CN210376254U - Combined detection equipment for measuring mercury and arsenic in different forms in water body - Google Patents
Combined detection equipment for measuring mercury and arsenic in different forms in water body Download PDFInfo
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- CN210376254U CN210376254U CN201921157662.4U CN201921157662U CN210376254U CN 210376254 U CN210376254 U CN 210376254U CN 201921157662 U CN201921157662 U CN 201921157662U CN 210376254 U CN210376254 U CN 210376254U
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Abstract
The utility model provides a ally oneself with check out test set that is arranged in mercury of survey different forms and arsenic in water, include: the liquid chromatograph is used for separating mercury and arsenic in a water sample to be detected by using the chromatographic column; the inductively coupled plasma mass spectrometer is used for measuring mercury element and arsenic element; the liquid chromatograph is connected with an interface device of the inductively coupled plasma mass spectrometer through a PEEK pipe; the liquid chromatograph and the inductively coupled plasma mass spectrometer are also connected through a trigger line and are respectively connected with a data processing device. The utility model discloses a set up the trigger line, can directly start the electric induction coupling plasma mass spectrograph after liquid chromatograph advances a kind and finishes and gather the signal, avoided having improved response speed as intermediate equipment secondary transmission instruction through data processing apparatus.
Description
Technical Field
The utility model belongs to water environment check out test set field especially relates to a ally oneself with check out test set that is arranged in mercury of survey different forms and arsenic in the water.
Background
With the development of disciplines such as environmental science, biomedicine, etc., many scholars recognize that bioavailability, toxicity, and chemical activity and removability in the environment of heavy metals are not only related to the total amount of heavy metals, but to a greater extent are determined by their morphology, with different morphologies producing different environmental effects. A specific element can act on a living system and living organisms only in a specific concentration range and in a specific existing form. According to the International Union of Pure and Applied Chemistry (IUPAC) definition: the morphology of an element is the appearance or distribution of the element in different classes of compounds: morphological analysis is the qualitative and quantitative analysis activity of one or more chemical morphologies of elements in a sample. The element form analysis needs to carry out in-situ, on-line, micro-area and instantaneous high-sensitivity and high-resolution comprehensive analysis on the element form in an environment and a biochemical sample by using a modern analysis technology, a single instrument or technology is difficult to complete, and the adoption of a combined technology is an important research means of modern analysis science.
Due to the strong toxicity of the methyl mercury, the limit value of the methyl mercury is specified in the current environmental quality standard, and the measuring method of the methyl mercury is specified in the related standard method. The methyl mercury in air is measured by gas chromatography (GB/T17132-1997), the methyl mercury in water is measured by gas chromatography (GB/T14204-93), and the acid extraction method of sulfhydryl cotton (GB/T5009.17-2003) is used in food.
Arsenic morphological analysis is an analysis method for separating, identifying and measuring the content of various arsenide in a sample, and a silver salt method and a new silver salt method are mostly adopted in the early stage. In recent years, some new color development methods for detecting trace arsenic have appeared. Such as a tree in the state of H2SO4In the medium, trace As (III) can inhibit the fading reaction of potassium bromate, potassium bromide and zirconium reagents, and a method for measuring trace As (III) is established and used for measuring As (III) in wastewater. The new absorptiometry method for rapidly determining trace arsenic in crude oil is established in Junxing et al, wherein ammonium aluminate reacts with As (V) to generate ammonium arsenate-aluminate, rhodamine is used As a color developing agent to combine with the ammonium aluminate to generate a polyvinyl alcohol system of a ternary complex. Jiahuasheng etc. uses mercapto cotton to separate and enrich arsenic, then uses K2Cr2O7Oxidation of As (III) in a strongly acidic medium to produce Cr3+By means of the generation of Cr3+Catalytic luminol-H2O2Chemiluminescence established an indirect method for the determination of As (III). These methods can be applied to morphological analysis of arsenic, but the methods have low sensitivity and complicated operation, and are rarely used at present.
