CN104297240A - Method and device applied to detection of toxic metal ions in water - Google Patents
Method and device applied to detection of toxic metal ions in water Download PDFInfo
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- CN104297240A CN104297240A CN201410577988.8A CN201410577988A CN104297240A CN 104297240 A CN104297240 A CN 104297240A CN 201410577988 A CN201410577988 A CN 201410577988A CN 104297240 A CN104297240 A CN 104297240A
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Abstract
The invention discloses a method and a device applied to detection of toxic metal ions in water. The detection method comprises the following steps: taking 1-(2-pyridylazo)-2-naphthol solution as a color rendering solution, adding the color rendering solution into a to-be-detected water sample and carry outing color rendering reaction, and qualitatively judging whether the toxic metal ions exist in the to-be-detected water sample by judging whether the characteristic red color exists in a reaction system, wherein the toxic metal ions comprise one or more of Cd<2+>, Pb<2+>, Hg<2+>, Mn<2+>, Ti<3+>, V<3+>, Co<2+>, Ni<2+>, Cu<2+> and Zn<2+>. The detection device comprises a colorimetric tube with a plug and a color rendering capsule; the color rendering capsule is arranged in the colorimetric tube with the plug and is filled with the color rendering solution. The detection method and the detection device are capable of quickly detecting toxic metal ions in the water, low in cost and simple and convenient to operate.
Description
Technical field
The invention belongs to chemical field, relate to detection method and the pick-up unit of intoxicating metallic ion in a kind of water, particularly relate to a kind of method for quick and the pick-up unit that are applicable to intoxicating metallic ion in house or field environment Water Under.
Background technology
Water is Source of life, operation under field environment, and in daily life, relevant people is event of poisoning, factory discharges in violation of rules and regulations and causes the poisoning of heavy metal ion often to have report, as thallium salt, mercury salt etc.Therefore, on the basis obtaining water source, guarantee that water security is drinkable particularly important.And often some toxic agent not only strong toxicity, effect is fast, toxic effect lasting, discharge easily cause casualty-producing concentrations afterwards, cause by number of ways poisoning, and be difficult to discover and protect, stable in properties, contamination be lasting.Developed country headed by the U.S., Britain and Germany, successively have developed many generations based on detection techniques such as fluorescence, Fourier transform infrared spectroscopy (FT-IR), GC-MS instrument, electrochemical methods.These technology based on high-end scientific equipment and toxicological data bank, thus have precisely fast, advantage efficiently repeatedly, but have that equipment price is high, volume is very much not portable, testing conditions requirement is high simultaneously, be difficult to show one's capabilities in the wild.For detecting of heavy metal ion in water, existing market has occurred that quality based on electrochemical principle is at the Portable heavy metal detector that can detect contents of many kinds of heavy metal ion of about 0.5kg, but unit price is up to about 100,000 yuan, be difficult to realize carry-on single equipment, spread to family.During due to operation in the wild, the not specialized detection of the complexity that Portable belt is large-scale, and most of practitioner and resident do not possess special knowledge, therefore, need to simplify and even reject complicated loaded down with trivial details sample pretreatment process, the various possible background interference of quick removal, realize effectively detecting and identifying of trace target compound in complex matrices, produce a set of that can carry with, with low cost, that be suitable for intoxicating metallic ion in the water source promoted method for quick and device, there is very important practical value.
Summary of the invention
The technical problem to be solved in the present invention overcomes the deficiencies in the prior art, provide a kind of can the detection method of intoxicating metallic ion and pick-up unit in intoxicating metallic ion, water with low cost, simple to operation in detection water fast.
