CN206876566U - A kind of water body bivalent nickel ion device for fast detecting - Google Patents

A kind of water body bivalent nickel ion device for fast detecting Download PDF

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CN206876566U
CN206876566U CN201720732136.0U CN201720732136U CN206876566U CN 206876566 U CN206876566 U CN 206876566U CN 201720732136 U CN201720732136 U CN 201720732136U CN 206876566 U CN206876566 U CN 206876566U
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nickel ion
reagent
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water
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欧阳永中
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Foshan University
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Foshan University
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Abstract

The utility model discloses a kind of water body bivalent nickel ion device for fast detecting, the earth's surface water gaging water sample in water sample case is handled by the first reagent in nickel ion kit, the second reagent and the 3rd reagent to obtain colour developing sample, and the absorbance by spectrophotometer measurement colour developing sample under maximum absorption wavelength, and the concentration of bivalent nickel ion is obtained by nickel ion concentration measurement apparatus.With it is simple to operate, analyze speed is fast, the degree of accuracy is high, low cost and other advantages; the demand in market and the convenience and accuracy of heavy metal nickel ion detection are catered to well; solves the live discomfort of great instrument in water environment pollution detection and analysis, by the detection on the spot of heavy metal pollution in water and long-term monitoring, the protection of water resource and field of comprehensive utilization have great significance and potential application prospect.

Description

A kind of water body bivalent nickel ion device for fast detecting
Technical field
Water pollution detection field is the utility model is related to, particularly a kind of water body bivalent nickel ion device for fast detecting.
Background technology
Compared with other transition metals, nickel is a kind of moderately toxic element, it is well known that in certain concentration In the range of, the compound such as nickel sulphur compound of nickel and nickel has severe toxicity, and nickel concentration is higher than 0.1 μ g/mL natural water pair Aquatile and by irrigate plant be harmful.In addition, nickel can produce toxic effects to tissue, and human body is caused Harm.Nickel is widely distributed in the earth's crust, has the performances such as good anticorrosion, high temperature resistant, this causes the compound of nickel and nickel to exist It is widely used in the fields such as plating, battery production, mining, intermetallic composite coating and forging, annual substantial amounts of nickeliferous industrial wastewater Discharge causes serious pollution to environment, causes nickel concentration in environment water higher, if from Sources controlling and controlled not in time Reason, it will cause to seriously endanger to environment and human body, therefore, in surface water pollution heavy metal nickel ion it is quick, accurate, The exploitation of real-time detection method and technology is very necessary.
The conventional analysis detection method of domestic and international water quality heavy metal mainly includes:AAS, atomic absorption spectrography (AAS) (AAS), atomic fluorescence spectrometry (AFS), x ray fluorescence spectrometry, inductively coupled plasma emission spectrography (ICP- AES), stripping voltammetry, mass spectrography (MS) etc..However, these methods are generally deposited in the detection and analysis on the spot of water environment pollution In the live discomfort of great instrument, it is impossible to meet the needs that scene is detected real-time.
Utility model content
To solve the above problems, the purpose of this utility model is to provide, simple to operate, analyze speed is fast, the degree of accuracy is high, A kind of water body bivalent nickel ion device for fast detecting that cost is low, the scene of completing is detected in real time.
Technical scheme is used by the invention for solving the technical problem:
A kind of water body bivalent nickel ion device for fast detecting, including:
Nickel ion kit, the reagent for being handled sample is stored, including,
First reagent storing device, for storing Ni in water sample2+It is oxidized to Ni4+The first reagent ammonium persulfate solution,
Second reagent storing device, for storage and Ni4+The the second reagent dimethylglyoxime and screening agent of reaction generation complex compound Mixed solution,
3rd reagent storing device, for being stored as Ni2+Oxidation provide alkaline environment the 3rd reagent sodium hydroxide solution;
Water sample case, for depositing water sample to be measured and as water sample to be measured and the chemical reaction field of nickel ion kit Institute;
Extraction element, for obtaining the first reagent, the second reagent and the 3rd reagent from nickel ion kit and adding successively Enter into water sample case, obtain the sample that develops the color;
Spectrophotometer, absorbance of the measurement colour developing sample under maximum absorption wavelength;
Nickel ion concentration measurement apparatus, the absorbance according to measured by spectrophotometer calculate the concentration of bivalent nickel ion.
