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Standardizing Nanomaterials
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ACS Nano

Cite this: ACS Nano 2016, 10, 11, 9763–9764
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https://doi.org/10.1021/acsnano.6b07629
Published November 22, 2016

Copyright © 2016 American Chemical Society. This publication is available under these Terms of Use.

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One of the greatest challenges in materials science is determining how best to characterize the increasing numbers of complex structures and materials being created by chemists, physicists, and engineers. Without agreed upon methods of characterization, both reproducibility and quality control are rendered impossible, and the impact of the entire field is endangered by the inability to replicate data, syntheses, and properties. Where these properties are to be applied, in catalysis, energy conversion, photonics, sensors, and elsewhere, or modeled and understood with theory and simulation, having standards of characterization would enable better connections between laboratories and between synthesis, understanding, and application. While the incredible diversity of materials that can be created by molecular synthesis is one of the most appealing aspects of the field, this panorama of possibilities also poses challenges.

The field of organic chemistry has long had highly established methods for characterizing new chemical compounds, and refining those processes and protocols has been going on for close to a century. Conversely, the global fascination with nanoscale materials has not been accompanied by the same degree of rigor, and the nanomaterials community has been much slower to standardize characterization procedures and requirements.

In an update on methods for organic compound characterization in 1952, Peck and Gale pointed out that “The accepted requirements for full characterization of an organic compound include establishment of purity of sample, determination, of physical properties, determination of elementary composition, functional groups, and empirical formula, and elucidation of structural formula and spatial relationships.” (1) This thought was written well over half a century ago, but few papers on nanoscale materials today would meet these ideal requirements.

It is now time for the nanomaterials community to consolidate and to agree on methods of characterization and minimum levels of analysis of materials.

One reason for this situation is that nanoscale materials are often fabricated or synthesized in different ways, sometimes by biologists, sometimes by physicists or engineers, and of course also by chemists. Each group has preferred processes and methods. Different dimensions, compositions, and structural hierarchies are involved, and materials may be amorphous, composite, or polycrystalline. Another issue is that nanoscale materials may be formed as thin films, dry powders, or solution-dispersed materials. Common characterization methods are neither obvious nor applicable to all different classes of nanomaterials. We note that protein chemists faced with the analogous difficulties of characterization recognized and agreed on the need for the arduous process of protein crystallization in order to carry out X-ray diffraction of protein structures.

It is now time for the nanomaterials community to consolidate and to agree on methods of characterization and minimum levels of analysis of materials. These methods and analyses may need to be updated as Peck and Gale did in their review, but systematic procedures and protocols recognized and demanded by research journals would create well-defined benchmarks for the field.

A further benefit of prescribed characterization methods and reporting of properties is a dramatic reduction in the duplication of known synthetic steps in manuscripts. Many manuscripts reproduce well-understood procedures as part of the research outcomes, whereas they are really part of the everyday workload of the chemist. Many figures and outcomes from research could readily be relegated to Supporting Information sections, as is common in organic chemistry, where absorption spectra, nuclear magnetic resonance (NMR) spectra, X-ray data, and infrared (IR) spectra are routinely carried out but are subsumed into the SI for the interested reader.

A further benefit of prescribed characterization methods and reporting of properties is a dramatic reduction in the duplication of known synthetic steps in manuscripts.

A further consequence of this lack of rigor has been the use of “chemicals as supplied”. This route has actually slowed down research in some cases since it has turned out that impurities in solvents such as trioctylphosphine oxide (TOPO) or surfactants such as cetrimonium bromide (CTAB) had significant and dominating effects on the outcomes of chemical reactions. (2) Poor characterization and lack of purification meant that it took considerable time for these problems to be recognized. Inorganic chemists tended to focus on characterization of the inorganic materials under investigation with the result that organic chemical effects were often not recognized.

