Determination of Cr(Ⅵ) by Spectrophotometry Combined with Ionic Liquid Aqueous Two-Phase Extraction
摘 要
移取水样2.0 mL,用水定容至20.0 mL,加入1.0 mL硫酸(1+7)溶液,2.5 g·L-1二苯碳酰二肼溶液1.0 mL,立即混匀。10.0 min后,依次加入24.0 g·L-1溴化1-丁基-3-甲基咪唑溶液1.0 mL,24.0 g磷酸氢二钾,混匀后,进行双水相萃取,以3 500 r·min-1转速离心2.0 min。将上层离子相移出,用水定容至3.0 mL,以试剂空白为参比液,于波长533 nm处测量吸光度。Cr (Ⅵ)的质量浓度在0.015~0.300 mg·L-1内与其吸光度呈线性关系,检出限(3s/k)为7.8×10-4mg·L-1,富集倍数为6.67倍。方法应用于测定实际水样中的Cr (Ⅵ),加标回收率在95.3%~111%之间。
Abstract
The water sample (2.0 mL) was diluted to 20.0 mL with water, then 1.0 mL of sulfuric acid (1+7) solution and 1.0 mL of 2.5 g·L-1 diphenylcarbazide solution were added and mixed immediately. After 10.0 min, 1.0 mL of 24.0 g·L-1 1-butyl-3-methylimidazolium bromide solution, 24.0 g dipotassium hydrogen phosphate were added in sequence, and then mixed well for aqueous two-phase extraction. Then the mixture was centrifuged at 3 500 r·min-1 for 2.0 min. The upper ionic phase was taken, and made up to 3.0 mL with water. The absorbance at 533 nm was measured with blank sample solution as reference. Linear relationship was found between the absorbance and the mass concentration of Cr(Ⅵ) in the range of 0.015-0.300 mg·L-1, with detection limit (3s/k) of 7.8×10-4mg·L-1 and enrichment factor of 6.67 times. The method was applied to determination of Cr(Ⅵ) in actual water samples, giving values of recovery obtained by standard addition method in the range of 95.3%-111%.
中图分类号 O657.32 DOI 10.11973/lhjy-hx201903014
所属栏目 工作简报
基金项目 国家自然科学基金面上项目(21375117);连云港市博士后项目(ZKK20171030);江苏省"六大人才高峰"高层次人才培养项目(XCL-181);淮海工学院研究生科研创新计划项目(XKY-CXX2017-16);连云港市"海燕计划"项目(2018-21)
收稿日期 2018/5/28
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联系人作者沙鸥(7993259@163.com)
备注王钰,硕士研究生,研究方向为样品前处理
引用该论文: WANG Yu,SHA Ou,FENG Yanli,SONG Yue,SHI Lishu. Determination of Cr(Ⅵ) by Spectrophotometry Combined with Ionic Liquid Aqueous Two-Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(3): 319~323
王钰,沙鸥,冯艳丽,宋跃,施礼数. 离子液体双水相萃取-分光光度法测定水中铬(Ⅵ)[J]. 理化检验-化学分册, 2019, 55(3): 319~323
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【6】TAFTI E N, DADFARNIA S, SHABANI A M H. Supramolecular dispersive liquid-liquid microextraction-based solidification of floating organic drops combined with electrothermal atomic absorption spectrometry for determination of chromium species[J]. International Journal of Environmental Analytical Chemistry, 2017,97(5):444-455.
【7】JORGE E O, ROCHA M M, FONSECA I T E, et al. Studies on the stripping voltammetric determination and speciation of chromium at a rotating-disc bismuth film electrode[J]. Talanta, 2010,81(1/2):556-564.
【8】OUYANG R, ZHANG W, ZHOU S, et al. Improved Bi film wrapped single walled carbon nanotubes for ultrasensitive electrochemical detection of trace Cr (Ⅵ)[J]. Electrochimica Acta, 2013,113:686-693.
【9】谭芳维.原子荧光光谱法测定食品中碘,铬及锑锭中汞的应用研究[D].南宁:广西大学, 2013:26-31.
【10】刘平.利用X荧光能谱仪快速测定合金钢中铬元素[J].分析仪器, 2017(1):29-33.
【11】沈兵,王练,奚奇辉,等.高效液相色谱法测定皮革中的六价铬[J].中国皮革, 2008(11):39-41.
【12】侯艳芳,周桂友.高效液相色谱法快速测定怀药中的六价铬[J].理化检验-化学分册, 2016,52(11):1306-1309.
【13】SUN Y C, LIN C Y, WU S F, et al. Evaluation of on-line desalter-inductively coupled plasma-mass spectrometry system for determination of Cr(Ⅲ), Cr(Ⅵ), and total chromium concentrations in natural water and urine samples[J]. Spectrochimica Acta Part B:Atomic Spectroscopy, 2006,61(2):230-234.
【14】GB/T 5750.6-2006生活饮用水标准检验方法金属指标[S].
【15】金洪洙,张晓霞,刘东方,等.浊点萃取-分光光度法测定水中痕量六价铬[J].环境监测管理与技术, 2009(4):51-53.
【16】TANG A N, JIANG D Q, JIANG Y, et al. Cloud point extraction for high-performance liquid chromatographic speciation of Cr (Ⅲ) and Cr (Ⅵ) in aqueous solutions[J]. Journal of Chromatography A, 2004,1036(2):183-188.
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