Toxicity dose descriptors from animal inhalation studies of 13 nanomaterials and their bulk and ionic counterparts and variation with primary particle characteristics

Figures & data

Table 1. Explanation of the columns in the Excel data library.

Column number	Title of column	Description
A	Number [can be used to reset the database after sorting by other columns]	This field can be used to reset the data library if the user has sorted the data based on other columns
B	Substance primary	This gives a description of the material by chemical element name and forms the basis of the alphabetical ordering of the materials
C	Literature reference (journal given in cases where each author has more articles per year)	The references are given as the first author’s last name followed by the year of publication. In the case of multiple publications from the same first author, the journal name is also given. The exact literature references can be found in the results section of this article, and thus also in the reference list
D	Product name	This can be used to identify products of interest
E	Companies and manufacturers, collection points, synthesized	Information on companies and manufacturers that delivered the material. Collection points and synthesized explains whether the materials were collected or synthesized
F	Material synthesized or collected by authors of the specific article?	Is given as a yes/no answer to provide information on whether the material was synthesized by the authors
G	Diameter (min) [nm]	This is the minimum reported diameter of the pristine material. For carbon nanotubes, this describes the diameter
H	Used size (nm) (diameter for particle and length for fibers) (ions are set to 0.3 for inclusion on graphs)	The diameter of the primary particles we applied in the graphical depictions. Except for fibers where the length was applied as this was considered to have the greatest impact on toxicity (Poland et al. 2012).
		For graphene the size was estimated on the basis of TEM pictures measured lengthwise (Han et al. 2015).
		For ions, the size was set to 0.3 nm based on the average size of an atom.
		If a particle size was reported as a range, a mean value was calculated, based on the mean of the lower and higher range.
		If only a smaller than (<) size was given, the maximum size was used.
		If particle size (or surface area) was not reported in the retrieved paper but had been characterized in another article (e.g. the silica DQ12 particle, the carbon black Elftex-12 Furnace Black, the carbon black Printex-90, and the carbon nanotube MWCNT-7), the size reported in the cited publication was used.
		For plates (graphene), the size was based on TEM pictures.
I	M-size d(minimum) (nm)	Size determined by microscopy (M is an abbreviation of microscopy)
J	M size d(maximum) (nm)	Size determined by microscopy
K	M-size d(length) (nm)	Size determined by microscopy
L	Count Mean d (nm)	–
M	Number of particles measured	–
N	XRD-size	Crystallite size as derived based on powder X-ray diffraction data
O	Apparatus for measurement	–
P	Crystal structure	–
Q	Phase	–
R	Shape	–
S	Specific surface area (m^2/g)	The sspecific surface area given in the articles
T	Agglomerated/aggregate size (nm) and reported	–
U	Size notes	–
V	GMD (nm)	Geometric Mean Diameter
W	GSD (nm)	Geometric Standard Deviation
X	CMAD (nm)	Count Median Aerodynamic Diameter
Y	Exposure particle size (nm)	Exposure size by the given method
Z	Notes on exposure particle size	–
AA	Surface chemical modification	Nanomaterials were pristine in the sense that only materials composed of one material were included. We provided an entry to confirm this and allow notes on detected impurities
AB	Mode of exposure	Noted as inhal as an abbreviation of inhalation
AC	Animal species	The animal species name is given
AD	Dose and information on exposure duration	Details are provided on the exposure level and duration
AE	Cumulative exposure duration (hours)	To calculate a cumulative dose the cumulative exposure duration is reported
AF	NOAEC neutrophils in BAL (mg/m^3)	–
AG	LOAEC neutrophils in BAL (mg/m^3)
AH	Recovery time from end of exposure until BAL was collected	–
AI	NOAEC genotoxicity/ carcinogenicity (mg/m^3)	The retrieved number is given
AJ	LOAEC genotoxicity/ carcinogenicity (mg/m^3)	The retrieved number is given
AK	Genotoxicity/carcinogenicity endpoint description	The used endpoint is described
AL	T25: potential for calculation of this value?	We evaluated whether the data were sufficient to calculate a T25
AM	T25 (mg/kg bw/day) [calculated by us directly based on the specific articles]	The calculation of this dose descriptor is described in a designated section below
AN	T25 (mg/m^3) based on 8 hours of inhalation 5 days per week	The calculation of this dose descriptor is described in a designated section below
AO	NOAEC neutrophils in BAL (cm^2/m^3)	This gives the dose descriptor based on dosed particle surface area
AP	LOAEC neutrophils in BAL (cm^2/m^3)	This gives the dose descriptor based on dosed particle surface area
AQ	NOAEC genotoxicity/ carcinogenicity (cm^2/m^3)	This gives the dose descriptor based on dosed particle surface area
AR	LOAEC genotoxicity/carcinogenicity (cm^2/m^3)	This gives the dose descriptor based on dosed particle surface area

