., Infante, H. G., Deumer, J., Gollwitzer, C., Krumrey, M., Murphy, K. E., Johnson, M. E., Bustos, A. R. M., Strenge, I. H., Faure, B., Hoghoj, P., Tong, V., Burr, L., Norling, K., Hook, F., Roesslein, M., Kocic, J., Hendriks, L., Kestens, V., Ramaye, Y., Lopez, M. C. C., Auclair, G., Mehn, D., Gilliland, D., Potthoff, A., Oelschlagel, K., Tentschert, J., Jungnickel, H., Krause, B. C., Hachenberger, Y. U., Reichardt, P., Luch, A., Whittaker, T. E., Stevens, M. M., Gupta, S., Singh, A., Lin, F. H., Liu, Y. H., Costa, A. L., Baldisserri, C., Jawad, R., Andaloussi, S. E. L., Holme, M. N., Lee, T. G., Kwak, M., Kim, J., Ziebel, J., Guignard, C., Cambier, S., Contal, S., Gutleb, A. C., Tatarkiewicz, J., Jankiewicz, B. J., Bartosewicz, B., Wu, X. C., Fagan, J. A., Elje, E., Runden-Pran, E., Dusinska, M., Kaur, I. P., Price, D., Nesbitt, I., O'Reilly, S., Peters, R. J. B., Bucher, G., Coleman, D., Harrison, A. J., Ghanem, A., Gering, A., McCarron, E., Fitzgerald, N., Cornelis, G., Tuoriniemi, J., Sakai, M., Tsuchida, H., Maguire, C., Prina-Mello, A., Lawlor, A. J., Adams, J., Schultz, C. L., Constantin, D., Thanh, N. T. K., Tung, L., Panariello, L., Damilos, S., Gavriilidis, A., Lynch, I., Fryer, B., Quevedo, A. C., Guggenheim, E., Briffa, S., Valsami-Jones, E., Huang, Y. X., Keller, A. A., Kinnunen, V. T., Peramaki, S., Krpetic, Z., Greenwood, M., and Shard, A. G., "Versailles project on advanced materials and standards (VAMAS) interlaboratory study on measuring the number concentration of colloidal gold nanoparticles," Nanoscale, 14, 4690-4704 (2022). 

3. Zangmeister, C. D., Radney, J. G., Benkstein, K. D., and Kalanyan, B., "Common Single-Use Consumer Plastic Products Release Trillions ofSub-100 nm Nanoparticles per Liter into Water during Normal Use," Environ. Sci. Technol., 56, 5448-5455 (2022). 

4. Johnson, M. E., Bennett, J., Bustos, A. R. M., Hanna, S. K., Kolmakov, A., Sharp, N., Petersen, E. J., Lapasset, P. E., Sims, C. M., Murphy, K. E., and Nelson, B. C., "Combining secondary ion mass spectrometry image depth profiling and single particle inductively coupled plasma mass spectrometry to investigate the uptake and biodistribution of gold nanoparticles in Caenorhabditis elegans," Analytica Chimica Acta, 1175, (2021). 

5. Zangmeister, C. D., Radney, J. G., Staymates, M. E., Vicenzi, E. P., and Weaver, J. L., "Hydration of Hydrophilic Cloth Face Masks Enhances the Filtration of Nanoparticles," Acs Applied Nano Materials, 4, 2694-2701 (2021). 

6. Petersen, E. J., Bustos, A. R. M., Toman, B., Johnson, M. E., Ellefson, M., Caceres, G. C., Neuer, A. L., Chan, G., Kemling, J. W., Mader, B., Murphy, K., and Roesslein, M., "Determining what really counts: modeling and measuring nanoparticle number concentrations,"  Environmental Science-Nano, 6, 2876-2896 (2019). 

7. Bustos, A. R. M., Purushotham, K. P., Possolo, A., Farkas, N., Vladar, A. E., Murphy, K. E., and Winchester, M. R., "Validation of Single Particle ICP-MS for Routine Measurements of Nanoparticle Size and Number Size Distribution," Analytical Chemistry, 90, 14376-14386 (2018). 

8. Calderon-Jimenez, B., Johnson, M. E., Bustos, A. R. M., Murphy, K. E., Winchester, M. R., and Baudrit, J. R. V., "Silver Nanoparticles: Technological Advances, Societal Impacts, and Metrological Challenges," Frontiers in Chemistry, 5, (2017). 

9. Johnson, M., Hanna, S., Bustos, A. M., Sims, C., Elliott, L., Lingayat, A., Johnston, A., Nikoobakht, B., Elliott, J., Holbrook, D., Scott, K., Murphy, K., Petersen, E., Yu, L., and Nelson, B., "Separation, sizing, and quantitation of engineered nanoparticles in an organism model using inductively coupled plasma mass spectrometry and image analysis," Abstracts of Papers of the American Chemical Society, 253, (2017). 

10. Liu, J. Y., Murphy, K. E., Winchester, M. R., and Hackley, V. A., "Overcoming challenges in single particle inductively coupled plasma mass spectrometry measurement of silver nanoparticles," Analytical and Bioanalytical Chemistry, 409, 6027-6039 (2017). 

11. Liu, W. Y., Mahynski, N. A., Gang, O., Panagiotopoulos, A. Z., and Kumar, S. K., "Directionally Interacting Spheres and Rods Form Ordered Phases," Acs Nano, 11, 4950-4959 (2017). 

