CN115753287A - Device and method for detecting total phosphorus in water samples - Google Patents
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Abstract
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Description
Translated fromChinese技术领域technical field
本发明涉及水质分析，特别涉及水样中总磷检测装置和方法。The invention relates to water quality analysis, in particular to a device and method for detecting total phosphorus in water samples.
背景技术Background technique
水中磷可以以元素磷、正磷酸盐、缩合磷酸盐、焦磷酸盐、偏磷酸盐和有机团结合的磷酸盐等形式存在。其主要来源为生活污水、化肥、农药及洗涤剂所用的磷酸盐增洁剂等。磷酸盐会干扰水厂中的混凝过程。水体中的磷也是藻类生长需要的一种关键元素，水体中磷含量过高可造成藻类的过量繁殖，大量消耗水中溶解氧，从而加速水体的富营养化，若直接排放，会造成湖泊、河流透明度降低，水质变坏。因此，准确测定水体中总磷含量是非常重要的。Phosphorus in water can exist in the form of elemental phosphorus, orthophosphate, condensed phosphate, pyrophosphate, metaphosphate and organic group-bound phosphate. Its main sources are domestic sewage, chemical fertilizers, pesticides, and phosphate builders used in detergents. Phosphate interferes with the coagulation process in waterworks. Phosphorus in water is also a key element needed for the growth of algae. Excessive phosphorus content in water can cause excessive reproduction of algae and consume a large amount of dissolved oxygen in water, thus accelerating the eutrophication of water. If it is discharged directly, it will cause lakes, rivers, etc. The transparency is reduced and the water quality is deteriorated. Therefore, it is very important to accurately determine the total phosphorus content in water.
目前，在环境监测中，水质总磷的测定标准方法主要包括《GB11893-89水质总磷的测定钼酸铵分光光度法》、《HJ 670-2013水质磷酸盐和总磷的测定连续流动-钼酸铵分光光度法》、《HJ 671-2013水质总磷的测定流动注射-钼酸铵分光光度法》等方法。At present, in environmental monitoring, the standard methods for the determination of total phosphorus in water mainly include "GB11893-89 Determination of Total Phosphorus in Water Quality Ammonium Molybdate Spectrophotometry", "HJ 670-2013 Determination of Phosphate and Total Phosphorus in Water Quality Continuous Flow-Molybdenum Ammonium Molybdate Spectrophotometry", "HJ 671-2013 Determination of Total Phosphorus in Water Quality Flow Injection-Ammonium Molybdate Spectrophotometry" and other methods.
《GB11893-89》规定了总磷包括溶解的、颗粒的、有机的和无机磷，水样需采用未过滤的样品进行测试，测试过程均需手工完成。当样品量较大时，受限于时间、设备、人员等条件，效率很低，不利于实验室批量化测试。《HJ670-2013》和《HJ 671-2013》均为仪器方法，所有测试过程由仪器自动完成，测试效率高，应用广泛，但也有以下问题需要解决："GB11893-89" stipulates that total phosphorus includes dissolved, granular, organic and inorganic phosphorus. Water samples must be tested with unfiltered samples, and the test process must be done manually. When the sample volume is large, it is limited by time, equipment, personnel and other conditions, and the efficiency is very low, which is not conducive to batch testing in the laboratory. "HJ670-2013" and "HJ 671-2013" are both instrument methods, all the test process is automatically completed by the instrument, the test efficiency is high, and it is widely used, but there are also the following problems to be solved:
1.样品浊度对测试结果有明显干扰，需要通过补偿测量进行校正或通过透析单元进行消除，操作步骤繁琐，透析单元随着样品量的增加透析能力逐渐下降，透析膜堵塞，还需要定期维护。1. The turbidity of the sample has obvious interference on the test results, which needs to be corrected by compensation measurement or eliminated by the dialysis unit. The operation steps are cumbersome, and the dialysis capacity of the dialysis unit gradually decreases with the increase of the sample volume, and the dialysis membrane is blocked. Regular maintenance is also required .
