CN107328723A - A kind of quick detection reagent of heavy metal lead and preparation method thereof - Google Patents
A kind of quick detection reagent of heavy metal lead and preparation method thereof Download PDFInfo
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- CN107328723A CN107328723A CN201710387906.7A CN201710387906A CN107328723A CN 107328723 A CN107328723 A CN 107328723A CN 201710387906 A CN201710387906 A CN 201710387906A CN 107328723 A CN107328723 A CN 107328723A
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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Abstract
The invention discloses a kind of quick detection reagent of heavy metal lead, it is made up of reagent A and reagent B, the reagent A is made up of the raw material below according to parts by weight：12 16 parts of ethylenediamine tetra-acetic acid, 69 parts of hydroxy ethylene diphosphonic acid, 10 14 parts of sodium citrate；The reagent B is made up of the raw material below according to parts by weight：15 18 parts of hydrochloric acid solution, 47 parts of sodium acetate, 25 parts of thiocarbamide, 58 parts of gentian violet solution.The invention also discloses the preparation method of the quick detection reagent of the heavy metal lead and application method.Quick detection reagent of the present invention, it is easy to use.The degree of accuracy is high, and without large-scale precision instrument, the approximate range of content of heavy metal lead just can be substantially judged by simply estimating, and detection speed is fast, disclosure satisfy that the field quick detection of the samples such as food, water sample.
Description
Technical field
The present invention relates to heavy metal analysis technical field, the quick detection reagent of specifically a kind of heavy metal lead and its preparation
Method.
Background technology
Lead is a kind of widely used heavy metal, is human body non-essential element.With the development of industrial and agricultural production, lead and its
Pollution of the compound to environment and food is increasingly serious.Lead and its compound are entered by respiratory tract, alimentary canal, skin and mucous membrane
In vivo, wherein most is stored in bone, and fraction flows with blood circulation and is distributed to whole body respectively tissue and organ, and and egg
Sulfydryl in white matter, enzyme and amino acid is combined, so as to have a strong impact on nerve system of human body, hemopoietic system, digestive system and kidney
Function.
According to correlative study, the people of Long Term Contact micro lead, the lead of savings can hinder the formation of haemocyte, cause under intelligence
Drop, study, job performance are low；Accumulation can make one to occur to a certain extent phrenoblabia, bad dream, insomnia, headache etc. it is chronic in
Toxication shape；Even there are the phenomenons such as weak, poor appetite, nausea, abdominal distension, stomachache, diarrhoea in severe patient.Lead can be entered by blood
Brain tissue, infringement cerebellum and cerebral cortex, disturb metabolic activity, make nutriment not enough with oxygen supply, cause the small capillary of brain
Blood vessel endothelium confluent monolayer cells swelling, and then develop into diffusivity brain damage.
The common detection methods of heavy metal lead mainly have sampling Graphite Furnace Atomic method, flame atomization, colorimetric method, atom glimmering
Light method etc..These methods are required to use large-scale precision instrument, and detection time is long, it is impossible to applied to samples such as food, water samples
Field quick detection.
The content of the invention
It is above-mentioned to solve it is an object of the invention to provide a kind of quick detection reagent of heavy metal lead and preparation method thereof
The problem of being proposed in background technology.
To achieve the above object, the present invention provides following technical scheme：
A kind of quick detection reagent of heavy metal lead, is made up of, the reagent A is by below according to weight reagent A and reagent B
The raw material composition of part：12-16 parts of ethylenediamine tetra-acetic acid, 6-9 parts of hydroxy ethylene diphosphonic acid, 10-14 parts of sodium citrate；The examination
Agent B is made up of the raw material below according to parts by weight：15-18 parts of hydrochloric acid solution, 4-7 parts of sodium acetate, 2-5 parts of thiocarbamide, gentian violet solution
5-8 parts.
It is used as further scheme of the invention：The mass fraction of the hydrochloric acid solution is 32-35%.
It is used as further scheme of the invention：The gentian violet solution is the mass fraction 1.8-2.0% gentian violet aqueous solution.
