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CN115266621A - A kind of in-situ water body microplastic detection device and detection method thereof - Google Patents

A kind of in-situ water body microplastic detection device and detection method thereof Download PDF

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CN115266621A
CN115266621A CN202210898858.9A CN202210898858A CN115266621A CN 115266621 A CN115266621 A CN 115266621A CN 202210898858 A CN202210898858 A CN 202210898858A CN 115266621 A CN115266621 A CN 115266621A
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detected
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filter membrane
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陈池来
袁凡
高晓明
许安
郑重
李跃
杨晨光
陈家金
刘赟
曹会彬
朱利凯
李文波
王贵师
张瑞
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Hefei Institutes of Physical Science of CAS
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Abstract

The invention relates to the technical field of environmental detection and pollutant purification, in particular to an in-situ water body micro-plastic detection device and a detection method thereof. The in-situ water body plastic detection device comprises a flow channel; a large-aperture filter screen is arranged at the inlet of the flow passage, and a small-aperture filter screen and a heating resistance screen are sequentially arranged at the outlet from inside to outside; and a water pump, a flowmeter, a biological cracking sprayer, an optical detection instrument, an ultrasonic generator and a fan are embedded in the middle section of the flow channel. The detection device and the detection method thereof can realize real-time detection of the micro-plastics in the water body in various complex environments.

Description

一种原位水体微塑料检测装置及其检测方法An in-situ water body microplastic detection device and detection method thereof

技术领域technical field

本发明涉及环境检测和净化污染物技术领域,具体涉及一种原位水体微塑料检测装置及其检测方法。The invention relates to the technical field of environmental detection and purification of pollutants, in particular to an in-situ water body microplastic detection device and a detection method thereof.

背景技术Background technique

由于多数微塑料降解缓慢,会在自然环境中不断积存,使污染程度加剧恶化,因此,水体微塑料污染已成为一个严重而又广泛的全球性环境议题。Since most microplastics degrade slowly and accumulate in the natural environment, the degree of pollution will be exacerbated. Therefore, microplastic pollution in water bodies has become a serious and extensive global environmental issue.

现有的微塑料研究方法都是以“水体取样-实验室分析”为主,受限于检测原理,无法实现微塑料质量的原位直接检测。微塑料在运输过程中会发生老化、破碎,这将影响检测结果的准确性。而且采样和检测方法的不同,很多研究结果表现形式也截然不同,对微塑料污染程度没有统一的评判标准,微塑料的检测艰难险阻。除了以上方法,新研究出了TGA(热重分析法),即在程序控制温度下,测量物质质量与温度关系的热分析技术,可以绘制微塑料定量标准曲线,从而能对微塑料的质量含量有定量的分析,此种方法对环境温度要求高,原位检测的不确定性明显,而且只能判断出质量含量,对颗粒浓度却无法判断,不能完整的检测出微塑料的各个指标。The existing microplastic research methods are mainly based on "water sampling-laboratory analysis", which is limited by the detection principle and cannot directly detect the quality of microplastics in situ. Microplastics will age and break during transportation, which will affect the accuracy of test results. Moreover, the sampling and detection methods are different, and many research results are expressed in completely different forms. There is no unified evaluation standard for the degree of microplastic pollution, and the detection of microplastics is difficult and dangerous. In addition to the above methods, TGA (thermogravimetric analysis) has been newly developed, which is a thermal analysis technique for measuring the relationship between material quality and temperature under program-controlled temperature. It can draw a quantitative standard curve for microplastics, so that the mass content of microplastics Quantitative analysis is available. This method requires high ambient temperature, and the uncertainty of in-situ detection is obvious. Moreover, it can only judge the mass content, but cannot judge the particle concentration, and cannot completely detect various indicators of microplastics.

中国专利CN 111175199 A公开了一种海水微塑料快速自动多功能检测设备及其方法,其目的是缩短检测时间,减少由时间引起的检测结果一致性差的问题,但不具有体现海水的原位、现场或在线检测的功能,例如没有自适应的检测范围调整和节能的控制策略。Chinese patent CN 111175199 A discloses a rapid automatic multi-functional detection device and method for seawater microplastics, the purpose of which is to shorten the detection time and reduce the problem of poor consistency of detection results caused by time, but it does not have the in-situ, On-site or online detection functions, such as no adaptive detection range adjustment and energy-saving control strategy.

因此,发展原位的水体微塑料探测装置,是未来微塑料精准检测的大势所趋。Therefore, the development of in-situ detection devices for microplastics in water bodies is the general trend for the precise detection of microplastics in the future.

发明内容Contents of the invention

本发明的目的在于提供一种原位水体微塑料检测装置及其检测方法,该检测装置及其检测方法可以实现各种复杂环境的实时水体微塑料检测。The object of the present invention is to provide an in-situ water body microplastic detection device and a detection method thereof, which can realize real-time detection of water body microplastics in various complex environments.

为实现上述目的,本发明采用了以下技术方案:To achieve the above object, the present invention adopts the following technical solutions:

一种原位水体塑料检测装置,包括流道;所述流道入口处设有滤网,出口处由内向外依次设有滤膜和加热电阻网;所述流道中段安装有水泵、流量计、生物裂解喷洒器、光学检测仪器、超声波发生器和风机。An in-situ water body plastic detection device, comprising a flow channel; the inlet of the flow channel is provided with a filter screen, and the outlet is provided with a filter membrane and a heating resistance net sequentially from the inside to the outside; the middle section of the flow channel is equipped with a water pump and a flow meter , biological cracking sprayer, optical detection instrument, ultrasonic generator and fan.

所述流道入口处安装有液位传感器,出口处安装有电子阀门。A liquid level sensor is installed at the inlet of the flow channel, and an electronic valve is installed at the outlet.