2.仪器法流路管径相对较细，不适用于测定含悬浮物颗粒物较多或颗粒粒径大于250μm的样品。2. The diameter of the flow path of the instrument method is relatively small, so it is not suitable for the determination of samples containing more suspended solids or particles with a particle size greater than 250 μm.
发明内容Contents of the invention
为解决上述现有技术方案中的不足，本发明提供了一种水样中总磷检测装置。In order to solve the shortcomings in the above-mentioned prior art solutions, the present invention provides a detection device for total phosphorus in water samples.
本发明的目的是通过以下技术方案实现的：The purpose of the present invention is achieved through the following technical solutions:
水样中总磷检测装置，所述水样中总磷检测装置包括依次连接的进样单元、消解单元和分析单元，所述分析单元包括分析仪和第一废液罐；所述水样中总磷检测装置还包括：The total phosphorus detection device in the water sample, the total phosphorus detection device in the water sample includes a sampling unit, a digestion unit and an analysis unit connected in sequence, and the analysis unit includes an analyzer and a first waste liquid tank; The total phosphorus detection device also includes:
过滤器，所述过滤器设置在所述消解单元和分析单元之间的流路上；a filter, the filter is arranged on the flow path between the digestion unit and the analysis unit;
第一切换模块和第二切换模块，所述第一切换模块用于使所述消解单元选择性地连通所述过滤器的进口或管道，所述第二切换模块用于使所述分析单元选择性地连通所述过滤器的出口或所述管道；A first switching module and a second switching module, the first switching module is used to selectively connect the digestion unit to the inlet or pipeline of the filter, and the second switching module is used to make the analysis unit select Sexually communicate with the outlet of the filter or the pipeline;
清洗单元，所述清洗单元根据需要地将总磷已知的清洗液送入所述过滤器出口和第二切换模块间的第一流路，所述过滤器内的清洗液在所述第一切换模块和过滤器进口间的第二流路排出。A cleaning unit, the cleaning unit sends the cleaning liquid with known total phosphorus into the first flow path between the filter outlet and the second switching module as required, and the cleaning liquid in the filter is The second flow path between the module and the filter inlet is exhausted.
本发明的目的还在于提供了一种水样中总磷检测方法，该发明目的是通过以下技术方案得以实现的：The purpose of the present invention is also to provide a method for detecting total phosphorus in water samples, which is achieved by the following technical solutions:
水样中总磷检测方法，所述水样中总磷检测方法包括以下步骤：The total phosphorus detection method in the water sample, the total phosphorus detection method in the water sample comprises the following steps:
(A1)进样单元预处理承载位处的水样，吸取预处理后的水样，送消解单元；(A1) The sample injection unit preprocesses the water sample at the holding position, absorbs the pretreated water sample, and sends it to the digestion unit;
(A2)试剂送所述消解单元，水样消解；(A2) The reagent is sent to the digestion unit, and the water sample is digested;
(A3)第一切换模块和第二切换模块切换，使得消解单元内的消解后水样依次经过第一切换模块、过滤器和第二切换模块，进入分析单元，获得水样中总磷含量；(A3) switching between the first switching module and the second switching module, so that the digested water sample in the digestion unit passes through the first switching module, the filter and the second switching module in sequence, and enters the analysis unit to obtain the total phosphorus content in the water sample;
(A4)第一切换模块和第二切换模块切换，使得消解单元内的剩余水样依次经过第一切换模块、管道和第二切换模块，进入分析单元内排废；同时，总磷已知的清洗液送入所述过滤器出口和第二切换模块间的第一流路，所述过滤器内的清洗液在所述第一切换模块和过滤器进口间的第二流路排出；(A4) The first switching module and the second switching module are switched, so that the remaining water samples in the digestion unit pass through the first switching module, the pipeline and the second switching module successively, and enter the analysis unit to discharge waste; at the same time, the known total phosphorus The cleaning liquid is sent into the first flow path between the filter outlet and the second switching module, and the cleaning liquid in the filter is discharged through the second flow path between the first switching module and the filter inlet;
(A5)第一切换模块和第二切换模块切换，清洗液依次经过第一切换模块、所述管道和第二切换模块，进入分析单元内排废。(A5) The first switching module and the second switching module are switched, and the cleaning liquid passes through the first switching module, the pipeline and the second switching module in sequence, and enters the analysis unit for waste discharge.
