CN103728264A - Lead detection method - Google Patents
Lead detection method Download PDFInfo
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- CN103728264A CN103728264A CN201310755143.9A CN201310755143A CN103728264A CN 103728264 A CN103728264 A CN 103728264A CN 201310755143 A CN201310755143 A CN 201310755143A CN 103728264 A CN103728264 A CN 103728264A
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Abstract
The invention relates to a lead detection method, which comprises the following steps: sequentially adding a reducing agent, a masking agent and a color developing agent into a sample; carrying out photometric determination, wherein the concentration of lead in the sample can be obtained by determining the absorbance A. The lead detection method has the advantages of being free from a highly-toxic reagent, good in safety, strong in anti-interference capability, high in accuracy and the like.
Description
Technical field
The present invention relates to a kind of plumbous detection method.
Background technology
Lead and compound thereof are a kind of noxious materials with the property accumulated, polyaffinity, can with external a series of protein, enzyme and amino acid in functional group's (sulfydryl) combination, the biochemistry of interference body and physiological activity, so cause poisoning, particularly serious to hematopoiesis, hepatic and/or renal infringement.Lead in nature water comes from the waste water of the industry discharges such as mining, metallurgy, plating, battery and chemical industry mostly.The public's sight line is focused on to lead contamination detection and early warning to the group lead contamination poisoning explosively that taken place frequently since 2006.Therefore, plumbous detection, particularly detects online, has become one of monitoring project of greatest concern.
At present, detect plumbous method more, have GFAAS (graphite furnace atomic absorption spectrometry) (GFAAS), flame atomic absorption spectrometry (AAS), Electrothermal Atomic Absorption spectroscopic methodology (ETAAS), inductively coupled plasma mass spectrometry method (ICP-MS), hydride generation-inductively coupled plasma-atomic emission spectrometry (HG-ICP-AES), anodic stripping voltammetry/polarography, spectrophotometric method etc.Wherein, spectrophotometric method with low cost with it, be easy to promote the use of and become and detect plumbous the most frequently used analyzing detecting method.
Dithizone spectrophotometry is that micro lead detects the most frequently used analytical approach, this analytical approach need to be used potassium cyanide impact on measurement with removal interfering ion as screening agent, and potassium cyanide is poisonous reagent, can bring infringement to operating personnel healthy, can cause secondary pollution to environment simultaneously.Now also there is report not adopt the plumbous detection method of potassium cyanide as screening agent, as used thiocarbamide, NH
4sCN, sodium potassium tartrate tetrahydrate etc. be as screening agent, but the use of these screening agents only can remove as Cu, Ni, the isoionic interference of Ca, Mg, and other cannot be removed as Cd, Zn, the isoionic interference of Cr, the poor anti jamming capability of this kind of plumbous detection method.In addition, dithizone spectrophotometry need to an organic solvent extract, and complex operation, reagent dosage are large.
To sum up, all there is poor anti jamming capability, complex operation and be mostly applicable to the shortcomings such as plumbous fast qualitative detection in the existing plumbous photometry that detects, can not meet people's needs now and accurately know in water and even the demand of the accurate content of the aspect lead such as food, blood, especially to detect application aspect gap very large online.So, research and develop the plumbous detection method that a kind of reagent safety is good, antijamming capability is strong, accuracy is high, be particularly useful for the online method detecting and seem very urgently and needs.
Summary of the invention
In order to solve above-mentioned deficiency of the prior art, the invention provides a kind of, plumbous detection method that antijamming capability strong, that accuracy high good without poisonous reagent, security.
For achieving the above object, the present invention adopts following technical scheme:
A kind of plumbous detection method, comprises the steps:
In sample, add successively reductive agent, screening agent, developer;
Carry out photometering, wherein, by measuring absorbance A and then obtaining concentration plumbous in sample.
As preferably, described reductive agent is aminated compounds.
As preferably, described reductive agent comprises at least one in ethylenediamine, poly-ethylene polyamine, oxammonium hydrochloride;
As preferably, described screening agent is hydroxylamine compound.
As preferably, described screening agent comprises at least one in triethanolamine, quinoline phenanthroline.
Further, after described screening agent adds, developer adds described buffering agent before adding.
Further, after adding, developer adds buffering agent.
As preferably, before developer adds and the volume ratio of the buffering agent adding be afterwards less than 4: 1.
