CN107064131A - A kind of detection carrier and its detection method for detecting various heavy - Google Patents
A kind of detection carrier and its detection method for detecting various heavy Download PDFInfo
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Abstract
The invention discloses a kind of detection carrier and its detection method for detecting various heavy, the detection carrier modifies microporous modified nitrocellulose membrane using xylenol orange, can as heavy metal ion chelating and colour developing carrier, the enrichment of heavy metal ion is carried out by using pin hole filter, and contrast standard colorimetric card carries out high sensitivity, sxemiquantitative, environment is detected real-time, food, heavy metal in industrial products, it is convenient and swift, substantial amounts of economy and manpower can be saved, be conducive to food, cosmetics safety and the real-time monitoring of environmental pollution, simultaneously for human body lead, the early prevention and treatment of mercury poisoning especially children and Patients of Occupational Disease play an important role, solving in traditional instrument detection needs large-scale instrument, instrumentation is difficult, it is costly, detection time is long, the problem of detection is inconvenient.
Description
Technical field：
The present invention relates to heavy metal rapid detection technical field, and in particular to a kind of detection carrier of detection various heavy
And its detection method.
Background technology：
Heavy metal is typically widely present in nature with natural concentration, but with expanding economy, domestic heavy metal
Exploitation, smelting, processing and business manufacturing activities it is increasing, cause many heavy metals such as copper, lead, mercury, chromium, cadmium, cobalt, arsenic etc.
Into in big gas and water, soil, cause serious environmental pollution.The biology of the heavy metal pollutions such as copper, lead, mercury, cadmium, chromium, cobalt, arsenic
Toxicity highly significant, high risks are caused to human health and environment.
The main method of current heavy metal analysis is spectroscopic methodology, including atom (absorption, transmitting, fluorescence etc.) spectrographic technique with
And AAS etc..In recent years, atom spectrum and the combination of plasma emission spectrum technology (ICP technologies), improve detection
Sensitivity, widened the range of linearity of detection, and made detection sensitiveer with mass spectrometry (ICP-MS), data analysis is more
It is convenient.But, costly, therefore the popularization and application in most of laboratories are restricted this quasi-instrument.
In addition to spectroscopic methodology, the AAS based on metal developer is also a kind of detection method conventional at present.
At present, the heavy metal inspection method national standard in food additives uses the light splitting that saturated hydrogen sulphide solution makees developer
Photometry.But the method is seriously polluted, preparing cumbersome and freshly prepared saturated hydrogen sulphide solution has strong fetid odour, poison
Property greatly, can make the CNS intoxication of people, produce dizzy, Nausea and vomiting phenomenon, severe one loss of consciousness, stupor, suffocate
It is even dead.Therefore, with toxicity is smaller and the obvious metal organicvisualization reagent of effect develops the color to substitute saturated hydrogen sulphide solution
New method obtains very big development.
General in most of organicvisualization reagents all to contain chromophore and auxochrome, they can be with the stable chelating of heavy metal generation
Thing simultaneously shows specific color.Unsaturated bond group energy absorbing wavelength in organic compound is more than 200nm light.This group
The referred to as chromophore of broad sense.Such as azo group (- N=N-), quinonyl etc..Some groups for having ring to electronics, they are with adding lustre to
Unsaturated bond interaction in group, can influence absorption of the organic compound to light, make color burn.These groups are referred to as helping
Color group.For example：Amido (- NH2), hydroxyl (- OH) etc., and halogeno-group (X-) etc., they can be with the unsaturated bond in chromophore
Interaction, causes permanent electric charge to move, thus reduce molecule intensify can, promote reagent to the absorption maximum of light to
Long wave direction is moved, so these groups are referred to as auxochrome.Organicvisualization reagent is used to detect heavy metal ion generation chelate tool
Have the advantage that：(1) color clear, general ε>104, sensitivity is high.(2) stabilization is combined, dissociation constant is small.(3) selectivity is high,
Specificity is strong.