Figure 1. Overview of content and placement of graphs for each material in the data library.

Table 2. Literature references used in the Excel data library and for graphs.

Material	Literature references
Silver (Ag)	(Braakhuis et al. 2014; Kwon et al. 2012a; Roberts et al. 2013; Seiffert et al. 2016; Sung et al. 2008)
Carbon black (CB)	(Driscoll et al. 1996; Elder et al. 2005; Gallagher et al. 2003; Heinrich et al. 1995; Henderson et al. 1992; Jackson et al. 2012; Ma-Hock et al. 2013; Mauderly et al. 1994; Saber et al. 2005; Wolff et al. 1990)
Carbon nanotubes (CNT)	(Mitchell et al. 2007; Shvedova et al. 2008; Pauluhn 2010; Kim et al. 2012; Porter et al. 2013; Ma-Hock et al. 2013; Mercer et al. 2013; Rydman et al. 2014; Sargent et al. 2014; Pothmann et al. 2015; Kasai et al. 2015; 2016; Catalan et al. 2016; Kinaret et al. 2017; Francis et al. 2018)
Graphene	(Ma-Hock et al. 2013; Han et al. 2015; Shin et al. 2015; Kim et al. 2018)
Cerium oxide (CeO2)	(Srinivas et al. 2011; Demokritou et al. 2013; Aalapati et al. 2014; Gosens et al. 2014; Keller et al. 2014; Larsen et al. 2016; Cordelli et al. 2017; Schwotzer et al. 2017)
Cobalt compounds (Co)	(Wehner et al. 1977; Wehner, Stuart, Sanders et al. 1979; Johansson, Curstedt, and Camner 1991; Johansson et al. 1992; Bucher et al. 1999; Behl et al. 2015; Sisler et al. 2016)
Copper compounds (Cu)	(Adamcakova-Dodd et al. 2015; Areecheewakul et al. 2022)
Iron compounds (Fe)	(Warheit et al. 1997; Zhou et al. 2003; Pauluhn 2009; Srinivas et al. 2012; Sutunkova et al. 2016)
Nickel compounds (Ni)	(Sunderman and Donnelly 1965; Wehner et al. 1975; Wehner, Moss, Milliman, Dagle, and Schirmer et al. 1979; Horie et al. 1985; Johansson et al. 1992; Dunnick et al. 1995; NTP 1996; Oller et al. 2008; Sutunkova et al. 2019; Katsnelson et al. 2021)
Silicium compounds (Si)	(Warheit, McHugh, and Hartsky 1995; Muhle et al. 1995; Johnston et al. 2000; Porter et al. 2002, 2004; Arts et al. 2007; Chen et al. 2008; Rossi, Pylkkanen, Koivisto, Vippola, et al. 2010; Sayes et al. 2010; Umbright et al. 2017; Shin et al. 2017; Brandão et al. 2021)
Titanium dioxide (TiO2)	(Lee, Trochimowicz, and Reinhardt 1985; Muhle et al. 1995; Heinrich et al. 1995; Warheit et al. 1997; Bermudez et al. 2002, 2004; Ma-Hock et al. 2009; Rossi, Pylkkanen, Koivisto, Nykasenoja, et al. 2010; Rossi, Pylkkanen, Koivisto, Vippola, et al. 2010; Noel et al. 2012; Kwon et al. 2012b; Lindberg et al. 2012; Baisch et al. 2014; Leppänen et al. 2015; Larsen et al. 2016; Brandão et al. 2021; Yamano et al. 2022a; Yamano et al. 2022b)
Zinc compounds (Zn)	(Conner et al. 1988; Ho et al. 2011; Adamcakova-Dodd et al. 2014; Chuang et al. 2014; Chen et al. 2015; Larsen et al. 2016; Huang et al. 2019)

