吹扫捕集气相色谱质谱法测定黄原酸的关键问题探究
The key problems in determination of xanthic acid by purge and trap gas chromatography-mass spectrometry
-
摘要: 通常状况下,黄原酸一般以黄原酸盐的状态存在,主要作为捕收剂广泛应用于矿产浮选.本研究采用吹扫捕集/气相色谱-质谱法测定黄原酸总量,对测定涉及的关键操作环节及重点技术问题进行了深入研究.研究了黄原酸种类、酸加入时间、pH、酸加入量和酸种类等样品前处理步骤中的影响因素,讨论了重金属、含盐量、氧化物以及化学性质相同的共存物质等方法干扰问题.其中水样中氧化物对测定的干扰问题较为突出,可通过加入5—20 mg硫代硫酸钠去除.此外,硫代硫酸钠的加入还可将样品保存时间由1 d延长到2周.Abstract: Under normal circumstances,xanthic acid generally exists in the state of xanthate, and is used as a collector in mineral flotation mainly. In this research, the total amount of xanthic acid was determined by purge and trap/gas chromatography-mass spectrometry. The key operational steps and technical issues were further studied, including the influence factors of xanthogen type, acid addition time, pH, acid addition amount, acid type, et al in the sample preparation step. The problems of method interference were discussed, such as heavy metals, salinity, oxides and coexisting substances with same chemical nature. The interference of oxides in the water sample was more prominent, which could be removed by adding 5-20 mg sodium thiosulfate. Besides, sample storage time was extended from one day to two weeks by using sodium thiosulfate.
-
[1] 宋小霞,朱静,张承屏,等,黄药的研制、应用和水污染处理研究进展[J]. 贵州化工, 2012,37(3):19-23. SONG X X,ZHU J,ZHANG C P,et al. Advance in research of production,application and treatment process of xanthate in dressing wastewater[J]. Guizhou Chemical Industry, 2012,37(3):19-23(in Chinese).
[2] 朱照照. 黄原酸盐的危害[J]. 有色金属, 2011,63(2):276-279. ZHU Z Z. Hazards of xanthate[J]. Nonferrous Metals, 2011,63(2):276-279(in Chinese).
[3] 朱红霞,徐秀艳,于建钊,等. 铜试剂亚铜分光光度法测定丁基黄原酸方法的探讨[J]. 光谱实验室,2013,30(1):341-348. ZHU H X, XU X Y, YU J Z, et al. Discussion of determining butyl xanthate by sodium diethyldithiocarbamate cuprous spectrophotometry[J]. Chinese Journal of Spectroscopy Laboratory, 2013,30(1):341-348(in Chinese).
[4] 王美飞,胡思宇,杨丽莉. 吹扫捕集-气相色谱-质谱法测定水中痕量丁基黄原酸[J]. 中国环境监测,2011,27(增刊):12-14. WANG M F, HU S Y, YANG L L. Determination for butylxanthic acid in water by purge and trap-gas chromatography-mass spectrometry[J]. Environmental Monitoring in China, 2011 ,27(Suppl):12-14(in Chinese).
[5] 彭涛,王超,吕怡兵,等. 超高效液相色谱法快速检测地表水中丁基黄原酸[J]. 中国环境监测,2013,29(2):65-68. PENG T, WANG C, LV Y B, et al. Rapid analysis of butylxanthic acid in surface water by ultra performance liquid chromatography[J]. Environmental Monitoring in China, 2013,29(2):65-68(in Chinese).
[6] 刘景泰,李振国. 超高效液相色谱-质谱法测定地表水中丁基黄原酸[J]. 中国环境监测,2012,28(5):76-78. LIU J T, LI Z G. Determination of butylxanthate in ground water by UPLC-MS[J]. Environmental Monitoring in China, 2012,28(5):76-78(in Chinese).
