CN107247049A - The test paper of cadmium content in a kind of detection cereal with screening agent - Google Patents
The test paper of cadmium content in a kind of detection cereal with screening agent Download PDFInfo
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- CN107247049A CN107247049A CN201710436969.7A CN201710436969A CN107247049A CN 107247049 A CN107247049 A CN 107247049A CN 201710436969 A CN201710436969 A CN 201710436969A CN 107247049 A CN107247049 A CN 107247049A
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Abstract
The present invention relates to a kind of test paper of cadmium content in detection cereal with screening agent, the test paper from top to bottom includes solid layer, color layer, support basic unit and solid layer successively, and support basic unit is additionally equipped with standard color comparison card；The support basic unit is the filter paper with screening agent and sensitizer；The solid layer is two layers, and two layers of solid layer is to have the xanthans with screening agent and sensitizer；The display layer is that cadmium is combined developer.The present invention has test paper using middling speed quantitative filter paper as basic backing material, cheap and easy to get, is easy to carry.The main support thing filter paper outer layer of test paper is covered to form barrier film by xanthans, plays a part of protecting and fixed developer, the advantages of adding the shelf-life of test paper.
Description
Technical field
The invention belongs to detect cadmium ion content technical field in cereal, and in particular to the invention belongs to detect cadmium in cereal
Ion concentration technical field, and in particular to the method and test paper of cadmium ion in a kind of quick detection cereal with screening agent.
Background technology
In recent years, with industry, agricultural, the fast development of the industry such as processing industry, the pollution problem of heavy metal has been in environment
Increasingly aggravate.And the heavy metal in environment can constantly be accumulated by food chain, existence and the health, such as Hunan of the mankind is jeopardized
Cadmium rice event.And cadmium content excessive aggregation can make muscular atrophy in human body, textured bone has an effect on enzyme system in liver kidney organ
Normal function, can be dead because of hepatorenal syndrome when serious.And the probability that the long-term intake of cadmium can make women suffer from breast cancer increases
Plus.Therefore, it is the content of heavy metal cadmium in control grain, it is necessary to which, to the water quality in grain producing region, soil and process are carried out
Monitoring, and set up quick, the convenient method suitable for Site Detection cadmium ion is particularly important.
At present, the analysis method of conventional detection heavy metal cadmium ion has a ultraviolet spectrophotometry, atomic absorption spectrography (AAS),
Atomic emission spectrometry, electrochemical process, inductively coupled plasma mass spectrometry.Ultraviolet spectrophotometry is multiple due to test process
Miscellaneous, stability and repeatability are poor, and other method sensitivity when analyzing cadmium ion content is high, and error is small, as a result accurately, but
Large-scale instrument and professional operator are needed, the detection cycle is long, complex operation, and expensive equipment, be not suitable for live fast
Speed detection.
Retrieve and find by prior art literature, number of patent application is 201410021261.1 Chinese patent, entitled
The test paper of detection Chinese herbal medicine cadmium content with screening agent, the test paper that the patent is invented includes the tape test overlapped successively
Hole, the sample-adding substrate of control wells, the fibrous layer of the glass with screening agent, reaction substrate with cadmium developer and with two
Individual peephole respectively with instrument connection, control wells are corresponding.It is colour developing using p-nitrophenyl diazonium azobenzene and its homologous series material
Agent, by developer, Substrate Protection agent, excipient, sensitizer is dried in vacuo after buffer grinding, is being coated on reaction substrate.
Sample liquid is added dropwise in instrument connection, phosphate buffer is added dropwise in control wells, the actual colour developing degree of control and colorimetric card, so as to examine
Measure out rapid determination of content of cadmium element in Chinese herbal medicine.Screening agent is fixed on test paper by the test paper first, is easy to carry, but it has the disadvantage system
Make process cumbersome, test paper is made up of four layers of backing material, need extemporaneous preparation phosphate buffer solution to do pair in test process
According to.
The research about detecting cadmium ion test paper domestic at present is less, and Triazene used in the present invention is being done
Larger technological difficulties are how developer being fixed on support carrier during into test paper, and such organicvisualization reagent typically exists
Dissolubility in water is poor.Less in the developer remained with the test paper of its alcohol solution dipping, detection limit does not meet detection
It is required that, it is larger using limitation.