与现有技术相比，本发明具有的有益效果为：Compared with prior art, the beneficial effect that the present invention has is:
1.在线消除样品浊度对测试结果的影响；1. Eliminate the influence of sample turbidity on test results online;
样品浊度对测试结果的影响，通过在线过滤器被消除，然后对在线过滤器进行自动化清洗，操作简单，无需维护，检测效率高；The influence of sample turbidity on the test results is eliminated through the online filter, and then the online filter is automatically cleaned, which is easy to operate, requires no maintenance, and has high detection efficiency;
2.含悬浮物颗粒物较多或颗粒粒径大于250μm的样品可以直接进样检测；2. Samples containing more suspended solids or particles with a particle size greater than 250 μm can be directly injected for detection;
对于含悬浮物颗粒物较多或颗粒粒径大于250μm的样品，高剪切乳化分散机对水样进行高速剪切乳化，将水样中的颗粒物高速剪切成粒径小于250μm，然后直接进行检测，测试结果准确，适用性强。For samples containing more suspended solids or particles with a particle size greater than 250 μm, the high-shear emulsification and disperser performs high-speed shear emulsification on the water sample, and shears the particles in the water sample to a particle size of less than 250 μm at high speed, and then directly detects , the test result is accurate and the applicability is strong.
附图说明Description of drawings
参照附图，本发明的公开内容将变得更易理解。本领域技术人员容易理解的是：这些附图仅仅用于举例说明本发明的技术方案，而并非意在对本发明的保护范围构成限制。图中：The disclosure of the present invention will become more comprehensible with reference to the accompanying drawings. Those skilled in the art can easily understand that these drawings are only used to illustrate the technical solution of the present invention, and are not intended to limit the protection scope of the present invention. In the picture:
图1是根据本发明实施例的水样中总磷检测方法的流程示意图。Fig. 1 is a schematic flowchart of a method for detecting total phosphorus in water samples according to an embodiment of the present invention.
具体实施方式Detailed ways
图1和以下说明描述了本发明的可选实施方式以教导本领域技术人员如何实施和再现本发明。为了解释本发明技术方案，已简化或省略了一些常规方面。本领域技术人员应该理解源自这些实施方式的变型或替换将在本发明的范围内。本领域技术人员应该理解下述特征能够以各种方式组合以形成本发明的多个变型。由此，本发明并不局限于下述可选实施方式，而仅由权利要求和它们的等同物限定。Figure 1 and the following description describe an alternative embodiment of the invention to teach those skilled in the art how to implement and reproduce the invention. In order to explain the technical solutions of the present invention, some conventional aspects have been simplified or omitted. It should be understood by those skilled in the art that modifications or substitutions from these embodiments will be within the scope of the present invention. Those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple variations of the invention. As such, the invention is not limited to the alternative embodiments described below, but only by the claims and their equivalents.
实施例1：Example 1:
本发明实施例的水样中总磷检测装置，所述水样中总磷检测装置包括：The total phosphorus detection device in the water sample of the embodiment of the present invention, the total phosphorus detection device in the water sample comprises:
依次连接的进样单元、消解单元和分析单元，所述分析单元包括泵、分析仪和第一废液罐；A sampling unit, a digestion unit and an analysis unit connected in sequence, the analysis unit includes a pump, an analyzer and a first waste liquid tank;
过滤器，所述过滤器设置在所述消解单元和分析单元之间的流路上；a filter, the filter is arranged on the flow path between the digestion unit and the analysis unit;
第一切换模块和第二切换模块，所述第一切换模块用于使所述消解单元选择性地连通所述过滤器的进口或管道，所述第二切换模块用于使所述分析单元选择性地连通所述过滤器的出口或所述管道；A first switching module and a second switching module, the first switching module is used to selectively connect the digestion unit to the inlet or pipeline of the filter, and the second switching module is used to make the analysis unit select Sexually communicate with the outlet of the filter or the pipeline;
清洗单元，所述清洗单元根据需要地将总磷已知的清洗液送入所述过滤器出口和第二切换模块间的第一流路，所述过滤器内的清洗液在所述第一切换模块和过滤器进口间的第二流路排出。A cleaning unit, the cleaning unit sends the cleaning liquid with known total phosphorus into the first flow path between the filter outlet and the second switching module as required, and the cleaning liquid in the filter is The second flow path between the module and the filter inlet is exhausted.
