CN104931491B - A kind of 61 test paper of conjunction for heavy-metal residual quick detection - Google Patents
A kind of 61 test paper of conjunction for heavy-metal residual quick detection Download PDFInfo
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Abstract
The present invention relates to a kind of quick, sensitive, easily 1 test paper of the conjunction of heavy-metal residual quick detection 6, including 6 mercury, cadmium, lead, copper, chromium, nickel heavy metal indexs, belong to food and environmental water quality monitoring field.The present invention is only made up of paper substrate and colour developing scraps of paper two parts, structurally and operationally all very simple；Using 3mm chromatography filter papers as carrier, test paper is set to be used for quickly detecting in 1 3min to mercury, cadmium, lead, copper, chromium, the heavy metal species content of nickel 6 in food, environment and water quality；It can be drawn by visual observation and accurately quantify test result, be not required to be shown with expensive instrument, user, which is not required to specialized training, can just grasp；Simultaneously cheap, production cost is low, is disposable and without repair and maintenance, accuracy is higher, repeatability, and the scene that is extremely suitable for is detected real-time and monitoring.
Description
Technical field
The present invention relates to it is a kind of it is quick, sensitive, easily heavy-metal residual quick detection 6 close 1 test paper, including mercury, cadmium,
6 lead, copper, chromium, nickel heavy metal indexs, belong to food and environmental water quality monitoring field.
Background technology
Heavy metal refer to periodic table of elements Midst density be more than 4.5 metal, totally 45 kinds, most common heavy metal have copper, lead,
Zinc, tin, nickel, cobalt, antimony, mercury, cadmium and bismuth.Heavy metal pollution refers to people or environment are damaged due to heavy metals exceeding standard
Phenomenon.Heavy metal pollution problem is long-standing in other countries, caused by the heavy metal Hg occurred such as Japanese Minamata bay in 1956
Itai-itai diseases case caused by several cadmiums occurs for minamata disease, nineteen fifty-five to Japanese fuji county in 1972.With China's expanding economy,
The heavy metal pollution problem in China also increasingly highlights.In the past few decades due to coal and other fossil fuels exploitation and use to
Substantial amounts of heavy metal is discharged into environment and the ecosystem, some illegal business administrations are improper, violation operation, without good
Regulations, any discharge are administered in the management of heavy metal discarded object, waste water etc. so that substantial amounts of heavy metal enters river and soil
In.Heavy metal can not be biodegradable, while have bioaccumulation, therefore they will be in the ecosystem and food chain
In it is permanent preserve, show high-caliber heavy metal pollution in the top (i.e. the life of people and people) of food chain.
The method of inspection of heavy metal is a lot, based on the inspection of authoritative institution at present is still mainly examined with large-scale instrument, and
And there is in method and very big development on material.Large-scale instrument method assay is accurately feasible, but time-consuming, technology
Be not suitable for the quick sampling observation in scene with the features such as equipment requirement is high, cost is high.Therefore, heavy-metal residual is quick, Sensitive Detection is for I
State's development of food industry and water quality safety monitor key technology difficulty in the urgent need to address, have important practical significance and answer
Use prospect.
In recent years, " test paper " is the food security to attract people's attention very much a quick detection platform.Test paper detecting method has
There is the features such as simple, cost is low to be adapted to field quick detection.It not only overcomes that Instrumental Analysis sample treatment is numerous and diverse, instrument uses
The high limitation of cost, a kind of quick, sensitive and simple to operate analysis method is more provided, is had in heavy metal quick detection
It is widely applied.Patent 200510013377.1 is disclosed with the test paper of quick detection heavy metal Hg, preparation method and answered at present
With patent 201210028922.4 discloses a kind of quantitative and semi-quantitative lead Test paper and its application, patent
201020288154.2 disclose a kind of quick detection test paper of copper ion, but these test paper only limit a certain index of detection,
It can not be realized during exclusive use and multiple indexes detection is carried out to a sample.Also patent 201020521531.2 discloses one kind
The detection card of various heavy is detected, but the detection card belongs to colloidal gold immunochromatographimethod sensor, need to prepare high specificity
Monoclonal antibody, sample pad is further related to, gold standard pad, the optimization and assembling of detecting pad and absorption pad, not only step is complicated, Er Qiecheng
This is higher.Therefore, it is necessary to find, a kind of high sensitivity, response time are short, with short production cycle, stability is strong, long shelf-life, possess
The technology of the very strong market competitiveness, for it is quick, quantitatively detect residual quantity of heavy metal in food and ambient water quality.
