Investigating the potential of tandem inductively coupled plasma mass spectrometry (ICP-MS/MS) for Ca determination in concrete

• Published in: Journal of analytical atomic spectrometry Vol. 36; no. 4; pp. 845 - 855
• Main Authors: Russell, B, Mohamud, H, Miranda, M. Garcia, Ivanov, P, Thompkins, H, Scott, J, Keen, P, Goddard, S
• Format: Journal Article
• Language: English
• Published: 13.04.2021
• ISSN: 0267-9477; 1364-5544
• DOI: 10.1039/d1ja00027f

Concrete is a common structural material used in nuclear reactors for biological shielding, containment buildings, and waste storage ponds. Calcium is a significant component of concrete, with neutron activation of stable 40 Ca (96.94% abundance) leading to the production of 41 Ca (half-life 1.002(17) × 10 5 years). The long half-life combined with the significant amount of concrete at nuclear facilities makes 41 Ca a key radionuclide for characterisation of low and intermediate level waste, as well as for long-term waste monitoring. Measurement of 41 Ca by inductively coupled plasma mass spectrometry (ICP-MS) is theoretically achievable, but has previously been prevented by multiple interferences, some of which cannot be removed by offline chemical separation. This study tests the potential of tandem ICP-MS/MS and its enhanced interference separation for the detection of 41 Ca in concrete samples. The instrument setup was initially optimised using stable element standards, with a combination of NH 3 , H 2 and He proving to be most effective, achieving an instrument detection limit of 0.32 Bq g −1 (0.099 ng g −1 ). The procedure was validated on several concrete samples, which required the optimisation of automated borate fusion sample digestion and four-stage chemical separation, with recoveries of 73-77%. Successful detection of 41 Ca was achieved at activity concentrations down to 0.67 Bq g −1 (0.21 ng g −1 ) at 41 Ca/ 40 Ca ratios of 10 −6 -10 −7 . This represents the first known measurement of 41 Ca using ICP-MS, and recommendations are made on how instrument capabilities can be further improved so that routine measurement can be realised. First measurement of 41 Ca and 41 Ca/ 40 Ca by ICP-MS using tandem quadrupole setup and collision-reaction cell separation of interferences.