In general, the content of mercury and arsenic in an environmental water body is low, a set of analysis method with high sensitivity and strong selectivity is needed for accurately measuring the forms of compounds of mercury and arsenic, and the comprehensive analysis of in-situ, on-line, micro-area and instantaneous high sensitivity and high resolution of mercury and arsenic elements in a sample is difficult to complete by a single instrument or technology. Therefore, the research of the technologies of pretreatment, separation and detection of samples for measuring arsenide by using the coupling technology is always the key point of the environmental analytical chemistry research.
However, no instrument and equipment capable of measuring mercury and arsenic in different forms with high accuracy, high efficiency and practicability is disclosed in the existing detection equipment for water samples.
In the actual operation process, mercury and arsenic in the natural environment need to be detected, but the content of various forms of arsenic compounds and mercury compounds in an environmental sample is low, the structure is complex, and therefore the adoption of a detector with high sensitivity is the key of success.
SUMMERY OF THE UTILITY MODEL
The utility model aims at prior art not enough, provide a ally oneself with check out test set that is arranged in mercury of survey different forms and arsenic in the water for the content of mercury and arsenic detects among the natural environment, and arsenic compound and mercury compound content detection precision and efficiency provide convenience in the sample for promote detection ring border.
According to an aspect of the utility model, a ally oneself with check out test set that is arranged in mercury of survey different forms and arsenic in the water is proposed, include: the liquid chromatograph is used for separating mercury and arsenic in a water sample to be detected by using the chromatographic column; the inductively coupled plasma mass spectrometer is used for measuring mercury element and arsenic element; a PEEK (polyether ether ketone, PEEK for short) tube disposed between the liquid chromatograph and the inductively coupled plasma mass spectrometer, the PEEK tube connecting an outlet end of a chromatographic column of the liquid chromatograph to an interface device of the inductively coupled plasma mass spectrometer; a trigger line for synchronously starting the liquid chromatograph and the inductively coupled plasma mass spectrometer, wherein the trigger line is connected to a control signal input interface of the inductively coupled plasma mass spectrometer from a signal output interface of the liquid chromatograph; a data processing device for collecting and processing data, the data processing device being connected to the liquid chromatograph and the inductively coupled plasma mass spectrometer, respectively, wherein the interface device comprises: the device comprises a liquid inlet, an auxiliary gas inlet and an atomizing gas inlet which are connected with a mixer, wherein the front end of the mixer is sequentially connected with a first heater and a discharge structure, the front end of the discharge structure is provided with a sample flow channel, the outer side of the sample flow channel is provided with a nitrogen channel and a nitrogen heater, the first heater is provided with a plurality of layers of channels, and connecting pieces are arranged among the channels; the discharge structure is a multi-stage corona needle discharge structure.
In some embodiments, a quaternary gradient pump may be disposed within the liquid chromatograph.
In some embodiments, the interface device may be an atmospheric pressure chemical ionization interface.
In some embodiments, the first heater includes a first heating layer having a tubular shape, a second heating layer, and a third heating layer having a cylindrical shape, and the first heating layer, the second heating layer, and the third heating layer are fixedly connected to each other by the cylindrical connecting member.
In some embodiments, the first heating layer, the second heating layer, the third heating layer and the cylindrical connecting piece are provided with ceramic layers on the outer sides.
In some embodiments, the multi-stage corona needle discharge structure is a secondary corona needle discharge structure, which specifically includes: the corona discharge device comprises a first fusiform ionization chamber and a second fusiform ionization chamber which are sequentially connected, wherein a first corona needle is arranged in the middle of the first fusiform ionization chamber, and a second corona needle is arranged in the middle of the second fusiform ionization chamber.
In some embodiments, a second heater is disposed between the first and second shuttle-shaped electrical de-ionized bins.
In some embodiments, the first corona needle and the second corona needle are provided in a plurality and are respectively and annularly arranged in the middle of the first fusiform ionization chamber and the second fusiform ionization chamber.