For solving the problems of the technologies described above, the present invention by the following technical solutions:
The detection method of intoxicating metallic ion in a kind of water, described detection method is for chromophoric solution with 1-(2-pyridylazo)-beta naphthal solution, chromophoric solution is added in water sample to be measured and carry out chromogenic reaction (i.e. complex reaction), according to whether occurring in reaction system that feature redness qualitatively judges whether containing intoxicating metallic ion in water sample to be measured, described intoxicating metallic ion comprises Cd
2+, Pb
2+, Hg
2+, Mn
2+, Ti
3+, V
3+, Co
2+, Ni
2+, Cu
2+, Zn
2+in one or more.
In above-mentioned detection method, preferably, the solvent of described 1-(2-pyridylazo)-beta naphthal solution is ethanol, more preferably absolute ethyl alcohol.
In above-mentioned detection method, preferably, in described 1-(2-pyridylazo)-beta naphthal solution, the mass percent of 1-(2-pyridylazo)-beta naphthal is 1% ~ 6%.
In above-mentioned detection method, preferably, the condition of described chromogenic reaction is: normal temperature, and pH value is 2 ~ 12.
As a total technical conceive, intoxicating metal ion detection device in the water that the present invention also provides a kind of above-mentioned detection method to adopt, described pick-up unit comprises color-comparison tube and colour developing capsule, described colour developing capsule is positioned at described color-comparison tube, and described colour developing capsule is built with chromophoric solution.
In above-mentioned pick-up unit, preferably, the capsule shell of described colour developing capsule is sealed by the dropper head of plastic dropper to form.
In above-mentioned pick-up unit, preferably, described colour developing capsule is prepared by following methods: first adopt plastic dropper to draw chromophoric solution, then plastic dropper is inverted, chromophoric solution is made to flow in the dropper head of plastic dropper, remove dropper body, then hot-seal is added to dropper head, obtain the capsule that develops the color.
In above-mentioned pick-up unit, preferably, the volume of described colour developing capsule is 0.2mL ~ 10mL.
In above-mentioned pick-up unit, preferably, the volume of described color-comparison tube is 5mL ~ 25mL.
Compared with prior art, the invention has the advantages that:
1, the invention discloses the detection method of intoxicating metallic ion in a kind of quick detection water, this detection method with 1-(2-pyridylazo)-beta naphthal solution for chromophoric solution, whether 1-(2-pyridylazo)-beta naphthal (English 1-(2-Pyridylazo)-2-naphthol by name) is organicvisualization reagent, detected in water containing intoxicating metallic ion by chromogenic reaction.Chromogenic reaction mechanism of the present invention be according to developer and underwater gold belong to ion meet time, combined fast and the complex of morphogenesis characters redness by complex reaction, the object of quick detection is reached by visualization, utilize complex reaction to develop the color, phenomenon significantly, have good selectivity and service condition is wide in range.
2, the developer [1-(2-pyridylazo)-beta naphthal] in the present invention can be red with most of intoxicating metallic ion indicating characteristic, and show through great many of experiments, this developer can be used for the Cd fast and effeciently detected in water
2+, Pb
2+, Hg
2+, Mn
2+, Ti
3+, V
3+, Co
2+, Ni
2+, Cu
2+, Zn
2+deng metallic ion.This developer is only red to the complexing of metal ion reaction and display feature of intoxicating, and the Ca in the water sample larger with usual hardness
2+, Mg
2+the feature that ion does not show complex reaction is red.
3, [1-(the 2-pyridylazo)-beta naphthal] solution in the present invention can select ethanol (preferred absolute ethyl alcohol) as solvent, ethanol is the organic reagent of a kind of dissolving cheap and easy to get [1-(2-pyridylazo)-beta naphthal] part, can infinitely dissolve each other with water sample to be measured again, and alcohol solvent itself is a kind of nontoxic environment-friendly type solvent, after being prepared into chromogenic reagent solution with part, its physicochemical property are stablized and are easy to long-time storage.
When 4, detecting intoxicating metallic ion in water sample, only need at normal temperatures, can in the broad range that pH value is 2-12, do not need to do special processing, direct by the ethanolic solution of [1-(2-pyridylazo)-beta naphthal] and water sample to be detected mixing, as water sample is shown in red, survey water sample and be not suitable for drinking, thus reach quick detection object.
