CN103776823A - Heavy-metal detection method, as well as test paper and preparation method thereof - Google Patents
Heavy-metal detection method, as well as test paper and preparation method thereof Download PDFInfo
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- CN103776823A CN103776823A CN201310415165.0A CN201310415165A CN103776823A CN 103776823 A CN103776823 A CN 103776823A CN 201310415165 A CN201310415165 A CN 201310415165A CN 103776823 A CN103776823 A CN 103776823A
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Abstract
The invention discloses a heavy-metal detection method which comprises the following steps: to-be-detected solution preparation: preparing a to-be-detected sample into an aqueous solution, and adding an acid solution and a potassium iodide solution to obtain a to-be-detected solution; to-be-detected solution detection: delivering the to-be-detected solution, dropwise adding the to-be-detected solution on the test paper for color development for 15-180 seconds, wherein the test paper contains triarylmethane alkaline cationic dye; result judgment: comparing the developing test paper with a color comparing card to determine the concentration of heavy metal. The invention further discloses test paper for the heavy metal detection method and a preparation method for the test paper. According to the invention, the metal content, particularly the content of the heavy metal mercury in some samples including a water sample, sludge and cosmetics can be detected.
Description
Technical field
The present invention relates to environment measuring field, relate in particular to the detection method of a heavy metal species, Test paper and preparation method thereof.
Background technology
Relative density on physics meaning is at 4.5g/cm
3above metal, is called heavy metal.Atomic number is from 23(V) to 92(U) native metal unit have 60 kinds, wherein the relative density of 54 kinds is all greater than 4.5g/cm
3, therefore, from the meaning of relative density, these 54 kinds of metals are all heavy metals.But, in the time carrying out ultimate analysis, what wherein have belongs to rare earth metal, and what have has incorporated refractory metal into, at the industrial element that really puts heavy metal under is finally: copper, lead, zinc, tin, nickel, cobalt, antimony, mercury, cadmium and bismuth, these 10 kinds of metals are widely used in modern industry, be greater than 5 except thering is metal general character and density, in physics, there is no other special general character, but studies confirm that in a large number heavy metal has very strong bio-toxicity both at home and abroad, Long Term Contact, causes serious harm to human body.
At present, heavy metal detects still take large-sized analytic instrument as main, the detection method of current all heavy metals can be divided into spectrum colourimetry and electrode method two classes, and spectrum colourimetry is sample treatment difference, has utilized respectively atomic spectrum and the molecular spectrum of different spectral coverage.Recently there is successively report for the colorimetric detection method of indivedual metals, on market, also occur some detecting instruments, but do not have a kind of detection method can accurately accomplish the detection of the quantitative and qualitative analysis that the heavy metal in environment is carried out.
Summary of the invention
For this reason, the present invention proposes a kind of heavy metal detection method that can address the above problem or that at least can partly address the above problem, Test paper and preparation method.
According to an aspect of the present invention, provide a heavy metal species detection method, the method comprises the steps:
Liquid preparation steps to be measured: testing sample is mixed with to aqueous solution, adds acid solution and liquor kalii iodide, obtain liquid to be measured;
Liquid detecting step to be measured: pipette liquid to be measured, drop on test paper and develop the color 15～180 seconds, contain triarylmethane class alkaline cationic dye in described test paper;
Result determining step: colour developing test paper and colorimetric card are compared, determine heavy metal concentration.
Alternatively, the method according to this invention, in liquid preparation steps to be measured: also add screening agent solution and ascorbic acid solution,
Wherein, in 4～6 parts of testing sample aqueous solution, add that 0.1～0.5 part of acid solution, 0.5～2.5 part are sheltered, shake up after 0.4～0.8 part of ascorbic acid solution and 1.0～2.0 parts of liquor kalii iodides the constant volume that adds water, obtain liquid to be measured.
Alternatively, the method according to this invention, in liquid preparation steps to be measured, described acid solution is formulated with the volume ratio of 1:2～2:1 with red fuming nitric acid (RFNA) and water.
Alternatively, the method according to this invention, in liquid preparation steps to be measured, the concentration of described potassium iodide is 1～2.5mol/L.
Alternatively, the method according to this invention, in liquid preparation steps to be measured, the concentration of described ascorbic acid is 0.1～0.5mol/L.
Alternatively, according to the inventive method, in liquid preparation steps to be measured, described heavy metal is mercury, and described ascorbic acid concentrations is 0.1～0.25mol/L.