The content of the invention
It is improved that there is provided a kind of detection with screening agent it is an object of the invention to the defect for prior art
The test paper of cadmium content in cereal.The test paper is firstly introduced xanthans for solid agent, and with adsorption effect, makes simple, operation
Convenient, specificity is good, and sensitivity is high, and detection time is short, with low cost, and property is stable, and limited period reaches half a year, it is not necessary to large-scale expensive
Weight instrument auxiliary, it is adaptable to which in field quick detection, and detection process need not use phosphoric acid, reduce environmental pollution.
To achieve these goals, the test paper for detecting cadmium content in cereal provided according to the present invention, including following technology
Scheme：
A kind of test paper of cadmium content in detection cereal with screening agent, the test paper from top to bottom includes solid successively
Layer, color layer, support basic unit and solid layer, support basic unit are additionally equipped with standard color comparison card；The support basic unit is to carry to shelter
Agent and the filter paper of sensitizer；The solid layer is two layers, and two layers of solid layer is to have the xanthans with screening agent and sensitizer；Institute
State display layer and be combined developer for cadmium.
Further, the screening agent of the support basic unit and solid layer is mixed masking agent, including hydroxylamine hydrochloride, amino second
The sour sodium of acid, stone and thiocarbamide；The sensitizer be triton x-100, emulsifier op-10 or Tween-20 any one.
Further, the support basic unit and solid layer use the addition of screening agent：Each component is respectively 0.5-1 grams.
Further, it is that mesoporous silicon sphere loads 2- hydroxyl -5- sulfonic group phenyl diazoamino azos that the cadmium, which is combined developer,
Benzene cadmium, the cadmium is combined developer preparation method and is：2- hydroxyl -5- the sulfonic groups of 3 milliliters of addition in 100 milligrams of mesoporous silicon spheres
Phenyldiazonium aminoazabenzol ethanol solution, the concentration of 2- hydroxyl -5- sulfonic group phenyl diazoaminoazobenzenes is 1 milligram/milli
Rise, add 7mL deionized waters, the shape in 20 milliliters of deionized water is redissolved in centrifugation after the completion of 32h, loading is stirred at room temperature in lucifuge
Into compound chromogenic reagent solution.
Further, the preparation of the support basic unit comprises the following steps：The screening agent each component is taken to be dissolved in respectively
Formed in ionized water and shelter agent solution, added sensitizer, filter paper is soaked in above-mentioned solution 20 minutes, taken out, vacuum drying.
Further, the preparation of the color layer comprises the following steps：Support basic unit filter paper is laid in Buchner funnel, 1 is taken
The compound chromogenic reagent solution of milliliter stays in branch support group on the support basic unit filter paper of fixed size scope, making compound developer after suction filtration
On metafiltration paper.
Further, the preparation of the solid layer comprises the following steps：Take respectively the screening agent each component be dissolved in from
Formed in sub- water and shelter agent solution, add sensitizer, take 20 milliliters of the solution of screening agent and sensitizer, add 20 milligrams of Huangs
The colloid is evenly coated in the support basic unit for being fixed with compound developer by virgin rubber, heating stirring to colloid uniform bubble-free respectively
The upper surface of filter paper and the lower surface of support basic unit filter paper, form solid layer.
Further, the filter paper is middling speed quantitative analysis filter paper, low speed quantitative analysis filter paper or ordinary filter paper.From such
Backing material, the material of cellulose makes compound developer be easier to stay in support basic unit, and such material is cheap and easy to get, very
Big degree reduces cost.
Further, described standard color comparison card, is the cadmium-ion solution for preparing series of standards concentration, its pH is transferred to
11.30 or so, under the conditions of this pH, the developer for being combined developer and cadmium ion is most obvious, and test paper is separately immersed in into this
15 minutes in the cadmium-ion solution of series, color is taken, standard color range is fabricated to.
The invention also discloses the test paper of cadmium content in this detection cereal with screening agent, cadmium contains in detection cereal
The application of amount.