The preparation method of the quick detection reagent of the heavy metal lead, step is as follows：
1) hydroxy ethylene diphosphonic acid is weighed, the deionized water of 2 times of weight is added, after being uniformly mixed, first is obtained
Solution；
2) the first solution is warming up to 80-85 DEG C, adds ethylenediamine tetra-acetic acid and sodium citrate, stirring mixing 20-
30min, obtains the second solution；
3) the second solution is put into processor for ultrasonic wave, ultrasonically treated 40-50min, produces reagent A at 70-75 DEG C；
4) hydrochloric acid solution is weighed, thiocarbamide is then gradually added under agitation, after addition is finished, the 3rd solution is obtained；
5) gentian violet solution is weighed, sodium acetate is then gradually added under agitation, after addition is finished, the 4th solution is obtained；
6) the 3rd solution is merged with the 4th solution, the ultrasonically treated 25-30min at 40-45 DEG C produces reagent B.
The application method of the quick detection reagent of the heavy metal lead, step is as follows：1) sample treatment：For solid to be measured
Sample, takes 10g solid samples to be measured, is put into 10mL deionized waters, is polished into slurry, adds 5mL reagent As, stirring mixing 5-
6min, filtering takes filtrate, obtains pretreatment fluid；For liquid sample, 10mL liquid samples are taken, 5mL reagents are added
A, stirring mixing 5-6min, obtains pretreatment fluid；2) detect：8mL reagent B are taken, are added into pretreatment fluid, are mixed, are stood
1min, observes color change.
It is used as further scheme of the invention：Step 2) in, the μ g/L of lead tolerance in sample≤7.5, reagent is in purple, sample
Lead tolerance is more than 7.5 μ g/L and less than or equal to 90 μ g/L in product, gradually switchs to blueness, sample by purple as concentration increases reagent
Middle lead tolerance is more than 90 μ g/L and less than or equal to 150 μ g/L, gradually switchs to blue-green, sample as concentration increases reagent by blueness
Middle lead tolerance is more than 150 μ g/L, and reagent is in green.
Compared with prior art, the beneficial effects of the invention are as follows：
Quick detection reagent of the present invention, it is easy to use, just can be substantially by simply estimating without large-scale precision instrument
Judge the approximate range of content of heavy metal lead, detection speed is fast, disclosure satisfy that the field quick detection of the samples such as food, water sample.
The quick detection reagent degree of accuracy of the present invention is high, and testing cost is low, can promote the use of on a large scale.
Embodiment
Technical scheme is described in more detail with reference to embodiment.
Embodiment 1
A kind of quick detection reagent of heavy metal lead, is made up of, the reagent A is by below according to weight reagent A and reagent B
The raw material composition of part：12 parts of ethylenediamine tetra-acetic acid, 6 parts of hydroxy ethylene diphosphonic acid, 10 parts of sodium citrate；The reagent B by with
Under according to parts by weight raw material constitute：15 parts of hydrochloric acid solution, 4 parts of sodium acetate, 2 parts of thiocarbamide, 5 parts of gentian violet solution；The hydrochloric acid is molten
The mass fraction of liquid is 32%；The gentian violet solution is the gentian violet aqueous solution of mass fraction 1.8%.
In the present embodiment, the preparation method of the quick detection reagent of the heavy metal lead, step is as follows：
1) hydroxy ethylene diphosphonic acid is weighed, the deionized water of 2 times of weight is added, after being uniformly mixed, first is obtained
Solution；
2) the first solution is warming up to 80 DEG C, adds ethylenediamine tetra-acetic acid and sodium citrate, stirring mixing 20min is obtained
Second solution；
3) the second solution is put into processor for ultrasonic wave, ultrasonically treated 40min, produces reagent A at 70 DEG C；
4) hydrochloric acid solution is weighed, thiocarbamide is then gradually added under agitation, after addition is finished, the 3rd solution is obtained；
5) gentian violet solution is weighed, sodium acetate is then gradually added under agitation, after addition is finished, the 4th solution is obtained；
6) the 3rd solution is merged with the 4th solution, the ultrasonically treated 25min at 40 DEG C produces reagent B.