As preferably, described buffering agent is NaOH-sodium tetraborate or potassium pyrophosphate-anhydrous sodium acetate or ammoniacal liquor-ammonium chloride.
Further, described absorbance A is the absorbance measuring after developer adds.
Further, after described screening agent adds, the absorbance that measures before adding of developer is A1, the absorbance measuring after described developer adds is A2, described absorbance A=A2-A1.
Further, before adding, described reductive agent adds oxidizing acid in sample, for measuring the plumbous total amount of sample.
Further, before described reductive agent adds to the plumbous standard substance that adds concentration known in sample.
Further, plumbous standard reserving solution is added in sample, as mark-on sample, measure the lead concentration in mark-on sample, further draw the recovery of standard addition of mark-on sample.
Further, described plumbous detection method is for automatically detecting.
The present invention compared with prior art has following beneficial effect:
1, the reductive agent that the present invention selects and screening agent are all nontoxic reagent, to environment non-secondary pollution, harmless to human body.
2, the technology that redox+complexing that the present invention adopts is sheltered, can significantly strengthen antijamming capability.
3, the present invention adopts and in sample, adds standard substance to improve the method in the linearity of measuring low concentration sample, strengthens the sensitivity of the method.And before and after developer adds, gather absorbance, and further deduct reagent and add the absorbance deviation causing, improve the accuracy of measuring.In addition, after developer adds, add again buffering agent, avoided the measurement inconsistence problems that causes because developer is residual, can effectively guarantee the consistance of the method, improve and automatically detect plumbous reappearance.
4, the present invention is simple to operate, reagent dosage is few, without troublesome operation such as extractions, can be used for automatically detecting lead, detects especially online.
Accompanying drawing explanation
Fig. 1 is typical curve plumbous in embodiment 2;
Fig. 2 is typical curve plumbous in embodiment 3;
Fig. 3 is typical curve plumbous in embodiment 4;
Fig. 4 is typical curve plumbous in embodiment 5;
Fig. 5 is typical curve plumbous in embodiment 6.
Embodiment
A kind of plumbous detection method, comprises the steps:
In sample, add successively reductive agent, screening agent, developer;
Carry out photometering, wherein, by measuring absorbance A and then obtaining concentration plumbous in sample.
Interfering ion in sample first with reductive agent generation redox reaction, then with screening agent generation complex reaction, guarantee that the method can shelter Cu, Zn, Cd, Ni and Cr etc.
Further, described reductive agent is aminated compounds, and described screening agent is hydroxylamine compound.
Preferably, described reductive agent comprises at least one in ethylenediamine, poly-ethylene polyamine, oxammonium hydrochloride; Described screening agent comprises at least one in triethanolamine, quinoline phenanthroline.
Preferably, described reductant concentration scope is [50,300] g/L; Described screening agent concentration range is [10,100] g/L.
The present invention makes sample colour developing under alkaline environment, thus at the pilot process of plumbous detection method, adopt buffering agent to regulate pH value, and buffering agent is alkali lye; As long as can make sample develop the color under alkali condition, the addition sequence of buffering agent is not added to restriction, buffering agent can add in the arbitrary link that adds reductive agent, screening agent, developer.
As preferably, described buffering agent is NaOH-sodium tetraborate or potassium pyrophosphate-anhydrous sodium acetate or ammoniacal liquor-ammonium chloride.
The PH scope of preferred described buffering agent is [9,12].
The reductive agent that the present invention selects and screening agent are all nontoxic reagent, to environment non-secondary pollution, harmless to human body.
Redox+complexing technology of sheltering that the present invention adopts, can significantly strengthen antijamming capability, in addition simple to operate, reagent dosage is few.
Further, after described screening agent adds, developer adds described buffering agent before adding.
Further, except after described screening agent adds, developer adds described buffering agent before adding, also after developer adds, add buffering agent.After described screening agent adds, developer adds buffering agent before adding, and is for suitable pH environment is provided, guarantee masking effect; After developer adds, add again buffering agent, avoided the measurement inconsistence problems that causes because developer is residual, can effectively guarantee the consistance of the method, improve and automatically detect plumbous reappearance, strengthen the method and be applied to the operability of automatic monitoring.
Before described developer adds and the buffering agent adding afterwards can be for alkali lye of the same race, also can be the different alkali lye of planting; If during alkali lye of the same race, concentration can be the same or different.
