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“Real-world” precision, bias, and between-laboratory variation for surface area measurement of a titanium dioxide nanomaterial in powder form

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Abstract

Accurate characterization of nanomaterial properties is a critical component of any nanotoxicology testing strategy. Data that describes the performance of various laboratories in measuring the characteristics of the same nanomaterial are scarce. We conducted an inter-laboratory study to evaluate “real-world” precision and bias of specific surface area measurements using a powered material containing sub-30 nm primary crystallites. Each participant was provided a sample of NIST Standard Reference Material 1898 (Titanium Dioxide Nanomaterial) and a sample preparation and analysis protocol. Based on results from 19 laboratories, overall performance was good. Estimates of precision ranged from 0.10 to 3.96 % and measurement bias was generally within ±5 % of the certified surface area value of the material. Between-laboratory variability accounted for 91 % of the total variance and is likely explained by gravimetric errors. Reliable determination of intrinsic nanomaterial properties such as surface area will permit development of protocols for toxicity testing, verification of laboratory proficiency, and consistency in interpretation of toxicity study data.

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Notes

  1. The identification of any commercial product or trade name does not imply endorsement or recommendation by the National Institute of Standards and Technology.

  2. For gas sorption measurements, STP refers to 273.15 K or 0 °C and 101.325 kPa or 1 atm.

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Acknowledgments

The authors thank the participants of the inter-laboratory study, and acknowledge the Versailles Project on Advanced Materials and Standards (VAMAS) Technical Working Area 34, through which the study was conducted. The authors gratefully acknowledge Drs. R.F. LeBouf and M.A. Virji at NIOSH for helpful discussions on statistical programming and analysis. The author’s thank Drs. M.A. Virji at NIOSH and B. Toman in the NIST Statistical Engineering Division for insightful comments and critical review of this manuscript. The findings and conclusions in this report are those of the authors and do not necessarily represent the views of the National Institute for Occupational Safety and Health.

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Correspondence to Vincent A. Hackley.

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Hackley, V.A., Stefaniak, A.B. “Real-world” precision, bias, and between-laboratory variation for surface area measurement of a titanium dioxide nanomaterial in powder form. J Nanopart Res 15, 1742 (2013). https://doi.org/10.1007/s11051-013-1742-y

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