CN117589758A - Colorimetric mercury detection method based on solid direct sample injection - Google Patents
Colorimetric mercury detection method based on solid direct sample injection Download PDFInfo
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 title claims abstract description 61
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- 239000007787 solid Substances 0.000 title claims abstract description 44
- 238000001514 detection method Methods 0.000 title claims abstract description 38
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- 239000007924 injection Substances 0.000 title claims abstract description 29
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000000243 solution Substances 0.000 claims abstract description 35
- 238000002835 absorbance Methods 0.000 claims abstract description 14
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- 239000010931 gold Substances 0.000 claims description 7
- 229910052737 gold Inorganic materials 0.000 claims description 7
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- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 4
- 229940038773 trisodium citrate Drugs 0.000 claims description 4
- XYYVDQWGDNRQDA-UHFFFAOYSA-K trichlorogold;trihydrate;hydrochloride Chemical compound O.O.O.Cl.Cl[Au](Cl)Cl XYYVDQWGDNRQDA-UHFFFAOYSA-K 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 2
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- 238000004458 analytical method Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
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- 102000016938 Catalase Human genes 0.000 description 1
- 108010053835 Catalase Proteins 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229910004042 HAuCl4 Inorganic materials 0.000 description 1
- 241000282412 Homo Species 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
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- 238000001277 hydride generation atomic absorption spectroscopy Methods 0.000 description 1
- 238000001676 hydride generation atomic fluorescence spectroscopy Methods 0.000 description 1
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- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
Abstract
The invention discloses a colorimetric mercury detection method based on solid direct sample injection, which comprises the steps of steaming out and transmitting combined mercury in a solid sample in an atomic state form through a solid direct sample injection device, and capturing and adsorbing Hg atoms transmitted by adopting PVP-AuNPs quartz films; TMB and H are carried out on PVP-AuNPs quartz film with Hg atoms captured and adsorbed 2 O 2 To generate blue solution to be measured; and (3) quantitatively detecting mercury by observing the absorbance of the solution to be detected. The invention evaporates and transmits the combined mercury in the solid sample in an atomic state form through the solid direct sample injection device, then captures and adsorbs the evaporated Hg atoms by adopting the PVP-AuNPs quartz film, further enhances the peroxidase characteristic of AuNPs, and further obtains the solid mercury through TMB and H 2 O 2 To produce a solution to be tested, finally through observationAnd (5) quantitatively detecting mercury by observing the absorbance of the solution to be detected.
Description
Technical Field
The invention relates to the technical field of detection of heavy metal mercury, in particular to a colorimetric mercury detection method based on solid direct sample injection.
Background
Mercury (Hg) is one of the most toxic heavy metals, and has attracted much attention in all countries of the world because of its high concentration accumulation, biotoxicity, long distance migration, and the like, which creates serious harm to ecosystems and humans. It is well known that outbreaks of Japanese water disease event pay attention to human mercury pollution, and Hg emission has irreversible effect on global ecological environment and has serious harm to soil, water and various organisms. According to the World Health Organization (WHO) regulations, mercury is considered to be one of the ten most toxic chemicals, and various related policies have been put out internationally to standardize the limit of mercury. In addition, mercury causes serious damage to organs such as the central nervous system and kidneys of the human body through food chains. The current common mercury detection methods include hydride generation Atomic Absorption Spectrometry (AAS), hydride generation Atomic Fluorescence Spectrometry (AFS), inductively coupled plasma mass spectrometry (ICP-MS) and the like, and the methods have high sensitivity and good accuracy. However, these conventional methods can only be used in a laboratory, and all the methods are performed by liquid matrix injection, so that strong acid or alkali is required to digest the sample, which is time-consuming and complicated, causes environmental pollution, and cannot meet the requirement of on-site rapid detection.