As preferably, before developer adds and the volume ratio of the buffering agent adding be afterwards less than 4: 1.
Further, described absorbance A is the absorbance measuring after developer adds.
Further, after described screening agent adds, the absorbance that measures before adding of developer is A1, the absorbance measuring after described developer adds is A2, described absorbance A=A2-A1.Measuring absorbance A 1, is the accuracy of measuring actual sample in order to improve the method, and deduction reagent adds the absorbance causing to change.
Further, before described reductive agent adds, to the plumbous standard substance that adds concentration known in sample, object is to improve the linearity of sample between low concentration region, increases the sensitivity of the method.
Further, plumbous standard reserving solution is added in sample, as mark-on sample, measure the lead concentration in mark-on sample, further draw the recovery of standard addition of mark-on sample.
Further, described plumbous detection method detects the lead content in sample in can be used for automatically detecting in good time.
The present invention is simple to operate, reagent dosage is few, without troublesome operation such as extractions, can be used for automatically detecting lead, detects especially online.Further, before described reductive agent adds, in sample, add oxidizing acid, object is in order to clear up water sample, and the lead of being combined with organism is discharged, and then measures total amount plumbous in sample.
As preferably, the concentration range of oxidizing acid is: [1,9] mol/L.
The present embodiment is the application examples of embodiment 1, specific as follows:
In sample, add successively reductive agent, screening agent, buffering agent, developer, described buffering agent is NaOH-sodium tetraborate solution, is called for short sodium tetraborate solution:
Pipette 10mL actual water sample in 50mL color comparison tube, add successively the ethylenediamine of 6mL50g/L, the triethanolamine of 3.5mL10g/L, the sodium tetraborate solution of 12mL pH=9, shake up standing 2min, then add PAR developer 2mL, shake up and be settled to groove with pure water, normal temperature colour developing 5min afterwards;
Carry out photometering, by measuring absorbance A and then obtaining concentration plumbous in sample:
Wherein, at 525nm wavelength place, detect that the absorbance A of the sample after colour developing is completely 0.090.
According to the absorbance of the typical curve between the concentration of the lead solution of having set up and absorbance and testing sample, draw the lead concentration of testing sample:
The corresponding function expression of typical curve of having set up is Y=0.103X+0.076, and related coefficient is 0.994; By the procedural information of actual water sample, be that described absorbance A 0.090 brings above-mentioned expression formula into, the measured value that draws this actual water sample is 0.136mg/L.
Described typical curve can be the curve establishing in advance, can be also on-the-spot foundation; In the process of establishing of described typical curve, the determination step of standard model used is identical with the determination step of testing sample.
The present embodiment typical curve process of establishing is specific as follows:
Pipette the plumbous standard solution of different volumes 0,1,2,4,6,8,10mL5mg/L in 50mL color comparison tube, add successively the ethylenediamine of 6mL50g/L, the triethanolamine of 3.5mL10g/L, the sodium tetraborate solution of 12mL pH=9, shake up standing 2min, add again PAR developer 2mL, shake up and be settled to groove with pure water afterwards, normal temperature colour developing 5min, at 525nm wavelength, its absorbance is detected at place.According to concentration and the absorbance of each lead solution, drawing standard curve, as shown in Figure 1, corresponding function expression is Y=0.103X+0.076, related coefficient is 0.994.
Embodiment 3
A kind of plumbous detection method is different from the plumbous detection method described in embodiment 2:
After described screening agent adds, the absorbance A 1 that measures before adding of developer is 0.003, the absorbance measuring after described developer adds is that A2 is 0.090, described absorbance A=A2-A1=0.087.
Refer to Fig. 2, the corresponding function expression of typical curve of foundation is Y=0.102X+0.073, and related coefficient is 0.994; By described absorbance A, be 0.087 to bring above-mentioned expression formula into, the measured value that draws this actual water sample is 0.137mg/L.
Embodiment 4
A kind of plumbous detection method is different from the plumbous detection method described in embodiment 3: before described reductive agent adds, to the plumbous standard substance that adds concentration known in sample, to strengthen the linearity of the method between low concentration region, to put forward high measurement sensitivity.
If plumbous standard reserving solution is added in sample, as mark-on sample, measure the lead concentration in mark-on sample, further draw the recovery of standard addition of mark-on sample.