5, pick-up unit of the present invention is made up of color-comparison tube and colour developing capsule two parts, and creatively [1-(2-pyridylazo)-beta naphthal] solution is sealed in colour developing capsule, can make a distinction with feature redness intoxicating metallic ion, there is accurate detection effect, compensate for that existing chemical detection device involves great expense, the excessive drawback that can not carry with of equipment.Pick-up unit of the present invention is cheap, and the price of set of device is less than 50 yuan, and quality is less than 0.1kg, and volume is little, is applicable to carrying with, and simple to operation, can be used for the Rapid Detection of intoxicating ion in domestic water or wild exterior-applied liquid medicine.
6, the reaction vessel when packaging carrying device of pick-up unit of the present invention using color-comparison tube as developer and water sample detection, this design ensure that pick-up unit can be carried with, be applicable in house or outdoor life environment, detect fast such as whether intoxicating metallic ion in the water sources such as well water, natural water, pond water exists or exceed standard.
Accompanying drawing explanation
Fig. 1 is the chemical structural drawing of developer 1-in the present invention (2-pyridylazo)-beta naphthal.
Fig. 2 is the structural representation of intoxicating metal ion detection device in the water of the embodiment of the present invention 1.
Fig. 3 is the Making programme schematic diagram of pick-up unit in the embodiment of the present invention 1.
Fig. 4 is the operating process schematic diagram utilizing pick-up unit to detect intoxicating metallic ion in water in the embodiment of the present invention 1.
Marginal data:
1, color-comparison tube; 2, develop the color capsule; 3, plastic dropper; 4, chromophoric solution; 5, dropper head; 6, water sample to be measured; 7, in yellow solution system; 8, the solution system taken on a red color.
Embodiment
Below in conjunction with Figure of description and concrete preferred embodiment, the invention will be further described, but protection domain not thereby limiting the invention.
Embodiment 1:
The detection method of intoxicating metallic ion in a kind of water of the present invention, this detection method is for chromophoric solution with 1-(2-pyridylazo)-beta naphthal solution, chromophoric solution is added in water sample to be measured and carries out chromogenic reaction, according to whether occurring in reaction system that whether feature redness qualitatively judges in water sample to be measured containing intoxicating metallic ion, if occur in reaction system, feature is red, then contain intoxicating metallic ion in water sample to be measured, detectable intoxicating metallic ion comprises Cd
2+, Pb
2+, Hg
2+, Mn
2+, Ti
3+, V
3+, Co
2+, Ni
2+, Cu
2+, Zn
2+deng.
In the present embodiment, 1-(2-pyridylazo)-beta naphthal is a kind of organicvisualization reagent, its chemical structural formula as shown in Figure 1, be a kind of commercially be slightly soluble in the orange red powder that water is soluble in organic solvent.The solvent of 1-(2-pyridylazo)-beta naphthal solution is ethanol, more preferably absolute ethyl alcohol.In 1-(2-pyridylazo)-beta naphthal solution, the mass percent of 1-(2-pyridylazo)-beta naphthal is 1% ~ 6%.Chromogenic reaction can be carried out at normal temperatures, and pH value is 2 ~ 12.
A kind of pick-up unit of detection method employing of above-mentioned the present embodiment, as shown in Figure 2, this pick-up unit comprises color-comparison tube 1 and several colour developing capsules 2, colour developing capsule 2 is positioned at color-comparison tube 1, is sealed with chromophoric solution (i.e. 1-(2-pyridylazo)-beta naphthal solution) in colour developing capsule 2.
The color-comparison tube 1 of this pick-up unit both can be used as the packaging carrying device of colour developing capsule 2, and also can be used as reaction vessel during water sample detection, this design ensure that pick-up unit can be carried with.The volume of color-comparison tube 1 is usually in 5mL ~ 25mL scope.
