CN112285100A - 一种检测次氯酸钠水溶液中自由基浓度的方法 - Google Patents
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Abstract
本发明公开了一种检测次氯酸钠水溶液中自由基浓度的方法,步骤:(1)在比色管中加入捕获剂、硫酸亚铁水溶液、待测的次氯酸钠水溶液,加水,超声,溶液是否显紫色,显紫色则有自由基,测吸光度;(2)在11支比色管中分别加入捕获剂,再加入梯度为0.1ml的氯化铁水溶液,加水,超声,溶液显紫色梯度,测吸光度,得到吸光度与氯化铁水溶液浓度的对应曲线,由于自由基摩尔浓度与氯化铁水溶液摩尔浓度之比为1:1;得到吸光度与自由基摩尔浓度的标准曲线,将待测的次氯酸钠水溶液的吸光度值代入标准曲线即可得到自由基摩尔浓度。本发明对于组分复杂的***无需分离,自然氧化程度低,产物稳定性高,与自由基浓度线性关系良好,测量范围宽。
Description
技术领域
本发明涉及一种检测次氯酸钠水溶液中自由基浓度的方法,属于化学检测领域。
背景技术
随着水质不断恶化、水质标准不断提高,水处理领域中膜分离技术被越来越多的应用。膜分离技术是一种无相变、低能耗的物理分离过程,具有高效、节能、无污染、操作方便等特点,能有效截留污染物、细菌和病毒。但在使用过程中膜表面或膜孔内会吸附、沉积污染物,造成膜孔径变小或堵塞,引发的膜污染问题成为膜技术使用的限制因素。因此为有效减缓膜污染,常用次氯酸钠水溶液作化学清洗剂。此外次氯酸钠水溶液也被用作氧化剂、杀菌剂、消毒剂,在污水处理和饮用水处理领域广泛应用,作为一种能够释放活性氯和活性氧的氧化性药剂,在使用过程中会产生自由基。适量的自由基浓度可有效杀菌、消毒,减缓膜表面污染物,而自由基过量存在则会对膜的结构和性能造成严重损伤,影响膜的使用寿命和截留能力,因此掌握检测和控制次氯酸钠水溶液中自由基浓度的方法是有必要的。
目前水溶液中自由基的检测方法包括电子自旋共振法(ESR),是检测自由基最直接的一种方法,这种方法虽然简单有效,但仪器价格昂贵,定量分析不够准确,针对不同种类自由基需要选取不同的捕获剂;化学发光法(CL)廉价、灵敏度高、反应快速,但选择性差,对组分不能很好定性,实际应用中受到限制;高效液相色谱法(HPLC),其灵敏度高,检出限低,但也存在设备昂贵,反应过程复杂,易产生中间产物等不足。
发明内容
本发明的目的是克服现有技术的不足,提供一种检测次氯酸钠水溶液中自由基浓度的方法。
本发明的技术方案概述如下:
一种检测次氯酸钠水溶液中自由基浓度的方法,包括如下步骤:
(1)在比色管中加入2ml捕获剂、1-3ml浓度为8-10mM硫酸亚铁水溶液、0.5-5ml待测的次氯酸钠水溶液,加去离子水至15ml,超声10-30分钟,37℃水浴加热10-30分钟,观察比色管中溶液是否显紫色,显紫色则有自由基,用分光光度计测量吸光度;
(2)在11支比色管中分别加入2ml捕获剂,再加入范围在0-1ml、梯度为0.1ml的、pH=2-4的8-10mM氯化铁水溶液,加去离子水至15ml,超声10-30分钟,37℃水浴加热10-30分钟,比色管中溶液显紫色梯度,用分光光度计依次测量吸光度,得到吸光度与氯化铁水溶液浓度的对应曲线,由于自由基摩尔浓度与氯化铁水溶液摩尔浓度之比为1:1;得到吸光度与自由基摩尔浓度的标准曲线,将步骤(1)获得的吸光度值代入所述标准曲线即可得到自由基摩尔浓度。
捕获剂按比例由0.1ml无水乙醇、0.9ml去离子水和0.01mmol水杨酸组成。
用分光光度计测量吸光度时波长是510nm。
所述待测的次氯酸钠水溶液的pH范围为1-12。
本发明的优点:
本发明的方法,含水杨酸的捕获剂药品廉价易得,对于组分复杂的***无需分离,自然氧化程度低,产物稳定性高,与自由基浓度线性关系良好,测量范围宽。
附图说明
图1为吸光度与自由基摩尔浓度的标准曲线。
图2(a)为自由基浓度随pH变化规律,(b)次氯酸钠组分随pH变化。
