熔融制樣-X射線熒光光譜法測(cè)定輕稀土精礦中稀土總量
發(fā)布時(shí)間:2018-05-01 12:38
本文選題:X射線熒光光譜法(XRF) + 熔融法; 參考:《冶金分析》2017年12期
【摘要】:作為稀土工業(yè)的原料,稀土精礦中稀土總量的測(cè)定方法步驟多、流程長(zhǎng)。實(shí)驗(yàn)采用熔融制樣-X射線熒光光譜法測(cè)定輕稀土精礦中稀土總量,研究了制樣和測(cè)量條件。準(zhǔn)確稱取6.000 0g無(wú)水四硼酸鋰和偏硼酸鋰混合熔劑(質(zhì)量比2∶1)于鉑黃坩堝中,以0.500 0g硝酸鋰為氧化劑消除試樣中還原物質(zhì)對(duì)鉑黃坩堝的侵蝕,稱取0.600 0g稀土精礦試樣,再于試樣表面均勻覆蓋0.500 0g氧化硼防止試樣噴濺,滴加0.5mL 20mg/mL的溴化銨溶液作為脫模劑。將坩堝放進(jìn)預(yù)加熱到1 050℃的熔樣機(jī)內(nèi)熔融19min制備樣片,可消除礦物效應(yīng)、粒度效應(yīng)及表面效應(yīng)。通過(guò)各稀土元素X射線熒光譜線的選擇減少譜線干擾,以經(jīng)驗(yàn)系數(shù)法校正譜線干擾和基體效應(yīng),用稀土精礦標(biāo)樣建立各稀土元素校準(zhǔn)曲線。各組分校準(zhǔn)曲線的相關(guān)系數(shù)在0.991~0.999之間,試樣重復(fù)測(cè)量的相對(duì)標(biāo)準(zhǔn)偏差(RSD)小于0.5%,稀土總量測(cè)定結(jié)果與重量法一致。方法的精密度和正確度能夠滿足生產(chǎn)要求。
[Abstract]:As the raw material of rare earth industry, there are many steps and long process to determine the total amount of rare earth in rare earth concentrate. The total amount of rare earth in light rare earth concentrate was determined by melting sample preparation-X-ray fluorescence spectrometry. The conditions of sample preparation and measurement were studied. The mixture flux of 6.000 g anhydrous lithium tetraborate and lithium metaborate (mass ratio 2: 1) was accurately used in the platinum yellow crucible, 0.500 g lithium nitrate was used as oxidant to eliminate the erosion of the reducing substance to the platinum yellow crucible in the sample, and the 0.600 g rare earth concentrate sample was used as the sample. Then 0.500 g boron oxide was uniformly covered on the surface of the sample to prevent the sample from spattering, and the ammonium bromide solution of 0.5mL 20mg/mL was added as the release agent. When the crucible is put into the melting prototype heated to 1 050 鈩,
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