Alternatively, the method according to this invention, in liquid preparation steps to be measured, described screening agent is formulated with the volume ratio of 5:1 with the citric acid solution of 0.5～1% APDC solution and 0.2～1%.
Alternatively, the method according to this invention, at liquid detecting step to be measured, described triarylmethane class alkaline cationic dye is methyl violet 10B.
According to the detection method of heavy metal of the present invention, can detect accurately the content of beary metal of (as sewage, mud and cosmetics) in environment.Especially utilize the test paper that contains methyl violet 10B to detect heavy metal Hg, the sensitiveest, color developing effect the best, and can detect exactly the content of mercury ion in environment.Utilize 0.5～1% APDC solution and 0.2～1% citric acid solution can more effectively shelter other heavy metal elements outside the removal of mercury using the formulated mixed liquor of the volume ratio of 5:1 as screening agent, eliminate and disturb, can measure more accurately concentration and the content of heavy metal Hg.Wherein said APDC is pyrrolidinyl two bamic acid ammoniums.Wherein, APDC shelters the metallic ions such as arsenic, bismuth (III), cadmium (II), cobalt (II), copper (II), iron (III), manganese (II), nickel (II), plumbous (II), antimony (II), tin (II) and zinc (II) under acid condition, and citric acid can be sheltered Fe (III), Al(III), Ni(II) plasma; The following Fe(III of 100mg/L), Zn (II), Ni(II) and Al(III) do not disturb the mensuration of mercury; Cu(II below 10mg/L), Cd(II) and Pb(II) do not disturb the mensuration of mercury; Other common not with I
-the metallic ion of complexing is as K
+, Na
+, Ca
2+, Mg
2+, NH
4 +and negative ion is as Cl
-, NO
3 -deng the mensuration that does not affect Gold Samples and belong to mercury ion.In addition, heavy metal method for quick according to the present invention does not need pre-service, but can well realize detection effect, and simple to operate, can also reduce production costs.
According to a further aspect in the invention, provide a kind of preparation method of heavy metal detection test paper, the method comprises the steps:
Quantitative filter paper is put into the ethanol water of triarylmethane class alkaline cationic dye;
The described aqueous solution of putting into filter paper is spent to constant temperature oscillation 25～35 minutes 23～28;
Filter paper after described constant temperature oscillation is taken out and dried.
Alternatively, preparation in accordance with the present invention, wherein,
Be mercury at described heavy metal;
In described ethanol water, ethanol content is 1～2%;
Described triarylmethane class alkaline cationic dye is methyl violet 10B;
The mass concentration of described methyl violet 10B solution is 15～20ppm.
According to a further aspect in the invention, provide a kind of heavy metal detection test paper.
The preparation method of heavy metal detection test paper and the test paper for preparing according to the method according to the present invention, can be sensitive heavy metal is developed the color, the Test paper that especially contains methyl violet 10B is to the colour developing of heavy metal Hg more accurately and obviously.
Accompanying drawing explanation
By reading below detailed description of the preferred embodiment, various other advantage and benefits will become cheer and bright for those of ordinary skills.Accompanying drawing is only for the object of preferred implementation is shown, and do not think limitation of the present invention.And in whole accompanying drawing, represent identical parts by identical reference symbol.Wherein in the accompanying drawings, the multiple identical parts of alphabetic flag indication after reference number, in the time of these parts of general reference, will omit its last alphabetic flag.In the accompanying drawings:
Fig. 1 shows according to the detection method of the heavy metal of one embodiment of the present invention;
Fig. 2 shows according to the colorimetric card of one embodiment of the present invention heavy metal Hg;
Embodiment
The invention provides many applicable creative concepts, this creativeness concept can be reflected in a large number of in concrete context.The specific embodiment of describing in following embodiment of the present invention is only as the exemplary illustration of specific implementation of the present invention, and do not form limitation of the scope of the invention.
Set up in the present invention a kind of sensitive colorimetric detection method that facilitates, principle of the present invention is: first heavy metal ion and halogen ion or class halogen ionic reaction form complex anion; Complex anion and triarylmethane class alkaline cationic dye associate and form ternary complexes.This ternary complex reaction has not only improved the stability of color development system, has formed the ligand with larger conjugated system, have larger spectral absorption capacity and the area that effectively adds lustre to, and its molar absorptivity is large, and reaction sensitivity and selectivity are high.