The content of the invention
The invention discloses the 6 of a kind of quick, sensitive, convenient heavy-metal residual quick detection to close 1 test paper, can facilitate,
Quickly the residual quantity of mercury in the various food and ambient water quality of market sale, cadmium, lead, copper, chromium, the heavy metal species of nickel 6 is entered
Row judges, testing result is read in 1-3min.
The composition of the present invention：Including paper substrate and 6 colour developing scraps of paper two parts, the described colour developing scraps of paper first pass through reaction solution
It is fixedly connected after immersion, drying, shearing with described substrate.
The preparation process of the present invention：
(1) preparation of reaction solution：Reaction solution 1-6 is prepared, the wherein solvent of reaction solution 1 is 80-120ml hot ethanols, solute
For 0.8-1.2g diphenylcarbazides, 5-10g polyvinylpyrrolidones, 20-30ml 10% triton x-100, ultrasonic dissolution,
Adjust pH 8.5-9.5；The solvent of reaction solution 2 is 80-120ml ethanol, and solute is 0.3-0.5g sodium hydroxides, 5-10g polyethylene
Pyrrolidones, 0.1-0.3g cadions, 20-30ml 10% triton x-100, ultrasonic dissolution, regulation pH 6.5-7.5；Reaction
The solvent of liquid 3 is 80-120ml ultra-pure waters, and solute is 0.3-0.5g rhodizonic acids, 5-10g polyvinylpyrrolidones, 3-5g bad
5% triton x-100 of hematic acid sodium, 20-30ml, ultrasonic dissolution, regulation pH 1.5-2.5；The solvent of reaction solution 4 is 80-
120ml ultra-pure waters, solute is 0.1-0.3g DDTCs, 5-10g polyvinylpyrrolidones, 20-30ml 5% triton x-100,
Ultrasonic dissolution, regulation pH 6.5-7.5；Reaction solution 5 divides for reaction solution 5A and reaction solution 5B, and reaction solution 5A solvent is 80-
120ml ultra-pure waters, solute are 0.07-0.15g cetyl trimethylammonium bromides, 9-11g citric acids, ultrasonic dissolution, adjust pH
6.5-7.5, reaction solution 5B solvent are 80-120ml hot ethanols, and solute is 1-3g diphenylcarbazides, 5-10g polyvinyl pyrroles
Alkanone, ultrasonic dissolution, regulation pH 6.5-7.5；Reaction solution 6 divides is for reaction solution 6A and reaction solution 6B, reaction solution 6A solvent
80-120ml ultra-pure waters, solute are 2.5-3.5g sodium hydroxides, 1.0-1.5g ammonium persulfates, ultrasonic dissolution, adjust pH 6.5-
7.5, reaction solution 6B solvent are 80-120ml hot ethanols, and solute is 1-3g dimethylglyoximes, 5-10g polyvinylpyrrolidones, is surpassed
Sound dissolves, regulation pH 6.5-7.5.