所述流道用于检测水体的流通。所述水泵,用于向流道内抽入足量的待检测水体。所述水泵上方设有流量计,流量计用于控制进入流道的待检测水体的液体量,即检测量。所述生物裂解喷洒器,用于向流道内喷洒生物裂解液,将在流道中流淌的待检测水体中的微生物分解掉,提高检测精度。所述超声波发生器,用于对待检测水体中的生物杂质的细胞进行分层处理。所述风机,用于将超声波发生器处理后的细胞层吹至流道外侧,排出检测装置。所述光学检测仪器包括数据采集单元和数据处理单元。所述数据采集单元为摄像头。所述数据处理单元相当于控制器和执行器。经过预处理的检测水体流经光学检测仪器时,光学检测仪器对流经的检测水体拍照,采集待检测水体的显微结构图像,将采集的数据发送至光学检测仪器的数据处理器进行处理。所述数据处理器还用于通过流道入口处的液位传感器和流道出口处的电子阀门,对整个流道中的检测水体的流量进行控制。所述光学检测仪器安装在流道的后端,光学检测仪器要位于对相机有较好的连续光源的环境下且水流速度均匀的位置。The flow channel is used to detect the flow of water body. The water pump is used to draw a sufficient amount of water to be detected into the flow channel. A flow meter is arranged above the water pump, and the flow meter is used to control the liquid amount of the water body to be detected entering the flow channel, that is, the detection amount. The biological cracking sprinkler is used for spraying the biological cracking liquid into the flow channel to decompose the microorganisms in the water body to be detected flowing in the flow channel, so as to improve the detection accuracy. The ultrasonic generator is used for layering the cells to be detected for biological impurities in the water body. The blower is used to blow the cell layer treated by the ultrasonic generator to the outside of the flow channel and discharge it out of the detection device. The optical detection instrument includes a data acquisition unit and a data processing unit. The data acquisition unit is a camera. The data processing unit is equivalent to a controller and an actuator. When the pretreated testing water flows through the optical testing instrument, the optical testing instrument takes pictures of the passing testing water, collects microstructure images of the water to be tested, and sends the collected data to the data processor of the optical testing instrument for processing. The data processor is also used to control the flow of the detected water body in the entire flow channel through the liquid level sensor at the inlet of the flow channel and the electronic valve at the outlet of the flow channel. The optical detection instrument is installed at the rear end of the flow channel, and the optical detection instrument should be located in an environment with a better continuous light source for the camera and a position where the water flow velocity is uniform.

进一步的,所述大孔径滤网包括滤网主体和开设在滤网主体上的若干过滤孔一,所述过滤孔一的孔径的取值范围为1mm~1cm;所述大孔径过滤网采用不锈钢滤网。Further, the large-aperture filter screen includes a filter screen main body and a plurality of filter holes 1 provided on the filter screen main body, and the aperture value range of the filter hole 1 is 1 mm to 1 cm; the large-aperture filter screen is made of stainless steel strainer.

进一步的,所述小孔径滤膜包括滤膜主体和开设在滤膜主体上的若干过滤孔二,所述过滤孔二的孔径的取值范围为1nm~10μm;所述小孔径滤膜采用离子微孔膜。与传统的网状滤膜相比,离子微孔滤膜最大的特点是具有真实几何意义上的孔径,孔径尺寸可在很宽的范围内(0.01-15μm)严格控制,孔径大小均匀一致。离子微孔滤膜具有较高的分离选择性,绝对截留大于孔径的任何微粒,分离效率能达到100%。离子微孔滤膜选用聚酯膜材,不吸收滤液中的物质,可防止滤液中有效成分被吸收而损失,不会有任何可迁移的物质到滤液中,因而不会污染滤液。Further, the small-pore filter membrane includes a filter membrane main body and a plurality of filter holes 2 set on the filter membrane main body, and the pore diameter of the filter hole 2 ranges from 1 nm to 10 μm; microporous membrane. Compared with the traditional mesh filter membrane, the biggest feature of the ion microporous membrane is that it has a real geometric pore size, the pore size can be strictly controlled in a wide range (0.01-15μm), and the pore size is uniform. The ion microporous membrane has high separation selectivity, absolutely intercepts any particles larger than the pore size, and the separation efficiency can reach 100%. The ion microporous filter membrane is made of polyester membrane, which does not absorb the substances in the filtrate, and can prevent the effective components in the filtrate from being absorbed and lost. There will not be any migratable substances into the filtrate, so the filtrate will not be polluted.

进一步的,所述生物裂解喷洒器采用的是根据林业生物防害的药剂喷洒结构改装而成,在管道上下方都放置喷洒装置能对流过的流体裂解,裂解完的的流体经流道的出口流出至光学检测仪器。生物裂解喷洒器嵌入安装在管道上,安装时要保证管道的封闭性。Further, the biological cracking sprayer is modified according to the chemical spraying structure of forestry biological hazard prevention. Spraying devices are placed on the upper and lower sides of the pipeline to crack the flowing fluid, and the cracked fluid passes through the outlet of the flow channel. Outflow to optical detection instrument. The biological cracking sprinkler is embedded and installed on the pipeline, and the sealing of the pipeline must be ensured during installation.

进一步的,所述光学检测仪器采用可见光检测仪、红外光谱仪或拉曼光谱仪中的任意一种。Further, the optical detection instrument adopts any one of a visible light detector, an infrared spectrometer or a Raman spectrometer.

进一步的,所述超声波发生器则采用电路板控制信号传递超声波发射器,产生相应频率的超声波将微塑料高速震动至流体表面,随后排出流体管道,减少微塑料污染。Further, the ultrasonic generator uses the circuit board control signal to transmit the ultrasonic transmitter to generate ultrasonic waves of corresponding frequency to vibrate the microplastics to the surface of the fluid at high speed, and then discharge the fluid pipes to reduce the pollution of microplastics.

本发明还涉及一种上述原位水体塑料检测装置的检测方法,该方法包括以下步骤:The present invention also relates to a detection method of the above-mentioned in-situ water body plastic detection device, the method comprising the following steps:

S1、进样S1, sample injection

将本发明所述的检测装置放置在需微塑料检测位置,如家用水管进水口,水库检测阀,深海检测区域等位置处。打开水泵,抽取设定体积的待检测水体,待检测水体由流道入口进入到流道中,在待检测水体经过大孔径滤网时,待检测水体中的部分杂质被大孔径过滤网过滤掉,利用设置在水泵上的流量计采集每次进样的待检测水体的体积。The detection device of the present invention is placed in places where detection of microplastics is required, such as water inlets of household water pipes, detection valves of reservoirs, deep-sea detection areas, etc. Turn on the water pump to draw a set volume of water to be tested. The water to be tested enters the flow channel from the inlet of the flow channel. When the water to be tested passes through the large-aperture filter, some impurities in the water to be tested are filtered out by the large-aperture filter. The volume of the water body to be tested for each sample injection is collected by using a flow meter arranged on the water pump.