As one of the main direct solid sample injection means, the electrothermal evaporation technology can evaporate and release mercury in the solid in the form of atomic vapor under the high temperature condition, and the generated mercury vapor can be directly detected after being carried by carrier gas or after being captured. Common evaporator materials mainly comprise high-melting-point materials such as metal, quartz, carbon materials and the like, and are designed into various forms such as rods, wires, boats, tubes, sheets and the like. The sample introduction technology does not need complicated pretreatment, can greatly improve the sample detection efficiency, and reduces errors and analyte loss caused by experimental pollution. The sample injection method can be combined with different detectors to measure mercury and different forms thereof. The solid direct sample injection mercury meter based on the principle has realized commercialization, is the electric heating evaporation instrument which is most successfully applied at present, but is limited by the characteristics of high power consumption, large volume, pure oxygen and the like of the instrument, and the instrument cannot realize miniaturization and on-site rapid detection at present. In recent years, a colorimetric sensing detection means of mercury has been paid attention to because of the characteristics of simplicity, convenience, real-time and the like, wherein a gold nanomaterial is widely applied to on-site rapid detection of mercury in the aspects of environment and the like.
Compared with natural nano-enzyme, the nano-enzyme has the characteristics of good biocompatibility, controllable catalytic activity, mild reaction conditions and the like, and is widely applied to the fields of biology, food, environment, medicine and the like. Gold nanoenzymes are one of the most representative nanoenzymes, which have peroxidase activity, catalase activity, oxidase activity, and the like. But in general, the peroxidase activity is weak and Hg 2+ Can enhance its peroxidase activity. Mainly based on Hg 2+ Is reduced to Hg by sodium citrate 0 The activity of peroxidase is further improved by changing the surface property of the gold nanoparticles through the combination of Au-Hg bond and the gold nanoparticles. The most widely used AuNPs are capable of catalytic oxidation of 3,3', 5' -Tetramethylbenzidine (TMB) substrates in the presence of hydrogen peroxide to form blue oxidation products (ox-TMB) with strong uv absorbance at 370nm and 650 nm. The mercury can be quantitatively analyzed through color change, and signal amplification is realized through a chromogenic substrate, so that the detection capability is further improved. The method has good detection capability, stability and anti-interference capability, is simple to operate and short in time consumption, and can realize rapid detection of mercury. However, the method is mainly aimed at detection of liquid samples, mainly mercury in water samples is the most widely applied method, and direct detection of mercury in solid samples cannot be realized, which is also a main reason for limiting the development of the method in solid samples.
Disclosure of Invention
The invention provides a colorimetric mercury detection method based on solid direct sample injection, which is suitable for quantitative detection of mercury in solid samples such as soil, food, fertilizer, organisms and liquid samples such as surface water and wastewater.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a colorimetric mercury detection method based on solid direct sample injection comprises the following steps:
s1: evaporating and transmitting the combined mercury in the solid sample in an atomic state form through a solid direct sample injection device, and capturing and adsorbing the transmitted Hg atoms by adopting a PVP-AuNPs quartz film;
s2: TMB and H are carried out on PVP-AuNPs quartz film with Hg atoms captured and adsorbed 2 O 2 To generate blue solution to be detected, specifically, PVP-AuNPs quartz film captured with Hg atoms is put into a test tube, and TMB and H are respectively dripped into the test tube 2 O 2 Obtaining a solution to be measured after the reaction;
s3: and (3) quantitatively detecting mercury by observing the absorbance of the solution to be detected, and specifically, measuring the ultraviolet absorbance of the solution to be detected obtained in the step (S2) at 370nm or 650 nm.
The PVP-AuNPs quartz film is prepared through the following steps:
s1.1: preparing AuNPs by reducing chloroauric acid trihydrate by trisodium citrate, and synthesizing PVP-AuNPs by adopting 1mg/mL polyvinylpyrrolidone coated gold nanoparticles;
s1.2: and (3) dropwise adding the synthesized PVP-AuNPs onto the surface of the quartz film, and drying to form a PVP-AuNPs layer so as to obtain the PVP-AuNPs quartz film.
In some embodiments, the operation of S1.2 is repeated to form PVP-AuNPs layers of different thicknesses on the quartz film surface.