As preferably, the concentration range of described plumbous standard substance is [Isosorbide-5-Nitrae] mol/L.
The concentration of the plumbous standard substance that the present embodiment adds is 2mol/L.
Before developer adds and the absorbance measuring be afterwards respectively A1 be 0.003 and A2 be 0.192, described absorbance A=A2-A1=0.189.
Refer to Fig. 3, the corresponding function expression of typical curve of foundation is Y=0.102X+0.175, and related coefficient is 0.997; By described absorbance A, be 0.189 to bring above-mentioned expression formula into, the measured value that draws this actual water sample is 0.137mg/L.
Embodiment 5
A kind of plumbous detection method is different from the plumbous detection method described in embodiment 4:
1, before reductive agent adds, add the dilute nitric acid solution of 2.5mL6mol/L, for clearing up sample, measure total lead ion content.In practical operation, if desired in sample, add front standard substance, plumbous standard substance directly can be added to the acid solution for clearing up sample;
2, except after described screening agent adds, developer adds described buffering agent before adding, also after developer adds, add buffering agent; And before described developer adds and the buffering agent adding be afterwards same concentration alkali lye of the same race, be potassium pyrophosphate-anhydrous acetic acid sodium solution, be called for short anhydrous acetic acid sodium solution.
Specific as follows:
Refer to table 1, ion classification and concentration in plumbous standard substance.Pipette the actual lead ring border standard model (GSBZ50009-88 that contains disturbance ion (table 1) of 4mL, lot number 200928) in 50mL color comparison tube, add successively the dilute nitric acid solution (leaded titer 4mol/L) of 2.5mL6mol/L, the ethylenediamine of 6mL150g/L, the triethanolamine of 3.5mL50g/L, the anhydrous sodium acetate of 9.6mL pH=11, shake up standing 2min, at 525nm wavelength place, detecting its absorbance A1 is 0.002; Add again the anhydrous acetic acid sodium solution of PAR developer 2mL and 2.4mLpH=11, shake up and be settled to groove with pure water afterwards, normal temperature colour developing 5min, at 525nm wavelength place, detecting its absorbance A2 is 0.278, absorbance A=A2-A1=0.276.
Each ion classification and concentration (mg/L) in the plumbous standard substance of table 1
| Ionic species | Concentration |
| Cu | 1.02±0.04 |
| Pb | 1.02±0.04 |
| Zn | 5.05±0.22 |
| Cd | 0.102±0.006 |
| Ni | 0.502±0.022 |
| Cr | 0.503±0.025 |
The process of the mensuration of standard model and then Criterion curve, specific as follows:
Pipette different volumes 0, 1, 2, 4, 6, 8, the plumbous standard solution of 10mL5mg/L is in 50mL color comparison tube, add successively the dilute nitric acid solution (leaded titer 4mol/L) of 2.5mL6mol/L, the ethylenediamine of 6mL150g/L, the triethanolamine of 3.5mL50g/L, the anhydrous acetic acid sodium solution of 9.6mL pH=11, shake up standing 2min, at 525nm wavelength, its absorbance is detected at place, add again the anhydrous acetic acid sodium solution of PAR developer 2mL and 2.4mLpH=11, shake up and be settled to groove with pure water afterwards, normal temperature colour developing 5min, at 525nm wavelength, its absorbance is detected at place.According to concentration and the absorbance of each lead solution, drawing standard curve, as shown in Figure 4, corresponding function expression is Y=0.101X+0.174, related coefficient is 0.999.