In some embodiments, the liquid chromatograph is an LC 1200-type liquid chromatograph.
In some embodiments, the inductively coupled plasma mass spectrometer is a NexION 300Q-type inductively coupled plasma mass spectrometer.
The beneficial effects of the utility model reside in at least:
the utility model discloses a set up trigger line and connect liquid chromatograph and inductive coupling plasma mass spectrograph, through setting up the trigger line, can directly start inductive coupling plasma mass spectrograph after liquid chromatograph advances the appearance and finishes and gather the signal, avoided having improved response speed as intermediate equipment secondary transmission instruction through data processing apparatus.
The utility model discloses a set up trigger line connection liquid chromatograph and inductive coupling plasma mass spectrograph, through changing interface arrangement's first heater structure can improve heating efficiency, is favorable to the gasification of solvent.
The utility model discloses a set up trigger line connection liquid chromatograph and inductive coupling plasma mass spectrograph, through designing multistage corona needle discharge structure, can improve ionization efficiency, further improve the monitoring ability to trace mercury compound and arsenic compound.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts. Moreover, the components in the figures are not drawn to scale, but are merely illustrative of the principles of the invention. For convenience in illustrating and describing some portions of the present invention, corresponding parts of the drawings may be exaggerated, i.e., may be larger, relative to other components in an exemplary device actually manufactured according to the present invention. In the drawings:
FIG. 1 is a schematic view of a connection structure of a combined detection apparatus for detecting mercury and arsenic in different forms in a water body according to an embodiment of the present invention;
fig. 2 is a schematic structural view of an interface device of a combined detection apparatus for detecting mercury and arsenic in different forms in a water body according to an embodiment of the present invention;
fig. 3 is a cross-sectional view taken at a-a in fig. 2.
FIG. 4 is a schematic structural view of an interface device of a combined detection apparatus for detecting mercury and arsenic in different forms in a water body according to another embodiment of the present invention;
in the figure: 1-liquid chromatograph, 2-interface device, 201-mixer, 202-liquid inlet, 203-auxiliary gas inlet, 204-atomization gas inlet, 205-first heater, 2051-first heating layer, 2052-second heating layer, 2053-third heating layer, 2054-connector, 206-discharge structure, 2061-first shuttle ionization chamber, 2062-second shuttle ionization chamber, 2063-first corona needle, 2064-second corona needle, 2065-second heater, 207-sample flow channel, 208-nitrogen channel, 209-nitrogen heater, 3-inductive coupling plasma mass spectrometer, 4-trigger wire, 5-data processing device, 6-PEEK tube;
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the embodiments of the present invention are described in further detail below with reference to the accompanying drawings. The exemplary embodiments and descriptions of the present invention are provided to explain the present invention, but not to limit the present invention.
It should also be noted that, in order to avoid obscuring the invention with unnecessary details, only the structures and/or process steps that are closely related to the solution according to the invention are shown in the drawings, while other details that are not relevant to the invention are omitted.
To the less characteristics that are difficult to detect of mercury compound and arsenic compound content in the natural environment sample, the utility model provides a ally oneself with and use check out test set that is arranged in the mercury of survey different forms and arsenic in the water, improved the lower appearance of waiting to survey of content.
As shown in fig. 1, in an embodiment of the present invention, a combined detection apparatus for detecting mercury and arsenic in different forms in a water body is provided, which includes:
a liquid chromatograph 1 for separating mercury and arsenic in a water sample to be detected by using a chromatographic column;
an inductively coupled plasma mass spectrometer 2 for measuring mercury and arsenic;
a PEEK tube 6 disposed between the liquid chromatograph 1 and the inductively coupled plasma mass spectrometer 2, the PEEK tube 6 connecting an outlet end of a chromatography column of the liquid chromatograph 1 to the interface device 2 of the inductively coupled plasma mass spectrometer 3;
a trigger line 4 for synchronously starting the liquid chromatograph 1 and the inductively coupled plasma mass spectrometer 3, wherein the trigger line 4 is connected from a signal output interface (not shown) of the liquid chromatograph 1 to a control signal input interface (not shown) of the inductively coupled plasma mass spectrometer 4;
and the data processing device 5 is used for acquiring and processing data, and the data processing device 5 is respectively connected with the liquid chromatograph 1 and the inductively coupled plasma mass spectrometer 3.