In some examples, 80. Mu.L of each drop was applied to a quartz film surface of 6mm diameter and dried at 40℃for 1 hour to form a PVP-AuNPs layer.
The solid direct sampling device comprises an electrothermal evaporation component, a catalytic pyrolysis component and a capturing component constructed by PVP-AuNPs quartz film;
specifically, the electrothermal evaporation component comprises a metal ceramic cup, a metal heating wire is arranged in the cup wall of the metal ceramic cup, two ends of the metal heating wire are respectively led out from the bottom of the metal ceramic cup and welded with a power supply pin, the bottom of the metal ceramic cup is fixed on a rubber base, and the power supply pin penetrates through the rubber base and is connected with a power supply device;
the catalytic pyrolysis component comprises a catalytic pyrolysis tube arranged on a rubber base, a metal ceramic cup is arranged in the catalytic pyrolysis tube, a heating coil with adjustable temperature is arranged outside the catalytic pyrolysis tube and above the metal ceramic cup, a carrier gas connecting tube is arranged on one side of the bottom of the catalytic pyrolysis tube, an assembly port is arranged at the top end of the catalytic pyrolysis tube and used for assembling a capturing component, a capturing device for capturing mercury is constructed by utilizing PVP-AuNPs quartz films, the capturing effect is improved, and the visual detection of mercury can be realized by carrying out a color development experiment on PVP-AuNPs quartz films capturing Hg atoms.
The capturing component comprises a quartz reducer pipe for assembling the PVP-AuNPs quartz film, wherein the PVP-AuNPs quartz film is detachably arranged in the quartz reducer pipe, and the quartz reducer pipe is detachably connected with the assembling port.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, mercury in a solid sample is evaporated in an atomic state through a capturing device, and then the PVP-AuNPs quartz film is used for capturing and adsorbing the evaporated Hg atoms, so that the peroxidase characteristic of AuNPs is enhanced, and TMB and H are further catalyzed 2 O 2 And (3) generating a solution to be detected, and finally realizing semi-quantitative and quantitative detection of mercury by observing the color change of the solution to be detected or measuring the absorbance of specific wavelength.
2. The whole analysis system converts mercury in a solid sample into three states of combination state-gas state-amalgam for the first time, realizes high-sensitivity visual detection on nano enzyme, and provides a new research thought for on-site rapid sensing detection of heavy metal mercury.
Drawings
FIG. 1 is a schematic cross-sectional view of a solid direct injection device;
FIG. 2 is the adsorption capacity of quartz membranes containing different amounts of PVP-AuNPs for mercury at the same concentration;
FIG. 3 shows the quartz membrane containing 80. Mu.LPVP-AuNPs against different concentrations of Hg 0 Is used for the adsorption capacity of the catalyst;
FIG. 4 is a schematic diagram of a linear equation fitted to a standard solution of mercury, wherein the abscissa represents the concentration of Hg and the ordinate represents the absorbance of the solution at 370nm after development.
The attached drawings are identified: 1. the electric heating evaporation component 11, the ceramic cup 12, the metal heating wire 13, the power supply pin 2, the catalytic pyrolysis component 21, the catalytic pyrolysis tube 22, the heating coil 23, the carrier gas connecting tube 3, the capturing component 31, the PVP-AuNPs quartz film 32, the quartz reducer 4, the rubber base 5, the power supply equipment 6 and the connecting tube.
Detailed Description
For the purpose of making apparent the objects, technical solutions and advantages of the present invention, the present invention will be further described in detail with reference to the following examples and the accompanying drawings, wherein the exemplary embodiments of the present invention and the descriptions thereof are for illustrating the present invention only and are not to be construed as limiting the present invention.