In addition, the applicant's research show that the most effective developer is methyl violet 10B for heavy metal Hg, and wherein methyl violet 10B is the one in triarylmethane class alkaline cationic dye, and structural formula is as follows:
Methyl violet 10B is green with metallic luster crystallization or bottle green crystalline powder, is the hexamethyl derivant of paramagenta, contains derivant a small amount of four, pentamethyl; 1g is dissolved in 10ml ethanol, 15ml glycerine, water-soluble and chloroform, and aqueous solution and ethanol are purple, are dissolved in hardly ether.
According to above reaction principle, and single heavy metal and developer feature separately, the detection method of a heavy metal species is proposed, especially for the detection method of heavy metal Hg.Because detection method will be used colour developing test paper and colorimetric card, also develop on this basis a series of corresponding Test papers and preparation method thereof, and corresponding colorimetric card.
According to shown in Fig. 1 according to the heavy metal detection method of one embodiment of the present invention, the method comprises the steps: first to enter liquid preparation steps S1100 to be measured: add 0.1～0.5 part of acid solution, 0.5～2.5 part of screening agent, 0.4～0.8 part of ascorbic acid solution and 1.0～2.0 parts of liquor kalii iodides the constant volume that adds water in 4～6 parts of testing sample aqueous solution after, shake up, obtain liquid to be measured; Then enter liquid detecting step S1200 to be measured: pipette liquid to be measured, drop on test paper and develop the color 15～180 seconds, in described test paper, contain triarylmethane class alkaline cationic dye; Finally enter result determining step S1300: colour developing test paper and colorimetric card are compared, determine heavy metal concentration, so far step S1300 finishes, and the detection of heavy metal completes.
Wherein, at liquid preparation steps S1100 to be measured, acid solution is formulated with the volume ratio of 1:2～2:1 with red fuming nitric acid (RFNA) and water.Acid solution can be used hydrochloric acid, sulfuric acid or nitric acid, but preferably use red fuming nitric acid (RFNA) and water with the formulated solution of the volume ratio of 1:2～2:1, the acidity of liquid to be measured is very large on the impact of test paper, easy oxidation KI when the acid amount that adds is too much, thereby on test paper, separate out I2 and disturb colour developing, therefore preferably red fuming nitric acid (RFNA) and water are formulated with the volume ratio of 1:2～2:1, and preferably red fuming nitric acid (RFNA) and water are prepared from the volume ratio of 2:3～3:2 further.
Wherein, at liquid preparation steps S1100 to be measured, preferably 1～2.5mol/L of potassium iodide concentration.This is due to heavy metal ion (as Hg (II)) and excessive I
-form complex anion comparatively stable, complex anion forms ternary complexes with developer further, has improved sensitivity and the selectivity of test paper reaction, but the too high I that is easily oxidized to of the concentration of KI in liquid to be measured
2disturb colour developing thereby separate out on test paper, draw preferably 1～2.5mol/L of potassium iodide concentration through test of many times.
Wherein, at liquid preparation steps S1100 to be measured, ascorbic acid concentrations is 0.1～0.5mol/L preferably, when heavy metal is mercury, and further preferred 0.1～0.25mol/L of ascorbic acid concentrations.Ascorbic acid does not participate in chromogenic reaction, but in color development system, has very important effect.A certain amount of ascorbic acid can protect iodide ion not oxidized on the one hand; Ascorbic acid can play again the effect of sheltering the interfering ion such as Fe (III), Zn (II) on the other hand.But in the time that the concentration of ascorbic acid is less than 0.1mol/L, can not fully play protection and the effect of sheltering, and excessive ascorbic acid can be fought for heavy metal ion (as Hg (II)) with developer and makes measurement result on the low side.Therefore draw the preferably 0.1～0.5mol/L of concentration of ascorbic acid through lot of experiments, preferred 0.1～0.25mol/L further in the time that heavy metal is mercury.