Figure 2. Specific surface area as function of primary particle size. Specific surface area was plotted as function of size for nanomaterials included in the data library for which the information was available. For spherical nanomaterials, the size is presented as diameter (A and B). For carbon nanotubes, the size is presented as either length (C), diameter (D), or aspect ratio (E). For graphene, the size is presented as the length of the edge (lateral size) (F). P values are from the linear regression F-test to test if the slope was significantly non-zero.

Figure 3. Silver (Ag) dose descriptors.

Figure 4. Carbon black (CB) dose descriptors.

Figure 5. Carbon nanotubes (CNT) dose descriptors and length of the tubes.

Figure 6. Carbon nanotubes (CNT) dose descriptors and diameter of the tubes.

Figure 7. Graphene dose descriptors.

Figure 8. Cerium (CeO₂) dose descriptors.

Figure 9. Cobalt (Co) dose descriptors. The data are on CoO compounds, unless otherwise indicated on the graphs with italics.

Figure 10. Copper (Cu) dose descriptors.

Figure 11. Iron (Fe) dose descriptors. The data are on iron oxides, unless otherwise indicated on the graphs with italics.

Figure 12. Nickel (Ni) dose descriptors. The data are on NiO compounds, unless otherwise indicated on the graphs with italics.

Figure 13. Silica amorphous (Si amorphous) dose descriptors.

Figure 14. Quartz dose descriptors.

Figure 15. Titanium dioxide (TiO₂) dose descriptors.

Figure 16. Zinc (Zn) dose descriptors.

Figure 17. Graphical presentation of T25s calculated based on chronic inhalation studies included in the data library. CNT size for Kasai et al. 2016 depicted as length (diameter 74 nm). The upper panel shows T25s as mg/kg bw/day and the lower panel shows T25s as exposure air concentrations (mg/m³).

Figure 18. Linear regression of dose descriptors (NOAEC and LOAEC) expressed as mass concentration as function of study duration for all materials taken together. The P values for the F-test testing of whether the slope is significantly non-zero are inserted next to the legends.

Figure 19. Linear regression showing dose descriptors expressed as surface area exposure as function of study duration for all materials taken together. The unit on the X-axis is logarithm base 10 (hours). P values for the F-test testing if the slope is significantly non-zero are inserted next to the legends.

Figure 20. Linear regression of NOAEC and LOAEC for all materials taken together with dose descriptors expressed as cumulative inhaled dose as function of material size or mass median aerodynamic diameter. A shows all spherical particles, B ions and all spherical particles, C only nanoparticles with a diameter of less than 100 nm, D all materials except carbon nanotubes and graphene with mass median aerodynamic diameter (MMAD) on the x-axis. The P values for the F-test testing if the slope is significantly non-zero are inserted next to the legends. For studies where administration was in ionic form, we subtracted the molecular mass of accompanying salts from the administered mass. For particles and bulk materials consisting of oxides, we did not subtract the mass of oxygen.

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Data availability statement

The data that support the findings of this study are openly available are available in the Supplemental materials and on the Nanosafer website at www.nanosafer.org