The colour developing capsule packaging of this pick-up unit has two kinds of sources substantially: one is the dropper head (this is preferred) deriving from common plastics dropper, or by make close with dropper head shapes of other materials such as glass or container that volume is close; Two is the capsule shells buied from the market, and volume is in 0.2mL ~ 10mL scope.
The manufacturing process of this pick-up unit is as shown in Figure 3: be first dissolved in by developer in solvent (preferred absolute ethyl alcohol) and be mixed with chromophoric solution 4, then chromophoric solution 4 (preferred 1mL) is drawn with plastic dropper 3, plastic dropper 3 is inverted, chromophoric solution 4 is made to flow in the dropper head 5 of plastic dropper 3, remove dropper after one's death, hot-seal is added to dropper head 5, make colour developing capsule 2, finally the colour developing capsule 2 of good seal is placed in color-comparison tube 1 (preferred 10mL), build plug, namely obtain pick-up unit.
This pick-up unit detects the operating process of intoxicating metallic ion in water as shown in Figure 4: the color-comparison tube 1 in pick-up unit is chromogenic reaction room, is also the carrier of colour developing capsule 2.In use, open color-comparison tube 1, pour out all colour developing capsules 2, get wherein 1 colour developing capsule, cut off sealing, poured into by chromophoric solution in color-comparison tube 1, chromophoric solution is in yellow.Water sample 6 to be measured is added in color-comparison tube 1, builds colorimetric pipe close, after shaking up, observations.If the solution after shaking up is still in yellow, namely in yellow solution system 7, then water source can be drunk; If the solution after shaking up presents redness (solution system 8 namely taken on a red color) or occurs red precipitate, then contain intoxicating metallic ion in water source, be not suitable for drinking.
The pick-up unit Costco Wholesale of the present embodiment is within 50 yuan, can be used as carry-on equipment, be applicable in life at home or field environment, judge whether whether exceed standard containing intoxicating metallic ion or intoxicating metallic ion in water (as well water, natural water, pond water etc.), judge that whether water source is suitable for drinking fast.
Embodiment 2:
Adopt the detection method in embodiment 1 and pick-up unit, test detected to the intoxicating metallic ion of known actual concentrations:
Toxicological parameters refers to that smaller dose enters the index that body just can disturb the levels of toxic substances of normal biochemical process or physiological function.According to " GB5749-2006 drinking water sanitary standard ", the toxicological parameters of several heavy metal ion involved in the present invention is as shown in table 1.
In the ethanolic solution of 1-(2-the pyridylazo)-beta naphthal of the present embodiment, the mass percent of 1-(2-pyridylazo)-beta naphthal is 6%.Chromogenic reaction is carried out at normal temperatures, pH value 2 ~ 12 scope.The capsule shell of colour developing capsule 2 is sealed by the dropper head 5 of plastic dropper to form, and the volume of developer 2 capsule is 1mL (filling chromophoric solution, lower same), and the volume of color-comparison tube 1 is 10mL (filling standard solution, lower same).
In the present embodiment, with the existing Cd in laboratory
2+, Pb
2+, Hg
2+and Mn
2+for research object, be 1.0 × 10 with volumetric flask preparation actual concentrations
-2, 1.0 × 10
-3, 1.0 × 10
-4with 1.0 × 10
-5the series standard solution of mol/L, for Hg
2+intoxicating concentration is lower, adds that to have surveyed a concentration be 5.0 × 10
-6the sample of mol/L.According to the operating process shown in Fig. 4, chromophoric solution is mixed with standard solution and shakes up, observe phenomena, if mixed solution presents macroscopic redness, then for detecting; If without obviously red, then for detecting, result is as shown in table 1.Test and record the least concentration that often kind of ion detects, record in table 2.As shown in Table 2, for the existing Cd in laboratory
2+, Pb
2+, Hg
2+and Mn
2+ion, 4 kinds of ion detection results show: the least concentration (i.e. concentrations) of 4 kinds of ions of experiment is all less than or equal to toxicological parameters.For these 4 kinds of ions of inspection, detection method sensitivity of the present invention is very high, feasible.From reaction principle, the method also extends to Ti
3+, V
3+, Co
2+, Ni
2+, Cu
2+, Zn
2+deng trace and effectively the detecting of trace metal ion.