Further, water sample case water sample storage volume to be measured is 3mL;First reagent storing device deposits 5mL Mass percentage concentration is 3% ammonium persulfate solution;The second reagent storing device storage is that 3mL mass percentage concentrations are 1% Dimethylglyoxime solution and 15mL masking agent solution mixed solution;3rd reagent storing device deposits 4mL mass percentages Concentration is 5% sodium hydroxide solution.
Further, the masking agent solution is the EWNN solution that mass percentage concentration is 20%.
Further, the nickel ion concentration measurement apparatus includes,
Tetravalence nickel ion concentration measurement apparatus, pass through sample absorbance and the tetravalence nickel ion concentration-absorbance standard of developing the color Equation A=0.2303x+0.0071, the tetravalence nickel ion concentration of colour developing sample being calculated, wherein A is the absorbance of solution to be measured, X is the tetravalence nickel ion concentration value of solution to be measured;
The apparatus for measuring concentration of bivalent nickel ion, above-mentioned tetravalence nickel ion concentration value is scaled bivalent nickel ion concentration Value.
Further, in addition to,
Device is shaken up, is arranged at water sample case, is shaken up for being sufficiently stirred after the second reagent of addition and the 3rd reagent;
Timer, for the developing time after prompting stirring to shake up.
Specifically, the maximum absorbing wavelength that the spectrophotometer is set is 470nm.
Specifically, the spectrophotometric is calculated as V-1100D spectrophotometers.
The beneficial effects of the utility model are:A kind of water body bivalent nickel ion quick detection dress that the utility model uses Put, by the first reagent in nickel ion kit, the second reagent and the 3rd reagent to the earth's surface water gaging in water sample case Water sample is handled to obtain colour developing sample, and the extinction by spectrophotometer measurement colour developing sample under maximum absorption wavelength Degree, and the concentration of bivalent nickel ion is obtained by nickel ion concentration measurement apparatus.Required detection device small volume and phase To cheap so that the detection method is applied to Site Detection, has simple to operate, analyze speed is fast, the degree of accuracy is high, cost is low etc. Advantage, the demand in market and the convenience and accuracy of heavy metal nickel ion detection have been catered to well, solve water environment dirt The live discomfort of great instrument in dye detection and analysis, the detection on the spot of heavy metal pollution in water and long-term monitoring, water are provided The protection in source and field of comprehensive utilization have great significance and potential application prospect.
Brief description of the drawings
The utility model is described in further detail with example below in conjunction with the accompanying drawings.
Fig. 1 is the schematic diagram of the utility model water body bivalent nickel ion device for fast detecting;
Fig. 2 is Ni4+Concentration-absorbance standard curve figure.
Embodiment
Shown in reference picture 1, a kind of water body bivalent nickel ion device for fast detecting of the present utility model, including nickel ion reagent Box 1, the reagent for being handled sample is stored, including, nickel ion kit 1, store for being handled sample Reagent, including:
First reagent storing device 11, for storing Ni in water sample2+It is oxidized to Ni4+The first reagent ammonium persulfate solution,
Second reagent storing device 12, for storage and Ni4+Second reagent dimethylglyoxime of reaction generation complex compound and masking Agent mixed solution,
3rd reagent storing device 13, for being stored as Ni2+Oxidation provide alkaline environment the 3rd reagent sodium hydroxide it is molten Liquid;
Water sample case 2, for depositing water sample to be measured and as water sample to be measured and the chemical reaction of nickel ion kit 1 Place;
Extraction element 3, for obtaining the first reagent, the second reagent and the 3rd reagent and successively from nickel ion kit 1 Add into water sample case 2, obtain the sample that develops the color;
Spectrophotometer 4, absorbance of the measurement colour developing sample under maximum absorption wavelength;
Nickel ion concentration measurement apparatus 5, the absorbance according to measured by spectrophotometer 4 calculate the dense of bivalent nickel ion Degree.