Conventional developer has Phen class, porphyrin, dithizone, xylenol orange and Arsenazo etc. at present.Neighbour two
Nitrogen phenanthrene is a kind of conventional oxidation-reduction indicator.It is a bidentate heterocyclic compound part, similar to 2,2'- bipyridyls,
It is the assistant ligand commonly used during crystalline material is constructed, it has very strong chelation, can be with most metal ions formation very
Stable complex, application the most frequently used at present is Spectrophotometric Determination of Iron.Porphyrin (porphyrins) is porphines
(porphine) general name of the homologue of the substituted base of outer band and derivative, is a kind of special big ring conjugation aroma system,
It is widely used in the fields such as biochemistry, medical science, complexing analytical chemistry, materials chemistry, optical electro-chemistry and catalytic chemistry.Porphyrin
Most significant chemical characteristic is that it easily generates 1 with metal ion：1 complex, and the stability of complex is higher.Porphyrin chelating gold
The species of category is very more, can turn into the country in recent years with metal ion all in periodic table and semimetal ion complex
Most common AAS, fluorimetry and high performance liquid chromatography.Dithizone also known as hexichol vulcanization azo carbonyl hydrazides, be
The conventional detection reagent of lead, mercury, zinc, can be combined generation red complex with metal ion.Xylenol orange (3,3 '-bis- (dicarboxyl first
Base aminomethyl)-o-cresolsulfon-phthalein) belong to triphenylmethane developer, empurpled network can be given birth to most heavy metal ion
Compound.But the metal complex absworption peak of porphyrin is mostly in 420nm or so, and the naked eyes of the mankind are poor to its ability to see things in their true light, therefore
In terms of can be used only in spectrophotomelric assay.Dithizone is easy oxidation by air, need to add Aqueous Solution of Sulfur Dioxide protection, therefore examination
The stability and environmental protection aspect of agent are not enough.
Xylenol orange is purple crystal, soluble in water, and it has 6 grades of acid dissociation.Wherein H6In to H2In4-All it is yellow,
HIn5-To In6-It is red.In pH=5~6, xylenol orange is mainly with H2In4-Form is present.In pH>It is presented red when 6.3,
In pH<Yellow is presented when 6.3, during pH=pKa=6.3, intermediate colors are presented.Xylenol orange can be used for many heavy metal ion
Direct titration, in pH<Terminal is changed into reddish violet by glassy yellow when 6.3, and discoloration is sharp, it is adaptable to naked eyes detection application.Diformazan
The complex that phenol orange and metal ion are formed all is reddish violet, therefore it is only applicable in pH<In 6 acid solution.
Chitosan is also known as chitosan, is that the chitin (chitin) being widely present by nature is made by deacetylated
With what is obtained, chemical name is Chitosan (1-4) -2- amino-B-D glucose.Its structural formula is as follows：
The content of the invention：
It is an object of the invention to provide a kind of detection carrier and its detection method for detecting various heavy, the detection is carried
Body modifies microporous modified nitrocellulose membrane using xylenol orange, can as heavy metal ion chelating and colour developing carrier, by adopting
The enrichment of heavy metal ion is carried out with pin hole filter, and contrast standard colorimetric card carries out high sensitivity, real-time sxemiquantitative, inspection
Survey environment, food, the heavy metal in industrial products, it is convenient and swift, substantial amounts of economy and manpower can be saved, be conducive to food,
Cosmetics safety and the real-time monitoring of environmental pollution, simultaneously for human body lead, mercury poisoning especially children and Patients of Occupational Disease
Early prevention and treatment plays an important role, solve traditional instrument detection in need large-scale instrument, instrumentation it is difficult, costly, detection
The problem of time length, inconvenient detection.The present invention is achieved by the following technical programs：
It is a kind of detect various heavy detection carrier, the heavy metal in copper, lead, mercury, chromium, cadmium, cobalt, arsenic one
More than kind, the detection carrier is the modification nitrocellulose membrane for being coated with xylenol orange, and microporous modified nitre is modified using xylenol orange
Sour tunica fibrosa, the preparation method of the detection carrier comprises the following steps：
(1) using 0.45um nitrocellulose filters as basilar memebrane, lived with the 0.5wt%NaOH aqueous solution as activator in room temperature
Change 30min, the nitrocellulose filter after net drying is activated is washed with deionized water thereafter；
(2) the HCl PH=2 adjusted chitosan solution is added on the nitrocellulose filter after activation, room temperature reaction 2
Hour progress is chitin modified, and modified nitrocellulose filter is obtained after being washed with deionized water only；Nitrocellulose after activation
The mass ratio of film and the HCl PH=2 adjusted chitosan solution is 1:10-1:1000；
(3) 1wt% xylenol orange solution is added in modified nitrocellulose filter, regulation pH value is 5.5, room temperature reaction
Net drying is washed with deionized water after 1 hour and obtains target product.
