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Author(s) |
Mishra, V. G.; Das, M. K.; Shah, D. J.; Jeyakumar, S.; Tomar, B. S.; Ramakumar, K. L. (RACD)
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Source |
Journal of Chromatography-A, 2018. Vol. 1532: pp. 144-149 |
ABSTRACT
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Determination of concentrations of micronutrients in plant samples is important in order to assess thegrowth and quality of plants. An ion chromatography (IC) method was developed for the simultaneousdetermination of B, Cl and Mo (micronutrients present in their anionic form in aqueous samples) usinga gradient elution with d-mannitol and NaOH. Despite their different chemical nature, these elementscould be separated from the matrix by employing pyrohydrolysis. IC was employed for their sequentialdetermination from single aliquot injection into the IC column. It was observed that the optimised proce-dures developed earlier in our laboratory for the separation of B and halogens using d-Mannitol-NaOH orbicarbonate eluents could not be extended to B-Mo-Cl separation. The concentration levels of d-mannitolin the eluent required for separation of boron impeded the conductivity detection of Mo and the peaksensitivity was seen to be critically dependent on d-mannitol concentration in the eluent. In addition,d-mannitol in NaOH eluent altered the retention times of analytes (B, F−, Cl−, NO3−, SO42−and MoO42−)which were not observed in the case of bicarbonate eluent. The current study deals with the investigationon the influence of d-mannitol on the molybdate as well as its role on the retention time. Formation ofMo-mannitol complex at different pH conditions and de-protonation of mannitol were correlated to theobserved effects. Based on the observations, a gradient elution method was proposed for the simulta-neous separation and determination of B, Cl and Mo in the pyrohydrolysis distillates of plant samples.The method was calibrated for B (0.05–1 mg/L), Cl (0.1–10 mg/L) and Mo (0.5–10 mg/L) and the linearregression coefficients obtained were 0.9992, 0.9998 and 0.997 respectively. The limit of detection (LOD)for B, Cl and Mo was calculated to be 19, 23 and 96 μg/L, respectively. The developed IC method afterpyrohydrolytic separation of B, Cl and Mo was successfully applied for the analysis of real samples |
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