【作者】 余娟；

【导师】 卢家炯； 闵亚光；

【作者基本信息】 广西大学 ， 制糖工程， 2007， 硕士

【摘要】 二氧化硫含量是白砂糖的一项重要质量指标。目前，我国白砂糖中二氧化硫的国标测定方法是盐酸副玫瑰苯胺法。该法简单、准确，但也存在一些不足的地方：一是剧毒试剂HgCl₂的使用；二是二氧化硫标准溶液的不稳定；三是显色剂配制的不确定。前者剧毒试剂的使用，不仅造成环境污染，还危害到化验人员的安全。后两个不足直接影响到该法的精密度、准确度、灵敏度、不确定度等，造成较大的测定误差。因此，探讨一种无毒（或低毒）、稳定、重现性好的无汞盐酸副玫瑰苯胺分光光度法或其它方法势在必行。本课题研究了盐酸副玫瑰苯胺法（改良显色剂）、甲醛吸收—盐酸副玫瑰苯胺分光光度法、三乙醇胺吸收一盐酸副玫瑰苯胺分光光度法、离子色谱法在测定白砂糖中二氧化硫的应用。主要的研究内容有：1、国标方法的分析及盐酸副玫瑰苯胺法（改良显色剂）的研究。2、无汞盐酸副玫瑰苯胺分光光度法的探讨：（1）甲醛吸收—盐酸副玫瑰苯胺分光光度法：5mL白砂糖样液+5mL甲醛吸收工作液+1mL氨磺酸钠溶液+0.5mL氢氧化钠+1mL盐酸副玫瑰苯胺溶液，室温，20min，1cm比色皿，波长579nm；（2）三乙醇胺吸收—盐酸副玫瑰苯胺分光光度法：5mL白砂糖样液+5mL三乙醇胺吸收工作液+2mL甲醛+1mL盐酸副玫瑰苯胺溶液，室温，20min，1cm比色皿，波长579nm。3、离子色谱法的探讨：lonPac AS11型分离柱；NaOH作淋洗液，梯度洗脱，流速1.00mL／min；抑制电导检测器检测；以保留时间定性，外标法定量。4、对比分析各种方法的相关评价指标（精密度、准确度、灵敏度、不确定度），并作出综合评价。结果表明，论文研究的几种方法都不同程度的优于国标方法，其中，最具有应用前景的方法为甲醛吸收—盐酸副玫瑰苯胺分光光度法。盐酸副玫瑰苯胺法（改良显色剂）、甲醛吸收—盐酸副玫瑰苯胺分光光度法、三乙醇胺吸收—盐酸副玫瑰苯胺分光光度法、离子色谱法测定结果与国标法无显著差异，初步确定应可用于白砂糖中二氧化硫的测定。更多还原

【Abstract】 One of the most important qualitative indexes about white granulated sugaris the SO₂ content. At present, the national standard method for determinationthe SO₂ content in white granulated sugar is pararosaniline hydrochloridemethod. This method is brief and accurate; meanwhile this method has severaldisadvantages: Firstly, the oxious reagent HgCl₂ is used, which will causeenvironmental pollution and endanger the safety of analyst. Secondly, the SO₂standard solution is unstable and the chromomeric agent is uncertain, which willstraight influence the precision, the accuracy, the sensitivity and the uncertaintyof this method. So, the pararosaniline hydrochloride （without mercury salt）spectrophotometries and other methods which are innoxious or harmfulless,stable, better repeatability must be researched.This paper studied these methods: pararosaniline hydrochloride method（improved chromomeric agent）, formaldehyde sampling-pararosanilinehydrochloride spectrophotometry, triethanolamine sampling-pararosanilinehydrochloride spectrophotometry, chromatography of ions, and theseapplications in determination the SO₂ content in white granulated sugar. Themain research contents were as follows:1. The analysis of the national standard method and the research ofpararosaniline hydrochloride method （improved chromomeric agent）. 2. The research of pararosaniline hydrochloride （without mercury salt）spectrophotometries: （1）the process of formaldehyde sampling-pararosanilinehydrochloride spectrophotometry was: 5mL sugar solution+5mL formaldehydesolution+1mL sodium sulfamate+0.5mL sodium hydroxide+1mLpararosaniline hydrochloride, ambient temperature, 20min, 10mm cuvette,590nm wavelength; （2）the process of triethanolamine-sampling pararosanilinehydrochloride spectrophotometry was: 5mL sugar solution+5mLtriethanolamine solution+2mL formaldehyde+1 mL pararosanilinehydrochloride, ambient temperature, 20min, 10mm cuvette, 590nm wavelength.3. The research of chromatography of ions: IonPac AS11 splitter; NaOH aseluent, gradient elution, 1.00mL/min; suppressed conductively detection;qualitative analysis with retaining time, quantitative analysis with externalreference method.4. The comparison of these methods （the precision, the accuracy, thesensitivity and the uncertainty） and making comprehensive evaluation of them.The results indicated that these methods were more applicative than the nationalstandard method, and the method which had the best applicative prospect wasformaldehyde sampling-pararosaniline hydrochloride spectrophotometry.Comparing with the experimental results by the national standard method,these methods had no significant differences and could be applied indetermination the SO₂ content in white granulated sugar preliminarily.更多还原