Hydroxylamine hydrochloride in the formula of screening agent, amion acetic acid is mainly used in sheltering copper ion, cobalt ions, nickel ion, iron from
The interference of son and zinc ion；Sodium potassium tartrate tetrahydrate, thiocarbamide is mainly used in sheltering silver ion, mercury ion, copper ion, lead ion etc. it is dry
Disturb.
The present invention is first stayed compound developer on the support basic unit filter paper of FX, then compound using suction filtration
Xanthans is smeared on developer, successfully compound developer is fixed on filter paper, and by screening agent and sensitizer with more
Easy method introduces test paper, test paper cadmium content suitable for field quick detection cereal.Establish in Site Detection cereal
The new method of cadmium ion.Compared with prior art, this method has the advantage that：
1st, test paper is cheap and easy to get using middling speed quantitative filter paper as basic backing material, is easy to carry.
2nd, the main support thing filter paper outer layer of test paper is covered to form barrier film by xanthans, plays protection and fixes developer
Effect, adds the shelf-life of test paper.
3rd, test paper manufacturing process is simple, is combined using suction filtration with xanthans, by compound developer fixation a on filter paper,
It is suitable for producing in enormous quantities, and production cost is low.
4th, simple to operate, most of reagent required for determining is fixed on test paper, and detection process need not add again
Enter, and phosphoric acid need not be used, reduce environmental pollution.
5th, detection sensitivity high specific is strong.When recycling the cadmium content in the test paper quick detection grain of the present invention, inspection
Rising limit is 0.1ppm, and accuracy in detection is more or less the same with atomic absorption spectrophotometry substantially.Due to the introduction of screening agent, for
Sheltering for other metal ions is good, so as to improve the specificity of detection.
6th, it is widely used.The Test paper that the present invention is set up may apply to：Grain, soil, water quality, processed food,
The detection of cadmium content in the materials such as Chinese herbal medicine, cosmetics.In addition above-mentioned sample has to pass through digestion process before testing, by chemical combination
The cadmium element of state is digested to inorganic cadmium ion, then is measured.
Brief description of the drawings：
Fig. 1 is the installation drawing of cadmium content test paper in the quick detection cereal with screening agent.
Wherein, 1- solids layer, 2- supports basic unit, 3- color layers.
Embodiment
In order that the purpose of the present invention, technical scheme and advantage are more clearly understood, below in conjunction with accompanying drawing and example, to this
Invention is further elaborated.And instantiation described herein is used only for explaining the present invention, it is not used to limit
The present invention.Without departing from the inventive concept of the premise, the similar improvement that can be done, belongs in the scope of the present invention.
Embodiment 1
The test paper structure of the present invention is simple, only using filter paper as basic backing material, and successfully will be aobvious using xanthans
The composite of toner is fixed on filter paper, is exactly the manufacturing process of the test paper below：
1 cadmium developer and mesoporous silicon sphere it is compound：Selected silicon ball is diameter 50nm or so mesoporous silicon sphere, in 100 millis
3 milliliters of 2- hydroxyl -5- sulfonic group phenyl diazoaminoazobenzene ethanol solutions, 2- hydroxyl -5- sulphurs are added in gram mesoporous silicon sphere
The concentration of acidic group phenyldiazonium aminoazabenzol is 1 mg/ml, adds 7mL deionized waters, 32h is stirred at room temperature in lucifuge, is filled
Centrifugation is redissolved after the completion of load forms the compound chromogenic reagent solution of cadmium in 20 milliliters of deionized water.
2 prepare screening agent, the mixed solution of sensitizer：Hydroxylamine hydrochloride, amion acetic acid, wine are added in 90mL deionized waters
Stone acid potassium sodium, each 1g of thiocarbamide after being completely dissolved, adds Qula and leads to 110-X 10mL, ultrasound is completely dissolved to Qula is logical, standby
With.
3 preparations contain screening agent, sensitizer, the mixed colloidal solution of xanthans：20mL 2 is taken to match somebody with somebody screening agent, sensitizer
Mixed solution, add 20mg xanthans, heating stirring to colloid uniform bubble-free.