S2、前处理S2, pre-processing

经过大孔径滤网过滤后的待检测水体沿流道继续向前流淌,当待检测水体流经生物裂解喷洒器时,生物裂解喷洒器向流道中的待检测水体喷洒生物裂解液,生物裂解液将待检测水体中的部分微生物杀死,当裂解装置中的液体流出时,其中的部分微生物杀死,这样减少了微塑料检测的干扰。当待检测水体流经超声波发生器时,利用超声波发生器发出的超声波将待检测水体中的水体微生物、浮游生物或微生物尸体进行震动粉碎,提高微塑料检测的准确性。The water body to be tested after being filtered by the large-aperture filter continues to flow forward along the flow channel. Part of the microorganisms in the water to be detected are killed, and when the liquid in the cracking device flows out, part of the microorganisms are killed, thus reducing the interference of microplastic detection. When the water body to be detected flows through the ultrasonic generator, the ultrasonic waves emitted by the ultrasonic generator are used to vibrate and pulverize the microorganisms, plankton or microbial corpses in the water body to be detected, so as to improve the accuracy of microplastic detection.

S3、富集S3, enrichment

经前处理后的待检测水体到达小孔径滤膜处,待检测水体中的微塑料富集到小孔径滤膜上,其余物质随待检测水体通过小孔径滤膜后由流道出口流出。采用风机对富集在小孔径滤膜上的微塑料进行风干,采用加热电阻网对富集在小孔径滤膜上的微塑料进行加热烘干。After pretreatment, the water body to be detected reaches the small-pore filter membrane, and the microplastics in the water body to be detected are enriched on the small-pore filter membrane, and the remaining substances flow out from the outlet of the flow channel after the water body to be tested passes through the small-pore filter membrane. A fan is used to air-dry the microplastics enriched on the small-aperture filter membrane, and a heating resistor net is used to heat and dry the microplastics enriched on the small-aperture filter membrane.

S4、光学检测S4. Optical detection

采用光学检测仪器对富集在小孔径滤膜上的微塑料进行检测,获取微塑料的种类及浓度。光学检测的目的是检测微塑料的种类和其对应的浓度,在小孔径滤膜上,先采用显微摄像头以成像的方式对微塑料的数量做一个估计,再用拉曼与红外光谱利用不同微塑料物理性质不同确定微塑料的种类。Optical detection instruments are used to detect the microplastics enriched on the small-pore filter membrane to obtain the type and concentration of microplastics. The purpose of optical detection is to detect the types of microplastics and their corresponding concentrations. On the small-pore filter membrane, the microscopic camera is used to estimate the amount of microplastics in the form of imaging, and then Raman and infrared spectroscopy are used to make an estimate. The physical properties of microplastics are different to determine the type of microplastics.

和现有技术相比,本发明的优点为:Compared with prior art, the advantages of the present invention are:

(1)本发明采用流道式设计,使待检测液体在流道中流动的过程中即可在原位复杂的环境中建立一个密闭的空间,在原位环境中对待检测液体中的微塑料种类及浓度进行检测,提高检测结果的准确性及检测效率。基于不同种类的微塑料在形态上具有明显区别,本发明利用区分算法对微塑料的种类进行统计输出,从而实现了实时在线的输出微塑料的颗粒浓度以及颗粒种类。本发明所采用的算法的执行环境的控制器采用嵌入式系统,计算速度快,体积小,降低各单元相互配合的复杂度,又可以极大的减小仪器体积,同时结合闭环控制,已到达降低最小检测浓度下界和节能的目的。(1) The present invention adopts a flow channel design, so that a closed space can be established in a complex environment in situ during the flow of the liquid to be detected in the flow channel, and the types of microplastics in the liquid to be detected in the in situ environment and concentration to improve the accuracy and efficiency of the test results. Based on the obvious difference in morphology of different types of microplastics, the present invention uses a distinguishing algorithm to statistically output the types of microplastics, thereby realizing the real-time online output of particle concentration and particle types of microplastics. The controller of the execution environment of the algorithm used in the present invention adopts an embedded system, which has fast calculation speed and small size, reduces the complexity of the mutual cooperation of each unit, and can greatly reduce the volume of the instrument. At the same time, combined with closed-loop control, it has reached The purpose of reducing the minimum detection concentration lower bound and saving energy.

(2)由于本发明能够排除流体中微生物对检测结果的影响,微塑料结构是比较对称的,微生物的细胞由于细胞的分化,形态不会对称,而且微生物的细胞结构已经有成熟的判断标准,比如细胞核等,这与微塑料有很大的区别。因此,本发明通过拍摄到待检测液体中的微塑料及微生物的显微结构,利用现有技术中的的机器学习训练中的识别模型,就能够将微塑料和微生物区分开,提高原位水体中微塑料检测的检测精度。(2) Since the present invention can eliminate the influence of microorganisms in the fluid on the detection results, the structure of microplastics is relatively symmetrical, and the cells of microorganisms will not be symmetrical due to cell differentiation, and the cell structure of microorganisms has mature judging criteria. For example, cell nuclei, etc., which are very different from microplastics. Therefore, by photographing the microstructure of microplastics and microorganisms in the liquid to be detected, the present invention can distinguish microplastics and microorganisms by using the recognition model in machine learning training in the prior art, and improve the quality of in-situ water quality. Detection accuracy of microplastic detection.

(3)本发明在流体的颗粒检测中采取可见光检测与双光谱的联合检测,由于不同物质在不同的的光线下的折射率都各不相同,这使得在光源经过颗粒之后折射进镜头的光敏元件的光信号也不同,使得摄像头捕获的颗粒形态,以及种类都大大增加,利用光谱分析颗粒种类,两者结合提高检测精度以及检测范围而且提高了检测精度。(3) The present invention adopts the joint detection of visible light detection and dual spectrum in the particle detection of fluid, because the refractive index of different substances under different light is all different, this makes the photosensitizer refracted into the lens after the light source passes through the particles The optical signals of the components are also different, which greatly increases the particle shapes and types captured by the camera. Using the spectrum to analyze the particle types, the combination of the two improves the detection accuracy and detection range and improves the detection accuracy.