A kind of water body bivalent nickel ion device for fast detecting that the utility model uses, by nickel ion kit 1 First reagent, the second reagent and the 3rd reagent are handled the earth's surface water gaging water sample in water sample case 2 to obtain colour developing sample This, and absorbance of the colour developing sample under maximum absorption wavelength is measured by spectrophotometer 4, and measured by nickel ion concentration Device 5 obtains the concentration of bivalent nickel ion.Required detection device small volume and relatively cheap so that the detection method is fitted For Site Detection, have that simple to operate, analyze speed is fast, the degree of accuracy is high, low cost and other advantages, catered to market well The convenience and accuracy of demand and heavy metal nickel ion detection, solve great instrument in water environment pollution detection and analysis and show Discomfort, by water detection and long-term monitoring, the protection of water resource and the field of comprehensive utilization on the spot of heavy metal pollution have Important meaning and potential application prospect.
The measuring principle of wherein described spectrophotometer 4 is built upon the analysis method on the basis of molecular absorption spectrum, Follow Lambert-Beer's law A=ε × b × c (wherein, A:Absorbance;ε:Absorptivity;b:Cuvette thickness;c:Determinand is dense Degree), i.e., the absorbance at absworption peak peak wavelength and between the concentration of measured matter it is linear.Therefore, the utility model By the measure to the sample that develops the color, the calibration curve equation met between sample and absorbance that develops the color is obtained, passes through spectrophotometric Meter 4 measures its absorbance, then the absorbance generation that nickel ion concentration measurement apparatus 5 will measure under the maximum absorption wavelength of determinand Enter in testing concentration-absorbance standard curve equation, the specific concentration of the determinand is calculated, light is divided in the present embodiment The maximum absorbing wavelength that degree meter 4 is set is 470nm.
In the utility model nickel ion kit 1, the first reagent storing device 11 storage ammonium persulfate (NH4)2S2O8Solution is made For the first reagent, the mixed solution of the second reagent storing device 12 storage dimethylglyoxime solution and EWNN solution is as the second examination Agent, the 3rd reagent storing device 13 store sodium hydroxide NaOH solution and extract the first reagent as the 3rd reagent, extraction element 3 and add Into the water sample of water sample case 2, (the NH in the first reagent4)2S2O8For solution as oxidant, it can be by the Ni in water sample2+Oxygen It is melted into tetravalence nickel ion Ni4+(Ni2++S2O8 2-=2SO4 2-+Ni4+), the developer dimethylglyoxime of the second reagent can be with positive tetravalence Ni4+Reaction solution, claret complex compound is generated, for follow-up spectrophotometric analysis, extraction element 3 will be by the second reagent and the Three reagents are sequentially added into claret complex compound, and the sodium tartrate in the second reagent is as screening agent, because of adding for the second reagent Enter before the 3rd reagent, therefore the NaOH that can be better protected from the 3rd reagent is with the reaction of other metal ions and to experimental result Impact.3rd reagent is NaOH solution, and it can be (NH4)2S2O8To Ni2+Oxidation provide alkaline environment, make oxidation reaction Carry out more abundant.
Specifically, V-1100D spectrophotometers are used in the present embodiment.
Preferred embodiment is further used as, 2 water sample to be measured of the water sample case storage volume is 3mL;Described The ammonium persulfate solution that one reagent storing device 11 storage 5mL mass percentage concentrations are 3%;Second reagent storing device 12 is deposited The mixed solution of the dimethylglyoxime solution for being 1% for 3mL mass percentage concentrations and 15mL masking agent solution;3rd reagent Memory 13 deposits the sodium hydroxide solution that 4mL mass percentage concentrations are 5%.