Example 1
A colorimetric mercury detection method based on solid direct sample injection comprises the following steps:
s1: evaporating and transmitting the combined mercury in the solid sample in an atomic state form through a solid direct sample injection device, and capturing and adsorbing the transmitted Hg atoms by adopting a PVP-AuNPs paper-based film 31;
s2: TMB and H were performed on PVP-AuNPs quartz film 31 having Hg atoms trapped and adsorbed thereon 2 O 2 To generate blue solution to be detected, specifically, PVP-AuNPs Dan Yingmo 31 captured with Hg atoms is placed in a test tube, and TMB and H are respectively dripped into the test tube 2 O 2 Obtaining a solution to be measured after the reaction;
s3: and (3) quantitatively detecting mercury by observing the absorbance of the solution to be detected, and specifically, measuring the ultraviolet absorbance of the solution to be detected obtained in the step (S2) at 370nm or 650 nm.
The PVP-AuNPs quartz film 31 described above was prepared by the following steps:
s1.1: preparing AuNPs by reducing chloroauric acid trihydrate by adopting trisodium citrate, specifically, adding 2mL of 50mM HAuCl4 solution into 8mL of water, heating and stirring to boil, wherein the solution is light yellow; then 10mL of 1% trisodium citrate solution is added, the solution is boiled for 20min, at the moment, the solution turns from yellow to deep purple and then turns into wine red, the solution is cooled to room temperature, and the solution is preserved at 4 ℃ for standby;
s1.2: based on AuNPs, 1mg/mL polyvinylpyrrolidone PVP is used for coating gold nanoparticles to synthesize PVP-AuNPs, specifically, 5mLAuNPs are taken to be added into 45mL deionized water, 5mL1mg/mL PVP solution is added, stirring is carried out for 24 hours, and the mixture is kept for standby at 4 ℃ after centrifugation. S1.3: the synthesized PVP-AuNPs are dripped on the surface of a quartz film and dried to form PVP-AuNPs layers to obtain a PVP-AuNPs paper-based film 31 loaded with PVP, preferably, the operation of S1.2 is repeated, so that PVP-AuNPs layers with different thicknesses are formed on the surface of the quartz film, specifically, 80 mu L of PVP-AuNPs layers are dripped on the surface of the quartz film with the diameter of 6mm each time, and the quartz film is dried for 1h at 40 ℃ to form PVP-AuNPs layers.
The solid direct sample injection device shown in fig. 1 comprises an electrothermal evaporation component 1 and a catalytic pyrolysis component 2, and further comprises a capturing component 3 constructed by a PVP-AuNPs quartz film 31, wherein the electrothermal evaporation component 1 is used for evaporating Hg in a solid sample in an atomic form, and the catalytic pyrolysis component 2 is used for transferring fifteen atomic Hg evaporated to the capturing component 3 for capturing by the PVP-AuNPs quartz film 31.
Specifically, the electrothermal evaporation component 1 comprises a metal ceramic cup 11, a metal heating wire 12 is arranged in the cup wall of the metal ceramic cup 11, two ends of the metal heating wire 12 are respectively led out from the bottom of the metal ceramic cup 11 and welded with a power supply pin 13, the bottom of the metal ceramic cup 11 is fixed on a rubber base 4, and the power supply pin 13 penetrates through the rubber base 4 and is connected with a power supply device 5;
the catalytic pyrolysis component 2 comprises a catalytic pyrolysis tube 21 arranged on a rubber base 4, a metal ceramic cup 11 is arranged in the catalytic pyrolysis tube 21, a heating coil 22 with adjustable temperature is arranged outside the catalytic pyrolysis tube 21 and above the metal ceramic cup 11, a carrier gas connecting tube 23 is arranged on one side of the bottom of the catalytic pyrolysis tube 21, and an assembly port is formed in the top end of the carrier gas connecting tube and used for assembling the capturing component 3.
The capturing component 3 comprises a quartz reducer pipe 32 for assembling the PVP-AuNPs quartz film 31, the PVP-AuNPs quartz film 31 is detachably arranged in the quartz reducer pipe 32, the quartz reducer pipe 32 is detachably connected with the assembling port, preferably, the quartz reducer pipe 32 is detachably connected with the assembling port through a connecting pipe 6, and the position of the quartz reducer pipe 32 can be changed.
The catalytic pyrolysis tube 21 is filled with a catalyst layer at a position corresponding to the heating coil 22, and the catalyst layer is provided for removing organic interfering substances after mercury in the solid sample is evaporated in an atomic state, and specifically, the catalyst layer includes CaO and a manganese catalyst.
