Determination of Chromium in Beer Yeast by Color-Fading Spectrophotometry with Wright's Stain
摘 要
取啤酒酵母样品0.200 0 g,用硝酸及过氧化氢微波消解,所得透明溶液蒸发至近干,冷却,加水溶解盐类。在pH 12的条件下滴加高锰酸钾溶液将铬(Ⅲ)氧化至六价,过量高锰酸钾滴加乙醇使还原褪色,用稀硝酸调节酸度到近中性。过滤,滤液定容至50 mL。取此溶液2.0 mL,置于25 mL容量瓶中,随后依次加入50 g·L-1硫脲溶液2 mL,5 mol·L-1磷酸溶液1.0 mL,0.2 mol·L-1碘化钾溶液4.0 mL,10 g·L-1聚乙烯醇溶液3.5 mL和0.5 g·L-1瑞氏色素溶液4.0 mL,加水定容并摇匀。同时按相同操作制备试剂空白,但不加样品溶液。避光反应20 min,试样溶液中的铬(Ⅵ)在此体系中反应后导致瑞氏色素褪色。于波长662 nm处分别测得试样和空白溶液的吸光度A和A0,并计算ΔA(A0-A)。结果表明:ΔA与铬(Ⅵ)的质量浓度在0.40 mg·L-1以内呈线性关系,检出限(3s/k)为0.005 5 mg·L-1。实样的分析结果与原子吸收光谱法所测结果一致。测定值的相对标准偏差(n=5)在1.4%~2.3%之间,加标回收率在99.1%~102%之间。
Abstract
The beer yeast sample (0.200 0 g) was digested with HNO3 and H2O2 in microwave digestor. The clear solution obtained was evaporated to near dryness. The residue was taken up with water and its acidity was adjusted to pH 12. Solution of KMnO4 was added dropwise to oxide Cr(Ⅲ) to Cr(Ⅵ) and excess of KMnO4 was de-colorized by addition of few drops of C2H5OH. The solution was then neutralized by dilute HNO3, filtered and its volume was made up to 50 mL. 2.0 mL of this sample solution were transfered to a 25 mL volumetric flask, and 2 mL of 50 g·L-1 thiourea solution, 1.0 mL of 5 mol·L-1 H3PO4 solution, 4.0 mL of 0.2 mol·L-1 KI solution, 3.5 mL of 10 g·L-1 PVA solution and 4.0 mL of 0.5 g·L-1 Wright's stain solution were added in succession, and its volume was made up to 25 mL with water with thorough mixing. Simultanuously, a blank solution was prepared in the same way but without the addition of sample solution. The 2 solutions were set for 20 min in darkness. Due to the action of Cr(Ⅵ) in the reaction system, color-fading of Wright's stain was observed. Absorbance of sample solution (A) and blank solution (A0) were measured at the wavelength of 662 nm, and ΔA were calculated by A0-A. It was shown that linear relationship between values of ΔA and mass concentration of Cr(Ⅵ) was kept within 0.40 mg·L-1, with detection limit (3s/k) of 0.005 5 mg·L-1. In analysis of some substantial sample by this method, the results obtained were in consistency with those obtained by AAS. Values of RSDs (n=5) found were in the range of 1.4% to 2.3%. Test for recovery was made by the standard addition method, giving values of recovery in the range of 99.1% to 102%.
中图分类号 O657.3 DOI 10.11973/lhjy-hx201803016
所属栏目 工作简报
基金项目 2015年度国家自然科学基金面上项目(21571105);2014年江苏省高校“青蓝工程”资助项目;2015年度连云港市第五期“521工程”科研项目;2015年江苏省高等学校大学生创新创业训练计划项目(201511585003Y)
收稿日期 2017/3/10
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备注李人宇(1972-),男,山东烟台人,教授,博士,主要从事应用化学研究,lirenyu518@163.com
引用该论文: LI Renyu,HUANG Jinzhuang,LI Yongmei,ZHOU Jiahong. Determination of Chromium in Beer Yeast by Color-Fading Spectrophotometry with Wright's Stain[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(3): 322~325
李人宇,黄金状,李咏梅,周家宏. 瑞氏色素褪色分光光度法测定啤酒酵母中铬含量[J]. 理化检验-化学分册, 2018, 54(3): 322~325
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【9】杨慧,刘俊华,丁良,等.催化动力学分光光度法测定粉丝中的微量铬[J].食品研究与开发, 2014,35(6):75-78.
【10】李晓燕,朱樱,欧阳泉根,等.二苯碳酰二肼光度法测定微量铬的改进[J].理化检验-化学分册, 2016,52(6):729-731.
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【12】高向阳,高遒竹,张小燕,等.微波消解-流动注射化学发光法快速测定调味品中的微量铬[J].中国调味品, 2016,41(10):101-104.
【13】王征帆.库仑分析法测定富铬酵母中铬含量研究[J].中国调味品, 2013,38(8):102-103.
【14】周桂友,侯艳芳,封琳,等.反相高效液相色谱法测定陶瓷饰品中六价铬的溶出量[J].理化检验-化学分册, 2015,51(1):86-90.
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