(3) cutting of filter paper：3mm chromatography filter papers (hereinafter referred to as filter paper) are cut into paper-cutter 10cm × 15cm square
The shape scraps of paper, it is easy to follow-up immersion liquid and drying；
(4) immersion of reaction solution：The reaction solution 1-6 configured is poured into special glass ware, filter paper 1-6 is clamped with tweezers
10-20s is soaked in reaction solution 1-6 respectively, is hung over clip on dry boxboard；
(5) drying of filter paper：To prevent the interference in air reduces test paper from using function, the filter paper for completing immersion liquid is put
Enter in vacuum drying chamber and dry.No. 1 scraps of paper dry 30-40min in the environment of 50-60 DEG C of temperature, vacuum 100-110Pa.2
Number scraps of paper dry 30-40min in the environment of 50-60 DEG C of temperature, vacuum 100-110Pa.No. 3 scraps of paper in 50-60 DEG C of temperature,
30-40min is dried in the environment of vacuum 100-110Pa.No. 4 scraps of paper are in 50-60 DEG C of temperature, vacuum 100-110Pa ring
30-40min is dried under border.No. 5 scraps of paper pass through reaction solution 5A in advance, in 50-60 DEG C of temperature, vacuum 100-110Pa environment
Lower drying 30-40min；Dried by being soaked in the environment of 50-60 DEG C of temperature, vacuum 100-110Pa for reaction solution 5B
50-60min.No. 6 scraps of paper pass through reaction solution 6A in advance, and 50- is dried in the environment of 30-40 DEG C of temperature, vacuum 100-110Pa
60min；In the immersion by reaction solution 6B, 50-60min is dried in the environment of 30-40 DEG C of temperature, vacuum 100-110Pa.
(6) storage of the colour developing scraps of paper：Dried filter paper 1-6 be develop the color the scraps of paper 1-6, be cut into 1cm ×
15cm colour developing bar 1-6, every can be cut to 10, be enclosed in valve bag, be put into the drier for fill drier and retain
It is to be checked；
(7) making of paper substrate：PP synthetic papers are cut into paper-cutter the 7cm × 15cm rectangle scraps of paper, are easy to follow-up paper
The bonding of base and colour-development sheet and the cutting of test strips.
(8) bonding of paper substrate and colour-development sheet：By the 1cm × 15cm cut colour developing scraps of paper 1-6, existed with adhesive bonding
On 7cm × 15cm paper substrate, turn into test-paper；
(9) cutting of test strips：The test-paper binded is uniformly cut into 0.55cm × 7cm test paper with paper cutter
Bar；
(10) storage of test strips：It is sealed in 4-20 DEG C of dry environment and stores, must not be by direct sunlight.
The scope of application of the present invention：Mercury in food and ambient water quality, cadmium, lead, copper, chromium, the heavy metal species content of nickel 6 it is quick
Detection.
The detection range of the present invention：Mercury 0-100mg/L, cadmium 0-20mg/L, lead 0-500mg/L, copper 0-100mg/L, chromium 0-
100mg/L, nickel 0-100mg/L.
The sample treatment of the present invention：Fluid sample can be detected directly；1g solid samples (edible part) are taken to be crushed, with
1mL distilled water mixes, and soaks 5min, stirring can detect to it.
The operating method of the present invention：Appropriate sample is taken in the drying receptacle of cleaning, to submerge the colour developing panel region of test paper
For standard, taken out immediately after submergence, colour-development sheet is horizontal positioned upward, it can be quantitatively judged after 1-3min.
The result judgement of the present invention：By the color of test paper compared with standard color comparison card carry out preliminary judgement, with colorimetric
Numerical value corresponding to card color identical color range is the detected value of this sample, as the color of test paper takes two between two color ranges
The median of person.
The features of the present invention：Only it is made up of paper substrate and colour developing scraps of paper two parts, it is structurally and operationally all very simple；With 3mm layers
Analysis filter paper is carrier, enables test paper in 1-3min to mercury, cadmium, lead, copper, chromium, the heavy metal species of nickel 6 in food and ambient water quality
Content is used for quickly detecting；It can be drawn by visual observation and accurately quantify test result, be not required to be shown with expensive instrument,
User, which is not required to specialized training, can just grasp；Simultaneously cheap, production cost is low, is disposable and without overhauling dimension
Shield, accuracy is higher, repeatability, is extremely suitable for live detection real-time and monitoring.
Brief description of the drawings
Fig. 1 is the overlooking the structure diagram of the present invention；
Fig. 2 is the side structure schematic view of the present invention；
Fig. 3 is the standard color comparison card (mg/L) of the present invention, and colorimetric corresponds to hexadecimal color code.
