DD ISO/TS 13278:2011 pdf download.Nanotechnologies — Determination of elemental impurities in samples of carbon nanotubes usingi nductively coupled plasma mass spectrometry.
6 Sample pretreatment
6.1 Sample preparation for ICP-MS analysis
Harmonizing sample preparation procedL%es by using a protocol such as that described In References 1121 and [14) contributes to the quality of measurements by improving repeatabihty, reproducibility and reliability. This in turn ensures that measurement results can be compared with those generated in other laboratories. 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 [121. are described here. These riclude wet digestion under h.gh pressure, a combination of dry ashing with wet digestion, and a microwave-assisted sample preparation for dissolution of elemental impurities in the CNT samples before ICP-MS analysis. These methods have been shown to provide reliable and reproducible measurement results using ICP.MSII2I. 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 we 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 using dosed microwave-assisted acid digestion systems or sealed PTFE vessels under high pressure.
In each of the following procedures, a selected number of “spiked’ samples shall be prepared with each batch of “unspiked” samples. The number of spiked samples shall be at least 10 % of the number of urispiked samples. The purpose of the spiked samples is to allow analyte recovery to be calculated. Spike recovery is described in 8.2.
6.1 Sample preparation for ICP-MS analysis
Harmonizing sample preparation procedL%es by using a protocol such as that described In References 1121 and [14) contributes to the quality of measurements by improving repeatabihty, reproducibility and reliability. This in turn ensures that measurement results can be compared with those generated in other laboratories. 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 [121. are described here. These riclude wet digestion under h.gh pressure, a combination of dry ashing with wet digestion, and a microwave-assisted sample preparation for dissolution of elemental impurities in the CNT samples before ICP-MS analysis. These methods have been shown to provide reliable and reproducible measurement results using ICP.MSII2I. 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 we 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 using dosed microwave-assisted acid digestion systems or sealed PTFE vessels under high pressure.
In each of the following procedures, a selected number of “spiked’ samples shall be prepared with each batch of “unspiked” samples. The number of spiked samples shall be at least 10 % of the number of urispiked samples. The purpose of the spiked samples is to allow analyte recovery to be calculated. Spike recovery is described in 8.2.
