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用于测定葡萄酒中二氧化硫的光学传感器。

Optical sensor for sulfur dioxide determination in wines.

作者信息

Silva Karime R B, Raimundo Ivo M, Gimenez Iara F, Alves Oswaldo L

机构信息

Instituto de Química, UNICAMP, Caixa Postal 6154, 13084-971 Campinas, Brazil.

出版信息

J Agric Food Chem. 2006 Nov 15;54(23):8697-701. doi: 10.1021/jf061553h.

Abstract

A method for the determination of free and total sulfur dioxide in wines, based on the use of an optical sensor that employs a dichlorobis(diphenylphosphino)methane dipalladium I complex [Pd(2)(dppm)(2)Cl(2)] immobilized in a PVC membrane plasticized with o-nitrophenyloctylether (o-NPOE) is described. A sensing membrane [4.2% Pd(2)(dppm)(2)Cl(2), 20.8% PVC, and 75% o-NPOE] was adapted to the tip of a bifurcated optical fiber bundle to perform reflectance measurements at 550 nm. The detection system consisted of two cells (40 mL), which hold the sample solution (plus reagents) and the optical sensor, respectively. For the determination of free SO(2), a wine sample was mixed with H(2)SO(4) solution in the sample cell, into which N(2) was bubbled, providing mixing of the solutions and conducting the SO(2) formed toward the detection cell. For determination of total SO(2), a KOH solution was mixed with the wine in the sample cell. Afterward, an H(2)SO(4) solution was added to the cell, and then N(2) was bubbled to conclude the measurement. Linear responses up to 50 and 150 mg L(-1) were obtained for free and total SO(2), with detection limits of 0.37 and 0.70 mg L(-1), respectively. The repeatability of the method was evaluated by carrying out 10 measurements using a single wine sample, providing relative standard deviation values of 2.2 and 2.5% for free and total SO(2), respectively. The sensing membrane prepared from 10 muL of the cocktail solution lasted for 80 measurements, whereas those prepared from 200 muL can be used for 250 measurements. The method was applied to free and total SO(2) determination in wines, and the results did not show significant difference from those obtained with the Ripper reference method at a confidence level of 95%.

摘要

描述了一种测定葡萄酒中游离二氧化硫和总二氧化硫的方法,该方法基于使用一种光学传感器,该传感器采用固定在邻硝基苯基辛基醚(o-NPOE)增塑的PVC膜中的二氯双(二苯基膦基)甲烷二钯(I)配合物[Pd(2)(dppm)(2)Cl(2)]。将传感膜[4.2% Pd(2)(dppm)(2)Cl(2)、20.8% PVC和75% o-NPOE]适配到分叉光纤束的尖端,以在550 nm处进行反射率测量。检测系统由两个池(40 mL)组成,分别容纳样品溶液(加试剂)和光学传感器。为了测定游离SO(2),将葡萄酒样品与样品池中的H(2)SO(4)溶液混合,向其中通入N(2),使溶液混合并将形成的SO(2)导入检测池。为了测定总SO(2),将KOH溶液与样品池中的葡萄酒混合。然后,向池中加入H(2)SO(4)溶液,接着通入N(2)以完成测量。游离和总SO(2)的线性响应范围分别高达50和150 mg L(-1),检测限分别为0.37和0.70 mg L(-1)。通过使用单个葡萄酒样品进行10次测量来评估该方法的重复性,游离和总SO(2)的相对标准偏差值分别为2.2%和2.5%。由10 μL混合溶液制备的传感膜可进行80次测量,而由200 μL制备的传感膜可用于250次测量。该方法应用于葡萄酒中游离和总SO(2)的测定,在95%的置信水平下,结果与用里珀参考方法获得的结果没有显著差异。

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