Example 2
The PVP-AuNPs quartz film 31 is against Hg 0 The capture effect of (2) was verified as follows:
1. exploration of different content of PVP-AuNPs quartz film vs Hg 0 Capture capability of (c):
specifically, the capturing ability of the quartz membrane 31 of PVP-AuNPs of different volumes was examined using 500. Mu.g/L Hg standard solution (20. Mu.L), and the results of the experiment are shown in FIG. 2, which shows that the capturing efficiency is maximum when the PVP-AuNPs content is 80. Mu.L, and the capturing efficiency remains stable as the PVP-AuNPs content on the membrane increases.
2. The capture capacity of 80 μl PVP-AuNPs quartz membrane 31 for mercury at different concentrations was investigated:
specifically, by examining the capturing capacity of 50-500. Mu.g/L Hg standard solution, the examination results are shown in FIG. 3, and the results show that the maximum capturing amount of the membrane can reach 12.5ng.
3. The color development ability of PVP-AuNPs quartz film 31 after capturing Hg was investigated:
specifically, the color development was performed with the PVP-AuNPs quartz film 31 after capturing Hg, and the color development result thereof was analyzed, wherein the color development steps were as follows:
3.1, removing the PVP-AuNPs quartz membrane 31 with the Hg trapped therein from the quartz reducing tube 32;
3.2, the detached PVP-AuNPs Dan Yingmo was placed in a test tube and 100. Mu.L 0.4mg/mLTMB and 3%H were added dropwise to the tube 2 O 2 Then reacting at 55 ℃ for 25min to obtain a reacted solution;
3.3, measuring the ultraviolet absorbance of the obtained solution at 370 nm.
As shown in FIG. 4, the color development results showed good linearity in the range of 50 to 500. Mu.g/LHg.
Example 3
The colorimetric mercury detection method is verified by measuring an actual rice sample:
weighing 0.05g of the treated rice sample in an electric heating evaporator 11, inserting the electric heating evaporator 11 into a catalytic pyrolysis tube 21, arranging a capturing component 3 on the catalytic pyrolysis tube 21, injecting air into the catalytic pyrolysis tube 21 by using a carrier gas connecting tube 23, then supplying power to the electric heating evaporation component 1 and the catalytic pyrolysis component 2 to dry, ash, pyrolyze and evaporate the rice sample, wherein a PVP-AuNPs quartz film 31 captures evaporated Hg atoms, then taking off the PVP-AuNPs quartz film 31 after capturing Hg atoms, and placing the PVP-AuNPs quartz film 31 into a test tube, and respectively adding 100 mu L of 0.4mg/mL TMB and 3% H 2 O 2 Incubation was carried out at 55deg.C for 25min, then the absorbance of the reacted solution was measured at 370nm, and then mercury was quantitatively measured, and the experimental results are shown in Table 1:
TABLE 1
The detection limit of the method can reach 15 mug/L, the relative standard deviation of repeated measurement is less than 15%, the labeled recovery rate of the sample is 116%, and the method has good consistency in the measurement result of the standard method.
In summary, the colorimetric mercury detection method based on solid direct sample injection disclosed by the invention has a good capturing effect on Hg, the solid direct sample injection device constructed based on the supported PVP-AuNPs paper-based film 31 is used for evaporating and transmitting mercury in a solid sample in an atomic state by adopting an electrothermal evaporation means, and then the PVP-AuNPs quartz film 31 is used for capturing Hg atoms absorbed and transmitted, so that the HPR characteristic of AuNPs is enhanced, and TMB and H are further catalyzed 2 O 2 And (3) generating a solution to be detected, and finally realizing semi-quantitative and quantitative detection of mercury by observing the color change of the solution to be detected or measuring the absorbance of specific wavelength. The whole analysis system converts mercury in a solid sample into three states of combination state-gaseous state-amalgam for the first time, realizes high-sensitivity visual detection on nano enzyme, and is heavy metalThe on-site rapid sensing detection of mercury provides a new research idea.
