摘要
对双通道离子色谱同时测定陶质文物表面结晶盐中的CH3 COO-、HCOO-、F-、Cl-、SO2-4、NO-3 等 9 种阴离子和Li+、Na+、K+等6 种阳离子的测定方法进行优选.通过优化色谱条件,确定采用Metrosep A Supp7 色谱柱为阴离子分析柱,3 mmol/L碳酸钠为阴离子淋洗液,流速为 0.7 mL/min;Metrosep C4 型色谱柱为阳离子分析柱,0.8 mmol/L吡啶二羧酸-1.6 mmol/L硝酸为阳离子淋洗液,流速为 0.7 mL/min.在此方法下,净化后的滤液一次进样,电导检测器检测,各离子峰形好,分离时间适中,分离效果很好.各离子的标准曲线相关系数R＞0.999,具有良好的线性关系,检出限在0.005～0.05 mg/L之间,加标回收率在96%～106%之间,相对标准偏差为0.1%～4%(n =5).结果表明,瓦当表面结晶盐中主要含有Ca2+、Na+、CH3 COO-、Cl-、SO2-4、NO-3.该方法简单快速、准确度高,可有效分离文物表面结晶盐中的常见有机酸根离子和无机阴阳离子.
Abstract
The contents of 9 anions and 6 cations in the crystalloid salt on ancient pottery,such as CH3 COO-,HCOO-,F-,Cl-,SO2-4,NO-3,Na+,K+,NH4 +,Ca2+,Mg2+,were studied and determined by dual channel ion chromatography.Using Metrosep A Supp7 anion chromatographic column as the ana-lytical column,3 mmol/L NaCO3 as the eluent,the flow rate was 0.7 mL/min,using Metrosep C4 cations chromatographic column as the analytical column,0.8 mmol/L C7 H5 NO4-1.6 mmol/L HNO3 as the elu-ent,the flow rate was 0.7 mL/min.Under this method,the purified filtrate is measured by conductivity detector.Each ion formes a good,moderate separation.The detection limit was between 0.005～0.05 mg/L.The correlation coefficient(R)of the various ions in samples was greater than 0.999,it has a good linear relationship,the recovery was 96%～106%,and the relative standard deviation was 0.1%～4%(n = 5).The result showed that the crystal salt on the tile surface mainly contains:Ca2+,Na+,CH3 COO-,Cl-,SO2-4,NO-3.The method is fast and accurate,sensitive and reliable and can be used for the separation and determanation of common organic acid ions and inorganic ions in crystal salts on the surface of cultural relics.
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