为了自动地进入清洗过滤器，进一步地，所述清洗单元包括：In order to automatically enter the cleaning filter, further, the cleaning unit includes:
第一阀门和第二阀门，所述清洗液采用总磷含量为零的纯水，依次流过所述第一阀门、过滤器的出口、过滤器的进口和第二流路，进入第二废液罐。The first valve and the second valve, the cleaning liquid adopts pure water with zero total phosphorus content, flows through the first valve, the outlet of the filter, the inlet of the filter and the second flow path in sequence, and enters the second waste water liquid tank.
为了对水样预处理及取样，进一步地，所述进样单元包括：In order to pretreat and sample the water sample, further, the sampling unit includes:
进样针，所述进样针包括内管和外管组成的复合管，内管连通泵，气源连通所述内管和外管之间的夹层；A sampling needle, the sampling needle includes a composite tube composed of an inner tube and an outer tube, the inner tube communicates with the pump, and the gas source communicates with the interlayer between the inner tube and the outer tube;
承载件，所述承载件具有多个承载水样容器的承载位；a bearing member, the bearing member has a plurality of bearing positions for carrying water sample containers;
驱动模块，所述驱动模块用于驱动所述承载件或进样针，使得所述进样针进入和退出选择的水样容器。A driving module, the driving module is used to drive the carrier or the sampling needle, so that the sampling needle enters and exits the selected water sample container.
为了降低水样中颗粒物的粒径，以降低对后续测量的影响，进一步地，所述进样单元还包括：In order to reduce the particle size of the particles in the water sample to reduce the impact on subsequent measurements, further, the sampling unit also includes:
剪切乳化分散机，所述剪切孵化分散机设置在所述机械臂上，所述机械臂驱动所述进样针和剪切乳化分散机同步地三维移动。A shear emulsification disperser, the shear incubation disperser is arranged on the mechanical arm, and the mechanical arm drives the sampling needle and the shear emulsification disperser to move synchronously in three dimensions.
为了提高消解效率，进一步地，所述消解模块包括：In order to improve digestion efficiency, further, the digestion module includes:
紫外灯和消解管，所述消解管呈螺旋状，并环绕所述紫外灯。An ultraviolet lamp and a digestion tube, the digestion tube is in a spiral shape and surrounds the ultraviolet lamp.
图1示意性地给出了本发明实施例水样中总磷检测方法的流程图，如图1所示，所述水样中总磷检测方法包括以下步骤：Fig. 1 schematically provides the flow chart of the total phosphorus detection method in the water sample of the embodiment of the present invention, as shown in Fig. 1, the total phosphorus detection method in the water sample comprises the following steps:
(A1)进样单元预处理承载位处的水样，吸取预处理后的水样，送消解单元；(A1) The sample injection unit preprocesses the water sample at the holding position, absorbs the pretreated water sample, and sends it to the digestion unit;
(A2)试剂送所述消解单元，水样消解；(A2) The reagent is sent to the digestion unit, and the water sample is digested;
(A3)第一切换模块和第二切换模块切换，使得消解单元内的消解后水样依次经过第一切换模块、过滤器和第二切换模块，进入分析单元，获得水样中总磷含量；(A3) switching between the first switching module and the second switching module, so that the digested water sample in the digestion unit passes through the first switching module, the filter and the second switching module in sequence, and enters the analysis unit to obtain the total phosphorus content in the water sample;
(A4)第一切换模块和第二切换模块切换，使得消解单元内的剩余水样依次经过第一切换模块、管道和第二切换模块，进入分析单元内排废；同时，总磷已知的清洗液送入所述过滤器出口和第二切换模块间的第一流路，所述过滤器内的清洗液在所述第一切换模块和过滤器进口间的第二流路排出；(A4) The first switching module and the second switching module are switched, so that the remaining water samples in the digestion unit pass through the first switching module, the pipeline and the second switching module successively, and enter the analysis unit to discharge waste; at the same time, the known total phosphorus The cleaning liquid is sent into the first flow path between the filter outlet and the second switching module, and the cleaning liquid in the filter is discharged through the second flow path between the first switching module and the filter inlet;
(A5)第一切换模块和第二切换模块切换，清洗液依次经过第一切换模块、所述管道和第二切换模块，进入分析单元内排废。(A5) The first switching module and the second switching module are switched, and the cleaning liquid passes through the first switching module, the pipeline and the second switching module in sequence, and enters the analysis unit for waste discharge.
