离子色谱法测定灰尘中四种酸根阴离子
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摘要
用离子色谱快速测定文物表面灰尘中共存4种酸根阴离子(Cl~-、SO_4~(2-)、NO_3~-、PO_4~(3-))。灰尘样品经超纯水振荡浸提后,采用On Guard~Ⅱ RP(C18柱)固相萃取柱和On Guard~ⅡP固相预处理柱净化。溶液中共存的4种阴离子采用25 mmol/L的氢氧化钾溶液等度洗脱分离,依次通过Ion PacAG11-SH(50 mm×4.0 mm)保护柱、IonPac~AS11-SH(250 mm×4.0 mm)分析柱和抑制器,以电导检测器对共存的4种阴离子分析定量。该法各离子的检出限0.46~0.61 mg/kg,加标回收率89.90%~107.79%,相对标准偏差(n=7)0.26%~0.34%。
The contents of 4 anions including Cl~-、SO_4~(2-)、NO_3~-、PO_4~(3-) in dust were studied and determined by ion chromatography( IC). By means of oscillation,the sample of dust was extracted with water and purified through On Guard~Ⅱ RP( C18 column) and On Guard~ⅡP solid phase extraction columns.The 4 anions existing in the solution were separated by Ion PacAS11-SH( 250 mm × 4. 0 mm) column with Ion Pac~AG11-SH( 50 mm × 4. 0 mm) as guard column by elution with 25 mmol/L KOH solution and detected by inhibitory conductivity detection. Values of detection limit( 3 s/k) found were in the range of 0. 46 ~ 0. 61 mg/kg. Tests for recovery and precision were made,giving values of recovery from89. 90% ~ 107. 79%,and RSD's( n = 7) range from 0. 26% ~ 0. 34%.
The contents of 4 anions including Cl~-、SO_4~(2-)、NO_3~-、PO_4~(3-) in dust were studied and determined by ion chromatography( IC). By means of oscillation,the sample of dust was extracted with water and purified through On Guard~Ⅱ RP( C18 column) and On Guard~ⅡP solid phase extraction columns.The 4 anions existing in the solution were separated by Ion PacAS11-SH( 250 mm × 4. 0 mm) column with Ion Pac~AG11-SH( 50 mm × 4. 0 mm) as guard column by elution with 25 mmol/L KOH solution and detected by inhibitory conductivity detection. Values of detection limit( 3 s/k) found were in the range of 0. 46 ~ 0. 61 mg/kg. Tests for recovery and precision were made,giving values of recovery from89. 90% ~ 107. 79%,and RSD's( n = 7) range from 0. 26% ~ 0. 34%.
引文
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[3]张予南.潼南大佛与大足千手观音像髹漆贴金过程反思——试论文物修复实践中的文物保护理念[J].中国文化遗产,2016(5):65-75.
[4]胡东波,薛铁宁,王金华,等.重庆大足宝顶山千手观音的贴金材料分析研究[J].文物保护与考古科学,2008,20(3):44-51.
[5]沈璐,刘成,周雪松.山西大同下华严寺辽代贴金泥塑病害调查[J].陕西师范大学学报:自然科学版,2008,36(S1):141-143.
[6]Tian Xingling,Ma Qinglin,Zheng Mingtian,et al.Gold leaf corrosion in moisture acid atmosphere at ambient temperature[J].Rare Metal Materials and Engineering,2014,43(11):2637-2642.
[7]胡平,解彦平,任永红.固相萃取-离子色谱法测定土壤中亚硝酸盐和硝酸盐[J].理化检验:化学分册,2012,48(11):1318-1320.
[8]魏益华,张金艳,罗林广.离子色谱法测定农村饮用水中阴离子[J].理化检验:化学分册,2012,48(2):213-214.
[9]吴勣,孙明星,高运川,等.离子色谱法测定化肥中六种阴离子[J].理化检验:化学分册,2011,47(1):23-26.
[10]牟世芬,刘克纳.离子色谱方法及应用[M].北京:化学工业出版社,2000.
[11]范云场,朱岩.离子色谱分析中的样品前处理技术[J].色谱,2007(5):633-640.
[12]Fan Huixiu,Deng Zhipeng,Zhong Hao,et al.Development of new solid phase extraction technique in the last ten years[J].Journal of Chinese Pharmaceutical Sciences,2013,22(4):293-302.