Table 1 detects the test findings of intoxicating metallic ion standard sample
Table 2 detects toxicological parameters and the concentrations of object ion
| Ion title | Toxicological parameters/(mg/mL) | Concentrations/(mg/mL) |
| Cd 2+ | 0.005 | 0.00112 |
| Pb 2+ | 0.01 | 0.00207 |
| Hg 2+ | 0.001 | 0.00100 |
| Mn 2+ | 0.1 | 0.0055 |
Embodiment 3:
Adopt the detection method in embodiment 1 and pick-up unit, the Rapid Detection of intoxicating metallic ion in environmental water systems tested:
At Changsha periphery, the water sample under varying environment condition is have collected with the mineral water bottle of dried and clean, mainly contain: Liuyang river, river, Liuyang factory blow-off pipe saliva, natural pond water, white sand well water, the foot of a hill or mountain, high mountain mountain spring water, forest stream and the moon lake water, totally 7 kinds of water samples.According to the operating process shown in Fig. 4, chromophoric solution is mixed with natural water-like and shakes up, observe phenomena, if present obvious visible redness, then for detecting; If without obviously red, then for detecting.The situation that the detects result of often kind of water sample is as shown in table 3, and all environmental water samples all without obviously red, show that the concentration of intoxicating metallic ion contained by 7 water sources that Changsha periphery is got is very low, can not cause toxicological effect.
In the ethanolic solution of 1-(2-the pyridylazo)-beta naphthal of the present embodiment, the mass percent of 1-(2-pyridylazo)-beta naphthal is 6%.Chromogenic reaction is carried out at normal temperatures, pH value 2 ~ 12 scope.The capsule shell of colour developing capsule 2 is sealed by the dropper head 5 of plastic dropper to form, and the volume of colour developing capsule 2 is 1mL, and the volume of color-comparison tube 1 is 10mL.
Table 3 detects the test findings of field environment water sample
| Water sample is originated | Liuyang river | Blow-off pipe saliva | Pond water | White sand well water | The foot of a hill or mountain, high mountain mountain spring water | Forest stream | Month lake water |
| Solution colour | Yellow | Yellow | Yellow | Yellow | Yellow | Yellow | Yellow |
| Detect situation | No | No | No | No | No | No | No |
Embodiment 4:
Adopt the detection method in embodiment 1 and pick-up unit, the Rapid Detection specific test to intoxicating metallic ion in water source:
Water sample under difficult environmental conditions, except the intoxicating metallic ion that may contain, leading ion impurity derives from the Ca causing the water hardness to increase
2+and Mg
2+.The water hardness that China represents with calcium carbonate concentration is roughly divided into: 0 ~ 75mg/L dead-soft water; 75 ~ 150mg/L soft water; Hard water in 150 ~ 300mg/L; 300 ~ 450mg/L hard water; 450 ~ 700mg/L high hardness; 700 ~ 1000mg/L superelevation hard water; > 1000mg/L ultrahard water.
In the present embodiment, respectively with Ca
2+and Mg
2+for research object, prepare water sample with volumetric flask.Preparation CaCO
3concentration is respectively the serial hard water of 100mg/L, 200mg/L, 500mg/L and 1000mg/L.Prepare magnesium chloride series hard water again, represent the hardness of water sample with calcium carbonate concentration, be converted to calcium carbonate concentration by density of magnesium chloride and be respectively 100mg/L, 200mg/L, 500mg/L and 1000mg/L.According to the operating process shown in Fig. 4, chromophoric solution is mixed with standard solution and shakes up, observe phenomena.Experimental result is as shown in table 4, the Ca that the water of various hardness is corresponding
2+and Mg
2+the feature that ion does not all show complex reaction is red, shows thus, and detection method of the present invention only has specificity to detecting of intoxicating metallic ion, not by Ca
2+and Mg
2+impact.
