CN108490062A - The detection method of phosphorus and its compound in a kind of detection workplace air - Google Patents
The detection method of phosphorus and its compound in a kind of detection workplace air Download PDFInfo
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- CN108490062A CN108490062A CN201810226635.1A CN201810226635A CN108490062A CN 108490062 A CN108490062 A CN 108490062A CN 201810226635 A CN201810226635 A CN 201810226635A CN 108490062 A CN108490062 A CN 108490062A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
Abstract
The invention discloses the detection methods of phosphorus and its compound in a kind of detection air, which is characterized in that the detection method comprises the following steps：（1）Collect the phosphorus and its compound in air；（2）The phosphorus being collected into and compound are cleared up；（4）Ammonium molybdate is added in solution after resolution, ammonium phosphomolybdate is generated, with alkali tune PH to 5 ~ 7；（5）It is detected using composite modified electrode, obtains testing result.Detection method is easy to operate, testing cost is low, accuracy is high, high sensitivity.
Description
Technical field
The present invention relates to phosphorus and its compounds in air detection technical field more particularly to a kind of detection workplace air
Detection method.
Background technology
Phosphorus in workplace has very a variety of, widely applied phosphoric acid in the industries such as manufacture, medicine, printing, metallurgy；Quilt
It is widely used in plating, chemical industry, the phosphorus pentoxide of analytical reagent etc.；It is applied to malathion, the third bromine of pesticide field
Phosphorus, phenothiazide；Hydrogen phosphide etc. applied to tobacco business.
Phosphoric acid steam or mist have irritation effect to eyes, nose, larynx, the upper respiratory tract, and wrongly taking phosphoric acid liquid can cause to dislike
The heart, vomiting, abdominal pain, bloody stool or shock, be in direct contact skin or eyes can cause to burn, Atrophic nasal mucosas, perforation of nasal septum；Agriculture
The phosphorus-containing matter that medicine field uses is the high-toxic organic phosphorus insecticide that can induce delayed neuropathy, can inhibit cholinesterase
Vigor can generate headache, weak, nausea and vomiting, abdominal pain, salivation, hidrosis, eye-blurred, fasciculation even edema with the lung involved after poisoning
The symptoms such as swollen, stupor；The smoke stimulation mucous membrane of phosphorus pentoxide is irritating to the skin and is acted on calcination.To various workplaces
In phosphorus and its compound be measured, all have great importance to the protection of people and environment.
However the prior art does not have the technology being detected to total phosphorus content in air, and the sensitivity detected is inadequate,
The requirement being detected to total phosphorus in air is not achieved.
Based on this, a kind of method for adapting to a variety of workplaces, detecting a variety of phosphorus compounds in air is provided, detection is improved
The sensitivity of method is urgently to be resolved hurrily.
Invention content
For the skill for solving inadequate to phosphorus in air and its compound test adaptation of methods and sensitivity in the prior art
Art problem provides the detection method of phosphorus and its compound in a kind of detection workplace air, reach can detect it is total in air
The content of phosphorus, and there is very high sensitivity, it can be adapted for the technique effect of the measurement of total phosphorus content in air.
To achieve the above object, it is achieved by following technical solution：
The detection method of phosphorus and its compound in a kind of detection air, the detection method comprise the following steps：
（1）Collect the phosphorus and its compound in air；
（2）The phosphorus being collected into and compound are cleared up；
（4）Ammonium molybdate is added in solution after resolution, ammonium phosphomolybdate is generated, with alkali tune PH to 5 ~ 7；
（5）It is detected using composite modified electrode, obtains testing result.
It is preferably, described to use composite modified electrode to be detected for current potential from -0.6 ~ 0.8 V cyclic voltammetry scans,
Differential Pulse Voltammetry is carried out later, and record current-potential curve is built according to the correspondence of electric current and total phosphorus concentration
Day-mark directrix curve, for the measurement of phosphorus content in sample to be tested, electric current（I, μ A）With the concentration of phosphorus（C, mmol/L）1.9 ×
10-8~0.7×10-2In a linear relationship within the scope of mol/L, equation of linear regression is：I = 30.49c + 2.74（R =
0.999, n=13）.
