本文广泛讨论了使用热水解作为进一步测定卤素的样品制备方法,涵盖了过去30年发表的研究。这种方法与有机(如纤维素、化石燃料,碳纳米管,和石墨)和无机物(如岩石,硅酸盐,氧化铝,和核燃料)矩阵。它也被用于不同有机物含量的样品,比如煤炭,矿物质补充剂,和土壤。样品质量变化很大,取决于样品中的有机物含量,有机样品的范围从50毫克到500毫克,和高达4克的无机样品。不同的添加剂,如V2O5和纤维素,或阻燃剂,如二氧化硅,还可用于使用热水解来改善分析物回收。稀碱溶液甚至水已经被用作吸收溶液,主要是NaOH,NH4OH,以及施加NaHCO3和Na2CO3的混合物。此外,热解与离子色谱等检测技术兼容,电感耦合等离子体质谱,离子选择电极,电感耦合等离子体发射光谱,能量色散X射线荧光光谱法,分光光度法,和同位素比质谱。通常与该方法相关的其他优点是消化物的低残留碳浓度和低残留生成。与碱性提取的关键比较,碱性融合,Schöniger氧瓶燃烧,还提供了燃烧弹和微波诱导燃烧。
The use of pyrohydrolysis as a sample preparation method for further halogen determination is extensively discussed in this
review, covering studies published in the last 30 years. This method is compatible with both organic (such as cellulose, fossil fuels, carbon nanotubes, and graphite) and inorganic (such as rocks, silicates, alumina, and nuclear fuels) matrices. It has also been used for samples with different organic matter content, such as coal, mineral supplements, and soil. Sample masses vary greatly and are dependent on organic matter content in the samples, ranging from 50 mg to up to 500 mg for organic samples, and up to 4 g to inorganic samples. Different additives, such as V2O5 and cellulose, or flame retardants, such as silica, could also be used to improve analyte recovery using pyrohydrolysis. Dilute alkaline solutions or even water have been used as absorbing solutions, with mainly NaOH, NH4OH, and mixtures of NaHCO3 and Na2CO3 being applied. Furthermore, pyrohydrolysis is compatible with detection techniques such as ion chromatography, inductively coupled plasma mass spectrometry, ion selective electrode, inductively coupled plasma optical emission spectrometry, energy-dispersive X-ray fluorescence spectrometry, spectrophotometry, and isotope ratio mass spectrometry. Other advantages usually related to this method are the low residual carbon concentration of digests and the low residue generation. A critical comparison with alkaline extraction, alkaline fusion, Schöniger oxygen flask combustion, combustion bomb and microwave-induced combustion is also provided.