Embodiment
Prepare embodiment
Embodiment 1
Reaction solution 1 is prepared first, and its solvent is 100ml hot ethanols, and solute is 1g diphenylcarbazides, 5g polyvinyl pyrroles
10% triton x-100 of alkanone, 20ml, ultrasonic dissolution, pH 8.5 is adjusted, obtains reaction solution 1.By 3mm chromatography filter papers anti-
Answer and soaked in liquid 1, soak time 10s, 30min is dried in the environment of temperature 50 C, vacuum 100-110Pa.Will processing
Good test-paper is sealed in the drier for being put into and filling drier, must not be by direct sunlight.
Embodiment 2
Reaction solution 2 is prepared first, and its solvent is 100ml ethanol, and solute is 0.3g sodium hydroxides, 5g polyvinylpyrrolidines
Ketone, 0.1g cadions, 20ml 10% triton x-100, ultrasonic dissolution, pH 6.5 is adjusted, obtains reaction solution 2.3mm is chromatographed
Filter paper soaks in reaction solution 2, soak time 10s, is dried in the environment of temperature 50 C, vacuum 100-110Pa
30min.The test-paper handled well is sealed in the drier for being put into and filling drier, must not be by direct sunlight.
Embodiment 3
Reaction solution 3 is prepared first, and its solvent is 100ml ultra-pure waters, and solute is 0.3g rhodizonic acids, 5g polyvinyl pyrroles
The bad hematic acid sodium of alkanone, 3g, 20ml 5% triton x-100, ultrasonic dissolution, pH 1.5 is adjusted, obtains reaction solution 3.By 3mm layers
Analysis filter paper soaks in reaction solution 3, soak time 10s, is dried in the environment of temperature 50 C, vacuum 100-110Pa
30min.The test-paper handled well is sealed in the drier for being put into and filling drier, must not be by direct sunlight.
Embodiment 4
Reaction solution 4 is prepared first, and its solvent is that solvent is 100ml ultra-pure waters, and solute is 0.1g DDTCs, 5g polyethylene pyrroles
5% triton x-100 of pyrrolidone, 20ml, ultrasonic dissolution, pH 6.5 is adjusted, obtains reaction solution 4.By 3mm chromatography filter papers anti-
Answer and soaked in liquid 4, soak time 10s, 30min is dried in the environment of temperature 50 C, vacuum 100-110Pa.Will processing
Good test-paper is sealed in the drier for being put into and filling drier, must not be by direct sunlight.
Embodiment 5
Prepare reaction solution 5A first, its solvent be 100ml ultra-pure waters, solute be 0.07g cetyl trimethylammonium bromides,
10g citric acids, ultrasonic dissolution, pH 6.5 is adjusted, obtains reaction solution 5A.3mm chromatography filter papers are soaked in reaction solution 5A, soaked
Time is 10s, and 30min is dried in the environment of temperature 50 C, vacuum 100-110Pa.Reaction solution 5B is prepared again, and its solvent is
100ml hot ethanols, solute are 1g diphenylcarbazides, 5g polyvinylpyrrolidones, ultrasonic dissolution, adjust pH 6.5, are obtained anti-
Answer liquid 5B.3mm chromatography filter papers are soaked in reaction solution 5B, soak time 10s, in temperature 50 C, vacuum 100-110Pa
In the environment of dry 60min.The test-paper handled well is sealed in the drier for being put into and filling drier, must not be by sunlight
Direct projection.
Embodiment 6
Reaction solution 6A is prepared first, its solvent is 100ml ultra-pure waters, and solute is 2.5g sodium hydroxides, 1.0g ammonium persulfates,
Ultrasonic dissolution, adjust pH 7.5.3mm chromatography filter papers are soaked in reaction solution 6A, soak time 10s, in temperature 50 C, very
60min is dried in the environment of reciprocal of duty cycle 100-110Pa.Reaction solution 6B is prepared again, and its solvent is 100ml hot ethanols, and solute is 1g bis-
Dinitrodiphenyl carbazide, 5g polyvinylpyrrolidones, ultrasonic dissolution, pH 6.5 is adjusted, obtains reaction solution 6B.3mm chromatography filter papers are existed
Soaked in reaction solution 6B, soak time 10s, 60min is dried in the environment of temperature 50 C, vacuum 100-110Pa.Will place
The test-paper managed is sealed in the drier for being put into and filling drier, must not be by direct sunlight.