Embodiment 2
A kind of quick detection reagent of heavy metal lead, is made up of, the reagent A is by below according to weight reagent A and reagent B
The raw material composition of part：13 parts of ethylenediamine tetra-acetic acid, 7 parts of hydroxy ethylene diphosphonic acid, 10 parts of sodium citrate；The reagent B by with
Under according to parts by weight raw material constitute：16 parts of hydrochloric acid solution, 5 parts of sodium acetate, 3 parts of thiocarbamide, 5 parts of gentian violet solution；The hydrochloric acid is molten
The mass fraction of liquid is 32%；The gentian violet solution is the gentian violet aqueous solution of mass fraction 1.8%.
In the present embodiment, the preparation method of the quick detection reagent of the heavy metal lead, step is as follows：
1) hydroxy ethylene diphosphonic acid is weighed, the deionized water of 2 times of weight is added, after being uniformly mixed, first is obtained
Solution；
2) the first solution is warming up to 82 DEG C, adds ethylenediamine tetra-acetic acid and sodium citrate, stirring mixing 23min is obtained
Second solution；
3) the second solution is put into processor for ultrasonic wave, ultrasonically treated 40min, produces reagent A at 72 DEG C；
4) hydrochloric acid solution is weighed, thiocarbamide is then gradually added under agitation, after addition is finished, the 3rd solution is obtained；
5) gentian violet solution is weighed, sodium acetate is then gradually added under agitation, after addition is finished, the 4th solution is obtained；
6) the 3rd solution is merged with the 4th solution, the ultrasonically treated 28min at 40 DEG C produces reagent B.
Embodiment 3
A kind of quick detection reagent of heavy metal lead, is made up of, the reagent A is by below according to weight reagent A and reagent B
The raw material composition of part：14 parts of ethylenediamine tetra-acetic acid, 8 parts of hydroxy ethylene diphosphonic acid, 12 parts of sodium citrate；The reagent B by with
Under according to parts by weight raw material constitute：17 parts of hydrochloric acid solution, 5 parts of sodium acetate, 4 parts of thiocarbamide, 7 parts of gentian violet solution；The hydrochloric acid is molten
The mass fraction of liquid is 34%；The gentian violet solution is the gentian violet aqueous solution of mass fraction 1.9%.
In the present embodiment, the preparation method of the quick detection reagent of the heavy metal lead, step is as follows：
1) hydroxy ethylene diphosphonic acid is weighed, the deionized water of 2 times of weight is added, after being uniformly mixed, first is obtained
Solution；
2) the first solution is warming up to 83 DEG C, adds ethylenediamine tetra-acetic acid and sodium citrate, stirring mixing 25min is obtained
Second solution；
3) the second solution is put into processor for ultrasonic wave, ultrasonically treated 45min, produces reagent A at 73 DEG C；
4) hydrochloric acid solution is weighed, thiocarbamide is then gradually added under agitation, after addition is finished, the 3rd solution is obtained；
5) gentian violet solution is weighed, sodium acetate is then gradually added under agitation, after addition is finished, the 4th solution is obtained；
6) the 3rd solution is merged with the 4th solution, the ultrasonically treated 28min at 43 DEG C produces reagent B.
Embodiment 4
A kind of quick detection reagent of heavy metal lead, is made up of, the reagent A is by below according to weight reagent A and reagent B
The raw material composition of part：15 parts of ethylenediamine tetra-acetic acid, 9 parts of hydroxy ethylene diphosphonic acid, 13 parts of sodium citrate；The reagent B by with
Under according to parts by weight raw material constitute：17 parts of hydrochloric acid solution, 6 parts of sodium acetate, 2 parts of thiocarbamide, 6 parts of gentian violet solution；The hydrochloric acid is molten
The mass fraction of liquid is 35%；The gentian violet solution is the gentian violet aqueous solution of mass fraction 2.0%.
