SWCNT-1: Single-Wall Carbon Nanotube Certified Reference Material

This Certified Reference Material is primarily intended for use in the validation of procedures and development of methods for the determination of trace metals in carbon nanotubes or those of a similar matrix. It has been gamma sterilized to support studies of environmental health and safety and nanotoxicology. SWCNTs have been identified as an engineered nanomaterial for which thorough characterization is needed for assessments of environmental, health and safety testing. Parameters of interest include elemental/molecular composition, specific surface area, surface chemistry, particle size and distribution, morphology/shape/form, surface charge and crystal structure, amongst other variables. SWCNT-1 serves as a stable and homogeneous representative test material to foster development and validation of international consensus-based standards to further rigorous physico-chemical characterization of such materials.

A unit of SWCNT-1 CRM consists of a bottle containing nominally 100 mg of SWCNT material under an argon atmosphere.

Table 1 summarizes those trace metals for which certified values have been established for this material. The expanded uncertainty (UCRM) in the certified value is equal to UCRM = kuc where uc is the combined standard uncertainty calculated according to the JCGM Guide and k is the coverage factor. It is intended that UCRM accounts for every aspect that reasonably contributes to the uncertainty of the measurement. A coverage factor of 2 was applied for all elements. The table below lists certified values for SWCNT-1, expressed on a dry mass basis.

Table 1: Certified Mass Fraction Values for SWCNT-1

Element Mass fraction Units
Co (a,b) 15.9 ± 1.0 g/kg
Ni (b,c) 14.4 ± 0.8 g/kg
Mo (b,c) 7.3 ± 1.1 g/kg
Fe (b,c) 2.2 ± 0.2 g/kg
Pb (c) 6.8 ± 0.9 mg/kg
Hg (c) < 10 Table 1 note a mg/kg

Table notes

Table 1 note a

For the purposes of uncertainty propagation, this value (x) could be interpreted as x/2 ± x/(2√3) where the uncertainty value is derived assuming a rectangular (uniform) distribution within the interval 0 to x.

Return to table 1 note a referrer

Coding

  • a - inductively coupled plasma mass spectrometry; quantitation by method of additions
  • b - instrumental neutron activation analysis
  • c - isotope dilution inductively coupled plasma mass spectrometry

Table 2: Reference Mass Fraction Values for SWCNT-1

Element Mass Fraction Table 2 note a Units
Al 494 ± 94 mg/kg
Au 0.139 ± 0.017 mg/kg
B 107.3 ± 3.1 mg/kg
Ca 2650 ± 300 mg/kg
Cr 285 ± 26 mg/kg
H 423 ± 0.990 mg/g
K 3220 ± 200 mg/kg
La 0.96 ± 0.27 mg/kg
Mn 135.8 ± 1.8 mg/kg
Na 167 ± 7 mg/kg
Ti 193 ± 22 mg/kg
V 4.37 ± 0.31 mg/kg

Table notes

Table 2 note a

Uncertainty is an expanded uncertainty (k = 2) about the mean (n = 4) calculated by combining between-method and within-method variances following. A comprehensive description of the methodologies and comparison of individual results is available.

Return to table 2 note a referrer

Table 3 : Reference Value for Specific Surface Area of SWCNT-1

Surface area Table 3 note a Units
329 ± 6 Table 3 note b m2/g

Table notes

Table 3 note a

Average adsorbate (nitrogen) area per molecule of 0.162 nm2 used for the determination. Expanded uncertainty (k = 2), based on 3 replicate determinations.

Return to table 3 note a referrer

Table 3 note b

Dry mass basis

Return to table 3 note b referrer

Table 4: Reference Thermogravimetry-Derived Values for SWCNT-1

Parameter
Oxidation temperature
Value Table 4 note a Units
Peak 1 502.9 ± 1.2 °C
Peak 2 602.7 ± 0.9 °C
Residual mass Table 4 note b 83.0 ± 5.8 mg/g

Table notes

Table 4 note a

Expanded uncertainty calculated as U = k (standard deviation divided by square root of 21) for k = 2 based on replicate measurement cycles undertaken over a period of 4 months on fresh and "aged" samples.

Return to table 4 note a referrer

Table 4 note b

Dry mass basis.

Return to table 4 note b referrer

Table 5: Reference G/D Raman Peak Ratio for Excitation of SWCNT-1 at 514.5 nm

G/D Ration Table 5 note a
49.1 ± 4.8

Table notes

Table 5 note a

Mean of peak heights of 13 determinations conducted over an 18 month stability study at NRC. Expanded uncertainty is calculated as U = k(standard deviation divided by square root of 13) for k = 2.

Return to table 5 note a referrer

Table 6: RBM-Derived Nanotube Diameter

Tube diameter Table 6 note a, nm
1.5 ± 0.2 Table 6 note b

Table notes

Table 6 note a

Calculated following : ωRBM = 234/d + 10; TEM imaging provides 1.5 ± 0.2 nm (n = 54) and AFM imaging provides a height of 1.5 nm (n = 3).

Return to table 6 note a referrer

Table 6 note b

Expanded uncertainty calculated as U=k(standard deviation divided by square root of 17)
for k = 2 based on RBM frequencies in the range 125 – 225 cm-1 excited with 514.5, 632.8 and 785 nm sources.

Return to table 6 note b referrer

Date of issue: June, 2013
Date of expiry: June, 2023
Revised: March 2016 (editorial update), March 2018 (date of expiry extended and Mg value removed from table 2)

Date modified: