[1]戴苏云,王 娜,马雨璇,等.X-射线粉末衍射法定性定量分析蒙脱石(散)的 影响因素考察[J].南京师范大学学报(自然科学版),2019,42(02):115-121.[doi:10.3969/j.issn.1001-4616.2019.02.019]
 Dai Suyun,Wang Na,Ma Yuxuan,et al.Study on Influencing Factors of X-ray Diffraction both Qualitative and Quantitative Analysis in Montmorillonite(Powder)[J].Journal of Nanjing Normal University(Natural Science Edition),2019,42(02):115-121.[doi:10.3969/j.issn.1001-4616.2019.02.019]
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X-射线粉末衍射法定性定量分析蒙脱石(散)的 影响因素考察
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《南京师范大学学报》(自然科学版)[ISSN:1001-4616/CN:32-1239/N]

卷:
第42卷
期数:
2019年02期
页码:
115-121
栏目:
·生命科学·
出版日期:
2019-06-30

文章信息/Info

Title:
Study on Influencing Factors of X-ray Diffraction both Qualitative and Quantitative Analysis in Montmorillonite(Powder)
文章编号:
1001-4616(2019)02-0115-07
作者:
戴苏云王 娜马雨璇王 冰李 钢
南京师范大学生命科学学院,分析测试中心,江苏 南京 210023
Author(s):
Dai SuyunWang NaMa YuxuanWang BingLi Gang
School of Life Sciences,Nanjing Normal University,Test and Analysis Center,Nanjing 210023,China
关键词:
蒙脱石X-射线粉末衍射定性分析定量分析方英石
Keywords:
montmorilloniteX-ray powder diffractionqualitative analysisquantitative analysischristobalite
分类号:
TG146
DOI:
10.3969/j.issn.1001-4616.2019.02.019
文献标志码:
A
摘要:
蒙脱石广泛应用于医药、化工、食品等领域,随着人们健康意识的不断增强,对《中国药典》中所规定的蒙脱石(散)的质量要求也随之提高,相应的企业对测试结果的稳定性和重复性也提出了新的要求. 本实验中,使用X-射线粉末衍射仪(PXRD)考察了5种因素对蒙脱石鉴定以及方英石和其他杂质含量测定的影响. 结果表明,(1)研磨不会破坏蒙脱石的晶型结构,用玛瑙研钵研磨3 min为宜.(2)相对湿度和温度对蒙脱石的第一个特征峰(5.7°左右)影响明显. 相对湿度增大,向低角偏移,对应的晶面距增大; 温度升高,向高角偏移,对应的晶面距减小,但不影响方英石和其他杂质的检测.(3)蒙脱石的预处理是将其置于温度20 ℃~25 ℃、相对湿度75%的环境条件下,静置12 h为最佳.(4)蒙脱石散前处理的溶解、洗涤、过滤是定量检测结果好坏的关键,建议至少洗涤6次. 本实验结果为生产企业进行蒙脱石(散)定性定量分析提供了参考依据.
Abstract:
Montmorillonite is widely used in medicine,chemical industry,food and other fields. With the increasing awareness of people's health,the quality requirements of montmorillonite(powder)specified in the Chinese Pharmacopoeia have also increased. New requirements for the stability and repeatability of the test results are also placed on by the corresponding companies. In this experiment,the influence of five factors on the identification of montmorillonite,and the determination of cristobalite and the other impurity was investigated by X-ray powder diffractometer(PXRD). The results showed that,(1)The crystal structure of montmorillonite does not be destroyed by grinding,and it is suitable to grind with agate mortar for 3 min.(2)The effect of temperature and humidity on the first characteristic peak of montmorillonite(about 5.7°)is obvious. When the humidity increases,it shifts to a low angle,and the corresponding crystal face distance increases. When the temperature rises,it shifts to a high angle,and the corresponding crystal face distance decreases. They don't affect the detection of cristobalite and other impurities.(3)It is suitable to place the montmorillonite under the environmental conditions of temperature 20 ℃~25 ℃ and relative humidity 75% for 12 h for pretreatment.(4)Dissolution,washing and filtration of montmorillonite pretreatment are the key to the quantitative detection results. It is recommended to wash at least 6 times. The results of this experiment provide a reference in the qualitative and quantitative analysis of montmorillonite(dispersion)for production enterprises.