In the present embodiment, the preparation method of the quick detection reagent of the heavy metal lead, step is as follows：
1) hydroxy ethylene diphosphonic acid is weighed, the deionized water of 2 times of weight is added, after being uniformly mixed, first is obtained
Solution；
2) the first solution is warming up to 85 DEG C, adds ethylenediamine tetra-acetic acid and sodium citrate, stirring mixing 25min is obtained
Second solution；
3) the second solution is put into processor for ultrasonic wave, ultrasonically treated 48min, produces reagent A at 75 DEG C；
4) hydrochloric acid solution is weighed, thiocarbamide is then gradually added under agitation, after addition is finished, the 3rd solution is obtained；
5) gentian violet solution is weighed, sodium acetate is then gradually added under agitation, after addition is finished, the 4th solution is obtained；
6) the 3rd solution is merged with the 4th solution, the ultrasonically treated 29min at 45 DEG C produces reagent B.
Embodiment 5
A kind of quick detection reagent of heavy metal lead, is made up of, the reagent A is by below according to weight reagent A and reagent B
The raw material composition of part：16 parts of ethylenediamine tetra-acetic acid, 9 parts of hydroxy ethylene diphosphonic acid, 14 parts of sodium citrate；The reagent B by with
Under according to parts by weight raw material constitute：18 parts of hydrochloric acid solution, 7 parts of sodium acetate, 5 parts of thiocarbamide, 8 parts of gentian violet solution；The hydrochloric acid is molten
The mass fraction of liquid is 35%；The gentian violet solution is the gentian violet aqueous solution of mass fraction 2.0%.
In the present embodiment, the preparation method of the quick detection reagent of the heavy metal lead, step is as follows：
1) hydroxy ethylene diphosphonic acid is weighed, the deionized water of 2 times of weight is added, after being uniformly mixed, first is obtained
Solution；
2) the first solution is warming up to 85 DEG C, adds ethylenediamine tetra-acetic acid and sodium citrate, stirring mixing 30min is obtained
Second solution；
3) the second solution is put into processor for ultrasonic wave, ultrasonically treated 50min, produces reagent A at 75 DEG C；
4) hydrochloric acid solution is weighed, thiocarbamide is then gradually added under agitation, after addition is finished, the 3rd solution is obtained；
5) gentian violet solution is weighed, sodium acetate is then gradually added under agitation, after addition is finished, the 4th solution is obtained；
6) the 3rd solution is merged with the 4th solution, the ultrasonically treated 30min at 45 DEG C produces reagent B.
The application method of the quick detection reagent of the heavy metal lead, step is as follows：1) sample treatment：For solid to be measured
Sample, takes 10g solid samples to be measured, is put into 10mL deionized waters, is polished into slurry, adds 5mL reagent As, stirring mixing 5-
6min, filtering takes filtrate, obtains pretreatment fluid；For liquid sample, 10mL liquid samples are taken, 5mL reagents are added
A, stirring mixing 5-6min, obtains pretreatment fluid；2) detect：8mL reagent B are taken, are added into pretreatment fluid, are mixed, are stood
1min, observes color change, as the μ g/L of lead tolerance in sample≤7.5, reagent be in purple, sample lead tolerance be more than 7.5 μ g/L
And less than or equal to 90 μ g/L, with concentration increase reagent by purple gradually switch to lead tolerance in blueness, sample be more than 90 μ g/L and
Less than or equal to 150 μ g/L, it is more than 150 μ g/L as concentration increase reagent gradually switchs to lead tolerance in blue-green, sample by blueness,
Reagent is in green.
Compliance test result
100 kinds of various concentrations, different types of sample are taken, respectively with dithizone spectrophotometry and the quick inspection of the present invention
Test agent is detected, using the testing result of dithizone spectrophotometry as standard, judges quick detection reagent detection of the present invention
As a result accuracy.
Find that the degree of accuracy of quick detection reagent of the present invention reached 100% by above-mentioned experiment, can be used in food,
The field quick detection of the samples such as water sample, the degree of accuracy is high.
Quick detection reagent of the present invention, it is easy to use, just can be substantially by simply estimating without large-scale precision instrument
Judge the approximate range of content of heavy metal lead, detection speed is fast, disclosure satisfy that the field quick detection of the samples such as food, water sample.
The quick detection reagent degree of accuracy of the present invention is high, and testing cost is low, can promote the use of on a large scale.
The better embodiment to the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party
, can also be on the premise of present inventive concept not be departed from formula, the knowledge that one skilled in the relevant art possesses
Various changes can be made.