Preferred embodiment is further used as, in addition to shakes up device and timer, is arranged at water sample case 2, mesh Be to be sufficiently stirred to shake up after the second reagent and the 3rd reagent is added;When timer is used to prompt to stir the colour developing after shaking up Between, the developing time of prompting 20 minutes.
Preferred embodiment is further used as, the masking agent solution is the sodium tartrate that mass percentage concentration is 20% Solution.
Shown in reference picture 1, the nickel ion concentration measurement apparatus 5 includes tetravalence nickel ion concentration measurement apparatus 515 and two The apparatus for measuring concentration 52 of valency nickel ion, wherein described tetravalence nickel ion concentration measurement apparatus 515 is surveyed spectrophotometer 4 The absorbance obtained is substituted into tetravalence nickel ion concentration-absorbance standard equation A=0.2303x+0.0071 of setting, is calculated to be measured The tetravalence nickel ion concentration of solution, wherein, A is the absorbance of solution to be measured, and x is the tetravalence nickel ion concentration of solution to be measured.And Above-mentioned tetravalence nickel ion concentration value is then scaled bivalent nickel ion concentration value by the apparatus for measuring concentration 52 of bivalent nickel ion.
Shown in reference picture 2, Ni can be seen that by the experimental result of standard sample4+Concentration range is in 0-5mg/L, Ni4+ Meet linear equation A=0.2303x+0.0071 between concentration and absorbance, linearly dependent coefficient 0.9998, meet Bill and determine Rule.
Preferred embodiment is further used as, measuring process of the present utility model is as follows:
1st, by 5mL concentration be 3% (NH4)2S2O8Solution, in the first reagent storing device 11, is somebody's turn to do as the first reagent storage Solution, can be by Ni in water sample as oxidant2+It is oxidized to Ni4+, for subsequent reactions;
2nd, the dimethylglyoxime solution that 3mL concentration is 1% and the EWNN solution that 15mL concentration is 20% are mixed, as Second reagent storage is in the second reagent storing device 12, dimethylglyoxime solution energy and Ni4+The complex compound of reaction generation claret, is used for Spectrophotometer 4 is analyzed, and sodium tartrate can prevent the NaOH in the 3rd reagent from being reacted with other metal ions as screening agent, shadow Ring experimental result;
3rd, using 4mL concentration be 5% NaOH solution as the 3rd reagent storage in the 3rd reagent storing device 13, NaOH solution For Ni2+Oxidation provide alkaline environment so that (NH4)2S2O8Solution is by Ni2+It is oxidized to Ni4Reaction it is more abundant;
4th, using above-mentioned first reagent, the second reagent and the 3rd reagent as nickel ion kit 1, for detecting earth's surface water sample The concentration of middle heavy metal nickel ion;
5th, the first reagent in nickel ion kit 1 is first added in 3mL water samples of the extraction element 3 in water sample case 2, The second reagent and the 3rd reagent are sequentially added after question response is complete, is sufficiently stirred and shakes up, and it is developed the color 20 minutes;
6th, by obtaining colour developing sample in V-1100D spectrophotometers 4, it is measured under maximum absorption wavelength (470nm) Absorbance;
7th, the absorbance of acquisition is substituted into Ni by nickel ion concentration measurement apparatus 54+Concentration-absorbance standard curve equation A In=0.2303x+0.0071, corresponding Ni is calculated4+Concentration, finally convert thereof into Ni2+Concentration, reach in sample The purpose of the quick detection of heavy metal bivalent nickel ion.
Described above, simply preferred embodiment of the present utility model, the utility model is not limited to above-mentioned implementation Mode, as long as it reaches technique effect of the present utility model with identical means, it should all belong to the scope of protection of the utility model.

