Sulfur Fine Particles as Stationary Phase for TLC/FTIR Analysis†

doi:10.7503/cjcu20130998

Abstract

Abstract:

In situ thin-layer chromatography-Fourier transform infrared spectroscopy(TLC-FTIR) technique has tremendous potential in the analysis of complex mixtures. However, the progress in this technique was quite slow. The reason is that conventional stationary phase has strong absorption in FTIR spectrum and brings about severe interference in the detection of samples. This paper proposes to use sulfur fine particles, which is transparent in mid-infrared, as a new type of TLC stationary phase. Additionally, decreasing the particle size of sulfur is very important in TLC-FTIR analysis technique. By optimizing the experimental conditions, the sulfur particle with a size of 500 nm was prepared and the conventional TLC plate and the narrow TLC plate using the sulfur paticles as the stationary phase was prepared. TLC experimental results prove that the TLC plate can separate the mixture of rhodamine B and gentian violet successfully. FTIR analysis confirms that the FTIR spectra of the separated rhodamine B/gentian violet spots and rhodamine B/bromophenol blue spots are in good agreement with the FTIR spectra of pure rhodamine B, gentian violet and bromophenol blue.

Key words: Thin-layer chromatography, Fourier transform infrared spectroscopy(FTIR), Sulfur, Narrow-band thin-layer chromatography(TLC) plate

CLC Number:

O657

TrendMD:

FAN Xiaokun, JIANG Ye, SHI Jiajia, LIU Cuige, WEI Yongju, SONG Zengfu, WENG Shifu, YANG Zhanlan, XU Yizhuang, WU Jinguang. Sulfur Fine Particles as Stationary Phase for TLC/FTIR Analysis^†[J]. Chem. J. Chinese Universities, 2014, 35(4): 741.

Figures/Tables 7

Fig.1 XRD pattern of the product by the reaction between sodium thiosulfate and hydrochloric acid(A) and standard XRD pattern of sulfur particles(B)

Fig.2 FTIR spectrum of the sulfur particles

Fig.3 SEM image of the sulfur particles

Fig.4 Photographs of a traditional TLC plate(A) and a narrow-band TLC plate(B)

Fig.5 Photograph of a narrow-band TLC plate using sulfur particles as stationary phase to separate the mixture of rhodamine B and gentian violet(A) and the mixture of rhodamine B and bromophenol blue(B) after chromatographic experiment

Fig.6 FTIR spectra of gentian violet(A) and rhodamine B(B) on the sulfur narrow-band TLC plateMass fraction of sample: a. 100%; b. 0.5%; c. 0.2%; d. 0.1%. Mobile phase: tetrahydrofuran, methanol and ammonia water.

Fig.7 FTIR spectra of bromophenol blue(A) and rhodamine B(B) on the sulfur narrow-band TLC plate a. Pure sample; b. 0.2%(mass fraction) sample. Mobile phase: ethyl acetate, methanol and ammonia water.