12. Pitkanen, L., Bustos, A. R. M., Murphy, K. E., Winchester, M. R., and Striegel, A. M., "Quantitative characterization of gold nanoparticles by size-exclusion and hydrodynamic chromatography, coupled to inductively coupled plasma mass spectrometry and quasi-elastic light scattering," Journal of Chromatography A, 1511, 59-67 (2017). 

13. Sims, C. M., Hanna, S. K., Heller, D. A., Horoszko, C. P., Johnson, M. E., Bustos, A. R. M., Reipa, V., Riley, K. R., and Nelson, B. C., "Redox-active nanomaterials for nanomedicine applications," Nanoscale, 9, 15226-15251 (2017). 

14. El Hadri, H., Petersen, E. J., and Winchester, M. R., "Impact of and correction for instrument sensitivity drift on nanoparticle size measurements by single-particle ICP-MS," Analytical and Bioanalytical Chemistry, 408, 5099-5108 (2016). 

15. Pitkanen, L. and Striegel, A. M., "Size-exclusion chromatography of metal nanoparticles and quantum dots," Trac-Trends in Analytical Chemistry, 80, 311-320 (2016). 

16. Bustos, A. R. M., Petersen, E. J., Possolo, A., and Winchester, M. R., "Post hoc Interlaboratory Comparison of Single Particle ICP-MS Size Measurements of NIST Gold Nanoparticle Reference Materials," Analytical Chemistry, 87, 8809-8817 (2015). 

17. Davis, C. S., Grolman, D. L., Karim, A., and Gilman, J. W., "What do we still need to understand to commercialize cellulose nanomaterials?," Green Materials, 3, 53-58 (2015). 

18. Liu, J. Y., Murphy, K., Hackley, V., and Winchester, M., "Evaluation and improvement of sample preparation protocols for the single particle ICP-MS measurement of silver nanoparticles,"  Abstracts of Papers of the American Chemical Society, 250, (2015). 

19. Liu, J. Y., Murphy, K. E., MacCuspie, R. I., and Winchester, M. R., "Capabilities of Single Particle Inductively Coupled Plasma Mass Spectrometry for the Size Measurement of Nanoparticles: A Case Study on Gold Nanoparticles," Analytical Chemistry, 86, 3405-3414 (2014). 

20. Elzey, S., Tsai, D. H., Yu, L. L., Winchester, M. R., Kelley, M. E., and Hackley, V. A., "Real-time size discrimination and elemental analysis of gold nanoparticles using ES-DMA coupled to ICP-MS," Analytical and Bioanalytical Chemistry, 405, 2279-2288 (2013). 

21. Elzey, S., Tsai, D. H., Rabb, S. A., Yu, L. L., Winchester, M. R., and Hackley, V. A., "Quantification of ligand packing density on gold nanoparticles using ICP-OES," Analytical and Bioanalytical Chemistry, 403, 145-149 (2012). 

22. Elzey, S., Tsai, D. H., Rabb, S., Yu, L., Winchester, M., and Hackley, V., "Quantification of thiolated surface species on gold nanoparticles using ICP-OES and ICP-MS," Abstracts of Papers of the American Chemical Society, 243, (2012). 

23. Zaluzhna, O., Zangmeister, C., and Tong, Y. Y. J., "Synthesis of Au and Ag nanoparticles with alkylselenocyanates," Rsc Advances, 2, 7396-7399 (2012). 

24. Allison, T. C. and Tong, Y. J., "Evaluation of methods to predict reactivity of gold nanoparticles," Physical Chemistry Chemical Physics, 13, 12858-12864 (2011). 

25. Park, I. S., Xu, B. L., Atienza, D. O., Hofstead-Duffy, A. M., Allison, T. C., and Tong, Y. J., "Chemical State of Adsorbed Sulfur on Pt Nanoparticles," Chemphyschem, 12, 747-752 (2011). 

26. Rincon, L., Hasmy, A., Marquez, M., and Gonzalez, C., "A perturbatively corrected tight-binding method with hybridization: Application to gold nanoparticles," Chemical Physics Letters, 503, 171-175 (2011). 

27. Zaluzhna, O., Li, Y., Zangmeister, C., and Tong, Y. Y. J., "Characterization and interface study of the alkaneselenolate-protected gold nanoparticles synthesized from the organic selenocyanates," Abstracts of Papers of the American Chemical Society, 241, (2011). 

28. Lang, B., "Hybridization thermodynamics of DNA bound to gold nanoparticles," Journal of Chemical Thermodynamics, 42, 1435-1440 (2010). 

29. Winchester, M. R., Sturgeon, R. E., and Costa-Fernandez, J. M., "Chemical characterization of engineered nanoparticles," Analytical and Bioanalytical Chemistry, 396, 951-952 (2010). 

30. Zaluzhna, O., Li, Y., Zangmeister, C. D., and Tong, Y. Y., "Attachment chemistry between gold nanoparticles and chalcogen-containing alkyl ligands," Abstracts of Papers of the American Chemical Society, 238, (2009). 

31. Jahn, A., Reiner, J. E., Vreeland, W. N., Devoe, D. L., Locascio, L. E., and Gaitan, M., Preparation of nanoparticles by continuous-flow microfluidics," Journal of Nanoparticle Research, 10, 925-934 (2008).