The preparation of 4 test paper：The cadmium of gained in 1 is combined chromogenic reagent solution ultrasound uniformly, 1mL is taken in fixed size scope
Suction filtration on filter paper, makes composite stay on filter paper, takes match somebody with somebody mixed colloidal solution in 0.5mL 3 afterwards, is uniformly coated in and contains
On the filter paper for having developer composite, the reverse side of filter paper is also coated into colloidal solution after vacuum drying, again after vacuum drying
Filter paper part without developer is cut, sealing preserve, be the test paper of cadmium content in invented detection cereal.
The preparation of 5 standard color ranges：
3mL 10% ammoniacal liquor is added in 25mL volumetric flasks, now the pH of solution is 11.30 or so, is configured to a series of
The cadmium standard liquid of concentration, by the test paper made bubble 15 minutes in standard liquid, then claps the color of test paper with digital camera
Under, go out colorimetric card using Photoshop7.0 Software for Design on computers, and corresponding detectable concentration scope is marked out, prepare
Into standard color range.The detection range of this test paper is 0.1~10ppm.
Embodiment 2
1 cadmium developer and mesoporous silicon sphere it is compound：Selected silicon ball is diameter 50nm or so mesoporous silicon sphere, in 100 millis
3 milliliters of 2- hydroxyl -5- sulfonic group phenyl diazoaminoazobenzene ethanol solutions, 2- hydroxyl -5- sulphurs are added in gram mesoporous silicon sphere
The concentration of acidic group phenyldiazonium aminoazabenzol is 1 mg/ml, adds 7mL deionized waters, 32h is stirred at room temperature in lucifuge, is filled
Centrifugation is redissolved after the completion of load forms the compound chromogenic reagent solution of cadmium in 20 milliliters of deionized water.
2 prepare screening agent, the mixed solution of sensitizer：Hydroxylamine hydrochloride 0.5g, amino second are added in 90mL deionized waters
Acid 0.5, sodium potassium tartrate tetrahydrate 0.5, each 1g of thiocarbamide after being completely dissolved, adds emulsifier op-10 10mL, ultrasound to emulsifying agent
OP-10 is completely dissolved, standby.
3 preparations contain screening agent, sensitizer, the mixed colloidal solution of xanthans：Take and match somebody with somebody screening agent, enhanced sensitivity in 20mL 2
The mixed solution of agent, adds 20mg xanthans, heating stirring to colloid uniform bubble-free.
The preparation of 4 test paper：The cadmium of gained in 1 is combined chromogenic reagent solution ultrasound uniformly, 1mL is taken in fixed size scope
Suction filtration on filter paper, makes composite stay on filter paper, takes match somebody with somebody mixed colloidal solution in 0.5mL 3 afterwards, is uniformly coated in and contains
On the filter paper for having developer composite, the reverse side of filter paper is also coated into colloidal solution after vacuum drying, again after vacuum drying
Filter paper part without developer is cut, sealing preserve, be the test paper of cadmium content in invented detection cereal.
The preparation of 5 standard color ranges：
3mL 10% ammoniacal liquor is added in 25mL volumetric flasks, now the pH of solution is 11.30 or so, is configured to a series of
The cadmium standard liquid of concentration, by the test paper made bubble 15 minutes in standard liquid, then claps the color of test paper with digital camera
Under, go out colorimetric card using Photoshop7.0 Software for Design on computers, and corresponding detectable concentration scope is marked out, prepare
Into standard color range.The detection range of this test paper is 0.1~10ppm.
Embodiment 3
1 cadmium developer and mesoporous silicon sphere it is compound：Selected silicon ball is diameter 50nm or so mesoporous silicon sphere, in 100 millis
3 milliliters of 2- hydroxyl -5- sulfonic group phenyl diazoaminoazobenzene ethanol solutions, 2- hydroxyl -5- sulphurs are added in gram mesoporous silicon sphere
The concentration of acidic group phenyldiazonium aminoazabenzol is 1 mg/ml, adds 7mL deionized waters, 32h is stirred at room temperature in lucifuge, is filled
Centrifugation is redissolved after the completion of load forms the compound chromogenic reagent solution of cadmium in 20 milliliters of deionized water.