Through setting trigger line 4, this embodiment can be in liquid chromatograph 1 advances to advance to start immediately after accomplishing inductively coupled plasma mass spectrograph 3 realizes no differentiation, reduces the sample and runs off, can be more accurate to detect to the mercury compound and the arsenic compound that content is very little in the natural sample.
Further, since the liquid chromatograph 1 and the inductively coupled plasma mass spectrometer 3 used in this embodiment are not instruments of the same manufacturer, in order to implement the combination, the data processing device 5 stores and runs the combination software for integrally controlling the combination step, and is mainly used for controlling the inductively coupled plasma mass spectrometer 3 to implement continuous signal acquisition. The combined software can carry out integral calculation on the signals to realize quantitative calculation.
In some embodiments, a quaternary gradient pump is disposed within the liquid chromatograph 1.
In some embodiments, the interface device 2 is an atmospheric pressure chemical ionization interface.
The liquid chromatogram-prismoid combination combines the separation capability of the liquid chromatograph 1 for effectively separating the thermal instability and the high-boiling point compound and the strong component identification capability of the inductively coupled plasma mass spectrometer 3, is an effective means for separating and analyzing complex organic mixtures, and the online key is the development of an applicable interface device, the solvent must be removed before the sample components enter an ion source, and the interface device plays a great role in the process of removing the solvent and promoting the ionization of sample molecules.
In this embodiment, the combined detection apparatus for detecting mercury and arsenic in different forms in a water body employs an atmospheric pressure chemical ionization interface, which can increase the yield of an ionization product, and can be comprehensively applied to analysis and detection of polar or nonpolar compounds, and fragments of the ionization product are few, mainly an excimer ion peak, so that the molecular mass of the compound for detection is generally less than 1000 Da.
In some embodiments, as shown in fig. 2, the interface device 2 comprises: the device comprises a liquid inlet 202, an auxiliary gas inlet 203 and an atomizing gas inlet 204 which are connected with a mixer 201, wherein the front end of the mixer 201 is sequentially connected with a first heater 205 and a discharge structure 206, the front end of the discharge structure 206 is provided with a sample flow channel 207, the outer side of the sample flow channel 207 is provided with a nitrogen gas channel 208 and a nitrogen gas heater 209, the first heater 205 is provided with a plurality of layers of channels, and a connecting piece 2054 is arranged between each channel; the discharge structure 206 is a multi-stage corona needle discharge structure (not shown).
In this case, in order to further improve the solvent removal rate and the ionization rate, on the basis of the conventional atmospheric pressure chemical ionization interface, the structure of the first heater 205 is changed and is set to be a multilayer structure, so that the heat exchange area is increased; furthermore, through setting up multistage corona needle discharge structure, the ionization efficiency of improvement that can be very big has greatly improved in the natural sample, the ability and the degree of accuracy of examining of mercury compound and arsenic compound that the content is less.
In some embodiments, as shown in fig. 3, the first heater 205 includes a first heating layer 2051 having a tubular shape, a second heating layer 2052, and a third heating layer 2053 having a cylindrical shape, and the first heating layer 2051, the second heating layer 2052, and the third heating layer 2053 are fixedly connected to each other by a cylindrical connecting member 2054.
In this embodiment, in order to further improve the heating capacity of the first heater 205 to the liquid sample, thereby improving the detection effect, the first heater 205 is configured as a three-layer heating structure, after the sample is mixed with the assist gas and the atomizing gas, the sample flows through the space among the first heating layer 2051, the second heating layer 2052 and the third heating layer 2053, and forms a turbulent flow through the cylindrical connecting piece 2054, thereby further improving the contact area and time of the heat exchange surface, and improving the heat exchange efficiency.