Preferably, the method for the phosphorus in the step 1 in collection air and its compound is：The sampling of filter membrane will be installed
Filter membrane, with 0.5 ~ 4L/min flow collection 0.1 ~ 8h air samples, is then put into small beaker, and add ultra-pure water 5 ~ 15 by folder
ML impregnates 10 ~ 30 min.
Preferably, the filter membrane is：One kind of glass fiber filter paper, miillpore filter and Vinylidene Chloride filter membrane, a diameter of 20 ~
30mm。
Preferably, the filter membrane is：Glass fiber filter paper.
Preferably, the resolution step is：Take 5 ~ 15ml of the phosphorus being collected into step 1 and its compound, it is added 0.05 ~
5 ~ 10ml of 0.5M salpeter solutions, 0.01 ~ 0.8M, 1 ~ 10ml of sulfuric acid solution clear up 10 ~ 30min under acidic environment.
Preferably, the ascorbic acid polymer electrode is made by the steps and obtains：
（1）By pyrroles, LiClO4, cerous nitrate, zirconium nitrate be added acetonitrile in, stir evenly, it is molten that glass-carbon electrode is placed in the mixing
In liquid, prepared using cyclic voltammetry；
（2）It is 1 ~ 3 in mass ratio by graphene, Platinum Nanoparticles:2 ~ 5 ratio is dissolved in acetone soln, magnetic agitation 1 ~ 2 hour,
Form uniform dispersion liquid；
(3) modified electrode prepared by step (1) is placed in the solution of step (2) preparation, in the case of magnetic agitation, slowly
Dropwise addition aqueous slkali adjust pH=8 ~ 10,10 ~ 20h of time of repose；
(4) by prepared by step (3) modified electrode dry, and under indifferent gas nitrogen protection in 300 ~ 500 DEG C calcine 1h ~
3h obtains composite modified electrode.
Preferably, the actual conditions of the cyclic voltammetry are：In -1.5 ~ 1.0V voltage ranges, with 50 ~ 100 mV/
S's sweeps the circle of fast cyclic voltammetry scan 3 ~ 8, and by treated, electrode is fully eluted with ultra-pure water.
Preferably, step（1）Pyrrole concentrations are 0.05 ~ 2mol/L in the mixed solution；The LiClO4It is a concentration of
0.05~2mol/L；The cerous nitrate is 5 ~ 10g/L；The zirconium nitrate is 20 ~ 30g/L.
Preferably, a concentration of 30 ~ 50g/L of the ammonium molybdate.
Advantageous effect:
（1）Measure the total phosphorus in air using electrochemical method determining, overcome the large-sized analytic instruments such as chromatography cost of determination it is high,
The shortcomings that field assay energy force difference, has many advantages, such as that sample pre-treatments are simple, reagent consumption is few, high sensitivity, fast and convenient,
Foundation can be provided for the invention of miniature, sensitive field quick detection instrument.
（2）Using the poly- ascorbic acid modified electrode of polypyrrole-, the oxidation current by directly measuring ammonium phosphomolybdate is examined
It surveys, it is fast and convenient, of low cost by the way that preparation method and detection method is calculated.
（3）Total phosphorus electrochemical detection method in the air that the present invention establishes, selectivity is good, the range of linearity is wide, can be used for each
The quick detection of phosphorus in kind workplace.
（4）The method of modifying of electrode may extend to the microelectrodes such as screen printing electrode in the present invention, further develop miniature
Detecting instrument.
Description of the drawings
2 linear graph of Fig. 1 embodiments.
Specific embodiment
The detection method of phosphorus and its compound in a kind of detection air of embodiment 1
1. collecting the phosphorus and its compound in air：The sampling folder of glass fiber filter paper, a diameter of 20mm, with 0.5L/ will be installed
Filter membrane, is then put into small beaker by min flow collection 0.1h air samples, and adds 5 mL of ultra-pure water and impregnate 10 min.
