光谱学与光谱分析
光譜學與光譜分析
광보학여광보분석
Spectroscopy and Spectral Analysis
2015年
11期
3275-3280
,共6页
林海兰%甘杰%于磊%朱日龙%田耘%罗岳平
林海蘭%甘傑%于磊%硃日龍%田耘%囉嶽平
림해란%감걸%우뢰%주일룡%전운%라악평
微波酸溶%石墨炉原子吸收分光光度法%土壤和沉积物%铍
微波痠溶%石墨爐原子吸收分光光度法%土壤和沉積物%鈹
미파산용%석묵로원자흡수분광광도법%토양화침적물%피
Microwave-acid digestion%GFAA%Soil and sediment%Beryllium
旨在提出一种微波酸溶/石墨炉原子吸收分光光度法测定土壤和沉积物中铍的方法。文中优化了仪器工作条件、阐述了校准曲线的绘制情况、讨论了土壤和沉积物的前处理过程(包括微波升温程序及消解体系的选择)以及考察了共存元素的干扰情况。实验表明,采用硝酸/氢氟酸/盐酸体系‐微波消解进行样品前处理,应用塞曼扣背景‐石墨炉原子吸收光谱法测定土壤/沉积物中铍,具有操作简单、无需基体改进剂、共存离子无干扰、再现性和重复性好等优点。在最优的实验条件下,当取样量为0.2000g,定容体积为25mL,该方法测定土壤铍的方法检出限为0.0049 mg?kg -1,方法测定下限为0.020 mg?kg-1。该法用于测定土壤标样和实际样品,不管是实验室内的方法比对,还是实验室间的方法验证,都获得较好的准确度和精密度。
旨在提齣一種微波痠溶/石墨爐原子吸收分光光度法測定土壤和沉積物中鈹的方法。文中優化瞭儀器工作條件、闡述瞭校準麯線的繪製情況、討論瞭土壤和沉積物的前處理過程(包括微波升溫程序及消解體繫的選擇)以及攷察瞭共存元素的榦擾情況。實驗錶明,採用硝痠/氫氟痠/鹽痠體繫‐微波消解進行樣品前處理,應用塞曼釦揹景‐石墨爐原子吸收光譜法測定土壤/沉積物中鈹,具有操作簡單、無需基體改進劑、共存離子無榦擾、再現性和重複性好等優點。在最優的實驗條件下,噹取樣量為0.2000g,定容體積為25mL,該方法測定土壤鈹的方法檢齣限為0.0049 mg?kg -1,方法測定下限為0.020 mg?kg-1。該法用于測定土壤標樣和實際樣品,不管是實驗室內的方法比對,還是實驗室間的方法驗證,都穫得較好的準確度和精密度。
지재제출일충미파산용/석묵로원자흡수분광광도법측정토양화침적물중피적방법。문중우화료의기공작조건、천술료교준곡선적회제정황、토론료토양화침적물적전처리과정(포괄미파승온정서급소해체계적선택)이급고찰료공존원소적간우정황。실험표명,채용초산/경불산/염산체계‐미파소해진행양품전처리,응용새만구배경‐석묵로원자흡수광보법측정토양/침적물중피,구유조작간단、무수기체개진제、공존리자무간우、재현성화중복성호등우점。재최우적실험조건하,당취양량위0.2000g,정용체적위25mL,해방법측정토양피적방법검출한위0.0049 mg?kg -1,방법측정하한위0.020 mg?kg-1。해법용우측정토양표양화실제양품,불관시실험실내적방법비대,환시실험실간적방법험증,도획득교호적준학도화정밀도。
A method for determination of beryllium in soils and sediments by microwave‐acid digestion/graphite furnace atomic absorption (GFAA) is described .In this paper ,the working conditions of the instrument are optimized ,the drawing of calibration curve is expounded ,the pretreatment process of soil and sediments (in‐cluding microwave heating process and the selection of digestion system) is discussed ,and the interference of coexisting elements is examined .The sample was pretreated by microwave digestion parameters using HNO3/HCl/HF mixed acid system .The method is fast and simple without matrix modifier ,and has no interference by coexisting ions ,and has high repeatability and reproducibility .Under the optimal experimental conditions , the limit of detection (LOD) is 0.004 9 mg?kg -1 (sample quantity 0.200 0 g ,sample volume 25 mL) ,and the limits of quantitation (LOQ) is 0.020 mg? kg -1 .This method is used to measure the standard samples and actual samples ,whether in the laboratory ,or between laboratories ,has good accuracy and precision .