In some embodiments, the first heating layer 2051, the second heating layer 2052, the third heating layer 2053, and the cylindrical connecting member 2054 are provided with ceramic layers on the outer sides thereof.
Since the target of the present application is the mercury compound and the arsenic compound which are contained in the natural sample in small amounts, the content of the mercury compound and the arsenic compound is extremely small, and therefore, the mercury compound and the arsenic compound are influenced by the equipment during the detection process, and the detection is inaccurate.
In this affair example, through setting up the ceramic layer makes first heater 205 inner structure inertization, isolated to the influence of trace determinand, further promote the degree of accuracy that detects.
In some embodiments, as shown in fig. 2, the multi-stage corona needle discharge structure is a secondary corona needle discharge structure (not labeled in the figure), and specifically includes: the ionization chamber comprises a first fusiform ionization chamber 2061 and a second fusiform ionization chamber 2062 which are connected in sequence, wherein a first corona needle 2063 is arranged in the middle of the first fusiform ionization chamber 2061, and a second corona needle 2064 is arranged in the middle of the second fusiform ionization chamber 2062.
In the detection process of the inductively coupled plasma mass spectrometer 3, the ionization step is extremely important, and the degree of ionization directly influences the detection result. Under the premise that the object to be detected is in a trace amount, the ionization efficiency needs to be further improved so as to improve the detection precision.
In this case, a two-stage corona needle discharge structure is adopted, in which the first corona needle 2063 and the second corona needle 2064 are respectively disposed at the middle positions of the first and second fusiform ionization chambers 2061 and 2062, and when the mixture gas of the gasified liquid to be measured, the auxiliary gas and the atomizing gas flows through the middle large-radius positions of the first and second fusiform ionization chambers 2061 and 2062, the speed is reduced, and the two-stage discharge ionization is performed through the first corona needle 2063 and the second corona needle 2064, so that the ionization efficiency is greatly improved.
In some embodiments, as shown in fig. 4, a second heater 2065 is disposed between the first and second shuttle ionization chambers 2061 and 2062.
On the basis of the previous embodiment, due to the addition of the flow path, in order to prevent the solvent in the liquid to be detected from being liquefied again in the ionization process, the temperature can be effectively reduced by adding the second heater 2065, and the detection efficiency can be guaranteed.
In some embodiments, the first corona pin 2063 and the second corona pin 2064 are provided in a plurality, and are respectively arranged in the middle of the first and second fusiform ionization chambers 2061 and 2062 in an annular shape.
In this embodiment, a plurality of the first corona pins 2063 and the second corona pins 2064 are provided at the same position, and the electrodes are kept consistent, so as to ensure the ionization quality of corona.
In some embodiments, the liquid chromatograph 1 is an LC 1200-type liquid chromatograph.
In some embodiments, the inductively coupled plasma mass spectrometer 3 is a NexION 300Q-type inductively coupled plasma mass spectrometer.
The key point of the online method is the development of an applicable interface, a solvent must be removed before sample components enter an ion source, at present, a crawler-type heating conveyor belt is mostly adopted, the defects are that components with the boiling point close to or low than that of the solvent of ① cannot be detected, the advantages of HPLC (high performance liquid chromatography) separation of heat-instable substances are lost in a certain sense, ③ solvent is difficult to volatilize, the background effect is high, and the resolution is not facilitated, so the LC/MS is in a development stage and is not universal enough in application.