Claims (6)

  1. A kind of 1. water body bivalent nickel ion device for fast detecting, it is characterised in that including:
    Nickel ion kit, the reagent for being handled sample is stored, including,
    First reagent storing device, for storing Ni in water sample2+It is oxidized to Ni4+The first reagent ammonium persulfate solution,
    Second reagent storing device, for storage and Ni4+Second reagent dimethylglyoxime of reaction generation complex compound and screening agent mixing Solution,
    3rd reagent storing device, for being stored as Ni2+Oxidation provide alkaline environment the 3rd reagent sodium hydroxide solution;
    Water sample case, for depositing water sample to be measured and as the chemical reaction place of water sample to be measured and nickel ion kit;
    Extraction element, for obtained from nickel ion kit the first reagent, the second reagent and the 3rd reagent and sequentially add to In water sample case, the sample that develops the color is obtained;
    Spectrophotometer, absorbance of the measurement colour developing sample under maximum absorption wavelength;
    Nickel ion concentration measurement apparatus, the absorbance according to measured by spectrophotometer calculate the concentration of bivalent nickel ion.
  2. A kind of 2. water body bivalent nickel ion device for fast detecting according to claim 1, it is characterised in that:The water sample is deposited It is 3mL to put box water sample storage volume to be measured;The persulfuric acid that the first reagent storing device storage 5mL mass percentage concentrations are 3% Ammonium salt solution;The second reagent storing device storage is the masking of dimethylglyoxime solution and 15mL that 3mL mass percentage concentrations are 1% The mixed solution of agent solution;The sodium hydroxide solution that the 3rd reagent storing device storage 4mL mass percentage concentrations are 5%.
  3. A kind of 3. water body bivalent nickel ion device for fast detecting according to claim 2, it is characterised in that:The screening agent Solution is the EWNN solution that mass percentage concentration is 20%.
  4. 4. according to a kind of any described water body bivalent nickel ion device for fast detecting of claim 1-3, it is characterised in that:It is described Nickel ion concentration measurement apparatus includes,
    Tetravalence nickel ion concentration measurement apparatus, pass through sample absorbance and the tetravalence nickel ion concentration-absorbance standard equation A of developing the color =0.2303x+0.0071, the tetravalence nickel ion concentration of colour developing sample is calculated, wherein A is the absorbance of solution to be measured, and x is to treat Survey the tetravalence nickel ion concentration value of solution;
    The apparatus for measuring concentration of bivalent nickel ion, above-mentioned tetravalence nickel ion concentration value is scaled bivalent nickel ion concentration value.
  5. 5. according to a kind of any described water body bivalent nickel ion device for fast detecting of claim 1-3, it is characterised in that:It is described The maximum absorbing wavelength that spectrophotometer is set is 470nm.
  6. 6. according to a kind of any described water body bivalent nickel ion device for fast detecting of claim 1-3, it is characterised in that:It is described Spectrophotometric is calculated as V-1100D spectrophotometers.
CN201720732136.0U 2017-06-21 2017-06-21 A kind of water body bivalent nickel ion device for fast detecting Active CN206876566U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109856066A (en) * 2019-01-02 2019-06-07 厦门大学 The evaluation method and application thereof of nickel-containing material gram volume
CN114062355A (en) * 2021-11-10 2022-02-18 浙江信捷检测技术有限公司 Total nickel test pack and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109856066A (en) * 2019-01-02 2019-06-07 厦门大学 The evaluation method and application thereof of nickel-containing material gram volume
CN109856066B (en) * 2019-01-02 2020-09-11 厦门大学 Method for evaluating gram capacity of nickel-containing material and application thereof
CN114062355A (en) * 2021-11-10 2022-02-18 浙江信捷检测技术有限公司 Total nickel test pack and preparation method thereof
CN114062355B (en) * 2021-11-10 2022-08-16 浙江信捷检测技术有限公司 Total nickel test pack and preparation method thereof

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