附图说明Description of drawings

图1是本发明中检测装置的结构示意图;Fig. 1 is the structural representation of detection device among the present invention;

图2是本发明中检测方法的原理框图;Fig. 2 is the functional block diagram of detection method among the present invention;

图3是本发明中检测方法的方法流程图;Fig. 3 is the method flowchart of detection method among the present invention;

图4是本发明中光学检测仪器的原理框图;Fig. 4 is the functional block diagram of optical detection instrument among the present invention;

其中:in:

1、大孔径滤网,2、电子阀门,3、水泵,4、流量计,5、流道,6、生物裂解喷洒器,7、光学检测仪器,8、超声波发生器,9、风机,10、小孔径滤膜,11、加热电阻网。1. Large aperture filter, 2. Electronic valve, 3. Water pump, 4. Flow meter, 5. Flow channel, 6. Biological cracking sprinkler, 7. Optical detection instrument, 8. Ultrasonic generator, 9. Fan, 10 , Small pore diameter filter membrane, 11, heating resistance network.

具体实施方式Detailed ways

下面结合附图对本发明做进一步说明:The present invention will be further described below in conjunction with accompanying drawing:

如图1所示的一种原位水体塑料检测装置,包括流道5;所述流道5入口处设有大孔径滤网1,出口处由内向外依次设有小孔径滤膜10和加热电阻网11;所述流道5中段嵌入安装有水泵3、流量计4、生物裂解喷洒器6、光学检测仪器7、超声波发生器8和风机9。所述流道5入口处安装有液位传感器,出口处安装有电子阀门。A kind of in-situ water body plastic detection device as shown in Figure 1, comprises flow channel 5; The entrance of described flow channel 5 is provided with large-aperture filter screen 1, and the outlet is provided with small-aperture filter membrane 10 and heating successively from inside to outside. Resistance network 11; the middle section of the flow channel 5 is embedded with a water pump 3, a flow meter 4, a biolysis sprinkler 6, an optical detection instrument 7, an ultrasonic generator 8 and a fan 9. A liquid level sensor is installed at the inlet of the flow channel 5, and an electronic valve is installed at the outlet.

所述流道5用于检测水体的流通。所述水泵3,用于向流道内抽入足量的待检测水体。所述水泵3上方设有流量计4,流量计4用于控制进入流道的待检测水体的液体量,即检测量。所述生物裂解喷洒器6,用于向流道5内喷洒生物裂解液,将在流道5中流淌的待检测水体中的微生物分解掉,提高微塑料的检测精度。所述超声波发生器8,用于对待检测水体中的生物杂质的细胞进行分层处理。所述风机9,用于将超声波发生器8处理后的细胞层吹至流道5外侧,排出检测装置。所述光学检测仪器7包括数据采集单元和数据处理单元。所述数据采集单元为摄像头。所述数据处理单元包括控制器和执行器。经过预处理的检测水体流经光学检测仪器7时,光学检测仪器7对流经的待检测水体拍照,采集待检测水体的显微结构图像,将采集的数据发送至光学检测仪器7的数据处理器进行处理。所述数据处理器还用于通过流道5入口处的液位传感器和流道出口处的电子阀门,对整个流道中的检测水体的流量进行控制。所述光学检测仪器7安装在流道5的后端(即靠近流道的出口端),光学检测仪器7要位于对相机有较好的连续光源的环境下且水流速度均匀的位置。The flow channel 5 is used to detect the circulation of water body. The water pump 3 is used to draw a sufficient amount of water to be tested into the flow channel. A flow meter 4 is arranged above the water pump 3, and the flow meter 4 is used to control the liquid amount of the water body to be detected entering the flow channel, that is, the detection amount. The biolysis sprayer 6 is used to spray the biolysis liquid into the flow channel 5 to decompose the microorganisms in the water body to be detected flowing in the flow channel 5 and improve the detection accuracy of microplastics. The ultrasonic generator 8 is used for layering the cells to be detected for biological impurities in the water body. The blower 9 is used to blow the cell layer treated by the ultrasonic generator 8 to the outside of the flow channel 5 and out of the detection device. The optical detection instrument 7 includes a data acquisition unit and a data processing unit. The data acquisition unit is a camera. The data processing unit includes a controller and an actuator. When the pretreated water body for detection flows through the optical detection instrument 7, the optical detection instrument 7 takes pictures of the passing water body to be detected, collects microstructure images of the water body to be detected, and sends the collected data to the data processor of the optical detection instrument 7 to process. The data processor is also used to control the flow of the detected water body in the entire flow channel through the liquid level sensor at the inlet of the flow channel 5 and the electronic valve at the outlet of the flow channel. The optical detection instrument 7 is installed at the rear end of the flow channel 5 (i.e. close to the outlet end of the flow channel), and the optical detection instrument 7 should be located in an environment with a better continuous light source for the camera and a uniform water flow velocity.

进一步的,所述大孔径滤网1包括滤网主体和开设在滤网主体上的若干过滤孔一,所述过滤孔一的孔径的取值范围为1mm~1cm;所述大孔径过滤网采用不锈钢滤网。Further, the large-aperture filter screen 1 includes a filter screen main body and a plurality of filter holes 1 provided on the filter screen main body, and the aperture of the filter hole 1 ranges from 1 mm to 1 cm; the large-aperture filter screen adopts Stainless steel strainer.

