title: Determination of mercury in phosphate fertilizers by cold vapor atomic absorption spectrometry.
abstract: In this paper, a method for the determination of mercury in phosphate fertilizers using slurry sampling and cold vapor atomic absorption spectrometry (CV QT AAS) is proposed. Because mercury (II) ions form strong complexes with phosphor compounds, the formation of metallic mercury vapor requires the presence of lanthanum chloride as a release agent. Thiourea increases the amount of mercury that is extracted from the solid sample to the liquid phase of the slurry. The method is established using two steps. First, the slurry is prepared using the sample, lanthanum chloride, hydrochloric acid solution and thiourea solution and is sonicated for 20 min. Afterward, mercury vapor is generated using an aliquot of the slurry in the presence of the hydrochloric acid solution and isoamylic alcohol with sodium tetrahydroborate solution as the reducing agent. The experimental conditions for slurry preparation were optimized using two-level full factorial design involving the factors: thiourea and lanthanum chloride concentrations and the duration of sonication. The method allows the determination of mercury by external calibration using aqueous standards with limits of detection and quantification of 2.4 and 8.2 μg kg(-1), respectively, and precision, expressed as relative standard deviation, of 6.36 and 5.81% for two phosphate fertilizer samples with mercury concentrations of 0.24 and 0.57 mg kg(-1), respectively. The accuracy was confirmed by the analysis of a certified reference material of phosphate fertilizer that was provided by the National Institute of Standards & Technology (NIST). The method was applied to determine mercury in six commercial samples of phosphate fertilizers. The mercury content varied from 33.97 to 209.28 μg kg(-1). These samples were also analyzed employing inductively coupled plasma mass spectrometry (ICP-MS). The ICP-MS results were consistent with the results from our proposed method.
authors.affiliation: Universidade Federal da Bahia, Grupo de Pesquisa em Química e Quimiometria, CEP: 40170-270, Salvador, Bahia, Brazil.
authors.forename: Robson M
authors.initials: RM
authors.lastname: de Jesus
authors.forename: Laiana O B
authors.initials: LO
authors.lastname: Silva
authors.forename: Jacira T
authors.initials: JT
authors.lastname: Castro
authors.forename: Andre D
authors.initials: AD
authors.lastname: de Azevedo Neto
authors.forename: Raildo M
authors.initials: RM
authors.lastname: de Jesus
authors.forename: Sergio L C
authors.initials: SL
authors.lastname: Ferreira
mesh_terms: D001894:Borohydrides / Q000737:chemistry; D002138:Calibration; D002413:Cations, Divalent; D005308:Fertilizers / Q000032:analysis*; D005740:Gases; D007811:Lanthanum / Q000737:chemistry; D057230:Limit of Detection; D008628:Mercury / Q000032:analysis*; D010755:Organophosphates / Q000737:chemistry*; D013010:Sonication; D013054:Spectrophotometry, Atomic / Q000379:methods / Q000592:standards*; D013890:Thiourea / Q000737:chemistry; D014835:Volatilization
chemical_list: D001894:Borohydrides; D002413:Cations, Divalent; D005308:Fertilizers; D005740:Gases; D010755:Organophosphates; C028521:lanthanum chloride; D007811:Lanthanum; C025364:sodium borohydride; D008628:Mercury; D013890:Thiourea