为了自动化地反向清洗过滤器，进一步地，总磷含量为零的纯水依次经过第一阀门、第一流路、过滤器、第二流路和第二阀门。In order to automatically reverse clean the filter, further, the pure water with zero total phosphorus content passes through the first valve, the first flow path, the filter, the second flow path and the second valve in sequence.
为了降低水样中颗粒物粒径以及提高水样的均一性，进一步地，在预处理中，进样针和用于承载多个水样容器的承载件相对移动，使得进样针插入选择的水样容器；In order to reduce the particle size of the water sample and improve the uniformity of the water sample, further, in the pretreatment, the sampling needle and the carrier for carrying multiple water sample containers move relatively so that the sampling needle is inserted into the selected water sample. sample container;
进样针中内管和外管之间的夹层排出气体，混合了水样，同时，剪切孵化分散机降低了水样中颗粒物的半径；The interlayer between the inner tube and the outer tube in the injection needle exhausts the gas and mixes the water sample. At the same time, the shear hatch disperser reduces the radius of the particles in the water sample;
预处理后的水样进入所述内管内，送所述消解单元。The pretreated water sample enters the inner tube and is sent to the digestion unit.
为了提高消解效率，进一步地，在消解中，水样经过螺旋状消解管，所述消解管环绕紫外灯。In order to improve the digestion efficiency, further, during the digestion, the water sample passes through a spiral digestion tube, and the digestion tube surrounds the ultraviolet lamp.
实施例2：Example 2:
根据本发明实施例1的水样中总磷检测装置和方法的应用例。An application example of the device and method for detecting total phosphorus in water samples according to Embodiment 1 of the present invention.
在该应用例中，进样单元中，进样针包括内管和外管组成的复合管，内管连通泵，气源连通所述内管和外管之间的夹层；进样针和剪切乳化分散机设置在机械壁上，并在驱动模块驱动下三维移动，使得进样针进入选择的水样容器内，多个水样容器呈矩阵式地设置在承载件的承载位；第一蠕动泵的入口分别连通试剂瓶、内管的出口；In this application example, in the sampling unit, the sampling needle includes a composite tube composed of an inner tube and an outer tube, the inner tube communicates with the pump, and the gas source communicates with the interlayer between the inner tube and the outer tube; the sampling needle and the shear The emulsifying and dispersing machine is set on the mechanical wall and moves three-dimensionally under the drive of the drive module, so that the sampling needle enters the selected water sample container, and multiple water sample containers are arranged in a matrix on the bearing position of the carrier; the first The inlet of the peristaltic pump is respectively connected to the outlet of the reagent bottle and the inner tube;
第一切换模块和第二切换模块分别采用电磁三通阀，使得第一蠕动泵的出口选择性地连通过滤器的入口或清洗管道，分析单元的出口选择性地连通过滤器出口和清洗管道；The first switching module and the second switching module respectively use electromagnetic three-way valves, so that the outlet of the first peristaltic pump is selectively connected to the inlet of the filter or the cleaning pipeline, and the outlet of the analysis unit is selectively connected to the outlet of the filter and the cleaning pipeline;
消解单元内，消解管呈螺旋状，环绕紫外灯；In the digestion unit, the digestion tube is in a spiral shape and surrounds the ultraviolet lamp;
在清洗单元内，纯水容器依次连通抽吸泵、第一电磁阀和(过滤器出口和第二切换模块间的)第一流路，(过滤器入口和第二切换模块间的)第一流路依次连通第二电磁阀和第二废液罐；In the cleaning unit, the pure water container is sequentially connected with the suction pump, the first solenoid valve, the first flow path (between the filter outlet and the second switching module), and the first flow path (between the filter inlet and the second switching module) Connecting the second solenoid valve and the second waste liquid tank in sequence;
分析单元包括第二蠕动泵和分析仪，分析仪中检测过的水样送第一废液罐。The analysis unit includes a second peristaltic pump and an analyzer, and the water samples detected in the analyzer are sent to the first waste liquid tank.