进一步的,所述小孔径滤膜10包括滤膜主体和开设在滤膜主体上的若干过滤孔二,所述过滤孔二的孔径的取值范围为1nm~10μm;所述小孔径滤膜10采用离子微孔膜。与传统的网状滤膜相比,离子微孔滤膜最大的特点是具有真实几何意义上的孔径,孔径尺寸可在很宽的范围内(0.01-15μm)严格控制,孔径大小均匀一致。离子微孔滤膜具有较高的分离选择性,绝对截留大于孔径的任何微粒,分离效率能达到100%。离子微孔滤膜选用聚酯膜材,不吸收滤液中的物质,可防止滤液中有效成分被吸收而损失,不会有任何可迁移的物质到滤液中,因而不会污染滤液。Further, the small-pore filter membrane 10 includes a filter membrane main body and several filter holes 2 provided on the filter membrane main body, the pore diameter of the filter hole 2 ranges from 1 nm to 10 μm; the small-pore filter membrane 10 Using ionic microporous membrane. Compared with the traditional mesh filter membrane, the biggest feature of the ion microporous membrane is that it has a real geometric pore size, the pore size can be strictly controlled in a wide range (0.01-15μm), and the pore size is uniform. The ion microporous membrane has high separation selectivity, absolutely intercepts any particles larger than the pore size, and the separation efficiency can reach 100%. The ion microporous filter membrane is made of polyester membrane, which does not absorb the substances in the filtrate, and can prevent the effective components in the filtrate from being absorbed and lost. There will not be any migratable substances into the filtrate, so the filtrate will not be polluted.

进一步的,所述生物裂解喷洒器6采用的是根据林业生物防害的药剂喷洒结构改装而成,在流道5上下方都放置喷洒装置能对流过的流体裂解,裂解完的的流体经流道的出口流出至光学检测仪器7。生物裂解喷洒器6嵌入安装在流道5上,安装时要保证流道的封闭性。Further, the biological cracking sprinkler 6 is modified according to the spraying structure of the forestry biological hazard prevention. Spraying devices are placed on the upper and lower sides of the flow channel 5 to crack the fluid flowing through. The cracked fluid flows through the The outlet of the channel flows out to the optical detection instrument 7. The biological cracking sprinkler 6 is embedded and installed on the flow channel 5, and the sealing of the flow channel should be ensured during installation.

进一步的,所述光学检测仪器7采用可见光检测仪、红外光谱仪或拉曼光谱仪中的任意一种。光学检测仪器7的采集端使用千兆级的彩色高速相机,对采集的图像进行数据差异化分析,彩色图像对比等算法处理对流体的微塑料含量进行测量,侧面的光敏传感器对不同微塑料的折射率进行分辨辅助并检验相机检测结果。Further, the optical detection instrument 7 adopts any one of a visible light detector, an infrared spectrometer or a Raman spectrometer. The acquisition end of the optical detection instrument 7 uses a gigabit-level color high-speed camera to perform data differential analysis on the collected images, color image comparison and other algorithm processing to measure the microplastic content of the fluid, and the photosensitive sensor on the side to measure the microplastic content of different microplastics. The refractive index is used to assist in resolution and to verify camera detection results.

进一步的,所述超声波发生器8则采用电路板控制信号传递超声波发射器,产生相应频率的超声波将微塑料高速震动至流体表面,随后排出流道5,减少微塑料污染。Further, the ultrasonic generator 8 uses the circuit board control signal to transmit the ultrasonic transmitter to generate ultrasonic waves of corresponding frequencies to vibrate the microplastics to the surface of the fluid at high speed, and then discharge the flow channel 5 to reduce the pollution of microplastics.

本发明还涉及一种上述原位水体塑料检测装置的检测方法,该方法包括以下步骤:The present invention also relates to a detection method of the above-mentioned in-situ water body plastic detection device, the method comprising the following steps:

S1、进样S1, sample injection

将本发明所述的检测装置放置在需要检测水体中微塑料的位置,如家用水管进水口,水库检测阀,深海检测区域等位置处。打开水泵3,抽取设定体积的待检测水体,待检测水体由流道5入口进入到流道5中,在待检测水体经过大孔径滤网1时,待检测水体中的部分杂质被大孔径过滤网1过滤掉,利用设置在水泵3上的流量计4采集每次进样的待检测水体的体积。The detection device of the present invention is placed in places where microplastics in water bodies need to be detected, such as water inlets of household water pipes, reservoir detection valves, deep-sea detection areas, etc. Turn on the water pump 3 to extract a set volume of water to be tested. The water to be tested enters the flow channel 5 from the inlet of the flow channel 5. When the water to be tested passes through the large-aperture filter 1, some impurities in the water to be tested are filtered by the large-aperture filter. The filter screen 1 filters out, and the volume of the water body to be detected is collected by the flow meter 4 arranged on the water pump 3 for each sample injection.

S2、前处理S2, pre-processing

经过大孔径滤网过滤后的待检测水体沿流道5继续向前流淌,当待检测水体流经生物裂解喷洒器6时,生物裂解喷洒器6向流道5中的待检测水体喷洒生物裂解液,生物裂解液将待检测水体中的部分微生物杀死,这样减少了水体中的微生物对微塑料检测结果的干扰。当待检测水体流经超声波发生器8时,利用超声波发生器8发出的超声波将待检测水体中的水体微生物、浮游生物或微生物尸体(微生物尸体指的是前面被生物裂解液杀死的部分微生物的尸体)进行震动粉碎,进一步提高水体中微塑料检测的准确性。生物裂解液只能杀死一部分细胞,超声波相当于一种补充方法,会更彻底的清除细胞的干扰。超声波发生器发出的超声波会震碎所有细胞,震碎得到的碎片会通过小孔径滤膜过滤掉,但是超声波对微塑料没有影响。The water body to be detected after being filtered by the large-aperture filter continues to flow forward along the flow channel 5. When the water body to be detected flows through the biolysis sprinkler 6, the biolysis sprinkler 6 sprays biolysis to the water body to be detected in the flow channel 5. The biological lysate kills some microorganisms in the water body to be tested, which reduces the interference of microorganisms in the water body on the detection results of microplastics. When the water body to be detected flows through the ultrasonic generator 8, the water body microorganisms, plankton or microbial corpses in the water body to be detected are removed by the ultrasonic waves sent by the ultrasonic generator 8 (the microbial corpses refer to some microorganisms killed by the biological lysate in the front) dead bodies) to be vibrated and crushed to further improve the accuracy of microplastic detection in water bodies. The biological lysate can only kill a part of the cells, and the ultrasonic wave is equivalent to a supplementary method, which will more thoroughly remove the interference of the cells. The ultrasonic waves emitted by the ultrasonic generator will shatter all the cells, and the fragments obtained by the shattering will be filtered out through the small-pore filter membrane, but the ultrasonic waves have no effect on microplastics.