2. the phosphorus being collected into and compound are cleared up：The phosphorus being collected into step 1 and its compound 5ml are taken, is added
0.05M salpeter solution 10ml, 0.8M sulfuric acid solution 1ml, clear up 10min under acidic environment.
3. ammonium molybdate is added in the solution after resolution, ammonium phosphomolybdate is generated：30g/L ammonium molybdate solutions are added in digestion solution,
Ammonium phosphomolybdate is generated, with NaOH solution tune PH to 5.
4. the preparation of standard solution：Dried 0.1389 g of potassium dihydrogen phosphate is accurately weighed, is quantitatively shifted after being dissolved in water
Enter in 100 mL volumetric flasks, be settled to scale, be configured to the phosphate standard storing solution of a concentration of 1.0mol/L, dilutes as needed
At various concentration.
5. using composite modified electrode to be detected for current potential from -0.6 ~ 0.8 V cyclic voltammetry scans, carry out later micro-
Sectors rushes voltammetric determination, and record current-potential curve establishes standard curve according to the correspondence of electric current and total phosphorus concentration,
Measurement for phosphorus content in sample to be tested.
The composite modified electrode is made by the steps and obtains：
（1）Glass-carbon electrode is placed in acetonitrile, pyrroles, LiClO is added4, cerous nitrate, zirconium nitrate, prepared using cyclic voltammetry；
（2）It is 1 in mass ratio by graphene, Platinum Nanoparticles:2 ratio is dissolved in acetone soln, magnetic agitation 1 ~ 2 hour, is formed
Uniform dispersion liquid；
(3) modified electrode prepared by step (1) is placed in the solution of step (2) preparation, in the case of magnetic agitation, slowly
Dropwise addition aqueous slkali adjust pH=8,10 ~ 20h of time of repose；
(4) modified electrode prepared by step (3) is dried, and 1h is calcined in 300 DEG C under indifferent gas nitrogen protection, obtained
Composite modified electrode.
Step（1）Pyrrole concentrations are 0.05mol/L in the mixed solution；The LiClO4A concentration of 0.05mol/L；Institute
It is 5g/L to state cerous nitrate；The zirconium nitrate is 20g/L
The actual conditions of the cyclic voltammetry are：In -1.5V voltage ranges, swept with the fast cyclic voltammetric of sweeping of 50 mV/s
3 circles are retouched, electrode is fully eluted with ultra-pure water by treated.
6. selectivity：
It is control with 0.01mmol/L phosphate radical solution, investigates same concentrations, the sulfate radical of 10 times of concentration, nitrate anion situation.
The results show that the response current that phosphate radical after above-mentioned interfering substance is added shows the total phosphorus inspection that the present invention establishes without significant change
Survey method has good selectivity phosphorus.
7. the range of linearity and detection limit：It uses composite modified electrode to be detected and recycles volt from -0.6 ~ 0.8 V for current potential
Peace scanning, carries out Differential Pulse Voltammetry, record current-potential curve is corresponding with total phosphorus concentration according to electric current later
Relationship establishes standard curve, electric current（I, μ A）With the concentration of phosphorus（C, mmol/L）2.0 × 10-7~0.8×10-4 Mol/L ranges
Interior in a linear relationship, equation of linear regression is：I = 26.35c + 1.459（R2=0.9999, n=5）.Based on three times
Signal-to-noise ratio（S/N = 3）, obtain the modified electrode and 7.8 × 10 be limited to the detection of phosphorus-8 mol/L。
8. measuring the phosphorus content in air using this method, the rate of recovery is 96.4% ~ 102.3%, and relative standard deviation is：
2.0%。
The detection method of phosphorus and its compound in a kind of detection air of embodiment 2
1. collecting the phosphorus and its compound in air：The sampling folder of glass fiber filter paper, a diameter of 25mm, with 2L/min will be installed
Filter membrane, is then put into small beaker by flow collection 2h air samples, and adds ultra-pure water 10mL and impregnate 20 min.
