CN104374722A - Method for analyzing lead - Google Patents
Method for analyzing lead Download PDFInfo
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- CN104374722A CN104374722A CN201410629536.XA CN201410629536A CN104374722A CN 104374722 A CN104374722 A CN 104374722A CN 201410629536 A CN201410629536 A CN 201410629536A CN 104374722 A CN104374722 A CN 104374722A
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Abstract
The invention discloses a method for analyzing lead. According to the method, a porphyrin color-developing agent is adopted to complex lead ions in a water body to form a colored complex under a certain condition, interference of other substances in a sample can be eliminated by adding different masking agents so as to obtain a good testing. The method can be used for solving the problem of secondary pollution on the environment caused by complicated operation, time consumption and conventional testing methods in a lead analyzing process, has the advantages of high accuracy, strong interference resistance, low cost and the like, and can be used for quickly analyzing lead in a water sample.
Description
Technical field
The present invention relates to plumbous detection field, particularly relate to a kind of analytical approach of lead.
Background technology
Lead in environment and compound thereof mainly enter human body from alimentary canal and respiratory tract, flow to whole body with blood circulation.Saturnism can the thyroid function of coup injury humans and animals, reduces the ability of thyroid uptake iodine and plasma protein-bound iodine, reduces the secretion of pituitrin and adrenocortical function, also can damage reproduction cell and reduce sexual function.At present, mensuration plumbous in water quality, measure by atomic absorption method, atomic fluorescence method, inductively coupled plasma-mass spectroscopy, anodic stripping voltammetry/polarography etc. mostly, although these analytical approach accuracy are higher, good stability, but high to the requirement of instrument and operation, cost intensive, and can not fast-field evaluation be realized.
Based on above defect, testing staff has found spectrophotometric method, and this method equipment is simple, method reliable, and is easy to realize on-line monitoring, therefore becomes conventional analytical approach.Be mainly dithizone method in existing spectrophotometric method, its method is national method standard.But the method operate in analytic process more loaded down with trivial details, reagent be difficult to buy, test after waste liquid be difficult to process, environmental pollution is larger.Main manifestations is: dithizone method needs to adopt potassium cyanide as screening agent in analytic process, and potassium cyanide belongs to poisonous reagent, have very large harm to the health of operating personnel in analytic process, and when adopting other material as screening agent, its screening ability can not reach requirement; In addition, dithizone method needs to adopt methenyl choloride to extract in analytic process, and methenyl choloride belongs to pole extractant not environmentally, and environmental pollution is very large.Therefore, exist in the process of existing Spectrophotometric Determination of Lead reagent contamination large, easily to environment cause secondary pollution, complex operation, the content being not suitable for Fast Measurement lead, amount of reagent large, analyze the problems such as cost is higher.
Summary of the invention
In order to solve the technical matters existed in background technology, the present invention proposes a kind of analytical approach of lead, solving complex operation in analytic process, apparatus expensive, can not quick and precisely detect and problem that environmental pollution is serious.In addition, another one advantage of the present invention is, test sample accurately, stable and antijamming capability is strong.
The present invention proposes a kind of analytical approach of lead, comprise the following steps:
The first step, gets a certain amount of lead solution as testing sample;
Second step, adds a certain amount of screening agent, regulator solution and developer, mixes in described testing sample;
3rd step, carries out photometric measurement to the solution after mixing in second step, then calculates concentration plumbous in described testing sample according to the signal value measured.
Further, described analytical approach heats the mixed solution obtained, then cools after also comprising the steps: to add screening agent, regulator solution, developer in described testing sample.
Further, the maximum temperature of heating is 80 DEG C-130 DEG C.
Further, the heat time is 1-20 minute.
Further, cooled solution temperature is less than 55 DEG C.
Further, described analytical approach also adds a certain amount of sensitizer after also comprising the steps: solution to be mixed cooling in mixed solution.
Further, described sensitizer is one or more in Qu Latong-100, oxine, Qu Latong-114, Qu Latong-80.
Further, described screening agent is one or several in anhydrous sodium acetate, tartrate, ascorbic acid, phenanthroline, oxalic acid, thiocarbamide.
Further, described regulator solution is one or several mixing in anhydrous sodium acetate, potassium hydroxide, NaOH, ammoniacal liquor.
Further, after adding regulator solution, the pH value of mixed solution is between 7.5-10.
Further, before adding described developer, need by developer solution in organic solvent.