微生物不可只用滤网过滤,因为据了解,海水中除了用滤网处理较大体积的杂质外,与微塑料大小量级相近且最有干扰因素的便只有微生物,另外微生物体内也附着有一定量的微塑料,所以杀死微生物,并取出其中的微塑料也是原位水体微塑料检测的关键步骤。本发明采用生物裂解和超声波震动的方式,对微生物进行处理。Microorganisms cannot be filtered only with a filter, because it is understood that in addition to using a filter to deal with larger volumes of impurities in seawater, only microorganisms are similar in size to microplastics and have the most disturbing factors. In addition, microorganisms also adhere to a certain amount Therefore, killing microorganisms and removing the microplastics is also a key step in the in situ detection of microplastics in water bodies. The invention adopts biological cracking and ultrasonic vibration to process microorganisms.

S3、富集S3, enrichment

经前处理后的待检测水体到达小孔径滤膜10处,待检测水体中的微塑料富集到小孔径滤膜10上,其余物质随待检测水体通过小孔径滤膜10后由流道5出口流出。采用风机9对富集在小孔径滤膜10上的微塑料进行风干,采用加热电阻网11对富集在小孔径滤膜10上的微塑料进行加热烘干。After pretreatment, the water body to be tested reaches the small-pore filter membrane 10, and the microplastics in the water body to be tested are enriched on the small-pore filter membrane 10, and the remaining substances pass through the small-pore filter membrane 10 along with the water body to be tested. Outflow. The fan 9 is used to air-dry the microplastics enriched on the small-aperture filter membrane 10 , and the heating resistor net 11 is used to heat and dry the microplastics enriched on the small-aperture filter membrane 10 .

S4、光学检测S4. Optical detection

采用光学检测仪器对富集在小孔径滤膜上的微塑料进行检测,获取微塑料的种类及浓度。光学检测的目的是检测微塑料的种类和其对应的浓度,在最后一个平面上,先采用显微摄像头以成像的方式对微塑料的数量做一个估计,再用拉曼与红外光谱利用不同微塑料物理性质不同确定微塑料的种类。Optical detection instruments are used to detect the microplastics enriched on the small-pore filter membrane to obtain the type and concentration of microplastics. The purpose of optical detection is to detect the types of microplastics and their corresponding concentrations. On the last plane, the microscopic camera is used to estimate the amount of microplastics in the form of imaging, and then Raman and infrared spectroscopy are used to use different microplastics. The different physical properties of plastics determine the types of microplastics.

由于双光谱只能检测一个点的微塑料信息,若采用点扫描的方式,不仅设计复杂,扫描时间也会很长。光学检测仪器的摄像机拍摄检测完,选取几个微塑料分布较多的位置作为微塑料分布坐标。光学检测仪器是利用摄像头对富集在小孔径滤膜上的微塑料进行拍照,从照片上能够看到哪些区域微塑料较多,哪些区域微塑料较少,多选取几个微塑料分布较多的位置,作为微塑料分布坐标。双光谱检测只需要根据微塑料分布坐标去对应的点进行检测即可,这大大减小了检测时间。双光谱检测指的是采用红外光谱和拉曼光谱对微塑料进行检测,这两种光谱检测微塑料是现有技术。本发明通过微塑料分布坐标,确定双光谱检测的检测位置,而不是对全区域进行扫描,这会大大缩减双光谱的工作时间,得到的结果也会相对准确。Since the dual spectrum can only detect the microplastic information of one point, if the point scanning method is used, not only the design is complicated, but also the scanning time will be very long. After the camera of the optical detection instrument has finished shooting and detecting, several locations where there are more microplastics are selected as the distribution coordinates of microplastics. The optical detection instrument uses a camera to take pictures of the microplastics enriched on the small-pore filter membrane. From the photos, it can be seen which areas have more microplastics and which areas have less microplastics. Select a few more microplastics to distribute more The location of , as the distribution coordinates of microplastics. Dual-spectrum detection only needs to detect the corresponding points according to the distribution coordinates of microplastics, which greatly reduces the detection time. Dual-spectrum detection refers to the detection of microplastics using infrared spectroscopy and Raman spectroscopy, which are existing technologies for detecting microplastics with these two spectra. The present invention determines the detection position of dual-spectrum detection through the distribution coordinates of microplastics, instead of scanning the whole area, which will greatly reduce the working time of dual-spectrum and obtain relatively accurate results.

由于水中微生物在前处理过程中没有完全去除干净,为了提高系统的鲁棒性,在采用光学检测仪器进行检测时候,利用图像处理方法对微塑料与微生物进行区分与筛查。根据图片识别不同物体,类似于AI的人脸识别,从图像中识别微塑料和微生物。由于微生物的形状相对对称、整齐,例如像一个圆、椭圆,或者触角对称。而微塑料的形状并没有明显的规律,对称性不强,因此从这些特征点出发,可以很好地区分微生物与微塑料。如何区分检测物体形状的对称性或非对称性,采用现有的AI技术实现。Since the microorganisms in the water were not completely removed during the pretreatment process, in order to improve the robustness of the system, when using optical detection instruments for detection, image processing methods were used to distinguish and screen microplastics and microorganisms. Recognize different objects based on pictures, similar to AI face recognition, and identify microplastics and microorganisms from images. Since the shape of microorganisms is relatively symmetrical and neat, such as a circle, an ellipse, or symmetrical antennae. The shape of microplastics has no obvious rules, and the symmetry is not strong. Therefore, starting from these characteristic points, microorganisms and microplastics can be well distinguished. How to distinguish the symmetry or asymmetry of the shape of the detected object is realized by using the existing AI technology.

