CN110646414A - 一种水中氯离子浓度快速检测试剂与用法 - Google Patents
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Abstract
本发明属于环保检测技术领域，更具体的涉及一种水中氯离子浓度快速检测试剂与用法。本发明以酒石酸、乙二胺四乙酸、柠檬酸中任意一种或两种以上的混合物为掩蔽剂；以硫酸、硝酸、三氟甲磺酸或对甲基苯磺酸中的任意一种为酸性试剂；以铁离子的盐为络合试剂三者组成水中氯离子浓度快速检测试剂。本发明基于氯离子与三价铁离子形成的络合物氯化铁在紫外可见区的吸收效应，本发明方法容易操作，方便储运，结果准确，价格低廉，且适合现场快速检测的水中氯离子快速检测试剂。
Description
技术领域
本发明属于环保检测技术领域，更具体的涉及一种水中氯离子浓度快速检测试剂与用法。
背景技术
氯离子是水中一种常见的阴离子，几乎所有的天然水中都有氯离子存在。氯离子是生物体内含量最丰富的阴离子，通过跨膜转运和离子通道参与机体多种生物功能。而在工业循环水中，氯离子的存在浓度如果过高，则会对系统造成危害，一是破坏钝化膜；二是降低pH值。在pH值偏低的环境下，不锈钢对Cl-将会更加敏感，其常见的腐蚀类型为点蚀。另外Cl-又是引起金属孔蚀、缝隙腐蚀、应力腐蚀和选择性腐蚀的主要原因。尤其是当Cl-含量达2％时，大多数不锈钢已不能使用。因此，对水中的氯离子含量进行监控，尤为重要。水中氯离子的测定方法众多，但多数要在实验室中进行，如：络合滴定法、分光光度法、原子吸收法、色谱分析法、电化学法等，上述方法各有优缺点，络合滴定法操作复杂，且成本较高；分光光度法用的试剂毒性较大，对环境不友好，且测量范围相对来讲比较窄，测试高浓度样品时需要进行稀释；原子吸收法和色谱分析法主要在仪器昂贵，不易在野外使用，且只能在实验室完成，对操作人员要求较高；电化学法则主要应用在生活用水，地表水领域无法很好的在工业水或污水中应用。
发明内容
本发明所要解决的技术问题就是，提供一种水中氯离子浓度快速检测试剂与用法，该检测试剂为一种试剂，方便携带且使用简单，测试过程快速，而且配合Pyxis SP-910便携式多参数水质分析仪，可对工业循环水、污水、天然水中的氯化物含量进行快速准确检测。
本发明基于氯离子与三价铁离子形成的络合物氯化铁在紫外可见区的吸收效应，本发明方法容易操作，方便储运，结果准确，价格低廉，且适合现场快速检测的水中氯离子快速检测试剂。
本发明是通过如下技术方案实现上述目的的，一种水中氯离子浓度快速检测试剂，包括掩蔽剂、酸性试剂和络合剂；
优选的，所述掩蔽剂为酒石酸、乙二胺四乙酸、柠檬酸中任意一种或两种以上的混合物；掩蔽剂主要为掩蔽水体中干扰离子对氯离子测试的干扰，如利用EDTA(乙二胺四乙酸)掩蔽钙镁离子，柠檬酸掩蔽金属离子等；
优选的，所述酸性试剂主要为测试提供一个最佳的pH的环境，如利用强酸硫酸、硝酸、三氟甲磺酸、对甲基苯磺酸等提供一个强酸性环境等；
优选的，所述络合试剂主要为一种铁离子的盐，如三氟甲磺酸铁、高氯酸铁等。
根据本发明的另一个方面，本发明提供了一种水中氯离子浓度快速检测试剂的用法，包括如下步骤：将掩蔽剂，酸性试剂，络合试剂按一定比例称量后，混合均匀，然后按照要求分装成单独定量包装。使用时，直接将装有10ml的水样比色瓶作为空白样，放入PyxisSP-910多参数水质分析仪中，按zero键，进行背景校准，然后将分装好的氯离子测定试剂包加入装有10ml水样的比色瓶中，然后上下翻转试剂瓶使水样与试剂混合均匀，作为样品，如果水样中含有氯离子，则迅速产生黄色，黄色的深浅与水中氯离子的浓度呈正比，放入Pyxis SP-910多参数水质分析仪中，按read键，进行读值，界面显示值即为水中氯离子浓度值。
本发明仅含有一个试剂包，络合试剂与水体中的氯离子反应迅速，反应时间相对于传统法，大大减少，而且试剂包中掩蔽剂的加入，大大降低水体的复杂性对测试的干扰，保证了测试结果的准确度，具有操作简便、结果准确、价格便宜、便于储运、适合现场快速检测等优点。
与现有技术相比，本发明具有如下有益效果:
1)检测试剂仅包含有一个试剂包，使用方便，且方便野外操作使用；
2)检测原理基于分光光度法测定，区别于传统滴定法与电极法，操作简便，准确度高，对操作人员专业性要求较低；
3)通过配方中各组分比例调整，测量范围可以从几个ppm到几百ppm。
附图说明
图1为氯离子浓度为5-80ppm与吸光度线性关系图。
图2为氯离子浓度为50-600ppm与吸光度线性关系图。
具体实施方式
实施例一
本试剂为一个试剂，具体制作方法为：
将0.2g掩蔽剂柠檬酸，4ml酸性试剂三氟甲磺酸，0.6g络合试剂三氟甲磺酸铁按比例称量后，然后用纯水定容到5ml，混合均匀，然后按照要求分装成单独定量包装。