Wherein, in liquid preparation steps to be measured, when heavy metal to be measured is mercury, screening agent preferably uses the citric acid solution of 0.5～1% APDC solution and 0.2～1% formulated with the volume ratio of 5:1.Screening agent is in the time selecting a kind of compound to shelter the metal outside heavy metal to be measured, and masking effect is bad, more serious to the interference ratio of metal to be measured, and impact detects effect.According to the inventive method, when heavy metal is detected, selecting, the potpourri of APDC solution and citric acid solution is better as the masking effect of screening agent, the APDC solution that preferred concentration is 0.5～1% further and 0.2～1% citric acid solution use as join masking agents, further select the citric acid solution of 0.5～1% APDC solution and 0.2～1% formulated with the volume ratio of 5:1.APDC shelters the metallic ions such as arsenic, bismuth (III), cadmium (II), cobalt (II), copper (II), iron (III), manganese (II), nickel (II), plumbous (II), antimony (II), tin (II) and zinc (II) under acid condition; The following Fe(III of 100mg/L), Zn (II), Ni(II) and Al(III) do not disturb the mensuration of mercury; Cu(II below 10mg/L), Cd(II) and Pb(II) do not disturb the mensuration of mercury; Other common not with I
-the metallic ion of complexing is as K
+, Na
+, Ca
2+, Mg
2+, NH
4 +and negative ion is as Cl
-, NO
3 -deng the mensuration that does not affect Gold Samples and belong to mercury ion.
In addition, at liquid detecting step S1200 to be measured, developing time preferably 15～180 seconds.With concentration be 20mg/L, 10mg/L, 5mg/L, 1.0mg/L, 0.1mg/L, 0mg/L series solution, react by the most preferably parameter of the inventive method, and in the time of 15s, 30s, 60s, 120s, 180s, colour developing situation is absorbed, colour developing variation presents the rear downward trend that first rises, and effect is best in the time of 60 seconds.
In addition, at liquid detecting step S1200 to be measured, triarylmethane class alkaline cationic dye is methyl violet 10B.In the time that metal to be measured is mercury, when the triarylmethane class alkaline cationic dye on test paper is methyl violet 10B, color developing effect is the sensitiveest, simple and quick.
In heavy metal detection method of the present invention, use Test paper and develop the color, the preparation method of this colour developing test paper comprises the steps: quantitative filter paper to put into the ethanol water of triarylmethane class alkaline cationic dye; The aqueous solution of putting into filter paper is spent to constant temperature oscillation 25～35 minutes 23～28; Filter paper after constant temperature oscillation is taken out and dried, keep in Dark Place.Wherein, when the preferred mercury of heavy metal, ethanol content preferably 1～2% in ethanol water; The purple 10B of triarylmethane class alkaline cationic dye preferable methyl; Preferably 15～20ppm of the mass concentration of methyl violet 10B solution.
Wherein, at result detecting step, test paper color and standard color comparison card after colour developing are compared, determine the concentration of heavy metal.And in the preparation process of standard color comparison card, select the best color condition of every heavy metal species detection, and choose the heavy metal solution of fixed concentration, carry out after chromogenic reaction, take and make standard color comparison card.
The detection method of heavy metal according to the present invention, optional parameter and many factors, can design the embodiment of different detection methods according to different parameters and factor, the detection method take heavy metal Hg be carried out to exemplary illustration to detection method of the present invention as embodiment below.
Before heavy metal detection method is carried out, first to be prepared heavy metal detection test paper, the factor and the parameter that in the preparation method due to Test paper, relate to are more, below the Test paper take mercury metal are described as example.
Embodiment 1
Get the beaker of a 2L, 500 milliliters of the ethanol waters that the ethanol content that adds the methyl violet 10B that the mass concentration for preparing is 15ppm is 1%, put into diameter and are 5 of the quantitative filter papers of 11 centimetres; The beaker of putting into filter paper and aqueous solution is placed on constant temperature oscillator, and 23 degree constant temperature oscillation 25 minutes, after taking-up, in cool place, dried at dry place, is cut into the test strips of 8mm*6mm with cutting knife, and low temperature saves backup.
Embodiment 2
Get the beaker of a 2L, 500 milliliters of the ethanol waters that the ethanol content that adds the methyl violet 10B that the mass concentration for preparing is 20ppm is 2%, put into diameter and are 5 of the quantitative filter papers of 11 centimetres; The beaker of putting into filter paper and aqueous solution is placed on constant temperature oscillator, and 28 degree constant temperature oscillation 35 minutes, after taking-up, in cool place, dried at dry place, is cut into the test strips of 8mm*6mm with cutting knife, and low temperature saves backup.
Embodiment 3
Get the beaker of a 2L, 500 milliliters of the ethanol waters that the ethanol content that adds the methyl violet 10B that the mass concentration for preparing is 18ppm is 1.5%, put into diameter and are 5 of the quantitative filter papers of 11 centimetres; The beaker of putting into filter paper and aqueous solution is placed on constant temperature oscillator, and 25 degree constant temperature oscillation 30 minutes, after taking-up, in cool place, dried at dry place, is cut into the test strips of 8mm*6mm with cutting knife, and low temperature saves backup.