By absorbance A, be 0.276 to bring in the typical curve of foundation, the measured value that calculates this environmental sample is 1.011mg/L, accuracy 1.10%.Embodiment 6
Plumbous detection method in embodiment 5 is in the online plumbous application detecting in actual water sample, various reagent add dependence sequential injection system, concrete steps comprise:
A, determination step
A1, reference solution absorbance, the absorbance of reference solution is equivalent to the value at zero point in typical curve, and effect is as blank reference value:
Current-carrying is that pure water (4mL) is directed into reaction detection unit under the driving of syringe pump, then add the dilute nitric acid solution (leaded titer 2mol/L) of 0.30mL9mol/L, 130 ℃ of high-temperature closeds are cleared up 15min and are cooled to room temperature, each reagent adds successively the ethylenediamine of 0.40mL300g/L under the switching of hyperchannel option valve, the triethanolamine of 0.70mL100g/L, the sodium tetraborate solution of 0.90mL pH=12, mix standing 2min, under 525nm light source, gather voltage signal V1, add again the sodium tetraborate solution of PAR developer 0.20mL and 0.30mL pH=12, gather voltage signal V2, the absorbance A of reference solution
reference=lg (V1/V2),
A2, obtain plumbous standard model absorbance Criterion curve, with reference to the acquisition step of reference solution absorbance in steps A 1:
Sample hose is inserted in the plumbous standard solution of 2mg/L, according to the step in A1, automatically gather voltage signal V1 ' and voltage signal V2 ', and the absorbance A of display standard solution
standard solution=lg (V1 '/V2 ').According to the absorbance of reference solution and 2mg/L lead solution, draw the typical curve of concentration and absorbance, as shown in Figure 5, the function expression of typical curve is Y=0.107X+0.075, and coefficient A=0.107 and B=0.075 are stored in instrument microprocessing systems.
A3, obtain actual water sample absorbance, with reference to the acquisition step of reference solution absorbance in steps A 1:
Sample hose is inserted in actual water sample, according to the step in A1, gather voltage signal V1 ' ' and voltage signal V2 ' ', automatically calculate the absorbance A of actual water sample
actual sample=lg (V1 ' '/V2 ' '),
B, calculation procedure:
By the absorbance A of actual sample, be 0.078 to bring in typical curve, the lead concentration that shows this actual water sample is 0.030mg/L.
Described plumbous detection method also comprises recovery of standard addition detecting step C:
Plumbous standard reserving solution is added in testing sample, as mark-on sample, and according to steps A, B, obtain the lead concentration of mark-on sample, further draw the recovery of standard addition of mark-on sample: add the deviation of sample concentration and actual sample concentration after standard solution with respect to the number percent of the concentration of standard solution adding.
Pipette the actual water sample in 100mL steps A, add the plumbous standard reserving solution of 0.5mL200mg/L, shake up rear as mark-on water sample.Sample hose is inserted in mark-on water sample, and according to the step in steps A, instrument gathers voltage signal automatically, and calculates absorbance, further obtains the lead concentration value 0.102mg/L of mark-on water sample, and the recovery of standard addition that calculates this actual water sample is 99%.
Above-mentioned embodiment should not be construed as limiting the scope of the invention.Key of the present invention is: the technology that adopts redox+complexing to shelter, avoided in plumbous testing process, using poisonous screening agent, and efficiently solve the large problem of disturbing.In the situation that not departing from spirit of the present invention, within any type of change that the present invention is made all should fall into protection scope of the present invention.
Claims (10)
1. a plumbous detection method, comprises the steps:
In sample, add successively reductive agent, screening agent and developer;
Carry out photometering, wherein, by measuring absorbance A and then obtaining concentration plumbous in sample.
2. plumbous covering method according to claim 1, is characterized in that: described reductive agent is aminated compounds.
3. plumbous covering method according to claim 2, is characterized in that: described reductive agent comprises at least one in ethylenediamine, poly-ethylene polyamine, oxammonium hydrochloride;
4. plumbous covering method according to claim 1, is characterized in that: described screening agent is hydroxylamine compound.
5. plumbous covering method according to claim 4, is characterized in that: described screening agent comprises at least one in triethanolamine, quinoline phenanthroline.
6. plumbous detection method according to claim 1, is characterized in that: after described screening agent adds, developer adds described buffering agent before adding.
7. plumbous detection method according to claim 6, is characterized in that: after developer adds, add buffering agent.
8. plumbous detection method according to claim 1, is characterized in that: described buffering agent is NaOH-sodium tetraborate or potassium pyrophosphate-anhydrous sodium acetate or ammoniacal liquor-ammonium chloride.
9. plumbous detection method according to claim 1, it is characterized in that: after described screening agent adds, the absorbance that measures before adding of developer is A1, the absorbance measuring after described developer adds is A2, described absorbance A=A2-A1.
10. plumbous detection method according to claim 1, is characterized in that: before described reductive agent adds to the plumbous standard substance that adds concentration known in sample.
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| CN113720833A (en) * | 2021-07-26 | 2021-11-30 | 杭州春来科技有限公司 | Lead detection method and device |
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Application publication date: 20140416 |