Embodiment 7
PP synthetic papers are cut into the 7cm × 15cm rectangle scraps of paper as substrate by the use of paper-cutter, by No. 1-6 point of the scraps of paper that develop the color
1cm × 15cm strip is not cut to and is affixed on substrate according to this, turns into test-paper；It is with paper cutter that the test-paper binded is uniform
0.55cm × 7cm test strips are cut into, is sealed in 4-20 DEG C of dry environment and stores, must not be by direct sunlight.
Detect embodiment
Embodiment 8
5 parts of the Drinking Water Samples from supermarket are purchased, using the colour developing panel region for submerging test paper as standard, are taken immediately after submergence
Go out, colour-development sheet is horizontal positioned upward, it can be quantitatively judged after 3min, number corresponding with colorimetric card color identical color range
Value is the detected value of this sample, as the color of test paper takes both medians between two color ranges.Measure 5 portions of drinking water
6 mercury, cadmium, lead, copper, chromium, nickel residual quantity of heavy metal are 0mg/L in sample, are qualified samples.
Embodiment 9
Above-mentioned 5 parts of Drinking Water Samples are subjected to mark-on experiment, add 6 kinds of mercury, cadmium, lead, copper, chromium, nickel huge sum of moneys in the sample
The standard substance of category, concentration are 20mg/L.Using the colour developing panel region for submerging test paper as standard, taken out immediately after submergence, will be aobvious
Color chips is horizontal positioned upward, can be quantitatively judged after 3min, and numerical value corresponding with colorimetric card color identical color range is
The detected value of this sample, as the color of test paper takes both medians between two color ranges.Measure in 5 parts of Drinking Water Samples
6 mercury, cadmium, lead, copper, chromium, nickel residual quantity of heavy metal are 20mg/L, consistent with the standard substance concentration added.
In addition, the national standard method GB/T 5750 according to heavy metal analysis in China's water quality《Drinking water standard is examined
Proved recipe method》AAS verifies that specific standards are as follows to above-mentioned 5 parts drinking-water samples：Mercury uses GB/T 5750《Life
The drinking water standard method of inspection》In 8.3 dithizone spectrophotometries；Cadmium uses GB/T 5750《Drinking water standard inspection party
Method》In 9.3 dithizone spectrophotometries；Lead uses GB/T 5750《The drinking water standard method of inspection》In 11.3 dithizones
AAS；Copper uses GB/T 5750《The drinking water standard method of inspection》In 4.3 sodium diethyldithiocarbamates
AAS；Chromium uses GB/T 5750《The drinking water standard method of inspection》In 10.1 diphenylcarbazide spectrophotometrics
Method；Nickel uses GB11910-1989《Dimethylglyoxime AAS in water quality nickel-silicon nitride》.The examination of testing result and the present invention
Paper result is consistent, it was demonstrated that the practicality and accuracy of the present invention.