Embodiment 5
Get the beaker of a 2L, 500 milliliters of the ethanol waters that the ethanol content that adds the methyl violet 10B that the mass concentration for preparing is 16ppm is 1.6%, put into diameter and are 5 of the quantitative filter papers of 11 centimetres; The beaker of putting into filter paper and aqueous solution is placed on constant temperature oscillator, and 30 degree constant temperature oscillation 32 minutes, after taking-up, in cool place, dried at dry place, is cut into the test strips of 8mm*6mm with cutting knife, and low temperature saves backup.
Embodiment 6
Get the beaker of a 2L, 500 milliliters of the ethanol waters that the ethanol content that adds the methyl violet 10B that the mass concentration for preparing is 19ppm is 1.9%, put into diameter and are 5 of the quantitative filter papers of 11 centimetres; The beaker of putting into filter paper and aqueous solution is placed on constant temperature oscillator, and 27 degree constant temperature oscillation 28 minutes, after taking-up, in cool place, dried at dry place, is cut into the test strips of 8mm*6mm with cutting knife, and low temperature saves backup.
Secondly, need to be according to the present invention the optimum reaction condition of heavy metal detection method prepare colorimetric card for use.Prepare colorimetric card as an example of mercury metal example below, the preparation method of colorimetric card is as follows in the present embodiment: pipette in the round bottom of each 5 milliliters in 10 milliliters of titer of the Hg that concentration range is 0～25mg/L (II) test tube with cover, chosen respectively in the present embodiment concentration and be the titer of 0mg/L, 0.1mg/L, 0.5mg/L, 2.5mg/L, 5mg/L, 10mg/L, 20mg/L each 5 milliliters in round bottom test tube with cover; Add successively respectively with red fuming nitric acid (RFNA) and water with 0.2 milliliter of the formulated salpeter solution of the volume ratio of 2:3; APDC solution with 0.9%, 0.6% citric acid solution are with 1.2 milliliters of the formulated screening agents of volume ratio of 5:1; 0.6 milliliter of the ascorbic acid solution of 0.15mol/L; 1.8 milliliters of the liquor kalii iodides of 1.8mol/L; Then add water and be settled to 10 milliliters and shake up.The mercury test-paper of well cutting is placed in the reactive tank of polystyrene microflute reaction plate fixing simultaneously, getting successively Hg (II) series concentration with micro liquid sampler mixes liquid 10uL to be measured and drops on the test paper of reactive tank, under indoor natural light, react and take and make colorimetric card afterwards for 60 seconds, prepare the colorimetric card of mercury as shown in Figure 2.
Application the said method test paper and the colorimetric card that prepare, and the various parameters that provide according to the present invention and reaction factor design obtain the detection method of heavy metal, refers more particularly to the detection method of heavy metal Hg.Detection method using following mercury metal describes detection method of the present invention as embodiment.
Embodiment 6
According to shown in Fig. 1 according to the heavy metal detection method of one embodiment of the present invention, the method comprises the steps: liquid preparation steps S1100 to be measured: in 4 milliliters of testing sample aqueous solution, add 0.1 milliliter of acid solution, 0.5 milliliter of screening agent, after 0.4 milliliter of ascorbic acid solution and 1.0 milliliters of liquor kalii iodides the constant volume that adds water, shake up, obtain liquid to be measured, acid solution is formulated with the volume ratio of 1:2 with red fuming nitric acid (RFNA) and water, potassium iodide concentration is 1mol/L, ascorbic acid concentrations is 0.1mol/L, 0.5% APDC solution for screening agent, 0.2% citric acid solution is formulated with the volume ratio of 5:1, enter afterwards liquid detecting step S1200 to be measured: pipette 9uL liquid to be measured, drop on test paper and develop the color 15 seconds, in test paper, contain methyl violet 10B, finally enter result determining step S1300: colour developing test paper and colorimetric card are compared, determine the concentration of heavy metal Hg, draw the content of mercury in sample through converting.