本发明实施例水样中总磷检测方法，也即本实施例检测装置的工作方法，如图1所示，所述水样中总磷检测方法包括以下步骤：The method for detecting total phosphorus in the water sample of the embodiment of the present invention, that is, the working method of the detection device in this embodiment, as shown in Figure 1, the method for detecting total phosphorus in the water sample includes the following steps:
(A1)进样单元内，机械臂在驱动下三维移动，使得取样针进入选择的水样容器内，气源提供的气体穿过内管和外管之间的夹层，之后进入水样中，混合了水样；同时，插入水样容器内的剪切乳化分散机降低了水样中颗粒物的半径；(A1) In the sampling unit, the mechanical arm moves three-dimensionally under the drive, so that the sampling needle enters the selected water sample container, and the gas provided by the gas source passes through the interlayer between the inner tube and the outer tube, and then enters the water sample. The water sample is mixed; at the same time, the shear emulsification disperser inserted into the water sample container reduces the radius of the particles in the water sample;
待预处理完成后，在第一蠕动泵抽吸下，水样容器内的水样穿过取样针的内管，进入消解单元；After the pretreatment is completed, under the suction of the first peristaltic pump, the water sample in the water sample container passes through the inner tube of the sampling needle and enters the digestion unit;
(A2)试剂通过第一蠕动泵送所述消解单元，水样消解；(A2) The reagent is sent to the digestion unit through the first peristaltic pump, and the water sample is digested;
(A3)第一切换模块和第二切换模块切换，第二蠕动泵抽吸，使得消解单元内的消解后水样依次经过第一切换模块、过滤器和第二切换模块，进入分析单元，获得水样中总磷含量，水样中的颗粒物被过滤器截留；(A3) The first switching module and the second switching module are switched, and the second peristaltic pump pumps, so that the digested water sample in the digestion unit passes through the first switching module, the filter and the second switching module in sequence, and enters the analysis unit, obtaining The total phosphorus content in the water sample, the particulate matter in the water sample is intercepted by the filter;
(A4)第一切换模块和第二切换模块切换，使得消解单元内的剩余水样依次经过第一切换模块、清洗管道和第二切换模块，进入分析单元，之后送入第一废液罐排废；同时，在抽吸泵作用下，总磷含量是零的纯水依次经过第一电磁阀、第一流路、过滤器、第二流路和第二电磁阀，之后进入第二废液罐；(A4) Switch between the first switching module and the second switching module, so that the remaining water samples in the digestion unit pass through the first switching module, the cleaning pipeline and the second switching module in turn, enter the analysis unit, and then send them to the first waste liquid tank row At the same time, under the action of the suction pump, the pure water with zero total phosphorus content passes through the first solenoid valve, the first flow path, the filter, the second flow path and the second solenoid valve in sequence, and then enters the second waste liquid tank ;
(A5)第一切换模块和第二切换模块切换，清洗液依次经过第一蠕动泵、第一切换模块、所述清洗管道和第二切换模块，进入分析单元，之后送第一废液罐排废。(A5) Switching between the first switching module and the second switching module, the cleaning liquid passes through the first peristaltic pump, the first switching module, the cleaning pipeline and the second switching module in sequence, enters the analysis unit, and then sends it to the first waste liquid tank waste.
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