Table 4 detects the specific test result of intoxicating metallic ion in water
In the ethanolic solution of 1-(2-the pyridylazo)-beta naphthal of the present embodiment, the mass percent of 1-(2-pyridylazo)-beta naphthal is 6%.Chromogenic reaction is carried out at normal temperatures, pH value 2 ~ 12 scope.The capsule shell of colour developing capsule 2 is sealed by the dropper head 5 of plastic dropper to form, and the volume of colour developing capsule 2 is 1mL, and the volume of color-comparison tube 1 is 10mL.
The above is only preferred embodiment of the present invention, not does any pro forma restriction to the present invention.Although the present invention discloses as above with preferred embodiment, but and be not used to limit the present invention.Any those of ordinary skill in the art, when not departing from Spirit Essence of the present invention and technical scheme, the Method and Technology content of above-mentioned announcement all can be utilized to make many possible variations and modification to technical solution of the present invention, or be revised as the Equivalent embodiments of equivalent variations.Therefore, every content not departing from technical solution of the present invention, according to technical spirit of the present invention to any simple modification made for any of the above embodiments, equivalent replacement, equivalence change and modification, all still belongs in the scope of technical solution of the present invention protection.
Claims (9)
1. the detection method of intoxicating metallic ion in a water, it is characterized in that, described detection method is for chromophoric solution with 1-(2-pyridylazo)-beta naphthal solution, chromophoric solution is added in water sample to be measured and carries out chromogenic reaction, according to whether occurring in reaction system that feature redness qualitatively judges whether containing intoxicating metallic ion in water sample to be measured, described intoxicating metallic ion comprises Cd
2+, Pb
2+, Hg
2+, Mn
2+, Ti
3+, V
3+, Co
2+, Ni
2+, Cu
2+, Zn
2+in one or more.
2. detection method according to claim 1, is characterized in that, the solvent of described 1-(2-pyridylazo)-beta naphthal solution is ethanol.
3. detection method according to claim 1 and 2, is characterized in that, in described 1-(2-pyridylazo)-beta naphthal solution, the mass percent of 1-(2-pyridylazo)-beta naphthal is 1% ~ 6%.
4. detection method according to claim 1 and 2, is characterized in that, the condition of described chromogenic reaction is: normal temperature, and pH value is 2 ~ 12.
5. intoxicating metal ion detection device in the water that adopts of a detection method according to any one of Claims 1 to 4, it is characterized in that, described pick-up unit comprises color-comparison tube and colour developing capsule, described colour developing capsule is positioned at described color-comparison tube, and described colour developing capsule is built with chromophoric solution.
6. pick-up unit according to claim 5, is characterized in that, the capsule shell of described colour developing capsule is sealed by the dropper head of plastic dropper to form.
7. the pick-up unit according to claim 5 or 6, it is characterized in that, described colour developing capsule is prepared by following methods: first adopt plastic dropper to draw chromophoric solution, then plastic dropper is inverted, chromophoric solution is made to flow in the dropper head of plastic dropper, remove dropper body, then hot-seal is added to dropper head, obtain the capsule that develops the color.
8. the pick-up unit according to claim 5 or 6, is characterized in that, the volume of described colour developing capsule is 0.2mL ~ 10mL.
9. the pick-up unit according to claim 5 or 6, is characterized in that, the volume of described color-comparison tube is 5mL ~ 25mL.
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|---|---|---|---|
| CN201410577988.8A CN104297240A (en) | 2014-10-24 | 2014-10-24 | Method and device applied to detection of toxic metal ions in water |
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|---|---|---|---|
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Application publication date: 20150121 |
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