The key technology of the liquid chromatogram-mass spectrum combination is an interface device of a liquid chromatograph and a mass spectrometer. The device plays a great role in removing the solvent and promoting the ionization process of sample molecules. The research of the liquid chromatography-mass spectrometry technology began in the 70 s of the 20 th century, and the liquid chromatography-mass spectrometry technology underwent a much longer exploration process compared with the gas chromatography-mass spectrometry technology. Early interface devices, such as conveyor belt interfaces, thermal spray interfaces, particle beam interfaces, etc., have not been commercially available for use with liquid chromatography-mass spectrometry due to the varying degrees of defects. The advent of atmospheric pressure chemical ionization source (APCI) did not bring a historical revolution to the liquid chromatography-mass spectrometry technology until the 90 s, and it was its advent that further pushed the pace at which liquid chromatography-mass spectrometry technology was put into commercial use.
In the description herein, reference to the description of the terms "one embodiment," "a particular embodiment," "some embodiments," "for example," "an example," "a particular example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. The sequence of steps involved in the embodiments is for illustrative purposes, and the sequence of steps is not limited and may be adjusted as desired.
The above-mentioned embodiments, further detailed description of the objects, technical solutions and advantages of the present invention, it should be understood that the above-mentioned embodiments are only specific embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (7)
1. A combination test device for use in the determination of different forms of mercury and arsenic in a body of water, the test device comprising:
the liquid chromatograph is used for separating mercury and arsenic in a water sample to be detected by using the chromatographic column;
the inductively coupled plasma mass spectrometer is used for measuring mercury element and arsenic element;
a PEEK tube disposed between the liquid chromatograph and the inductively coupled plasma mass spectrometer, the PEEK tube connecting an outlet end of a chromatography column of the liquid chromatograph to an interface device of the inductively coupled plasma mass spectrometer;
a trigger line for synchronously starting the liquid chromatograph and the inductively coupled plasma mass spectrometer, wherein the trigger line is connected to a control signal input interface of the inductively coupled plasma mass spectrometer from a signal output interface of the liquid chromatograph;
the data processing device is used for acquiring and processing data and is respectively connected with the liquid chromatograph and the inductively coupled plasma mass spectrometer;
the interface device includes: the device comprises a liquid inlet, an auxiliary gas inlet and an atomizing gas inlet which are connected with a mixer, wherein the front end of the mixer is sequentially connected with a first heater and a discharge structure, the front end of the discharge structure is provided with a sample flow channel, the outer side of the sample flow channel is provided with a nitrogen channel and a nitrogen heater, the first heater is provided with a plurality of layers of channels, and connecting pieces are arranged among the channels; the discharge structure is a multi-stage corona needle discharge structure.
2. The joint detection apparatus of claim 1, wherein a quaternary gradient pump is disposed inside the liquid chromatograph.
3. The joint detection device according to claim 2, wherein the first heater comprises a first heating layer having a tubular shape, a second heating layer, and a third heating layer having a cylindrical shape, and the first heating layer, the second heating layer, and the third heating layer are fixedly connected to each other by the cylindrical connecting member.
4. The joint detection apparatus of claim 3, wherein the first heating layer, the second heating layer, the third heating layer, and the cylindrical connecting member are provided with ceramic layers on outer sides thereof.
5. The joint detection device according to claim 4, wherein the multi-stage corona needle discharge structure is a two-stage corona needle discharge structure, and specifically comprises: the corona discharge device comprises a first fusiform ionization chamber and a second fusiform ionization chamber which are sequentially connected, wherein a first corona needle is arranged in the middle of the first fusiform ionization chamber, and a second corona needle is arranged in the middle of the second fusiform ionization chamber.
6. The joint detection apparatus as claimed in claim 5, wherein a second heater is provided between the first and second shuttle-shaped ionization chambers.
7. The combination detection device according to claim 5, wherein the first corona needle and the second corona needle are provided in a plurality of numbers, and are respectively and annularly arranged in the middle of the first fusiform electric discharging bin and the second fusiform electric discharging bin.
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| CN114965831A (en) * | 2022-05-19 | 2022-08-30 | 厦门大学 | Zero dead volume interface device for combination of chromatograph and mass spectrum and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114965831A (en) * | 2022-05-19 | 2022-08-30 | 厦门大学 | Zero dead volume interface device for combination of chromatograph and mass spectrum and application thereof |
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