There are, of course, many other embodiments of the invention that can be made by those skilled in the art in light of the above teachings without departing from the spirit or essential scope thereof, but that such modifications and variations are to be considered within the scope of the appended claims.
Claims (8)
1. The colorimetric mercury detection method based on solid direct sample injection is characterized by comprising the following steps of:
s1: evaporating and transmitting the combined mercury in the solid sample in an atomic state form through a solid direct sample injection device, and capturing and adsorbing the transmitted Hg atoms by adopting a PVP-AuNPs quartz film (31);
s2: TMB and H were performed on PVP-AuNPs quartz film (31) having Hg atoms trapped and adsorbed thereon 2 O 2 To generate blue solution to be measured;
s3: and (3) quantitatively detecting mercury by observing the absorbance of the solution to be detected.
2. The colorimetric mercury detection method based on direct solid sample injection according to claim 1, characterized in that the PVP-AuNPs quartz film (31) in S1 is prepared by the following steps:
s1.1: preparing AuNPs by reducing chloroauric acid trihydrate by trisodium citrate, and synthesizing PVP-AuNPs by coating gold nanoparticles with 1mg/mL polyvinylpyrrolidone (PVP);
s1.2: and (3) dropwise adding the synthesized PVP-AuNPs onto the surface of the quartz film, and drying to form a PVP-AuNPs layer so as to obtain the PVP-AuNPs quartz film.
3. The colorimetric mercury detection method based on direct solid sample injection according to claim 2, wherein the operation of S1.2 is repeated to form PVP-AuNPs layers with different thicknesses on the surface of the quartz film.
4. The colorimetric mercury detection method based on direct solid sample injection according to claim 3, wherein 80 μl of the solution is added dropwise to a quartz film surface with a diameter of 6mm, and the solution is dried at 40deg.C for 1h to form PVP-AuNPs layer.
5. The colorimetric mercury detection method based on direct solid sample injection according to claim 1, characterized in that in S2, PVP-AuNPs quartz film (31) with Hg atoms captured is placed in a test tube, and TMB and H are respectively added dropwise into the test tube 2 O 2 And obtaining the solution to be measured after the reaction.
6. The colorimetric mercury detection method based on direct solid sample injection according to claim 1, wherein the ultraviolet absorbance of the obtained solution to be detected is measured at 370nm or 650nm in S3.
7. The colorimetric mercury detection method based on direct solid sample injection according to claim 1, characterized in that the direct solid sample injection device comprises an electrothermal evaporation component (1) and a catalytic pyrolysis component (2), and further comprises a capturing component (3) constructed by a PVP-AuNPs quartz film (31);
the electrothermal evaporation component (1) comprises a metal ceramic cup (11), a metal heating wire (12) is arranged in the cup wall of the metal ceramic cup (11), two ends of the metal heating wire (12) are respectively led out from the bottom of the metal ceramic cup (11) and welded with a power supply pin (13), the bottom of the metal ceramic cup (11) is fixed on a rubber base (4), and the power supply pin (13) penetrates through the rubber base (4) to be connected with a power supply device (5);
the catalytic pyrolysis component (2) comprises a catalytic pyrolysis tube (21) arranged on a rubber base (4), a metal ceramic cup (11) is arranged in the catalytic pyrolysis tube (21), a heating coil (22) with adjustable temperature is arranged outside the catalytic pyrolysis tube (21) and above the metal ceramic cup (11), a carrier gas connecting tube (23) is arranged on one side of the bottom of the catalytic pyrolysis tube (21), and an assembly port is formed in the top end of the catalytic pyrolysis tube and used for assembling the capturing component (3).
8. The colorimetric mercury detection method based on direct solid sample injection according to claim 7, characterized in that the capturing component (3) comprises a quartz reducer pipe (32) for assembling the modified quartz membrane (31), the modified quartz membrane (31) is detachably arranged in the quartz reducer pipe (32), and the quartz reducer pipe (32) is detachably connected with an assembling port.
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