本发明中的光学检测采用了可见光检测与双光谱的联合检测以及检测仪器对于微塑料与微生物的区分算法。本发明所采用的光学检测仪器的原理框图如图4所示。本发明在光学检测仪器的摄像头的对面光源处,切换光源。由于不同物质在不同的光线下的折射率都各不相同,这使得在光源经过颗粒之后折射进镜头的光敏元件的光信号也不同,使得摄像头捕获的颗粒形态,以及种类都大大增加。可见光检测与双光谱的联合检测不仅提高了检测精度,而且能够提高检测能力,检测范围扩大。The optical detection in the present invention adopts the joint detection of visible light detection and dual spectrum and the detection instrument's algorithm for distinguishing microplastics and microorganisms. The principle block diagram of the optical detection instrument adopted in the present invention is shown in FIG. 4 . The invention switches the light source at the light source opposite to the camera of the optical detection instrument. Since the refractive index of different substances is different under different light, this makes the light signal of the photosensitive element refracted into the lens after the light source passes through the particles is also different, so that the shape and type of particles captured by the camera are greatly increased. The joint detection of visible light detection and dual spectrum not only improves the detection accuracy, but also improves the detection ability and expands the detection range.

由于能够拍摄显微的结构,可以通过识别算法来区分微塑料与微生物,原因在于,微塑料结构是比较对称的,微生物的细胞由于细胞的分化,形态不会对称,而且微生物的细胞结构已经有成熟的判断标准,比如细胞核等,这与微塑料有很大的区别;所以只要能拍摄到显微结构加上成熟的机器学习训练的识别模型,能够将二者区分,这能够提高检测精度,而且对后面的质量浓度的检测奠定基础。Because microscopic structures can be photographed, microplastics and microorganisms can be distinguished through recognition algorithms. The reason is that the structure of microplastics is relatively symmetrical, and the morphology of microbial cells will not be symmetrical due to cell differentiation, and the cell structure of microorganisms has already Mature judgment criteria, such as cell nuclei, are quite different from microplastics; so as long as the microstructure can be photographed and a mature machine learning-trained recognition model can be used to distinguish the two, this can improve detection accuracy. And it lays the foundation for the subsequent detection of mass concentration.

本发明所述的原位水体微塑料检测装置的检测方法的具体流程如图3所示:The specific process of the detection method of the in-situ water body microplastic detection device described in the present invention is shown in Figure 3:

(1)检测进行之前先判断上次检测是否完成,主要通过判断加热电阻网11的温度是否已经降低至未工作时的温度值A,并判断光学检测仪器7工作是否结束,结束时会对控制单元返回信号。(1) Before the detection is carried out, judge whether the last detection is completed, mainly by judging whether the temperature of the heating resistor network 11 has been reduced to the temperature value A when not working, and judging whether the work of the optical detection instrument 7 is over. The unit returns the signal.

(2)确定上次检测完成后打开进电子阀门2,流体经过大孔径滤网1之后,流量计4检测总水体体积,当总水体体积达到设定的阈值N时,关闭进水阀门(即电子阀门2)。(2) Open the electronic inlet valve 2 after confirming that the last detection is completed. After the fluid passes through the large-aperture filter screen 1, the flow meter 4 detects the total water body volume. When the total water body volume reaches the set threshold N, close the water inlet valve (i.e. Electronic valve 2).

(3)由于不同水域微生物含量不同,所以需判断,若微生物含量超过阈值C,则选择生物裂解喷洒器6喷洒生物裂解液和开启超声波发生器8发出超声波的方式对待检测水体中的微生物进行生物裂解和超声波处理。生物裂解液的喷洒是一个相对封闭的罐体,进样阀和出样阀均有喷洒装置。当罐体中的流体体积达到设定值之后开始喷洒裂解液停留相应时间后流出。(3) Due to the different microbial content in different waters, it needs to be judged. If the microbial content exceeds the threshold C, then select the biological cracking sprinkler 6 to spray the biological cracking liquid and turn on the ultrasonic generator 8 to send out ultrasonic waves. Lysis and sonication. The spraying of the biological lysate is a relatively closed tank, and both the sampling valve and the sampling valve have spraying devices. When the fluid volume in the tank reaches the set value, it starts to spray the lysate and then flows out after staying for a corresponding period of time.

(4)经过生物裂解和超声波去除生物杂质之后流体经过小孔径滤膜10,采用小孔径滤膜10进行第二次过滤。待检测水体中的微塑料富集到小孔径滤膜10上,其余物质随待检测水体通过小孔径滤膜10由流道5出口流出。采用风机9对富集在小孔径滤膜10上的微塑料进行风干以降低水分含量,采用加热电阻网11对富集在小孔径滤膜10上的微塑料进行加热烘干。(4) After biolysis and ultrasonic removal of biological impurities, the fluid passes through the small-pore filter membrane 10, and the small-pore filter membrane 10 is used for second filtration. The microplastics in the water body to be detected are enriched on the filter membrane 10 with a small pore size, and the remaining substances flow out from the outlet of the flow channel 5 through the filter membrane 10 with a small pore size along with the water body to be detected. The fan 9 is used to air-dry the microplastics enriched on the small-aperture filter membrane 10 to reduce the moisture content, and the heating resistor net 11 is used to heat and dry the microplastics enriched on the small-aperture filter membrane 10 .

(5)对富集在小孔径滤膜10上的微塑料进行光学检测,光学检测仪器7处的光源分别为可见光,拉曼光谱,和红外光谱,分别射出不同的光线,摄像头对可见光下的颗粒进行数据收集,光学检测仪器7中的光敏传感器则收集其他光谱照射时,微塑料对其折射的光线从而判断其颗粒种类。(5) Optical detection is carried out on the microplastics enriched on the small-aperture filter membrane 10. The light sources at the optical detection instrument 7 are respectively visible light, Raman spectrum, and infrared spectrum, which emit different light rays respectively. The camera detects the microplastics under visible light Particles collect data, and the photosensitive sensor in the optical detection instrument 7 collects light refracted by microplastics when other spectra are irradiated to determine the type of particles.

(6)根据光学检测仪器的综合检测进行计数,检测出各种微塑料浓度X1、X2……。若X1、X2……太小,或等于0,则说明抽取的总水体体积不够可以继续开阀门加水,以达到可检测最小浓度;再做一次检测,若重复实验结果不变则说明不足以得到检测最小浓度范围。若达到最小值,则对流体进行重复检测并输出检测结果各微塑料浓度为Xi/N。(6) Count according to the comprehensive detection of the optical detection instrument, and detect the concentrations of various microplastics X 1 , X 2 . . . If X 1 , X 2 ... are too small, or equal to 0, it means that the total volume of water drawn is not enough. You can continue to open the valve and add water to reach the minimum detectable concentration; do another test, if the repeated test results remain unchanged, it means insufficient In order to obtain the detection minimum concentration range. If the minimum value is reached, the fluid is repeatedly detected and the detection result is output as the concentration of each microplastic is X i /N.

