光谱学与光谱分析
光譜學與光譜分析
광보학여광보분석
SPECTROSCOPY AND SPECTRAL ANALYSIS
2015年
1期
208-211
,共4页
方丽%赵南京%孟德硕%袁静%汤洁%王寅%余洋%马明俊%胡丽%张大海%肖雪%王煜%刘建国%刘文清
方麗%趙南京%孟德碩%袁靜%湯潔%王寅%餘洋%馬明俊%鬍麗%張大海%肖雪%王煜%劉建國%劉文清
방려%조남경%맹덕석%원정%탕길%왕인%여양%마명준%호려%장대해%초설%왕욱%류건국%류문청
光谱学%激光诱导击穿光谱%标准加入法%ICP-MS%固体废弃物
光譜學%激光誘導擊穿光譜%標準加入法%ICP-MS%固體廢棄物
광보학%격광유도격천광보%표준가입법%ICP-MS%고체폐기물
Spectroscopy%LIBS%Standard addition method%ICP-MS%Solid waste
利用激光诱导击穿光谱结合标准加入法定量分析了铅蓄电池厂含铅污泥中重金属铅元素含量，标准加入法有效避免了外标法与内标法制作标准曲线时基质不同对L IBS检测结果的影响，且样品处理过程简单。实验采用中心波长为1064 nm的Nd∶YAG脉冲激光器作为激发光源，以高分辨率、宽光谱段的中阶梯光栅光谱仪和增强型电荷耦合器件为谱线分离与探测器件，选取铅的PbⅠ：405.78 nm特征谱线作为分析线，以FeⅠ：404.58 nm特征谱线作为内标线进行结果计算。预实验确定较佳的实验条件后（激光脉冲能量：128.5 mJ ，延时：2.5μs ，门宽：3μs），对铅蓄电池厂的未知铅泥样品中铅元素进行定量分析，结果表明加入铅在0～25000 mg?kg －1范围内谱线不会产生自吸收，PbⅠ：405.78 nm信号强度与铅加入量呈很好的线性关系，由此确定合适的铅加入量为0～25000 mg?kg －1。在此基础上配制四个样品，基质均为铅蓄电池厂含铅污泥，加入铅浓度分别为5000，10000，15000，20000 mg?kg －1，每个样品设置三个平行样，验证实验重复性及可靠性，并与IC P-M S检测结果对比，结果直线外推误差为－14.8％。12个样品单次计算结果误差介于为－24.6％～17.6％之间，含铅量平均值为43069 mg?kg －1，相对误差为－2.44％。
利用激光誘導擊穿光譜結閤標準加入法定量分析瞭鉛蓄電池廠含鉛汙泥中重金屬鉛元素含量，標準加入法有效避免瞭外標法與內標法製作標準麯線時基質不同對L IBS檢測結果的影響，且樣品處理過程簡單。實驗採用中心波長為1064 nm的Nd∶YAG脈遲激光器作為激髮光源，以高分辨率、寬光譜段的中階梯光柵光譜儀和增彊型電荷耦閤器件為譜線分離與探測器件，選取鉛的PbⅠ：405.78 nm特徵譜線作為分析線，以FeⅠ：404.58 nm特徵譜線作為內標線進行結果計算。預實驗確定較佳的實驗條件後（激光脈遲能量：128.5 mJ ，延時：2.5μs ，門寬：3μs），對鉛蓄電池廠的未知鉛泥樣品中鉛元素進行定量分析，結果錶明加入鉛在0～25000 mg?kg －1範圍內譜線不會產生自吸收，PbⅠ：405.78 nm信號彊度與鉛加入量呈很好的線性關繫，由此確定閤適的鉛加入量為0～25000 mg?kg －1。在此基礎上配製四箇樣品，基質均為鉛蓄電池廠含鉛汙泥，加入鉛濃度分彆為5000，10000，15000，20000 mg?kg －1，每箇樣品設置三箇平行樣，驗證實驗重複性及可靠性，併與IC P-M S檢測結果對比，結果直線外推誤差為－14.8％。12箇樣品單次計算結果誤差介于為－24.6％～17.6％之間，含鉛量平均值為43069 mg?kg －1，相對誤差為－2.44％。
이용격광유도격천광보결합표준가입법정량분석료연축전지엄함연오니중중금속연원소함량，표준가입법유효피면료외표법여내표법제작표준곡선시기질불동대L IBS검측결과적영향，차양품처리과정간단。실험채용중심파장위1064 nm적Nd∶YAG맥충격광기작위격발광원，이고분변솔、관광보단적중계제광책광보의화증강형전하우합기건위보선분리여탐측기건，선취연적PbⅠ：405.78 nm특정보선작위분석선，이FeⅠ：404.58 nm특정보선작위내표선진행결과계산。예실험학정교가적실험조건후（격광맥충능량：128.5 mJ ，연시：2.5μs ，문관：3μs），대연축전지엄적미지연니양품중연원소진행정량분석，결과표명가입연재0～25000 mg?kg －1범위내보선불회산생자흡수，PbⅠ：405.78 nm신호강도여연가입량정흔호적선성관계，유차학정합괄적연가입량위0～25000 mg?kg －1。재차기출상배제사개양품，기질균위연축전지엄함연오니，가입연농도분별위5000，10000，15000，20000 mg?kg －1，매개양품설치삼개평행양，험증실험중복성급가고성，병여IC P-M S검측결과대비，결과직선외추오차위－14.8％。12개양품단차계산결과오차개우위－24.6％～17.6％지간，함연량평균치위43069 mg?kg －1，상대오차위－2.44％。
The standard addition method with laser induced breakdown spectroscopy was used to analyze an unknown sample taken from a lead battery factory .the matrix influence on the results was effectively avoided when the external or internal stand-ard method was used ,and the pretreatment of samples was simple and quick .The Nd∶YAG pulse laser with wavelength 1 064 nm was used as the excitation source .The echelle spectroscopy with high resolution and wide spectral range was used as the spectral separation device ,and the intensified charge coupled device (ICCD ) as the spectral detection device in the experiment . The characteristic line at 405.78 nm was chosen as the analysis line to measure Pb concentration .FeⅠ :404.58 line was chosen as the internal standard .Pre-experiment was carried out to confirm the appropriate condition .Under the laser energy of 128.5 mJ ,the delay time of 2.5 μs ,and the gate width of 3 μs ,it was determined that with the addition of Pb to the sample in the range of 0 and 25 000 mg?kg -1 ,there wasn’t self-absorption .There was a good linear relationship between the intensity of the spectral line of 405.78 nm and the addition of Pb .The appropriate concentration of Pb added into the sample for analysis was de-termined by this series of samples .On this basis ,four samples were prepared with three parallel samples for each sample in or-der to verify the repeatability and reliability of the method ,i .e .5 000 ,10 000 ,15 000 ,20 000 mg?kg -1 Pb was added into the original sample .The results were compared with the result of ICP-MS .The twelve samples’ relative errors were between-24.6% and 17.6% .The average result was 43 069 mg?kg -1 with the relative error -2.44% .
