摘要
首先用碱熔融法分解试样，然后加抗坏血酸将试液中的Ｆｅ３＋还原为Ｆｅ２＋，再用离子色谱法测定试液中的Ｆｅ２＋，Ｍｇ２＋和Ｃａ２＋。采用Ｓｈｉｍ－ｐａｃｋＩＣ－Ｃｌ阳离子交换柱分离样品离子，以０．２５ｍｍｏｌ／Ｌ乙二胺－０．５０ｍｍｏｌ／Ｌ柠檬酸（ｐＨ４．５０）为流动相，以ＣＤＤ－６Ａ电导检测器检测，使被测组分得到满意的分离和检测。Ｆｅ，Ｍｇ和Ｃａ的加标回收率均在９０％以上。测定结果与原子吸收光谱法测定结果相近。
Determination of Fe, Mg and Ca in superheater tube scale and boiler scale by single column ion chromatography is described. The sample was dissolved after fusion at 650℃. Fe 3+ in the solution of sample was then reduced to Fe 2+ by ascorbic acid. Finally, Fe 2+ , Mg 2+ and Ca 2+ in the solution of sample were determind by ion chromatography. Chromatographic analysis was performed on an HIC 6A ion chromatograph (Shimadzu) with a CDD 6A conductivity detector. The separation column was Shim pack IC Cl cation exchange column(15cm×5.0mm i.d.). The solution containing 0.25mmol/L ethylenediamine 0.50mmol/L citric acid, pH 4.50, was used as the eluent with a flow rate of 1.0mL/min. The column oven temperature was controlled at 40℃. The injection volume was 20μL. The optimum concentration of eluent for the separation of Ni 2+ , Zn 2+ , Fe 2+ , Mg 2+ , Mn 2+ , Cd 2+ , Ca 2+ and Sr 2+ was investigated. Satisfactory separation and detection of Fe 2+ , Mg 2+ and Ca 2+ is presented with the proposed method. The detection limits (signal to noise ratio=2)for Fe 2+ , Mg 2+ and Ca 2+ were 0.10, 0.12 and 0.31mg/L, respectively. The relative standard deviations were lower than 2.2%(n=5) for all the three ions. The linear ranges for Fe 2+ , Mg 2+ and Ca 2+ were 0.10 20, 0.12 30 and 0.31 50mg/L(r=0.999), respectively. The recoveries of the added standard were over 90%. There was little difference between the results from ion chromatography and those from atomic absorption spectrometry.
出处
《色谱》
CAS
CSCD
北大核心
1998年第1期65-67,共3页
Chinese Journal of Chromatography
基金
黑龙江省教委基金
关键词
离子色谱法
过热器管垢
锅炉垢
铁
镁
钙
ion chromatography, superheater tube scale, boiler scale, iron, magnesium, calcium