实施例二
将0.1g掩蔽剂酒石酸，2ml酸性试剂硝酸，0.3g络合试剂高氯酸铁按比例称量后，然后用纯水定容到5ml，混合均匀，然后按照要求分装成单独定量包装。
实施例三
将0.3g掩蔽剂酒石酸和柠檬酸，3g酸性试剂对甲基苯磺酸，0.4g络合试剂三氟甲磺酸铁按比例称量后，将上述材料加入到玻璃研钵中，充分研磨至全部原材料混合均匀，然后按照要求分装成单独定量包装。
实施例四
取1000ppm的氯离子标准溶液为母液，配制一系列不同浓度的标准溶液，浓度分别为5、10、40、80ppm，取上述标准溶液装入10ml的比色瓶，作为空白样，放入Pyxis SP-910多参数水质分析仪中，按zero键，进行背景校准，将一包试剂加入装有10ml水样的另一比色瓶中，上下翻转试剂瓶使水样与试剂混合均匀，作为样品，然后放入Pyxis SP-910多参数水质分析仪中，按read键，进行吸光度测试。以浓度为横坐标，吸光度为纵坐标，看线性关系，氯离子浓度与吸光度线性关系良好，R2＝0.999，如图1所示。
实施例五
取1000ppm的氯离子标准溶液为母液，配制一系列不同浓度的标准溶液，浓度分别为50、100、200、300、400、500、600ppm，取上述标准溶液装入10ml的比色瓶，作为空白样，放入Pyxis SP-910多参数水质分析仪中，按zero键，进行背景校准，将一包试剂加入装有10ml水样的另一比色瓶中，上下翻转试剂瓶使水样与试剂混合均匀，作为样品，然后放入PyxisSP-910多参数水质分析仪中，按read键，进行吸光度测试。以浓度为横坐标，吸光度为纵坐标，看线性关系，氯离子浓度与吸光度线性关系良好，R2＝0.997，如图2所示。
实施例六
取五个实际工业循环水样品进行滴定与比色对比测试，测试数据如下，从测试数据看，如果以滴定测试值为真值，比色测试值为测试值，从对比数据看，比色测试值相对于滴定测试值在低浓度范围内，相对误差较大，大概在±10％左右，在高浓度范围内，比色测试值相对于滴定测试值在高浓度范围内，相对误差大概在±5％左右，结果如表1所示。
表1本发明测试方法与滴定测试的对比
| 水样编号 | 滴定测试值/ppm | 比色测试值/ppm | 相对误差 |
| 1# | 300 | 310.0 | 3.3％ |
| 2# | 90 | 97.1 | 7.9％ |
| 3# | 1240 | 1212.5 | -2.2％ |
| 4# | 14 | 9.5 | -32.1％ |
| 5# | 49 | 42.5 | -13.3％ |
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。
Claims (6)
1.一种水中氯离子浓度快速检测试剂，包括掩蔽剂、酸性试剂和络合剂；
所述掩蔽剂为酒石酸、乙二胺四乙酸、柠檬酸中任意一种或两种以上的混合物；
所述酸性试剂为硫酸、硝酸、三氟甲磺酸或对甲基苯磺酸中的任意一种；
所述络合试剂为铁离子的盐。
2.根据权利要求1所述的水中氯离子浓度快速检测试剂，其特征在于：所述铁离子的盐为三氟甲磺酸铁或高氯酸铁。
3.根据权利要求2所述的水中氯离子浓度快速检测试剂，其特征在于，具体制备成分及其制备方法为：将0.2g掩蔽剂柠檬酸，4ml酸性试剂三氟甲磺酸，0.6g络合试剂三氟甲磺酸铁按比例称量后，然后用纯水定容到5ml，混合均匀。
4.根据权利要求2所述的水中氯离子浓度快速检测试剂，其特征在于，具体制备成分及其制备方法为：将0.1g掩蔽剂酒石酸，2ml酸性试剂硝酸，0.3g络合试剂高氯酸铁按比例称量后，然后用纯水定容到5ml，混合均匀。
5.根据权利要求2所述的水中氯离子浓度快速检测试剂，其特征在于，具体制备成分及其制备方法为：将0.3g掩蔽剂酒石酸和柠檬酸，3g酸性试剂对甲基苯磺酸，0.4g络合试剂三氟甲磺酸铁按比例称量后，将上述材料加入到玻璃研钵中，充分研磨至全部原材料混合均匀。
6.一种权利要求1所述的水中氯离子浓度快速检测试剂的使用方法，包括如下步骤：
将掩蔽剂，酸性试剂，络合试剂按一定比例称量后，混合均匀，然后按照要求分装成单独定量包装；
使用时，直接将装有10ml的水样比色瓶作为空白样，放入Pyxis SP-910多参数水质分析仪中，按zero键，进行背景校准，然后将分装好的氯离子测定试剂包加入装有10ml水样的比色瓶中，上下翻转试剂瓶使水样与试剂混合均匀，作为样品；
如果水样中含有氯离子，则迅速产生黄色，黄色的深浅与水中氯离子的浓度呈正比，放入Pyxis SP-910多参数水质分析仪中，按read键，进行读值，界面显示值即为水中氯离子浓度值。
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