激光誘導(dǎo)擊穿光譜結(jié)合標(biāo)準(zhǔn)加入法定量分析土壤中鉛、鎘、鉻和銅(英文)
發(fā)布時間:2018-03-13 11:10
本文選題:激光誘導(dǎo)擊穿光譜 切入點:定量分析 出處:《光譜學(xué)與光譜分析》2017年10期 論文類型:期刊論文
【摘要】:利用課題組自主研制的便攜式激光誘導(dǎo)擊穿光譜測量系統(tǒng)定量分析土壤及固體廢棄物中四種重金屬元素Pb,Cd,Cr和Cu。實驗采用中心波長為1 064nm的Nd∶YAG脈沖激光器作為激發(fā)光源,工作頻率為3Hz,單脈沖能量為100mJ,脈沖寬度為6ns;以高分辨率、寬光譜段的中階梯光柵光譜儀和增強型電荷耦合器件為譜線分離與探測器件,探測范圍為200~500nm,分辨率為0.08~0.12nm。為了提高光譜強度及檢測靈敏度,通過半球空間約束裝置對等離子進行約束,并采用多芯光纖實現(xiàn)多通道不同角度光譜信號收集,接收角度為45°。實驗時激光重復(fù)頻率為2Hz,延時為1.5μs,門寬為1.05ms。文章創(chuàng)新性地將曲線擬合代替直線擬合用于標(biāo)準(zhǔn)加入法定量分析基質(zhì)未知樣品中重金屬元素,有效提高了測量結(jié)果的準(zhǔn)確性,尤其是低濃度的土壤樣品,直線擬合無法定量分析重金屬含量,相比而言,曲線擬合相關(guān)系數(shù)更高,測量結(jié)果更接近國標(biāo)方法,可以滿足一級土壤污染的檢測。七個土壤及固體廢棄物樣品檢測的相對誤差如下,直線擬合相對誤差分別為:Pb 1.26%~79.38%,Cr-22.44%~82.06%,Cu 15.09%~190.50%,Cd 32.76%~167.96%,曲線擬合相對誤差為分別Pb-4.19%~11.92%,Cr-38.31%~9.26%,Cu-7.24%~26.86%,Cd-10.52%~12.94%,相對誤差平均值為10.47%。
[Abstract]:A portable laser-induced breakdown spectrometric system was developed for quantitative analysis of four heavy metal elements in soil and solid waste. The Nd:YAG pulse laser with a central wavelength of 1064nm was used as the excitation source. The working frequency is 3Hz, the single pulse energy is 100mJ, the pulse width is 6ns, the high resolution, wide spectrum band middle step grating spectrometer and the enhanced charge coupled device are used as the line separation and detector. In order to improve the spectral intensity and detection sensitivity, the plasma is constrained by the hemispherical space confinement device, and the multi-channel and different angle spectral signal is collected by using multi-core fiber, the detection range is 200 ~ 500 nm and the resolution is 0.08 ~ 0.12 nm. The receiving angle is 45 擄, the laser repetition rate is 2 Hz, the delay is 1.5 渭 s, and the gate width is 1.05 Ms. This paper innovatively uses curve fitting instead of straight line fitting for quantitative analysis of heavy metal elements in unknown matrix samples by standard addition method. The accuracy of the measurement results is improved effectively, especially in the low concentration soil samples, the linear fitting can not quantitatively analyze the heavy metal content, in contrast, the curve fitting correlation coefficient is higher, and the measured results are closer to the national standard method. The relative errors of the seven soil samples and solid waste samples were as follows. The relative errors of the straight line fitting were 79.38 Cr-22.44440.06K, Cu 15.090.50cu 32.767.96, and the relative errors of curve fitting were Pb-4.1911.92Cr-38.31U 9.269.26Cu-7.248626.8626cd-10.52n 12.940.The average relative error was 10.4747.
【作者單位】: 中國科學(xué)院安徽光學(xué)精密機械研究所 中國科學(xué)院環(huán)境光學(xué)與技術(shù)重點實驗室;安徽省環(huán)境光學(xué)監(jiān)測技術(shù)重點實驗室;中國科學(xué)技術(shù)大學(xué);
【基金】:the support of the project of the Science and Technology program of Anhui province(1501041119) the science and technology major special program of Anhui province(15CZZ04125) the National Key Research and Development Plan(2016YFD0800902-3) National“863”program(2014AA06A513)
【分類號】:O657.31;X833
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