参考文献/References:

[1] 苏传芝. 思密达治疗婴幼儿腹泻疗效观察[J]. 黑龙江医学,2001,25(10):773-773.
[2]国家药典委员会. 中华人民共和国药典2015年版四部[M]. 北京:中国医药科技出版社,2015.
[3]谌刚,严春杰,寿瑾枫,等. 蒙脱石X射线衍射定量分析方法影响因素研究[J]. 非金属矿,2011,34(1):60-62.
[4]VAZQUEZ A,LóPEZ M,KORTABERRIA G,et al. Modification of montmorillonite with cationic surfactants. Thermal and chemical analysis including CEC determination[J]. Applied clay science,2008,41(1):24-36.
[5]SHOKRI E,YEGANI R,POURABBAS B,et al. Evaluation of modified montmorillonite with di-cationic surfactants as efficient and environmentally friendly adsorbents for arsenic removal from contaminated water[J]. Water science and technology water supply,2018,18(2):460-472.
[6]HERMES H E,FRIELINGHAUS H,PYCKHOUT-HINTZEN W,et al. Quantitative analysis of small angle neutron scattering data from montmorillonite dispersions[J]. Polymer,2006,47(6):2147-2155.
[7]OUESLATI W,RHAIEM H B,LANSON B,et al. Selectivity of Na-montmorillonite in relation with the concentration of bivalent cation(Cu,Ca,Ni)by quantitative analysis of XRD patterns[J]. Applied clay science,2009,43(2):224-227.
[8]ZHANG X,ZHANG L,ZOU X,et al. Semi-quantitative analysis of microbial production of oxalic acid by montmorillonite sorption and ATR-IR[J]. Applied clay science,2018,162:518-523.
[9]OUESLATI W,RHAIEM H B,AMARA A B H. XRD investigations of hydrated homoionic montmorillonite saturated by several heavy metal cations[J]. Desalination,2011,271(1-3):139-149.
[10]邱晶波,沈晓敏,谢梦雨,等. X-射线粉末衍射法对不同厂家蒙脱石的纯度考察[J]. 南京师大学报(自然科学版),2016,39(3):102-105.
[11]PAPATZANI S,BADOGIANNIS E G,PAINE K. The pozzolanic properties of inorganic and organomodified nano-montmorillonite dispersions[J]. Construction and building materials,2018,167:299-316.
[12]方生健. 温度与湿度成正(反)比吗[J]. 档案学研究,1990(2):80-82.
[13]翟建敏,南杰,原韶玲,等. 超声附加绘图定位甲状腺微小结节的临床应用[J]. 中华耳鼻咽喉头颈外科杂志,2013,48(9):730-733.
[14]张为胜,张梅雪,徐东峰,等. 一种药用蒙脱石X射线衍射图谱鉴别标准:中国,101504379[P]. 2009-08-12.
[15]QIU J B,LI G,SHENG Y,et al. Quantification of febuxostat polymorphs using powder X-ray diffraction technique[J]. Journal of pharmaceutical and biomedical analysis,2015,107:298-303.

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备注/Memo

备注/Memo:
收稿日期:2018-12-15.
基金项目:江苏省大型科学仪器设备共享服务平台资助(BZ201403).
通讯联系人:李钢,教授,研究方向:药物晶型结构的分析与研究. E-mail:40010@njnu.edu.cn; 王冰,博士,高级实验师,研究方向:药物晶型结构的分析与研究. E-mail:40388@njnu.edu.cn
更新日期/Last Update: 2019-06-30