Claims (6)
1. a kind of quick detection reagent of heavy metal lead, it is characterised in that be made up of reagent A and reagent B, the reagent A by with
Under according to parts by weight raw material constitute：12-16 parts of ethylenediamine tetra-acetic acid, 6-9 parts of hydroxy ethylene diphosphonic acid, sodium citrate 10-
14 parts；The reagent B is made up of the raw material below according to parts by weight：15-18 parts of hydrochloric acid solution, 4-7 parts of sodium acetate, thiocarbamide 2-5
Part, 5-8 parts of gentian violet solution.
2. the quick detection reagent of heavy metal lead according to claim 1, it is characterised in that the quality of the hydrochloric acid solution
Fraction is 32-35%.
3. the quick detection reagent of heavy metal lead according to claim 1, it is characterised in that the gentian violet solution is quality
The fraction 1.8-2.0% gentian violet aqueous solution.
4. a kind of preparation method of the quick detection reagent of heavy metal lead as described in claim 1-3 is any, it is characterised in that
Step is as follows：
1) hydroxy ethylene diphosphonic acid is weighed, the deionized water of 2 times of weight is added, after being uniformly mixed, the first solution is obtained；
2) the first solution is warming up to 80-85 DEG C, adds ethylenediamine tetra-acetic acid and sodium citrate, stirring mixing 20-30min is obtained
Obtain the second solution；
3) the second solution is put into processor for ultrasonic wave, ultrasonically treated 40-50min, produces reagent A at 70-75 DEG C；
4) hydrochloric acid solution is weighed, thiocarbamide is then gradually added under agitation, after addition is finished, the 3rd solution is obtained；
5) gentian violet solution is weighed, sodium acetate is then gradually added under agitation, after addition is finished, the 4th solution is obtained；
6) the 3rd solution is merged with the 4th solution, the ultrasonically treated 25-30min at 40-45 DEG C produces reagent B.
5. a kind of application method of the quick detection reagent of heavy metal lead as described in claim 1-3 is any, it is characterised in that
Step is as follows：1) sample treatment：For solid sample to be measured, 10g solid samples to be measured are taken, is put into 10mL deionized waters, beats
Slurry is worn into, 5mL reagent As are added, stirring mixing 5-6min, filtering takes filtrate, obtains pretreatment fluid；For liquid sample,
10mL liquid samples are taken, 5mL reagent As are added, stirring mixing 5-6min obtains pretreatment fluid；2) detect：Take 8mL reagents
B, is added into pretreatment fluid, is mixed, and stands 1min, observes color change.
6. the application method of the quick detection reagent of heavy metal lead according to claim 5, it is characterised in that step 2)
In, the μ g/L of lead tolerance in sample≤7.5, reagent be in purple, sample lead tolerance be more than 7.5 μ g/L and less than or equal to 90 μ g/L,
It is more than 90 μ g/L and less than or equal to 150 μ g/L as concentration increases reagent and gradually switchs in blueness, sample lead tolerance by purple, with
Concentration increase reagent lead tolerance is gradually switched in blue-green, sample by blueness and be more than 150 μ g/L, reagent is in green.
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| CN113358591A (en) * | 2021-07-09 | 2021-09-07 | 王春莲 | Edible fungus detection metal detection device for food quality safety detection |
| CN114088896A (en) * | 2022-01-20 | 2022-02-25 | 深圳市汇知科技有限公司 | Detection device and detection method for heavy metals in agricultural products |
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| CN113358591A (en) * | 2021-07-09 | 2021-09-07 | 王春莲 | Edible fungus detection metal detection device for food quality safety detection |
| CN113358591B (en) * | 2021-07-09 | 2023-01-31 | 王春莲 | Edible fungus detection metal detection device for food quality safety detection |
| CN114088896A (en) * | 2022-01-20 | 2022-02-25 | 深圳市汇知科技有限公司 | Detection device and detection method for heavy metals in agricultural products |
| CN114088896B (en) * | 2022-01-20 | 2022-04-05 | 深圳市汇知科技有限公司 | Detection device and detection method for heavy metals in agricultural products |
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| CN107328723B (en) | 2019-12-06 |
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