离子色谱法快速测定秦陵土遗址中无机阴、阳离子含量  

Rapid Determination of Inorganic Anions and Cations in Earthen Site of Qinshihuang′s Mausoleum by Ion Chromatography

作　　者：杜维莎 景博文 付菲 李华 夏寅[1,2] 周萍 DU Weisha;JING Bowen;FU Fei;LI Hua;XIA Yin;ZHOU Ping(Emperor Qin Shihuang′s Mausoleum Site Museum,Xi′an,Shaanxi 710600,China;Key Scientific Research Base of Ancient Polychrome Pottery Conservation of State Administration for Cultural Heritage,Xi′an,Shaanxi 710600,China)

机构地区：[1]秦始皇帝陵博物院,西安710600 [2]陶质彩绘文物保护国家文物局重点科研基地,西安710600

出　　处：《中国无机分析化学》2023年第10期1097-1103,共7页Chinese Journal of Inorganic Analytical Chemistry

基　　金：陕西省重点研发计划项目(2021ZDLSF06-01);秦陵博物院项目(2022QLBWY05-03)。

摘　　要：研究发现,可溶盐在土遗址内反复溶解重结晶产生的体积膨胀,是导致其产生酥粉、脱落、盐析病害的主要原因,严重影响着遗址类文物的安全与稳定。因此,对土遗址可溶盐组成、分布的系统性研究是判断文物病害成因、病害发展趋势的基础性工作。建立离子色谱技术快速测定秦陵土遗址中无机阴、阳离子的方法,有利于对土遗址或埋藏文物面临的潜在风险进行有效识别,从而为文物预防性保护提供数据支撑。以30 mmol/L氢氧化钾溶液作为淋洗液用于5种阴离子(F^(-)、Cl^(-)、SO_(4)^(2-)、NO_(3)^(-)、PO_(4)^(3-))的分离及20 mmol/L甲烷磺酸(MSA)溶液作为淋洗液用于5种阳离子(Na^(+)、NH_(4)^(+)、K^(+)、Mg^(2+)、Ca^(2+))的分离,测定中采用抑制电导检测器。结果表明,几种离子的质量浓度均在一定范围内呈线性关系,F^(-)、Cl^(-)、SO_(4)^(2-)、NO_(3)^(-)、PO_(4)^(3-)等5种阴离子的检出限分别为0.003、0.002、0.001、0.001、0.003 mg/L,Na^(+)、NH_(4)^(+)、K^(+)、Mg^(2+)、Ca^(2+)等5种阳离子的检出限分别为0.003、0.004、0.004、0.005、0.010 mg/L,阴离子的加标回收率在95.0%~101%,阳离子的加标回收率在91.0%~99.0%。方法具有精密度高、准确度好、分析速度快等优点,可用于秦陵土遗址中常见无机阴、阳离子的快速测定。It is found that the volume expansion caused by the repeated dissolution and recrystallization of soluble salt in the earthen sites is the main reason for the diseases of crisp powder,shedding and salting out,which seriously affects the safety and stability of relics in the ruins.Therefore,the systematic study on the composition and distribution of soluble salts in earthen sites is the basic work to judge the causes and development trend of diseases of cultural relics.In this paper,inorganic anions and cations in the earthen site of Qin Mausoleum were determined by ion chromatography(IC).30 mmol/L KOH solution were used for the separation of five anions(F^(-),Cl^(-),SO_4^(2-),NO_3^(-)and PO_4^(3-)) and 20 mmol/L MSA solution were used for the separation of five cations(Na^(+),NH_4^(+),K^(+),Mg^(2+) and Ca^(2+)).Suppressed conductivity detectors were adopted in the measurement.Linearity was found in the definite ranges for all 10 ions,with detection limits of 0.003,0.002,0.001,0.001 and 0.003 mg/L for F^(-),Cl^(-),SO_4^(2-),NO_3^(-) and PO_4^(3-) as well as 0.003,0.004,0.004,0.005 and 0.010 mg/L for Na^(+),NH_4^(+),K^(+),Mg^(2+),and Ca^(2+).The recoveries of anions and cations were 95.0%-101% and 91.0%-99.0%.The method has the advantages of high precision,good accuracy and fast analysis speed,and can be used for the rapid determination of common inorganic anions and cations in earthen sites of Qinshihuang′s Mausoleum.

关 键 词：离子色谱 秦陵土遗址 阴离子 阳离子 

分 类 号：O657.75[理学—分析化学] TH833[理学—化学]