2 prepare screening agent, the mixed solution of sensitizer：Hydroxylamine hydrochloride 1g, amion acetic acid are added in 90mL deionized waters
0.6, sodium potassium tartrate tetrahydrate 1, each 0.5g of thiocarbamide after being completely dissolved, adds Tween-20 10mL, ultrasound is completely molten to Tween-20
Solution, it is standby.
3 preparations contain screening agent, sensitizer, the mixed colloidal solution of xanthans：Take and match somebody with somebody screening agent, enhanced sensitivity in 20mL 2
The mixed solution of agent, adds 20mg xanthans, heating stirring to colloid uniform bubble-free.
The preparation of 4 test paper：The cadmium of gained in 1 is combined chromogenic reagent solution ultrasound uniformly, 1mL is taken in fixed size scope
Suction filtration on filter paper, makes composite stay on filter paper, takes match somebody with somebody mixed colloidal solution in 0.5mL 3 afterwards, is uniformly coated in and contains
On the filter paper for having developer composite, the reverse side of filter paper is also coated into colloidal solution after vacuum drying, again after vacuum drying
Filter paper part without developer is cut, sealing preserve, be the test paper of cadmium content in invented detection cereal.
The preparation of 5 standard color ranges：
3mL 10% ammoniacal liquor is added in 25mL volumetric flasks, now the pH of solution is 11.30 or so, is configured to a series of
The cadmium standard liquid of concentration, by the test paper made bubble 15 minutes in standard liquid, then claps the color of test paper with digital camera
Under, go out colorimetric card using Photoshop7.0 Software for Design on computers, and corresponding detectable concentration scope is marked out, prepare
Into standard color range.The detection range of this test paper is 0.1~10ppm.
The measure of cadmium content in embodiment 4, rice meal
The digestion pre-treatment of sample：Using mixed acid Wet, 3 kinds of rice meals by grinding sieving are taken, 80 mesh are crossed
Sieve, weighs 2g samples and is placed in beaker in tall form, adds 10mL concentrated nitric acids, soaked overnight, and 160 DEG C of heating, which disappear to boil to solution, becomes clear,
Increase chloric acid 5mL and continue to disappear and boil to clear, continue to be heated to acid solution amount about 2mL, add 2.1ppm lead standard liquid 1mL, adjusted with ammoniacal liquor
It is about 11.30 to save pH value of solution, and 25mL is being settled to the pH ammoniacal liquor-ammonium chloride buffer solutions for being about 11.30.
The detection of actual sample：In the digestion solution that the Test paper invented is immersed in three of the above rice, 15 minutes
The color of test paper is contrasted with standard color comparison card afterwards, and testing result is represented, is not detected and is not detected in three portions of rice.For above-mentioned molten
Liquid uses inductively coupled plasma-Mass Spectrometer Method again, and testing result is 0.094ppm, 0.0207ppm, 0.2736ppb.Two kinds
Testing result is consistent substantially, illustrates that invented Test paper meets the requirements.
The measure of cadmium content in embodiment 5, mung bean flour
In this example, digestion process is carried out from 3 kinds of different mung bean flours.To the processing method be the same as Example 4 of sample
It is identical.
The detection basic step of sample is identical with example 4.Testing result shows that the testing result of 3 parts of mung bean flours is two parts
Do not detect, a content is 0.1ppm, and with inductively coupled plasma-Mass Spectrometer Method, testing result is 0.1365ppb,
0.1454ppb, 0.1312ppm.
Above is instantiation of the present invention is described.In addition, the invention is not limited in above-mentioned specific implementation
Mode, the deformation or modification made within the scope of the claims to the present invention has no effect on the substantive content of the present invention.This hair
Bright Test paper production process is simple, with low cost, easy to use, can be widely used in Site Detection, before development
Scape is wide.
Claims (10)
1. the test paper of cadmium content in a kind of detection cereal with screening agent, it is characterised in that the test paper is from top to bottom successively
Including solid layer, color layer, support basic unit and solid layer, support basic unit is additionally equipped with standard color comparison card；It is described support basic unit be
Filter paper with screening agent and sensitizer；The solid layer is two layers, and two layers of solid layer is to carry screening agent and sensitizer
Xanthans；The display layer is that cadmium is combined developer.