图3为反应前后的紫外吸收光谱图。
具体实施方式
下面通过具体实施例对本发明作进一步的说明。
实施例1
一种检测次氯酸钠水溶液中自由基浓度的方法,包括如下步骤:
(1)在25mL具塞比色管中加入2ml捕获剂、2ml浓度为10mM硫酸亚铁水溶液、3ml待测的次氯酸钠水溶液(pH为7,在空气中暴露),加去离子水至15ml,超声20分钟,37℃水浴加热20分钟,观察比色管中溶液显紫色,显紫色则产生自由基,用分光光度在波长510nm处测量吸光度为0.658;
(2)在11支比色管中分别加入2ml捕获剂,再加入0、0.1、0.2、0.3、0.4、0.5、0.6、0.7、0.8、0.9、1ml、pH=3的10mM氯化铁水溶液,加去离子水至15ml(此时比色管中氯化铁水溶液浓度分别为0、0.067、0.133、0.2、0.267、0.333、0.4、0.467、0.533、0.6、0.667mM),超声20分钟,37℃水浴加热20分钟,经0.45μm滤膜滤出后,比色管中溶液显紫色梯度,用10mm比色皿在波长510nm处,以水为参比用分光光度计依次测量吸光度,得到吸光度与氯化铁水溶液浓度的对应曲线,由于自由基摩尔浓度与氯化铁水溶液摩尔浓度之比为1:1,以吸光度为纵坐标,以自由基摩尔浓度为横坐标,绘制吸光度与自由基摩尔浓度的标准曲线如图1所示,将步骤(1)获得的吸光度值代入标准曲线即可得到自由基摩尔浓度为0.476mM。
本发明可以检测的自由基浓度范围为0.05334-0.80004mM,检出限0.00156mM。
捕获剂按比例由0.1ml无水乙醇、0.9ml去离子水和0.01mmol水杨酸组成。
实施例2
一种检测次氯酸钠水溶液中自由基浓度的方法,包括如下步骤:
(1)在25mL具塞比色管中加入2ml捕获剂、1ml浓度为8mM硫酸亚铁水溶液、0.5ml待测的次氯酸钠水溶液(pH为1,在空气中暴露),加去离子水至15ml,超声10分钟,37℃水浴加热10分钟,观察比色管中溶液是否显紫色,显紫色则产生自由基,用分光光度计在波长510nm处测量吸光度为0.281;
(2)在11支比色管中分别加入2ml捕获剂,再加入0、0.1、0.2、0.3、0.4、0.5、0.6、0.7、0.8、0.9、1ml、pH=4的8mM氯化铁水溶液,加去离子水至15ml,(此时比色管中氯化铁水溶液浓度分别为0、0.053、0.107、0.16、0.213、0.267、0.32、0.373、0.427、0.48、0.53mM),超声10分钟,37℃水浴加热10分钟,经0.45μm滤膜滤出后,比色管中溶液显紫色梯度,用10mm比色皿在波长510nm处,以水为参比用分光光度计依次测量吸光度,得到吸光度与氯化铁水溶液浓度的对应曲线,由于自由基摩尔浓度与氯化铁水溶液摩尔浓度之比为1:1,以吸光度为纵坐标,以自由基摩尔浓度为横坐标,绘制吸光度与自由基摩尔浓度的标准曲线,将步骤(1)获得的吸光度值代入标准曲线即可得到自由基摩尔浓度为0.182mM。本发明可以检测的自由基浓度范围为0.05334-0.80004mM,检出限0.00156mM。
捕获剂按比例由0.1ml无水乙醇、0.9ml去离子水和0.01mmol水杨酸组成。
实施例3
一种检测次氯酸钠水溶液中自由基浓度的方法,包括如下步骤:
(1)在25mL具塞比色管中加入2ml捕获剂、3ml浓度为8mM硫酸亚铁水溶液、5ml待测的次氯酸钠水溶液(pH为12,在空气中暴露),加去离子水至15ml,超声30分钟,37℃水浴加热30分钟,观察比色管中溶液是否显紫色,显紫色则产生自由基,用分光光度计在波长510nm处测量吸光度为0.573;
