溶液陰極輝光放電光譜信號(hào)的內(nèi)標(biāo)法定量分析研究
發(fā)布時(shí)間:2018-07-11 10:21
本文選題:溶液陰極輝光放電-原子發(fā)射光譜 + 定量分析。 參考:《光譜學(xué)與光譜分析》2017年09期
【摘要】:溶液陰極輝光放電-原子發(fā)射光譜是一種新穎的快速、高效、實(shí)時(shí)在線的元素分析方法,它可用于水體金屬元素的檢測(cè)。為提高其測(cè)量精確度和穩(wěn)定性,將內(nèi)標(biāo)法應(yīng)用于溶液陰極輝光放電-原子發(fā)射光譜技術(shù)。對(duì)K元素建立了標(biāo)準(zhǔn)定標(biāo)曲線和以H_β為內(nèi)標(biāo)元素的定標(biāo)曲線,內(nèi)標(biāo)法測(cè)得樣品的相對(duì)誤差和相對(duì)標(biāo)準(zhǔn)偏差分別為1.11%,2.14%,精確度和穩(wěn)定性較之標(biāo)準(zhǔn)曲線法有一定的提高。實(shí)驗(yàn)考察了元素譜線強(qiáng)度在同一時(shí)段的波動(dòng)情況,發(fā)現(xiàn)元素K和H_β的譜線強(qiáng)度變化趨勢(shì)稍有不同,而同主族元素K和Rb,Ca和Mg的譜線強(qiáng)度有相同的變化趨勢(shì),提出選擇與待測(cè)元素同主族且譜線強(qiáng)度變化趨勢(shì)較為一致的元素作為內(nèi)標(biāo)元素能更大化校正實(shí)驗(yàn)波動(dòng)的觀點(diǎn)。同時(shí)探討了K以Rb為內(nèi)標(biāo)元素、Ca以Mg為內(nèi)標(biāo)元素以及Mg以Ca為內(nèi)標(biāo)元素時(shí)的內(nèi)標(biāo)法測(cè)量的精確度和穩(wěn)定性,得其相對(duì)誤差分別為0.49%,0.02%和0.30%,相對(duì)標(biāo)準(zhǔn)偏差分別為1.11%,1.13%和0.87%,與標(biāo)準(zhǔn)曲線法和以H_β為內(nèi)標(biāo)元素的內(nèi)標(biāo)法相比效果更佳。測(cè)得自來水樣品中Ca元素以Mg為內(nèi)標(biāo)的相對(duì)誤差和相對(duì)標(biāo)準(zhǔn)偏差為0.58%,1.03%,Mg元素以Ca為內(nèi)標(biāo)的相對(duì)誤差和相對(duì)標(biāo)準(zhǔn)偏差為1.57%和1.10%。研究結(jié)果表明,將溶液陰極輝光放電-原子發(fā)射光譜技術(shù)應(yīng)用于水體金屬元素檢測(cè)時(shí),內(nèi)標(biāo)法可以有效校正實(shí)驗(yàn)波動(dòng)的影響,提高測(cè)量的精確度和穩(wěn)定性。
[Abstract]:Solution cathodic glow discharge-atomic emission spectroscopy is a novel, fast, efficient and real-time on-line element analysis method, which can be used for the detection of metal elements in water. In order to improve the measurement accuracy and stability, the internal standard method was applied to the cathodic glow discharge-atomic emission spectrometry. The standard calibration curve of K element and the calibration curve with H _ 尾 as internal standard element were established. The relative error and relative standard deviation of the sample measured by the internal standard method were 1.11 and 2.14, respectively. The accuracy and stability of the method were improved to some extent compared with the standard curve method. The variation trend of spectral line strength of element K and H _ 尾 is slightly different from that of element K, but the intensity of spectral line of elements K, RB, Ca and mg has the same trend. It is pointed out that the selection of elements with the same main family and the same trend of spectral intensity as internal standard elements can be used to correct the experimental fluctuations more greatly. At the same time, the accuracy and stability of the internal standard method for K with RB as internal standard element, Ca with mg as internal standard element and mg with Ca as internal standard element are discussed. The relative error is 0.490.2% and 0.30%, and the relative standard deviation is 1.11% and 0.87%, respectively, which is better than the standard curve method and the internal standard method with H _ 尾 as the internal standard element. The relative error and relative standard deviation of Ca in tap water samples with mg as internal standard and relative standard deviation are 0.58 and 1.03 respectively. The relative error and relative standard deviation of mg element with Ca as internal standard are 1.57% and 1.10% respectively. The results show that when the solution cathodic glow discharge-atomic emission spectroscopy is applied to the detection of metallic elements in water body, the internal standard method can effectively correct the influence of the experimental fluctuation and improve the accuracy and stability of the measurement.
【作者單位】: 重慶郵電大學(xué)光電工程學(xué)院;
【基金】:重慶市基礎(chǔ)與前沿研究計(jì)劃一般項(xiàng)目(cstc2016jcyjA0389);重慶市基礎(chǔ)與前沿研究計(jì)劃重點(diǎn)項(xiàng)目(cstc2015jcyjBX0016) 重慶市教委科技項(xiàng)目(KJ1500436) 留學(xué)歸國人員科研啟動(dòng)基金項(xiàng)目(教外司留[2015]1098號(hào))資助
【分類號(hào)】:O657.31;X832
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