2. the test paper of cadmium content in a kind of detection cereal with screening agent according to claim 1, it is characterised in that institute
The screening agent for stating support basic unit and solid layer is mixed masking agent, including the sour sodium of hydroxylamine hydrochloride, amion acetic acid, stone and thiocarbamide；
The sensitizer be triton x-100, emulsifier op-10 or Tween-20 any one.
3. the test paper of cadmium content in a kind of detection cereal with screening agent according to claim 2, it is characterised in that institute
State the addition of support basic unit and solid layer using screening agent：Each component is respectively 0.5-1 grams.
4. the test paper of cadmium content in a kind of detection cereal with screening agent according to claim 1, it is characterised in that institute
It is that mesoporous silicon sphere loads 2- hydroxyl -5- sulfonic group phenyl diazoaminoazobenzene cadmiums to state cadmium and be combined developer, and the cadmium is compound aobvious
Toner preparation method is：2- hydroxyl -5- sulfonic group phenyl diazoamino the azos of 3 milliliters of addition in 100 milligrams of mesoporous silicon spheres
Benzyl carbinol solution, the concentration of 2- hydroxyl -5- sulfonic group phenyl diazoaminoazobenzenes is 1 mg/ml, add 7mL go from
Sub- water, the compound developer solution of formation cadmium in 20 milliliters of deionized water is redissolved in centrifugation after the completion of 32h, loading is stirred at room temperature in lucifuge
Liquid.
5. the test paper of cadmium content in a kind of detection cereal with screening agent according to claim 3, it is characterised in that institute
The preparation for stating support basic unit comprises the following steps：Take the screening agent each component to be dissolved in deionized water respectively and form screening agent
Solution, adds sensitizer, and filter paper is soaked in above-mentioned solution 20 minutes, takes out, vacuum drying.
6. the test paper of cadmium content in a kind of detection cereal with screening agent according to claim 1 or 4, its feature exists
In the preparation of the color layer comprises the following steps：Support basic unit filter paper is laid in Buchner funnel, 1 milliliter of compound colour developing is taken
Agent solution is stayed on support basic unit filter paper on the support basic unit filter paper of fixed size scope, making compound developer after suction filtration.
7. the test paper of cadmium content in a kind of detection cereal with screening agent according to claim 3, it is characterised in that institute
The preparation for stating solid layer comprises the following steps：The screening agent each component is taken to be dissolved in formation screening agent in deionized water respectively molten
Liquid, adds sensitizer, takes 20 milliliters of the solution of screening agent and sensitizer, adds 20 milligrams of xanthans, heating stirring to glue
Body uniform bubble-free, the colloid is evenly coated in respectively upper surface and the support for the support basic unit filter paper for being fixed with compound developer
The lower surface of basic unit's filter paper, forms solid layer.
8. the test paper of cadmium content in a kind of detection cereal with screening agent according to claim 1, it is characterised in that institute
It is middling speed quantitative analysis filter paper, low speed quantitative analysis filter paper or ordinary filter paper to state filter paper.
9. the test paper of cadmium content in a kind of detection cereal with screening agent according to claim 1, it is characterised in that institute
The standard color comparison card stated, is the cadmium-ion solution for preparing series of standards concentration, its pH is transferred into 11.30 or so, by test paper point
It is not immersed in this series of cadmium-ion solution 15 minutes, takes color, is fabricated to standard color range.
10. the examination of cadmium content in a kind of a kind of detection cereal with screening agent according to claim 1-9 any one
The application of paper cadmium content in detection cereal.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109668875A (en) * | 2017-10-13 | 2019-04-23 | 中国科学院大连化学物理研究所 | It is a kind of for quickly detecting the test paper of pesticide sevin |
| CN112683889A (en) * | 2020-12-04 | 2021-04-20 | 西安建筑科技大学 | Binary chromogenic test paper and method for rapidly and semi-quantitatively detecting Cd (II) |
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| CN112683889A (en) * | 2020-12-04 | 2021-04-20 | 西安建筑科技大学 | Binary chromogenic test paper and method for rapidly and semi-quantitatively detecting Cd (II) |
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