The present invention also protects a kind of detection method for detecting various heavy, and this method comprises the following steps：
The salpeter solution configured first with deionized water extracts heavy metal ion present in sample, thereafter by qualitative filter
Particulate matter in the preliminary filtering solution of paper, then filtered by pin hole filter, the filter paper of pin hole filter laying is a variety of heavy for above-mentioned detection
The detection carrier of metal：The modification nitrocellulose membrane of xylenol orange is coated with, when solution is by filter paper, heavy metal ion and two
Cresols orange is combined and developed the color, and finally dismantles filter and filter paper and the standard color comparison card being provided previously by are carried out into color contrast, thus survey
Heavy metal ion content in random sample sheet；The heavy metal is selected from one or more of copper, lead, mercury, chromium, cadmium, cobalt, arsenic.
Xylenol orange molecule contains 4 carboxyls, two of which carboxyl and metal ion-chelant after it is combined with heavy metal,
Form the xylenol orange complex compound compound molecule as shown in formula I.Because the complex compound still has two free carboxies, therefore in pH<6
Acid solution in still exist with anionic form.
On the one hand modified nitrocellulose filter strengthens its mechanical performance and toughness, and on the other hand chitosan is consolidated
It is fixed, prevent the dissolving of chitosan in an acidic solution from causing filtering to be lost, so that chitosan can be steady under the conditions of pH value is 5.5
Surely xylenol orange is adsorbed, and does not influence the colour developing of xylenol orange complex compound.
The modification nitrocellulose membrane hydrophily for being coated with xylenol orange is strong, with the complex in the aqueous solution and showing
Color.
Especially, because xylenol orange can be chelated with contents of many kinds of heavy metal ion and occur color change, therefore by treating
Survey and add the influence that different anion sealers shield non-target metal ion in solution in buffer system in advance, for example, can use
NH4F shelters Al3+、Ti4+, ascorbic acid shelters Fe3+, Phen shelters Ni2+, acetylacetone,2,4-pentanedione shelters Th4+、Al3+Deng also may be used
General detection card is made to detect for the wide spectrum of contents of many kinds of heavy metal ion.
In addition the increase ions binding speed such as some surfactants such as tween-20, PEG can be also added in solution to be measured
And color developing effect is improved, increase detection sensitivity.Beneficial effects of the present invention are as follows：
1) Simple portable of the present invention, simple to operate, detection speed is fast, detected using colorimetric card form, with being provided previously by
Standard color comparison card carries out color contrast, thus determines heavy metal ion content in sample, visual result, and detection time is short, and 10
Minute in can sentence read result, without by supplementary instrument and and professional.
2) sensitivity is high：Due to carrying out the enrichment of heavy metal ion using pin hole filter, therefore the richness of ion can be realized
Collection, increase sensitivity, this has significant enhancement with traditional heavy metal colorimetric card in terms of sensitivity, using 20mL syringe as
Example, equivalent to improving 100 times, therefore can detect more micro heavy metal ion, Monitoring lower-cut reaches 0.1mg/L.
3) at a low price：It is thousands of or even up to ten thousand compared to a detection of heavy metal ion instrument or biology sensor so 100,000 valency
For lattice, price of the present invention is cheap, and general population also has the ability to buy.