The American Chemical Society (ACS) publishes the broadest range of chemistry research across the globe. Many ACS journals publish manuscripts on complex materials. It is appropriate to consider creating a prescribed or expected set of characterization requirements for publication that takes into account the nature of modern chemical research into complex nanomaterials and the wide range of new tools available for characterization such as scanning probe and electron microscopy. Having authors put more basic characterization into Supporting Information would allow them to focus on the novelty of their research. Thereby, we may define suitable benchmarks for publication within the ACS journals.

Due to the larger variety of nanomaterials, there is not one single characterization method for all materials. Often, for the characterization of certain properties, several similar or methodologies exist that give similar or related information. Concerning structural properties of nanomaterials, transmission electron microscopy (TEM), scanning electron microscopy (SEM), scanning tunnelling microscopy (STM), atomic force microscopy (AFM), electron diffraction pattern, X-ray diffraction (XRD), NMR, Fourier-transformed IR spectroscopy (FTIR), thermal gravimetry analysis (TGA), quartz crystal microbalance (QCM), inductively coupled plasma mass spectrometry (ICP-MS), elemental analysis, etc. are standard techniques. For nanomaterials dispersed in solvent, colloidal properties should also be investigated, in the solvent in which the nanomaterials will be applied. Typical characterization methods include dynamic light scattering (DLS), fluorescence correlation spectroscopy (FCS), titration against salt and pH, absorption spectroscopy, column chromatography, gel electrophoresis, etc. Where the sizes of the nanomaterials in solvent are bigger than the structural sizes, agglomeration has most likely occurred. Notably, there is also not only one “size” for nanomaterials, but different methods will lead to different “types” of sizes. (3) For fluorescent nanomaterials, optical characterization should be performed, such as ultraviolet/visible absorption spectra, fluorescence spectra, determination of quantum yield, etc. The nature of the respective study will largely determine which are the best characterization techniques to apply. However, using standard characterization is a good way to benchmark “new” nanomaterials against existing ones.

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  • Corresponding Author
    • Paul S. Weiss,  Editor-in-Chief
  • Authors
    • Paul Mulvaney,  Associate Editor
    • Wolfgang J. Parak,  Associate Editor
    • Frank Caruso,  Associate Editor, Chemistry of Materials
  • Notes
    Views expressed in this editorial are those of the authors and not necessarily the views of the ACS.

References

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This article references 3 other publications.

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    Detoxification of Gold Nanorods by Treatment with Polystyrenesulfonate
    Leonov, Alexei P.; Zheng, Jiwen; Clogston, Jeffrey D.; Stern, Stephan T.; Patri, Anil K.; Wei, Alexander
    ACS Nano (2008), 2 (12), 2481-2488CODEN: ANCAC3; ISSN:1936-0851. (American Chemical Society)
    We address an outstanding issue assocd. with the biocompatibility of gold nanorods (GNRs), a promising agent for biomedical imaging and theragnostics. GNRs are typically prepd. in the presence of cetyltrimethylammonium bromide (CTAB), a cationic surfactant whose rigorous removal is necessary due to its cytotoxicity and membrane-compromising properties. CTAB-stabilized GNRs can be partially purified by treatment with polystyrenesulfonate (PSS), an anionic polyelectrolyte often used as a surrogate peptizing agent, followed by chloroform extn. and ultrafiltration with minimal loss of dispersion stability. However, in vitro cytotoxicity assays of PSS-coated GNRs revealed IC50 values in the low to submicromolar range, with subsequent studies indicating the source of toxicity to be assocd. with a persistent PSS-CTAB complex. Further exchange of CTAB-laden PSS with fresh polyelectrolyte greatly improves biocompatibility, to the extent that 85 μg/mL of "CTAB-free" GNRs (the highest level evaluated) has comparable toxicity to a std. phosphate buffer soln. Ironically, PSS is not effective by itself at stabilizing GNRs in CTAB-depleted suspensions: while useful as a detergent for GNR detoxification, it should be replaced by more robust coatings for long-term stability under physiol. conditions.
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    Size Determination of (Bio)conjugated Water-Soluble Colloidal Nanoparticles: A Comparison of Different Techniques
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    Journal of Physical Chemistry C (2007), 111 (31), 11552-11559CODEN: JPCCCK; ISSN:1932-7447. (American Chemical Society)
    The size of inorg. colloidal nanoparticles coated with org. layers of different thickness was measured with different techniques, including TEM, gel electrophoresis, size exclusion chromatog., fluorescence correlation spectroscopy, and thermophoresis. The results are critically compared, and the advantages and disadvantages of the resp. methods are discussed.
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  • References

    This article references 3 other publications.