Claims (1)
- A kind of 1. 61 test paper of conjunction for heavy-metal residual quick detection, it is characterised in that：By paper substrate and 6 pieces of colour developing scraps of paper groups Into described paper substrate is fixedly connected with the described 6 pieces colour developing scraps of paper；6 pieces of described colour developing scraps of paper, including No. 1 scraps of paper, No. 2 scraps of paper, No. 3 scraps of paper, No. 4 scraps of paper, No. 5 scraps of paper, No. 6 scraps of paper, point Mercury, cadmium, lead, copper, chromium, the heavy metal species of nickel 6 Yong Yu not detected；No. 1 described scraps of paper：(1) the prior immersion for passing through reaction solution 1, soak time 10-20s, in 50-60 DEG C of temperature, very 30-40min is dried in the environment of reciprocal of duty cycle 100-110 Pa；(2) solvent of reaction solution 1 is 80-120ml hot ethanols, and solute is 0.8-1.2g diphenylcarbazides, 5-10g polyvinylpyrrolidones, 20-30ml 10% triton x-100, ultrasonic dissolution, adjust Save pH8.5-9.5；No. 2 described scraps of paper：(1) the prior immersion for passing through reaction solution 2, soak time 10-20s, in 50-60 DEG C of temperature, very 30-40min is dried in the environment of reciprocal of duty cycle 100-110 Pa；(2) solvent of reaction solution 2 is 80-120ml ethanol, solute 0.3- 0.5g sodium hydroxides, 5-10g polyvinylpyrrolidones, 0.1-0.3g cadions, 20-30ml 10% triton x-100, ultrasound Dissolving, adjust pH6.5-7.5；No. 3 described scraps of paper：(1) the prior immersion for passing through reaction solution 3, soak time 10-20s, in 50-60 DEG C of temperature, very 30-40min is dried in the environment of reciprocal of duty cycle 100-110 Pa；(2) solvent of reaction solution 3 is 80-120ml ultra-pure waters, and solute is The bad hematic acid sodium of 0.3-0.5g rhodizonic acids, 5-10g polyvinylpyrrolidones, 3-5g, 20-30ml 5% triton x-100, Ultrasonic dissolution, adjust pH1.5-2.5；No. 4 described scraps of paper：(1) the prior immersion for passing through reaction solution 4, soak time 10-20s, in 50-60 DEG C of temperature, very 30-40min is dried in the environment of reciprocal of duty cycle 100-110 Pa；(2) solvent of reaction solution 4 is 80-120ml ultra-pure waters, and solute is 0.1-0.3g DDTCs, 5-10g polyvinylpyrrolidones, 20-30ml 5% triton x-100, ultrasonic dissolution, adjust pH 6.5-7.5；No. 5 described scraps of paper：(1) in advance pass through reaction solution 5A immersion, soak time 10-20s, in 50-60 DEG C of temperature, 30-40min is dried in the environment of vacuum 100-110Pa；Again pass through reaction solution 5B immersion, soak time 10-20s, in 50-60min is dried in the environment of 50-60 DEG C of temperature, vacuum 100-110Pa；(2) reaction solution 5A solvent surpasses for 80-120ml Pure water, solute are 0.07-0.15g cetyl trimethylammonium bromides, 9-11g citric acids, ultrasonic dissolution, adjust pH 6.5- 7.5；(3) reaction solution 5B solvent is 80-120ml hot ethanols, and solute is 1-3g diphenylcarbazides, 5-10g polyvinyl pyrroles Alkanone, ultrasonic dissolution, regulation pH 6.5-7.5；No. 6 described scraps of paper：(1) in advance pass through reaction solution 6A immersion, soak time 10-20s, in 30-40 DEG C of temperature, 50-60min is dried in the environment of vacuum 100-110Pa；Again pass through reaction solution 6B immersion, soak time 10-20s, in 50-60min is dried in the environment of 30-40 DEG C of temperature, vacuum 100-110Pa；(2) reaction solution 6A solvent is 80-120ml Ultra-pure water, solute are 2.5-3.5g sodium hydroxides, 1.0-1.5g ammonium persulfates, ultrasonic dissolution, adjust pH 6.5-7.5；(3) it is anti- The solvent for answering liquid 6B is 80-120ml hot ethanols, and solute is 1-3g dimethylglyoximes, 5-10g polyvinylpyrrolidones, ultrasonic dissolution, Adjust pH6.5-7.5.
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| CN105738360A (en) * | 2016-04-25 | 2016-07-06 | 北京言必信科技有限公司 | Fast detecting test paper for mercury ions |
| CN107202788B (en) * | 2017-07-11 | 2018-12-11 | 海南职业技术学院 | Chinese medicine quality is quickly defined the level test paper and preparation method thereof |
| CN108844951B (en) * | 2018-06-28 | 2021-07-13 | 中国农业大学 | Mercury ion detection product and method and smartphone imaging analysis system |
| CN113155758A (en) * | 2021-03-03 | 2021-07-23 | 贵阳学通仪器仪表有限公司 | Automatic high-precision online heavy metal detector for boiler and manufacturing method thereof |
| CN114544607A (en) * | 2022-01-13 | 2022-05-27 | 广东省农业科学院农业质量标准与监测技术研究所 | Rapid screening method for nickel hyper-enriched plants |
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