Embodiment 7
According to shown in Fig. 1 according to the heavy metal detection method of one embodiment of the present invention, the method comprises the steps: liquid preparation steps S1100 to be measured: in 4 milliliters of testing sample aqueous solution, add 0.5 milliliter of acid solution, 2.5 milliliters of screening agents, after 0.8 milliliter of ascorbic acid solution and 2.0 milliliters of liquor kalii iodides the constant volume that adds water, shake up, obtain liquid to be measured, wherein testing sample aqueous solution is sewage sample, acid solution is formulated with the volume ratio of 2:1 with red fuming nitric acid (RFNA) and water, potassium iodide concentration is 2.5mol/L, ascorbic acid concentrations is 0.5mol/L, 1.0% APDC solution for screening agent, 1.0% citric acid solution is formulated with the volume ratio of 5:1, enter afterwards liquid detecting step S1200 to be measured: pipette 9uL liquid to be measured, drop on test paper and develop the color 15 seconds, in test paper, contain methyl violet 10B, finally enter result determining step S1300: colour developing test paper and colorimetric card are compared, determine the concentration of heavy metal Hg, draw the content of mercury in sample through converting.
Embodiment 8
According to shown in Fig. 1 according to the heavy metal detection method of one embodiment of the present invention, the method comprises the steps: liquid preparation steps S1100 to be measured: in 6 milliliters of testing sample aqueous solution, add 0.2 milliliter of acid solution, 0.8 milliliter of screening agent, after 0.7 milliliter of ascorbic acid solution and 1.3 milliliters of liquor kalii iodides the constant volume that adds water, shake up, obtain liquid to be measured, acid solution is formulated with the volume ratio of 2:3 with red fuming nitric acid (RFNA) and water, potassium iodide concentration is 1.5mol/L, ascorbic acid concentrations is 0.3mol/L, 0.9% APDC solution for screening agent, 0.8% citric acid solution is formulated with the volume ratio of 5:1, enter afterwards liquid detecting step S1200 to be measured: pipette 9uL liquid to be measured, drop on test paper and develop the color 50 seconds, in test paper, contain methyl violet 10B, finally enter result determining step S1300: colour developing test paper and colorimetric card are compared, determine the concentration of heavy metal Hg, draw the content of mercury in sample through converting.
Embodiment 9
According to shown in Fig. 1 according to the heavy metal detection method of one embodiment of the present invention, the method comprises the steps: liquid preparation steps S1100 to be measured: in 6 milliliters of testing sample aqueous solution, add 0.3 milliliter of acid solution, 1.5 milliliters of screening agents, after 0.6 milliliter of ascorbic acid solution and 1.8 milliliters of liquor kalii iodides the constant volume that adds water, shake up, obtain liquid to be measured, wherein testing sample aqueous solution is sewage sample, acid solution is formulated with the volume ratio of 3:2 with red fuming nitric acid (RFNA) and water, potassium iodide concentration is 2.5mol/L, ascorbic acid concentrations is 0.3mol/L, 0.7% APDC solution for screening agent, 0.8% citric acid solution is formulated with the volume ratio of 5:1, enter afterwards liquid detecting step S1200 to be measured: pipette 11uL liquid to be measured, drop on test paper and develop the color 180 seconds, in test paper, contain methyl violet 10B, finally enter result determining step S1300: colour developing test paper and colorimetric card are compared, determine the concentration of heavy metal Hg, show that through converting Gold Samples belongs to the content of mercury.
Embodiment 10
According to shown in Fig. 1 according to the heavy metal detection method of one embodiment of the present invention, the method comprises the steps: liquid preparation steps S1100 to be measured: in 5 milliliters of testing sample aqueous solution, add 0.3 milliliter of acid solution, 1.1 milliliters of screening agents, after 0.5 milliliter of ascorbic acid solution and 1.6 milliliters of liquor kalii iodides the constant volume that adds water, shake up, obtain liquid to be measured, acid solution is formulated with the volume ratio of 2:3 with red fuming nitric acid (RFNA) and water, potassium iodide concentration is 2.2mol/L, ascorbic acid concentrations is 0.25mol/L, screening agent is formulated with the volume ratio of 5:1 with the citric acid solution of 0.6% APDC solution and 0.7%, enter afterwards liquid detecting step S1200 to be measured: pipette 10uL liquid to be measured, drop on test paper and develop the color 70 seconds, in test paper, contain methyl violet 10B, finally enter result determining step S1300: colour developing test paper and colorimetric card are compared, determine the concentration of heavy metal Hg, and obtain the content of mercury in sample through converting.