4) flexibility ratio is high：Specific heavy metal ion in sample, or inspection can be detected by allocating metallic shield reagent
Several heavy metal ion are surveyed, therefore can also research and develop and promote a series of products for being used to detect other ions or heavy metal.
In a word, the present invention realizes high sensitivity, sxemiquantitative, the weight detected real-time in environment, food, industrial products
Metal, it is convenient and swift, substantial amounts of economy and manpower can be saved, is conducive to the real-time of food, cosmetics safety and environmental pollution
Monitoring, plays an important role simultaneously for the early prevention and treatment of human body lead, mercury poisoning especially children and Patients of Occupational Disease, solves biography
The problem of difficult, costly large-scale instrument, instrumentation, detection time length, inconvenient detection is needed in system instrument detection.
Brief description of the drawings：
Fig. 1 is the gray scale and the graph of a relation of heavy metal ion content in solution to be measured of the detection carrier colour developing of the present invention；
Wherein, abscissa is heavy metal ion content in solution to be measured, the gray scale that ordinate develops the color for detection carrier.
Embodiment：
Further illustrated the following is to the present invention, rather than limitation of the present invention.
Embodiment 1：
It is a kind of detect various heavy detection carrier, the heavy metal in copper, lead, mercury, chromium, cadmium, cobalt, arsenic one
More than kind, the carrier is the modification nitrocellulose membrane for being coated with xylenol orange, and it is fine to modify microporous modified nitric acid using xylenol orange
Film is tieed up, the preparation method of the detection carrier comprises the following steps：
(1) using 0.45um nitrocellulose filters as basilar memebrane, lived with the 0.5wt%NaOH aqueous solution as activator in room temperature
Change 30min, the nitrocellulose filter after net drying is activated is washed with deionized water thereafter；
(2) the HCl PH=2 adjusted chitosan solution is added on the nitrocellulose filter after activation, room temperature reaction 2
Hour progress is chitin modified, and modified nitrocellulose filter is obtained after being washed with deionized water only；Nitrocellulose after activation
The mass ratio of film and the HCl PH=2 adjusted chitosan solution is 1:100.
(3) 1wt% xylenol orange solution is added in modified nitrocellulose filter, regulation pH value is 5.5, room temperature reaction
Net drying is washed with deionized water after 1 hour and obtains target product.
Test result indicates that：The modified nitrocellulose filter on the one hand mechanical performance of enhancing nitrocellulose filter and tough
Property, on the other hand chitosan is fixed, prevents that the dissolving of chitosan in an acidic solution from causing filtering to be lost, so that
Chitosan can stablize absorption xylenol orange under the conditions of pH value is 5.5, and not influence the colour developing of xylenol orange complex compound, such as Fig. 1
Shown, the gray scale that detection carrier of the invention develops the color and heavy metal ion content in solution to be measured are in corresponding relation, can sxemiquantitative
Heavy metal ion content in quick detection solution to be measured.
Embodiment 2：
A kind of detection method for detecting various heavy, this method comprises the following steps：
The salpeter solution configured first with deionized water extracts heavy metal ion present in sample, and the heavy metal is selected from
One or more of copper, lead, mercury, chromium, cadmium, cobalt, arsenic, thereafter by particulate matter in the preliminary filtering solution of qualitative filter paper, then pass through
Pin hole filter is filtered, and the filter paper of pin hole filter laying is the detection carrier of detection various heavy prepared by embodiment 1：It is coated with
The modification nitrocellulose membrane of xylenol orange, when solution is by filter paper, heavy metal ion is combined and developed the color with xylenol orange, finally
Filter paper and the standard color comparison card being provided previously by are carried out color contrast by dismounting filter, are thus determined heavy metal ion in sample and are contained
Amount.Result is can obtain in 10 minutes, Monitoring lower-cut reaches 0.1mg/L.