    1. 1
      Peck, R. L.; Gale, P. H. Characterization of Organic Compounds Anal. Chem. 1952, 24, 116– 120 DOI: 10.1021/ac60061a022
      There is no corresponding record for this reference.
    2. 2
      Leonov, A. P.; Zheng, J.; Clogston, J. D.; Stern, S. T.; Patri, A. K.; Wei, A. Detoxification of Gold Nanorods by Treatment with Polystyrenesulfonate ACS Nano 2008, 2, 2481– 2488 DOI: 10.1021/nn800466c
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      Detoxification of Gold Nanorods by Treatment with Polystyrenesulfonate
      Leonov, Alexei P.; Zheng, Jiwen; Clogston, Jeffrey D.; Stern, Stephan T.; Patri, Anil K.; Wei, Alexander
      ACS Nano (2008), 2 (12), 2481-2488CODEN: ANCAC3; ISSN:1936-0851. (American Chemical Society)
      We address an outstanding issue assocd. with the biocompatibility of gold nanorods (GNRs), a promising agent for biomedical imaging and theragnostics. GNRs are typically prepd. in the presence of cetyltrimethylammonium bromide (CTAB), a cationic surfactant whose rigorous removal is necessary due to its cytotoxicity and membrane-compromising properties. CTAB-stabilized GNRs can be partially purified by treatment with polystyrenesulfonate (PSS), an anionic polyelectrolyte often used as a surrogate peptizing agent, followed by chloroform extn. and ultrafiltration with minimal loss of dispersion stability. However, in vitro cytotoxicity assays of PSS-coated GNRs revealed IC50 values in the low to submicromolar range, with subsequent studies indicating the source of toxicity to be assocd. with a persistent PSS-CTAB complex. Further exchange of CTAB-laden PSS with fresh polyelectrolyte greatly improves biocompatibility, to the extent that 85 μg/mL of "CTAB-free" GNRs (the highest level evaluated) has comparable toxicity to a std. phosphate buffer soln. Ironically, PSS is not effective by itself at stabilizing GNRs in CTAB-depleted suspensions: while useful as a detergent for GNR detoxification, it should be replaced by more robust coatings for long-term stability under physiol. conditions.
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    3. 3
      Sperling, R. A.; Liedl, T.; Duhr, S.; Kudera, S.; Zanella, M.; Lin, C.-A. J.; Chang, W. H.; Braun, D.; Parak, W. J. Size Determination of (Bio-) Conjugated Water-Soluble Colloidal Nanoparticles: A Comparison of Different Techniques J. Phys. Chem. C 2007, 111, 11552– 11559 DOI: 10.1021/jp070999d
      3
      Size Determination of (Bio)conjugated Water-Soluble Colloidal Nanoparticles: A Comparison of Different Techniques
      Sperling, R. A.; Liedl, T.; Duhr, S.; Kudera, S.; Zanella, M.; Lin, C.-A. J.; Chang, W. H.; Braun, D.; Parak, W. J.
      Journal of Physical Chemistry C (2007), 111 (31), 11552-11559CODEN: JPCCCK; ISSN:1932-7447. (American Chemical Society)
      The size of inorg. colloidal nanoparticles coated with org. layers of different thickness was measured with different techniques, including TEM, gel electrophoresis, size exclusion chromatog., fluorescence correlation spectroscopy, and thermophoresis. The results are critically compared, and the advantages and disadvantages of the resp. methods are discussed.
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      https://chemport.cas.org/services/resolver?origin=ACS&resolution=options&coi=1%3ACAS%3A528%3ADC%252BD2sXns1ens7g%253D&md5=0f42edd02fe41e3a6959c3c7753817aa