(2)在11支比色管中分别加入2ml捕获剂,再加入0、0.1、0.2、0.3、0.4、0.5、0.6、0.7、0.8、0.9、1ml、pH=2的10mM氯化铁水溶液,加去离子水至15ml,(此时比色管中氯化铁水溶液浓度分别为0、0.067、0.133、0.2、0.267、0.333、0.4、0.467、0.533、0.6、0.667mM),超声30分钟,37℃水浴加热30分钟,经0.45μm滤膜滤出后,比色管中溶液显紫色梯度,用10mm比色皿在波长510nm处,以水为参比用分光光度计依次测量吸光度,得到吸光度与氯化铁水溶液浓度的对应曲线,由于自由基摩尔浓度与氯化铁水溶液摩尔浓度之比为1:1,以吸光度为纵坐标,以自由基摩尔浓度为横坐标,绘制吸光度与自由基摩尔浓度的标准曲线,将步骤(1)获得的吸光度值代入标准曲线即可得到自由基摩尔浓度为0.376mM。
本发明可以检测的自由基浓度范围为0.05334-0.80004mM,检出限0.00156mM。
捕获剂按比例由0.1ml无水乙醇、0.9ml去离子水和0.01mmol水杨酸组成。
次氯酸钠水溶液中的组分受到pH影响有不同存在形态。pH1-5范围内,次氯酸钠水溶液中的组分是HClO和Cl2,并随着pH增加,次氯酸浓度逐渐增加而氯气浓度逐渐降低,羟基自由基的浓度随之增加。此范围内ClO-是自由基形成的限制性物质,酸性条件下形成的HO·浓度低,反应机理方程式为:
HClO→HO·+Cl·……(1)
Cl·+HClO→HO·+Cl2……(2)
总方程式为:2HClO→2HO·+Cl2……(3)
pH5-9范围内,次氯酸钠水溶液中的组分是HClO和ClO-,两者之间的比率应在降解动力学中起主要作用。其中随着pH增加,次氯酸浓度逐渐降低而次氯酸根离子浓度逐渐增加,产生自由基浓度高。次氯酸钠水溶液会生成羟基自由基与氧氯自由基,反应机理方程式为:
HClO+ClO-→ClO·+Cl-+HO·……(4)
HO·+ClO-→ClO·+OH-……(5)
ClO·+ClO-+OH-→2Cl-+O2+HO·……(6)
总方程式为:HClO+3ClO-→ClO·+HO·+O2+3Cl-……(7)
pH9-12范围内,HClO是自由基形成的限制性物质,其浓度逐渐降低,导致溶液中的自由基浓度明显降低。次氯酸钠溶液pH>12时,会生成Fe(OH)3沉淀,抑制紫色络合物生成。因此水杨酸分光光度法测试自由基的范围在pH1-12,如图2所示。
羟基自由基和氧氯自由基再分别与亚铁离子反应,生成三价铁离子,反应机理方程式为:
Fe2++HO·→Fe3++OH-……(8)
Fe2++ClO·→Fe3++ClO-……(9)
以上可知,自由基摩尔浓度与三价铁离子摩尔浓度之比为1:1。
而后三价铁离子再与水杨酸捕获剂反应生成一种紫色络合物,通过反应前后紫外-可见吸收光谱测定,认为该物质在510nm波长处有最大吸收峰,如图3所示。
Claims (4)
1.一种检测次氯酸钠水溶液中自由基浓度的方法,其特征在于包括如下步骤:
(1)在比色管中加入2ml捕获剂、1-3ml浓度为8-10mM硫酸亚铁水溶液、0.5-5ml待测的次氯酸钠水溶液,加去离子水至15ml,超声10-30分钟,37℃水浴加热10-30分钟,观察比色管中溶液是否显紫色,显紫色则有自由基,用分光光度计测量吸光度;
(2)在11支比色管中分别加入2ml捕获剂,再加入范围在0-1ml、梯度为0.1ml的、pH=2-4的8-10mM氯化铁水溶液,加去离子水至15ml,超声10-30分钟,37℃水浴加热10-30分钟,比色管中溶液显紫色梯度,用分光光度计依次测量吸光度,得到吸光度与氯化铁水溶液浓度的对应曲线,由于自由基摩尔浓度与氯化铁水溶液摩尔浓度之比为1:1;得到吸光度与自由基摩尔浓度的标准曲线,将步骤(1)获得的吸光度值代入所述标准曲线即可得到自由基摩尔浓度。
2.根据权利要求1所述的方法,其特征在于所述捕获剂按比例由0.1ml无水乙醇、0.9ml去离子水和0.01mmol水杨酸组成。
3.根据权利要求1所述的方法,其特征在于,用分光光度计测量吸光度时波长是510nm。
4.根据权利要求1所述的方法,其特征在于所述待测的次氯酸钠水溶液的pH范围为1-12。
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