Claims (6)
1. it is a kind of detect various heavy detection carrier, it is characterised in that the heavy metal be selected from copper, lead, mercury, chromium, cadmium,
One or more of cobalt, arsenic, the detection carrier are the modification nitrocellulose membrane for being coated with xylenol orange, are modified using xylenol orange
Microporous modified nitrocellulose membrane, the preparation method of the detection carrier comprises the following steps：
(1) using 0.45um nitrocellulose filters as basilar memebrane, activated with the 0.5wt%NaOH aqueous solution as activator in room temperature
30min, is washed with deionized water thereafter the nitrocellulose filter after net drying is activated；
(2) the HCl PH=2 adjusted chitosan solution is added on the nitrocellulose filter after activation, reacted at room temperature 2 hours
Progress is chitin modified, and modified nitrocellulose filter is obtained after being washed with deionized water only；Nitrocellulose filter after activation with
The mass ratio of the PH=2 of HCl regulations chitosan solution is 1:10-1:1000；
(3) 1wt% xylenol orange solution is added in modified nitrocellulose filter, regulation pH value is 5.5, and room temperature reaction 1 is small
When after net drying be washed with deionized water obtain target product.
2. a kind of detection method for detecting various heavy, it is characterised in that this method comprises the following steps：Deionization is used first
The salpeter solution of water configuration extracts heavy metal ion present in sample, thereafter by particle in the preliminary filtering solution of qualitative filter paper
Thing, then filtered by pin hole filter, the filter paper of pin hole filter laying is the detection of the detection various heavy described in claim 1
Carrier：The modification nitrocellulose membrane of xylenol orange is coated with, when solution is by filter paper, heavy metal ion is combined with xylenol orange
And develop the color, finally dismantle filter and filter paper and the standard color comparison card being provided previously by are subjected to color contrast, thus determine weight in sample
Metal ion content；The heavy metal is selected from one or more of copper, lead, mercury, chromium, cadmium, cobalt, arsenic.
3. the detection method of detection various heavy according to claim 2, it is characterised in that by solution to be measured
The influence that different anion sealers shield non-target metal ion is added in buffer system in advance.
4. the detection method of detection various heavy according to claim 3, it is characterised in that be added with solution to be measured
NH4F shelters Al3+、Ti4+, ascorbic acid shelters Fe3+, Phen shelters Ni2+, acetylacetone,2,4-pentanedione shelters Th4+、Al3+。
5. the detection method of detection various heavy according to claim 2, it is characterised in that add table in solution to be measured
Face activating agent.
6. the detection method of detection various heavy according to claim 5, it is characterised in that the surfactant choosing
From any of tween-20, PEG.
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| CN109187384A (en) * | 2018-08-14 | 2019-01-11 | 广东省测试分析研究所（中国广州分析测试中心） | Mercury method is surveyed in mercury enrichment material and head space enrichment in a kind of water sample |
| CN109541149A (en) * | 2018-12-29 | 2019-03-29 | 广东工业大学 | A kind of bion atmosphere heavy metal pollution detection discriminating gear and application |
| CN109975471A (en) * | 2019-02-27 | 2019-07-05 | 海南医学院 | A kind of preparation method of the information pattern paper base sensor of detection of heavy metal ion |
| CN110261605A (en) * | 2019-06-25 | 2019-09-20 | 陕西科技大学 | A kind of method of chitin modified enhancing test paper detection sensitivity |
| CN111808916A (en) * | 2020-07-24 | 2020-10-23 | 上海安翰医疗技术有限公司 | Trypsin detection film, preparation method and application thereof and trypsin detection kit |
| CN114295608A (en) * | 2021-12-31 | 2022-04-08 | 南京化学试剂股份有限公司 | Method for rapidly determining heavy metal in edetate disodium |
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| US11771311B2 (en) | 2020-07-24 | 2023-10-03 | AnX Robotica Corp | Systems and methods for collecting and screening of pancreatic secretions |
| CN114295608A (en) * | 2021-12-31 | 2022-04-08 | 南京化学试剂股份有限公司 | Method for rapidly determining heavy metal in edetate disodium |
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Application publication date: 20170818 |