(7)最后清理流道1、大孔径滤网1和小孔径滤膜10,复位装置准备下一次检测。(7) Finally, the flow channel 1, the large-aperture filter screen 1 and the small-aperture filter membrane 10 are cleaned, and the reset device is ready for the next detection.

综上所述,本发明将进样、前处理、富集和光学检测技术集成为一体,能够对水体微塑料丰度、种类原位进行实时探测。In summary, the present invention integrates sampling, pretreatment, enrichment and optical detection technologies, and can detect the abundance and types of microplastics in water in real time in situ.

以上所述的实施例仅仅是对本发明的优选实施方式进行描述,并非对本发明的范围进行限定,在不脱离本发明设计精神的前提下,本领域普通技术人员对本发明的技术方案作出的各种变形和改进,均应落入本发明权利要求书确定的保护范围内。The above-mentioned embodiments are only descriptions of preferred implementations of the present invention, and are not intended to limit the scope of the present invention. Variations and improvements should fall within the scope of protection defined by the claims of the present invention.

Claims (8)

1. The utility model provides an normal position water plastics detection device which characterized in that: comprises a flow passage; a filter screen is arranged at the inlet of the flow channel, and a filter membrane and a heating resistance net are sequentially arranged at the outlet from inside to outside; and the middle section of the flow channel is provided with a water pump, a biological cracking sprayer, an optical detection instrument, an ultrasonic generator and a fan.
2. The in-situ water body plastic detection device according to claim 1, wherein: and a liquid level sensor is installed at the inlet of the flow channel, and an electronic valve is installed at the outlet of the flow channel.
3. The in-situ water body plastic detection device according to claim 1, wherein: the flow channel is used for detecting the circulation of the water body; the water pump is used for pumping sufficient water to be detected into the flow channel; a flow meter is arranged above the water pump and used for controlling the liquid amount of the water body to be detected entering the flow channel, namely the detected amount; the biological cracking sprayer is used for spraying biological cracking liquid into the flow channel and decomposing microorganisms in the water body to be detected flowing in the flow channel; the ultrasonic generator is used for carrying out layering treatment on cells of biological impurities in the water body to be detected; and the fan is used for blowing the cell layer processed by the ultrasonic generator to the outer side of the flow channel and discharging the cell layer out of the detection device.
4. The in-situ water body plastic detection device according to claim 1, wherein: the optical detection instrument comprises a data acquisition unit and a data processing unit; the data acquisition unit is a camera; the data processing unit comprises a controller and an actuator; the optical detection instrument is used for photographing the flowing water body to be detected, acquiring the microstructure image of the water body to be detected, and sending the acquired image data to the data processor of the optical detection instrument for processing; the data processor is also used for controlling the flow of the water body to be detected in the whole flow channel through the liquid level sensor at the inlet of the flow channel and the electronic valve at the outlet of the flow channel.
5. The in-situ water body plastic detection device according to claim 1, wherein: the filter screen is a large-aperture filter screen; the large-aperture filter screen comprises a filter screen main body and a plurality of first filter holes arranged on the filter screen main body, wherein the aperture of the first filter holes ranges from 1mm to 1cm; the large-aperture filter screen is a stainless steel filter screen.
6. The in-situ water body plastic detection device according to claim 1, wherein: the filter membrane is a small-aperture filter membrane; the small-aperture filter membrane comprises a filter membrane main body and a plurality of second filter holes formed in the filter membrane main body, and the aperture of the second filter holes ranges from 1nm to 10 microns; the small-aperture filter membrane adopts an ion microporous membrane.
7. The in-situ water body plastic detection device according to claim 1, wherein: the optical detection instrument adopts any one of a visible light detector, an infrared spectrometer or a Raman spectrometer.
8. The detection method of the in-situ water body plastic detection device according to any one of claims 1 to 7, characterized by comprising the following steps: the method comprises the following steps:
s1, sample introduction
Opening a water pump, extracting a water body to be detected with a set volume, enabling the water body to be detected to enter a flow channel from a flow channel inlet, filtering part of impurities in the water body to be detected by a large-aperture filter screen when the water body to be detected passes through the large-aperture filter screen, and collecting the volume of the water body to be detected of each sample introduction by using a flowmeter arranged on the water pump;
s2, pretreatment
The water body to be detected after being filtered by the large-aperture filter screen continuously flows forwards along the flow channel, when the water body to be detected flows through the biological cracking sprinkler, the biological cracking sprinkler sprays biological cracking liquid to the water body to be detected in the flow channel, the biological cracking liquid kills part of microorganisms in the water body to be detected, and when the water body to be detected flows through the ultrasonic generator, the ultrasonic waves emitted by the ultrasonic generator are utilized to vibrate and crush the microorganisms, plankton or microorganism corpses in the water body to be detected;
s3, enrichment
The pretreated water body to be detected reaches the small-aperture filter membrane, the micro-plastic in the water body to be detected is enriched on the small-aperture filter membrane, and the rest substances flow out of the runner outlet after passing through the small-aperture filter membrane along with the water body to be detected; air-drying the micro-plastics enriched on the small-aperture filter membrane by using a fan, and heating and drying the micro-plastics enriched on the small-aperture filter membrane by using a heating resistance net;
s4, optical detection
And detecting the micro-plastic enriched on the small-aperture filter membrane by using an optical detection instrument to obtain the type and the concentration of the micro-plastic.
CN202210898858.9A 2022-07-28 2022-07-28 A kind of in-situ water body microplastic detection device and detection method thereof Pending CN115266621A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117388135A (en) * 2023-10-30 2024-01-12 山东建筑大学 Device and method for in-situ enrichment detection of rubber asphalt pavement runoff water body microplastic

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117388135A (en) * 2023-10-30 2024-01-12 山东建筑大学 Device and method for in-situ enrichment detection of rubber asphalt pavement runoff water body microplastic

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