Further, described organic solvent is at least one in alcohol, normal hexane, DMF, sherwood oil.
The analytical approach of a kind of lead provided by the invention, compared with prior art, owing to adopting the porphyrin organism of organic solvent dissolution as developer, sensitizer and screening agent go interference effect under and regulator solution pH value regulating action under, make lead and porphyrin can generate stable complex compound fast, the Stability of Metal Complexes generated in this solution preparation process is very strong, antijamming capability is strong, this complex compound has characteristic absorption peak under certain wavelength, lead concentration direct proportionality in the peak height of this absorption peak and peak area and testing sample, therefore, concentration plumbous in testing sample can be calculated according to the plumbous characteristic absorption peak generated with organism porphyrin.In the method, do not need to use poisonous solution or extract, and simple to operate, and do not need the equipment of Price-dependent costliness, stable complex compound is conducive to quick and precisely detecting and on-line checkingi; In addition, in the method, reagent dosage is few, and reagent cost is low.
Accompanying drawing explanation
Fig. 1 is lead concentration in the specific embodiment of the invention and the linear figure of absorbance.
Embodiment
The specific embodiment of the invention provides a kind of analytical approach of lead, specifically comprises the following steps:
First, getting a certain amount of dibromo hydroxy-porphyrin is dissolved in DMF solution, stir and mix, as stand-by developer, developer has characteristic absorption peak in visible wavelength region, and in course of reaction, developer and lead ion form complex compound.
Then, get the testing sample of many parts of 12ml containing lead at different concentrations, the screening agent that 0.7ml mass ratio is the Phen configuration of 2.53% is added in every part of testing sample, 1.3ml mass ratio is the regulator solution of the NaOH configuration of 4%, the PH of solution is made to maintain between 7.5-10,1.5ml developer is heated to 95 DEG C, heating is stopped after 3min, be cooled to room temperature (25 DEG C), add the sensitizer that 0.82ml configures with the Qu Latong-100 that volume ratio is 5%, shake up standing 3min, in its absorbance of 469nm place test.
Above-mentioned screening agent can be one or several in anhydrous sodium acetate, tartrate, ascorbic acid, phenanthroline, oxalic acid, thiocarbamide, it is phenanthroline in this specific embodiment, the Main Function of the screening agent that the present invention selects in reaction system is shelter the disturbed test of other metallic ion to lead in plumbous test process, to ensure the stability of test result, its ion that can shelter is cadmium, zinc, copper, arsenic, nickel, total chromium etc.; Regulator solution is one or several in strong base-weak acid salt, is NaOH in this specific embodiment, and regulator solution Main Function in whole reaction system is the pH value regulating color development system, provides the complexing environment that best; Sensitizer is one or more in Qu Latong-100, oxine, Qu Latong-114, Qu Latong-80, is Qu Latong-100 in this specific embodiment, and sensitizer Main Function is in the reaction the complex compound of catalyzed coloration agent and lead ion.
It should be noted that, heating is conducive to the formation accelerating complex compound, makes reaction more thorough, the reflection of porphyrin organism and metallic ion needs the time longer, even can not reflect, but can accelerated reaction by heating, and under heating state, 3-5min can complete reaction.Meanwhile, if add some screening agents not only can shelter metallic ion, improve selectivity, reaction also can be made to carry out instantaneously.After adding certain screening agent, room temperature reaction a period of time can normally develop the color without the need to heating
The solution to be measured of above-mentioned different lead concentration records corresponding absorbance, table specific as follows:
| Lead concentration (mg/L) | Absorbance |
| 0 | 0.0002 |
| 0.1 | 0.0699 |
| 0.2 | 0.1470 |
| 0.3 | 0.2174 |
| 0.4 | 0.2838 |
According to the Plotting data one-tenth linear graph as shown in Figure 1 in above table, have good linear relationship between known absorbance and lead concentration, i.e. y=0.714x+0.001, wherein y represents absorbance, x represents lead concentration.Therefore according to analytical approach of the present invention, utilize the linear relationship between lead concentration as shown in Figure 1 and absorbance, as long as measure absorbance, the concentration accurately calculating lead in solution to be measured that just can be simple and quick, therefore must ensure that lead forms complex compound (perfect condition all forms complex compound) as much as possible here, but without the need to the operation of complexity and the equipment of costliness.