Embodiment 11
According to shown in Fig. 1 according to the heavy metal detection method of one embodiment of the present invention, the method comprises the steps: liquid preparation steps S1100 to be measured: in 4.5 milliliters of testing sample aqueous solution, add 0.25 milliliter of acid solution, 0.8 milliliter of screening agent, after 0.5 milliliter of ascorbic acid solution and 1.6 milliliters of liquor kalii iodides the constant volume that adds water, shake up, obtain liquid to be measured, acid solution is formulated with the volume ratio of 3:2 with red fuming nitric acid (RFNA) and water, potassium iodide concentration is 2mol/L, ascorbic acid concentrations is 0.1mol/L, screening agent is formulated with the volume ratio of 5:1 with the citric acid solution of 0.8% APDC solution and 0.8%, enter afterwards liquid detecting step S1200 to be measured: pipette 10uL liquid to be measured, drop on test paper and develop the color 80 seconds, in test paper, contain methyl violet 10B, finally enter result determining step S1300: colour developing test paper and colorimetric card are compared, determine the concentration of heavy metal Hg.
Can find out according to embodiment 6-11, the method according to this invention, can detect easy, fast the content of beary metal in sample, especially can utilize the detection paper that contains methyl violet 10B to go out content and the concentration of heavy metal Hg, according to the present invention, the detection method of heavy metal can detect the content of water sample and Heavy Metals in Sludge.In addition, the inventive method can also be applied to cosmetics detection field, therefore has wide range of applications, and certain contribution is made in environment monitoring field.
In addition, according to the method for quick of embodiment 10, the mercury test paper that use contains methyl violet 10B has carried out Fast Measurement to natural water, sanitary sewage, industrial waste water and cosmetics etc., and testing result is contrasted with the testing result with instrument analytical method, results of comparison is as shown in the table:
Can find out according to upper table, while the mercury metal containing in sample being carried out to fast detecting with test paper method, obtain concentration range, in the time that quantitatively detecting, the mercury metal containing in to sample with atomic absorption method obtains concrete concentration value, wherein concentration range comprises concrete concentration value, hence one can see that, test paper method can Accurate Determining heavy metal Hg concentration range, simple to operate, and can Rapid Detection; In addition, when the heavy metal Hg concentration that detects with atomic absorption method is on the low side, test paper method inspection does not measure the content of mercury, show that according to experiment test paper method is limited to 0.1-20mg/L to the detection of heavy metal Hg.
It should be noted, the present invention will be described rather than limit for above-described embodiment, and those skilled in the art can design alternative embodiment in the situation that not departing from claims scope.In the claims, any reference symbol between bracket should be configured to limitations on claims.Word " comprises " not to be got rid of existence and is not listed as element or step in the claims.
Claims (10)
1. a heavy metal species detection method, the method comprises the steps:
Liquid preparation steps to be measured (S1100): testing sample is mixed with to aqueous solution, adds acid solution and liquor kalii iodide, obtain liquid to be measured;
Liquid detecting step to be measured (S1200): pipette liquid to be measured, drop on test paper and develop the color 15～180 seconds, contain triarylmethane class alkaline cationic dye in described test paper;
Result determining step (S1300): colour developing test paper and colorimetric card are carried out to visual comparison, determine heavy metal concentration.
2. according to the method for claim 1, in liquid preparation steps to be measured (S1100): also add screening agent solution and ascorbic acid solution;
Wherein, shake up add 0.1～0.5 part of acid solution, 0.5～2.5 part of screening agent, 0.4～0.8 part of ascorbic acid solution and 1.0～2.0 parts of liquor kalii iodides the constant volume that adds water in 4～6 parts of testing sample aqueous solution after, obtain liquid to be measured.
3. according to the method for claim 2, in liquid preparation steps to be measured (S1100),
Described acid solution is formulated with the volume ratio of 1:2～2:1 with red fuming nitric acid (RFNA) and water;
The concentration of described potassium iodide is 1～2.5mol/L.
4. according to the method for claim 2, in liquid preparation steps to be measured (S1100), the concentration of described ascorbic acid is 0.1～0.5mol/L.
5. according to the either method of claim 1-4, in liquid preparation steps to be measured (S1100), described heavy metal is mercury, and described ascorbic acid concentrations is 0.1～0.25mol/L.
6. according to the method for claim 5, in liquid preparation steps to be measured (S1100), described screening agent is formulated with the volume ratio of 5:1 with the citric acid solution of 0.5～1% APDC solution and 0.2～1%.
7. according to the method for claim 5, at liquid detecting step to be measured (S1200), described triarylmethane class alkaline cationic dye is methyl violet 10B.
8. a preparation method for heavy metal detection test paper, the method comprises the steps:
Quantitative filter paper is put into the ethanol water of triarylmethane class alkaline cationic dye;
The described aqueous solution of putting into filter paper is spent to constant temperature oscillation 25～35 minutes 23～28;
Filter paper after described constant temperature oscillation is taken out and dried.
