Abstract:Methyltin mercaptide is widely used as one of the best heat stabilizer in the polyvinylchloride (PVC) thermal processing due to its excellent stability, good transparency, high compatibility and weather resistance. The content of sulfur and tin significantly affects its quality and performance, so it is of great significance to develop an analytical method for the simultaneous determination of sulfur and tin. Inductively coupled plasma atomic emission spectrometry (ICP-OES) has been a powerful analytical tool for a myriad of complex samples owing to its advantages of the low detection limits, rapid and precise determinations over wide dynamic ranges, freedom from chemical inter-element interferences, the high sample throughput and above all, simultaneous multi-elements analysis. Microwave technique as a well-developed method for sample preparation can dramatically reduce the digestion time and the loss of volatile elements compared with the traditional open digestion. Hereby, a microwave-assisted acid digestion (MW-AAD) procedure followed by inductively coupled plasma optical emission spectroscopy (ICP-OES) analysis was developed for the simultaneous determination of Sn and S in methyltin mercaptide. This method has the advantages of simplicity, rapidness, good accuracy, green and less use of samples. Parameters affecting the MW-AAD such as the digestion solution and digestion time were optimized by using a chemical analyzed reference sample (DX-181) to attain tin and sulfur quantitative recoveries. HNO3-HCl-HClO4 (v/v/v=9∶3∶1) and 10 min were the optimum digestion solution and digestion time, respectively. Under optimum conditions, the standard addition method and the standard calibration curve method were both been used to detect Sn and S in DX-181. There was no significant difference between two methods and the relative deviations to the chemical analysis values were both less than 2%. Additionally, the accuracy of the MW-AAD method was examined by analyzing three methyltin mercaptide samples (DX-181,DX-990,DX-960). The results were satisfactory with the relative deviations (<3%) and the recoveries of standard addition (99%~102%).
[1] GB/T26026—2010. Methyltin Mercaptide(硫醇甲基锡). Inspection and Quarantine of the People’s Republic of China(中华人民共和国国家标准). [2] Thangavel S, Dash K, Dhavile S M et al. Talanta, 2015, 131: 505. [3] Villanueva-Alonso J, Pena-Vazquez E, Barciela-Alonso M C, et al. Atomic Spectroscopy, 2014, 35(1): 7. [4] Mketo N, Nomngongo P N, Ngila J C. Analytical Methods, 2014, 6(21): 8505. [5] Santelli R E, Oliveira E P, de Carvalho M d F B,et al. Spectrochimica Acta Part B: Atomic Spectroscopy, 2008, 63(7): 800. [6] Grindlay G, Maestre S, Gras L,et al. Journal of Analytical Atomic Spectrometry, 2006, 21(12): 1403. [7] Galbács G, Szorcsik A, Galbács Z,et al. Talanta, 2000, 52(6): 1061. [8] Burger K, Nagy L, Buzás N,et al. Journal of the Chemical Society, Dalton Transactions, 1993, 16: 2499. [9] Sánchez R, Todolí J L, Lienemann C P,et al. Spectrochimica Acta Part B: Atomic Spectroscopy, 2013, 88: 104. [10] Abu-Samra A, Morris J S, Koirtyohann S. Analytical Chemistry, 1975, 47(8): 1475. [11] ZHANG Liu-yi, FU Chuan, YANG Fu-mo,et al (张六一,付 川,杨复沫,等). Spectroscopy and Spectral Analysis(光谱学与光谱分析), 2014, 34(11): 3109. [12] Chand V, Prasad S. Microchemical Journal, 2013, 111: 53. [13] Sun Y C, Chi P H, Shiue M Y. Analytical Sciences, 2001, 17(12): 1395. [14] Kalembkiewicz J, Sitarz-Palczak E. Atomic Spectroscopy, 2001, 22(6): 433.