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (12)
1. a plumbous analytical approach, is characterized in that, comprises the following steps:
The first step, gets a certain amount of lead solution as testing sample;
Second step, adds a certain amount of screening agent, regulator solution and developer, mixes in described testing sample;
3rd step, carries out photometric measurement to the solution after mixing in second step, then calculates concentration plumbous in described testing sample according to the signal value measured.
2. the analytical approach of lead according to claim 1, is characterized in that, described analytical approach heats the mixed solution obtained, then cools after also comprising the steps: to add screening agent, regulator solution, developer in described testing sample.
3. the analytical approach of lead according to claim 2, is characterized in that, the maximum temperature of heating is 80 DEG C-130 DEG C.
4. the analytical approach of lead according to claim 2, is characterized in that, the heat time is 1-20 minute.
5. the analytical approach of lead according to claim 2, is characterized in that, cooled solution temperature is less than 55 DEG C.
6. the analytical approach of lead according to claim 5, is characterized in that, described analytical approach also adds a certain amount of sensitizer after also comprising the steps: solution to be mixed cooling in mixed solution.
7. the analytical approach of lead according to claim 6, is characterized in that, described sensitizer is one or more in Qu Latong-100, oxine, Qu Latong-114, Qu Latong-80.
8. the analytical approach of lead according to claim 2, is characterized in that, described screening agent is one or several in anhydrous sodium acetate, tartrate, ascorbic acid, phenanthroline, oxalic acid, thiocarbamide.
9. the analytical approach of lead according to claim 2, is characterized in that, described regulator solution is one or several in anhydrous sodium acetate, potassium hydroxide, NaOH, ammoniacal liquor.
10. the analytical approach of lead according to claim 2, is characterized in that: after adding regulator solution, the pH value of mixed solution is between 7.5-10.
The analytical approach of 11. lead according to claim 2, is characterized in that, before adding described developer, and need by developer solution in organic solvent.
The analytical approach of 12. lead according to claim 11, is characterized in that, described organic solvent is at least one in alcohol, normal hexane, DMF, sherwood oil.
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| CN201410629536.XA CN104374722A (en) | 2014-11-11 | 2014-11-11 | Method for analyzing lead |
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| CN201410629536.XA CN104374722A (en) | 2014-11-11 | 2014-11-11 | Method for analyzing lead |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105021558A (en) * | 2015-08-07 | 2015-11-04 | 齐鲁工业大学 | Lead and cadmium determination method for fruit of ficus carica linn. |
| CN113218897A (en) * | 2021-04-25 | 2021-08-06 | 深圳市长协新能源科技有限公司 | Reagent for measuring lead concentration and method for measuring lead concentration |
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| CN103543115A (en) * | 2013-10-31 | 2014-01-29 | 大连大公环境检测有限公司 | Method for detecting concentration of chromium ion in water body |
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| CN103940759A (en) * | 2013-08-06 | 2014-07-23 | 江苏天瑞仪器股份有限公司 | Method for detection of lead ions in water |
| CN103940760A (en) * | 2013-08-06 | 2014-07-23 | 江苏天瑞仪器股份有限公司 | Masking agent solution for reagent pack for detection of lead ions in water |
| CN103940756A (en) * | 2013-08-06 | 2014-07-23 | 江苏天瑞仪器股份有限公司 | Reagent pack for detection of lead ions in water |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103278471A (en) * | 2013-06-14 | 2013-09-04 | 沈阳飞机工业（集团）有限公司 | Method for monitoring COD (chemical oxygen demand) in fluorescent wastewater |
| CN103940759A (en) * | 2013-08-06 | 2014-07-23 | 江苏天瑞仪器股份有限公司 | Method for detection of lead ions in water |
| CN103940760A (en) * | 2013-08-06 | 2014-07-23 | 江苏天瑞仪器股份有限公司 | Masking agent solution for reagent pack for detection of lead ions in water |
| CN103940756A (en) * | 2013-08-06 | 2014-07-23 | 江苏天瑞仪器股份有限公司 | Reagent pack for detection of lead ions in water |
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| CN105021558A (en) * | 2015-08-07 | 2015-11-04 | 齐鲁工业大学 | Lead and cadmium determination method for fruit of ficus carica linn. |
| CN113218897A (en) * | 2021-04-25 | 2021-08-06 | 深圳市长协新能源科技有限公司 | Reagent for measuring lead concentration and method for measuring lead concentration |
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Application publication date: 20150225 |