9. preparation method according to Claim 8, wherein,
Described heavy metal is mercury;
In described ethanol water, ethanol content is 1～2%;
Described triarylmethane class alkaline cationic dye is methyl violet 10B;
The mass concentration of described methyl violet 10B solution is 15～20ppm.
10. the heavy metal detection test paper that the preparation method of a kind according to Claim 8 or 9 obtains.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104990919A (en) * | 2015-07-24 | 2015-10-21 | 天津凯英科技发展有限公司 | Method for quickly detecting heavy metal content, test paper, and preparation method thereof |
| CN106198518A (en) * | 2016-07-05 | 2016-12-07 | 河南城建学院 | A kind of copper ion quick detection test paper and preparation method thereof |
| CN107764818A (en) * | 2017-10-22 | 2018-03-06 | 贺州学院 | A kind of method for detecting content of beary metal |
| JP2021532337A (en) * | 2019-08-26 | 2021-11-25 | 江▲蘇▼大学 | Fluorescence test paper and detection method for detecting mercury ions |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1019786A (en) * | 1996-07-04 | 1998-01-23 | Agency Of Ind Science & Technol | Reagent for measuring heavy metal and transition metal |
| CN1687754A (en) * | 2005-04-29 | 2005-10-26 | 农业部环境保护科研监测所 | Test paper for detecting heavy metal lead, cadmium, and mercury rapidly, preparation method and application |
| CN101893576A (en) * | 2010-06-18 | 2010-11-24 | 北京欧凯纳斯科技有限公司 | Heavy metal detection test paper and preparation method and application thereof |
| CN103760154A (en) * | 2013-09-12 | 2014-04-30 | 天津凯英科技发展有限公司 | Rapid heavy metal detection method, and detection test paper and preparation method thereof |
| CN103776822A (en) * | 2013-09-12 | 2014-05-07 | 天津凯英科技发展有限公司 | Rapid heavy-metal detection method, as well as test paper and preparation method thereof |
-
2013
- 2013-09-12 CN CN201310415165.0A patent/CN103776823A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1019786A (en) * | 1996-07-04 | 1998-01-23 | Agency Of Ind Science & Technol | Reagent for measuring heavy metal and transition metal |
| CN1687754A (en) * | 2005-04-29 | 2005-10-26 | 农业部环境保护科研监测所 | Test paper for detecting heavy metal lead, cadmium, and mercury rapidly, preparation method and application |
| CN101893576A (en) * | 2010-06-18 | 2010-11-24 | 北京欧凯纳斯科技有限公司 | Heavy metal detection test paper and preparation method and application thereof |
| CN103760154A (en) * | 2013-09-12 | 2014-04-30 | 天津凯英科技发展有限公司 | Rapid heavy metal detection method, and detection test paper and preparation method thereof |
| CN103776822A (en) * | 2013-09-12 | 2014-05-07 | 天津凯英科技发展有限公司 | Rapid heavy-metal detection method, as well as test paper and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| I.WALTER,ET AL: "Heavy metal speciation and phytotoxic effects of three representative sewage sludges for agricultural uses", 《ENVIRONMENTAL POLLUTION》, vol. 139, no. 3, 28 February 2006 (2006-02-28), XP028012027, DOI: doi:10.1016/j.envpol.2005.05.020 * |
| 郭玉香: "试纸法快速测定环境水样中痕量重金属镉、汞、铅的研究", 《中国优秀硕士学位论文全文数据库工程科技I辑》, no. 03, 15 September 2007 (2007-09-15) * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104990919A (en) * | 2015-07-24 | 2015-10-21 | 天津凯英科技发展有限公司 | Method for quickly detecting heavy metal content, test paper, and preparation method thereof |
| CN106198518A (en) * | 2016-07-05 | 2016-12-07 | 河南城建学院 | A kind of copper ion quick detection test paper and preparation method thereof |
| CN107764818A (en) * | 2017-10-22 | 2018-03-06 | 贺州学院 | A kind of method for detecting content of beary metal |
| JP2021532337A (en) * | 2019-08-26 | 2021-11-25 | 江▲蘇▼大学 | Fluorescence test paper and detection method for detecting mercury ions |
| JP7032831B2 (en) | 2019-08-26 | 2022-03-09 | 江▲蘇▼大学 | Fluorescence test paper and detection method for detecting mercury ions |
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