石鹽中硼含量及其同位素的準(zhǔn)確測(cè)定
發(fā)布時(shí)間:2018-02-22 03:29
本文關(guān)鍵詞: 硼特效樹(shù)脂 ICP-OES 正熱電離質(zhì)譜(P-TIMS) 硼同位素 出處:《光譜學(xué)與光譜分析》2017年08期 論文類(lèi)型:期刊論文
【摘要】:基于Cs2BO+2的正熱電離質(zhì)譜法測(cè)定樣品中硼同位素時(shí),硼含量的準(zhǔn)確測(cè)定直接制約著硼同位素測(cè)定的成敗。目前,使用電感耦合等離子體原子發(fā)射光譜儀(ICP-OES)測(cè)定高鹽樣品的硼含量仍然存在很大問(wèn)題,主要體現(xiàn)在兩個(gè)方面:高鹽的基體干擾和儀器檢出限制約,而僅僅依靠簡(jiǎn)單的稀釋無(wú)法很好的解決這些困難。因此對(duì)樣品進(jìn)行硼元素的預(yù)富集以及基體離子的去除是十分必要的。在使用硼特效樹(shù)脂進(jìn)行硼元素的吸附時(shí)發(fā)現(xiàn)部分鈉離子也會(huì)被同時(shí)吸附,故采用3mol·L~(-1)的氨水可以洗脫大部分吸附的鈉離子而不造成硼的損失,達(dá)到了去除基體的目的。隨后使用10mL 75℃的0.1mol·L~(-1)鹽酸將硼特效樹(shù)脂吸附的硼洗脫實(shí)現(xiàn)了樣品中硼的富集。ICP-OES測(cè)定硼含量時(shí),選擇波長(zhǎng)為208.900nm,樣品的加標(biāo)回收率在106.00%~108.40%之間,檢出限為0.006mg·L~(-1),定量下限為0.02mg·L~(-1)。通過(guò)不同鹽度下的12次重復(fù)實(shí)驗(yàn),其相對(duì)標(biāo)準(zhǔn)偏差小于5%,在1.94%~3.37%之間,因此該方法是可行的,并不存在偶然誤差。聯(lián)合此方法和Cs2BO+2離子的正熱電離質(zhì)譜法,成功測(cè)定了8個(gè)地質(zhì)石鹽樣品的硼含量及硼同位素組成。
[Abstract]:The accurate determination of boron content directly restricts the success or failure of boron isotope determination in the determination of boron isotopes by positive thermoelectric ionization mass spectrometry based on Cs2BO 2. The determination of boron content in high salt samples by ICP-OESis still a big problem, which is mainly reflected in two aspects: the matrix interference of high salt and the limit of instrument detection. These difficulties can not be solved by simple dilution alone. Therefore, it is necessary to preenrich the samples and remove the matrix ions. Now some of the sodium ions are also adsorbed at the same time, Therefore, ammonia solution (3 mol 路L ~ (-1)) can elucidate most of the adsorbed sodium ions without causing boron loss. The removal of the matrix was achieved. The boron adsorbed by boron special effect resin was eluted with 10 mL 75 鈩,
本文編號(hào):1523535
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