DD ISO/TS 13278 pdf download – Nanotechnologies — Determination of elementalimpurities in samples ofcarbon nanotubes using inductively coupled plasmamass spectrometry.
4.3 Reagents
4.3.1 General
All reagents should be prepared and stored in polytetrafluoroelhylene (PTFE) containers precleaned by nitnc acid and ultrapure water. Precleaned containers made from polypropylene. quartz, or other matenals may also be suitable
4.3.2 Purity of adds
Ultra high purity acids (e.g. HNO. guaranteed reagent or equivalent grade) shall be used for sample dissolution
and preparation of calibration standards.
4.3.3 Purity 01 reagents
Guaranteed grade chemicals (99,99% or higher than 99,99 %) shall be used in all tests (e.g. H202. guaranteed reagent or equivalent grade) Certified reference materials should be used whenever available,
4.3.4 Purity of water
Ultrapure water having a resistivity of at least 18 MO cm shall be used in all tests.
4.4 Stock solutions
4.4.1 General
Stock solutions may be obtained directly as multi-element standards Iron, accredited cnrritaL,Il 1iuu Lii national metrology institutes as certified reference materials. They may also be prepared from single element standards or suitable starting materials in-house, although this can be difficult due 10 problems with cross- contamination. The following stock solutions shall be available for calibration of the Instrument. The purity of starling matenals should be assessed.
4.4.2 ICP-MS calibration standard stock solution No. 1
1 000 mgtl of each element (Ca, Ce. Gd, Ge. Hg, La. Li, Sb. Sm. TI. W. Yb) In 10 vol% HNO3 (1,6 molIl HNO3) in water.
4.4.3 ICP-MS calibration standard stock solution No. 2
100 mgil of each element (As, B, Be, Fe, Se, Zn)in 1,6 moUl HNO3 in waler,
4.4.4 ICP-MS calibration standard stock solution No. 3
10 mgll of each element (Ag, Al, Ba, Bi. Cd. Co. Cr, Cu, Ga, K, Li, Mg, Mn, Mo, Na. Ni, Pb, Rb. Sr. Te. TI. U, V) in 1,6 molll HNO3 in water,
NOTE The working standard shod be prepared daily.
4.5 Stock spike solutions
4.5.1 General
Multi-element spike standards are available from commercial vendors and national metrology institutes Alternatively, stock solutions of multi-element spike standards may be prepared wi-house giving due consideration to the purity of water and acids. The loltowing stock spde solutions shall be available.
5 Apparatus
Use an ICP-MS instrument with a quadrupole or sector field mass spectrometer, or another type of ICPMS instrument operating with at least I u (atomic mass unit) resolution for mule-element determinations. It is recommended that CCT or DRC technology[I413J[141sJ1e be used, if avadable, to efficiently remove or minimize spectral interferences.
6 Sample pretreatment
6.1 Sample preparation for ICP-MS analysis
Harmonizing sample preparation procedures by using a protocol such as that described in References (121 end [14J contributes to the quality of measurements by improving repeatabdity, reproducibility and reliability. This in turn ensures that measurement results can be compared with those generated in other laboratones. Given that different laboratories might have different types of sample preparation equipment It is helpful to provide more than one option for pretreatment of CNTs. Three different sample pretreatment methods, which can be found in Reference (12J, are described here. These include wet digestion under high pressure, a combination of dry ashong with wet digestion, and a microwave-assisted sample preparation for dissolution of elemental impunties In the CNT samples before ICP-MS analysis. These methods have been shown to provide reliable and reproducible measurement results using ICP-MSI12). They are all equivalent. Among the three procedures described, the appropriate choice for a particular laboratory can be made on the basis of the available equipment or other laboratory-specific factors, as well as a consideration of possible sample effects If elements of high volatility that are subject to thermal losses, such as Hg. Se, and As. are to be determined, then samples shall be digested usmg closed microwave-assisted acid digestion systems or sealed PTFE vessels under high pressure.
DD ISO/TS 13278 pdf download – Nanotechnologies — Determination of elementalimpurities in samples ofcarbon nanotubes using inductively coupled plasmamass spectrometry