[7] 付晓燕,李振国,刘景泰,等. 超高效液相色谱-串联质谱测定水中丁基黄原酸[J]. 环境工程,2018,36(增刊):19-22. FU X Y,LI Z G,LIU J T,et al. Determination of butyl xanthate in water by ultra performance liquid chromatography-tandem mass spectrometry[J]. Environmental Engineering, 2018 ,36(Suppl):19-22(in Chinese).
[8] 朱红霞,刀婿,彭涛. 离子色谱法测定丁基黄原酸[J]. 中国测试,2015,41(4):36-38. ZHU H X, DAO X, PENG T. Determination of butyl xanthate by ion chromatography[J]. China Measurement & Test, 2015,41(4):36-38(in Chinese).
[9] 朱红霞,白雪,黄颖霞. 离子色谱法测定水中的6种黄原酸盐[J]. 理化检验-化学分册,2016,52(9):1065-1067. ZHU H X, BAI X, HUANG Y X. Determination and separation of six kinds of xanthogenate with ion chromatography[J]. PTCA(Part B:CHEM.ANAL.), 2016,52(9):1065-1067(in Chinese).
[10] KEMPPINEN J, AALTONEN A, SIHVONEN T, et al. Xanthate degradation occurring in flotation process waters of a gold concentrator plant[J]. Minerals Engineering, 2015,80:1-7(in Chinese). [11] FONTENELE R S,PILAR HIDALGO, IVANO G R, et al. Flow injection analysis of ethyl xanthate by in-line dialysis and UV spectrophotometric detection[J]. Talanta,2007,72:1017-1022. [12] 林诗云,杨梅,李禹,等. 吹扫捕集-气相色谱-质谱法测定水中丁基黄原酸及27种挥发性有机物[J]. 理化检验-化学分册,2016,52(4):436-439. LIN S Y, YANG M, LI Y, et al. GC-MS Determination of butylxanthic acid and 27 volatile organic compounds in water with purging and trapping[J]. PTCA(Part B:Chem Anal), 2016,52(4):436-439(in Chinese).
[13] 吉正元,普学伟. 吹扫捕集-气相色谱/质谱法测定水中的乙醛、丙烯醛、丙烯腈、吡啶、松节油和丁基黄原酸[J]. 环境监控与预警, 2017,9(5):16-19. JI Z Y, PU X W. Determination of acetaldehyde, acrolein, acrylonitrile, pyridine, turpentine and butylxanthic acid in water by purge and trap-gas chromatography/mass spectrometry[J]. Environmental Monitoring and Forewarning, 2017,9(5):16-19(in Chinese).
[14] 李振国,王钢栋,吹扫捕集气相色谱-质谱法测定土壤中的代森锌[J].中国环境监测,2014,30(4):163-165. LI Z G, WANG G D. Determination of zlneb in soil by purge and trap GC/MS[J]. Environmental Monitoring in China, 2014,30(4):163-165(in Chinese).
[15] 周伟峰,王婷,马兴华, 等. 顶空-气相色谱法测定土壤中代森锌的残留[J].环境化学,2015,34(7):1380-1382. ZHOU W F, WANG T,MA X H,et al. Determination of zlneb in soil by headspace-gas chromatography[J]. Environmental Chemistry, 2015,34(7):1380-1382(in Chinese).
[16] YUKIO NAGAOSA, TORU MIZUYUKI. Determination of Cu(Ⅱ) and Ni(Ⅱ) as chelates with butyl xanthate by liquid chromatography with electrochemical and spectrophotometric detection[J]. Analytica Chimica Acta,1995,311:225-229. [17] RAO B S, RAMAKRISHNA K, VENKATESWARLU P. New extraction-spectrophotometric determination of iron(Ⅲ) with potassium isobutyl xanthate[J]. J Indian Chen Soc, 2003,80(8):295-296.
计量
- 文章访问数: 1637
- HTML全文浏览数: 1637
- PDF下载数: 44
- 施引文献: 0