References 22

[1]	He L.Y., Method and Application of Planar Chromatography(2nd Ed.), Chemical Industry Press, Beijing, 2005
	(何丽一. 平面色谱方法及应用, 北京: 化学工业出版社, 2005)
[2]	Sun Y.Q., Hu Y. Z., Selection and Optimization of HPLC Solvent System, Chemical Industry Press, Beijing, 2007
	(孙毓庆, 胡育筑. 液相色谱溶剂系统的选择与优化, 北京: 化学工业出版社, 2007)
[3]	Sherma J., Anal. Chem., 1988, 60, 74R—86R
[4]	Wu J.G., Modern Fourier Transform Infrared Spectroscopy Technology and Application, Press of Science and Technology, Beijing, 1994
	(吴瑾光. 近代傅里叶变换红外光谱技术及应用, 北京: 科学技术文献出版社, 1994)
[5]	Guo Q., Xu G. Y., Chang L. W., Chin. J. Anal. Chem., 1998, 26, 81—84
	(郭勍, 徐桂云, 常理文. 分析化学, 1998, 26, 81—84)
[6]	He K., Li X. G., Chen H. Y., Ye X. L., Deng Y. F., Chen X., Sun S. L., Chin. J. Anal. Chem., 2011, 39, 572—575
	(贺凯, 李学刚, 陈红英, 叶小利, 邓亚飞, 陈新, 孙胜亮. 分析化学, 2011, 39, 572—575)
[7]	McCoy N. R., Fiebig C. E., Anal. Chem., 1965, 37(4), 593—595
[8]	Sturm A. P., Parkhurst M. R., Skinner A. W., Anal. Chem., 1966, 38(9), 1244—1247
[9]	Percival J. C., Griffiths R. P., Anal. Chem., 1975, 47, 154—156
[10]	Fuller P.M., Griffiths R. P., Anal. Chem., 1978, 50, 1906—1910
[11]	Zuber E. G., Warren J. R., Begosh P. P., Anal. Chem., 1984, 56, 2935—2939
[12]	Lindsay B. L., Randall C. Y., Edward M. E., Anal. Chem., 1982, 54, 549—552
[13]	White L. R., Anal. Chem., 1985, 57, 1819—1822
[14]	Danielson D.N., Katon E. J., Bouffard P. S., Anal. Chem., 1992, 64, 2183—2186
[15]	Bouffard P.S., Katon E. J., Sommer J. A., Danielson D. N., Anal. Chem., 1994, 66, 1937—1940
[16]	Liu X., Pan Q. H., Ding J., Zhu Q., He A. Q., Yue S. J., Li X. P., Hu L. P., Xia J. M., Wei Y. J., Liu C. G., Yu J., Yang Z. L., Zhu X., Xu Y. Z., Wu J. G., Spectroscopy and Spectral Analysis,2011, 31(7), 1767—1771
	(刘溪, 潘庆华, 丁洁, 祝青, 贺安琪, 岳世娟, 李晓佩, 胡丽萍, 夏锦明, 魏永巨, 刘翠格, 余江, 杨展澜, 朱曦, 徐怡庄, 吴瑾光. 光谱学与光谱分析, 2011, 31(7), 1767—1771)
[17]	Zhu Q., Su X., Wu H. J., Zhai Y. J., Bu H. B. T. E., Xia J. M., Xu Y. Z., Wu J. G., Spectroscopy and Spectral Analysis,2012, 32(7), 1790—1794
	(祝青, 苏晓, 吴海军, 翟延君, 布和巴特, 夏锦明, 徐怡庄, 吴瑾光. 光谱学与光谱分析, 2012, 32(7), 1790—1794)
[18]	Liu W., Wu H. J., Wang X. P., Zhu Q., Kang T. G., He A. Q., Weng S. F., Yang Z. L., Xia J. M., Xu Y. Z., Wu J. G., Chem. J. Chinese Universities,2013, 34(6), 1347—1352
	(刘微, 吴海军, 王修鹏, 祝青, 康廷国, 贺安琪, 翁诗甫, 杨展澜, 夏锦明, 徐怡庄, 吴瑾光. 高等学校化学学报, 2013, 34(6), 1347—1352)
[19]	Zhu Q., Wu H. J., Wang F., He A. Q., Huang K., Wei Y. J., Liu C. G., Zhai Y. J., Weng S. F., Yang Z. L., Xu Y. Z., Noda I., Wu J. G., Journal of Planar Chromatography,2014, 27(2), 80—83
[20]	Wang F., Wu H. J., Anal. Methods,2013, 5, 4138—4144
[21]	Fan X. K., Guo R., Shi J. J., Wu H. J., He A. Q., Wei Y. J., Liu C. G., Weng S. F., Yang Z. L., Xu Y. Z., Isao N., Wu J. G., Journal of Spectroscopy,2013, doi:
[22]	Yao F.Y., Guo D. W., Du M. D., Inorganic Chemistry Books, Book Five, Science Press, Beijing, 1990
	(姚凤仪, 郭德威, 杜明德. 无机化学丛书, 第五卷, 北京: 科学出版社, 1990)