2. the phosphorus being collected into and compound are cleared up：The phosphorus being collected into step 1 and its compound 10ml are taken, is added
0.5M salpeter solution 8ml, 0.01M sulfuric acid solution 5ml, clear up 20min under acidic environment.
3. ammonium molybdate is added in the solution after resolution, ammonium phosphomolybdate is generated：30g/L ammonium molybdate solutions are added in digestion solution,
Ammonium phosphomolybdate is generated, with NaOH solution tune PH to 6.
4. the preparation of standard solution：Dried 0.1389 g of potassium dihydrogen phosphate is accurately weighed, is quantitatively shifted after being dissolved in water
Enter in 100 mL volumetric flasks, be settled to scale, be configured to the phosphate standard storing solution of a concentration of 1.0mol/L, dilutes as needed
At various concentration.
5. using composite modified electrode to be detected for current potential from -0.6 ~ 0.8 V cyclic voltammetry scans, carry out later micro-
Sectors rushes voltammetric determination, and record current-potential curve establishes standard curve according to the correspondence of electric current and total phosphorus concentration,
Measurement for phosphorus content in sample to be tested.
（1）Glass-carbon electrode is placed in acetonitrile, pyrroles, LiClO is added4, cerous nitrate, zirconium nitrate, using cyclic voltammetry
It prepares；
（2）It is 2 in mass ratio by graphene, Platinum Nanoparticles:3 ratio is dissolved in acetone soln, magnetic agitation 1.5 hours, is formed
Uniform dispersion liquid；
(3) modified electrode prepared by step (1) is placed in the solution of step (2) preparation, in the case of magnetic agitation, slowly
Dropwise addition aqueous slkali adjust pH=9, time of repose 15h；
(4) modified electrode prepared by step (3) is dried, and 2h is calcined in 400 DEG C under indifferent gas nitrogen protection, obtained
Composite modified electrode.
Step（1）Pyrrole concentrations are 1mol/L in the mixed solution；The LiClO4A concentration of 1mol/L；The nitric acid
Cerium is 8g/L；The zirconium nitrate is 25g/L.
The actual conditions of the cyclic voltammetry are：In 0.5V voltage ranges, fast cyclic voltammetric is swept with 80 mV/s
5 circle of scanning, by treated, electrode is fully eluted with ultra-pure water.
6. selectivity：
It is control with 0.1 mmol/L phosphate radical solution, investigates same concentrations, the sulfate radical of 10 times of concentration, nitrate anion situation.
The results show that the response current that phosphate radical after above-mentioned interfering substance is added shows the total phosphorus inspection that the present invention establishes without significant change
Survey method has good selectivity phosphorus.
7. the range of linearity and detection limit：It uses composite modified electrode to be detected and recycles volt from -0.6 ~ 0.8 V for current potential
Peace scanning, carries out Differential Pulse Voltammetry, record current-potential curve is corresponding with total phosphorus concentration according to electric current later
Relationship establishes standard curve, electric current（I, μ A）With the concentration of phosphorus（C, mmol/L）1.9 × 10-8~0.7×10-2Mol/L ranges
Interior in a linear relationship, equation of linear regression is：I = 30.49c + 2.74（R2=1.0, n=5）.Signal-to-noise ratio based on three times
（S/N = 3）, obtain the modified electrode and 4.0 × 10 be limited to the detection of phosphorus-9mol/L。
8. measuring the phosphorus content in air using this method, the rate of recovery is 97.5% ~ 101.2%, and relative standard deviation is：
1.3%。
The detection method of phosphorus and its compound in a kind of detection air of embodiment 3
1. collecting the phosphorus and its compound in air：The sampling folder of glass fiber filter paper, a diameter of 30mm, with 4L/min will be installed
Filter membrane, is then put into small beaker by flow collection 0.1h air samples, and adds 15 mL of ultra-pure water and impregnate 30 min.
2. the phosphorus being collected into and compound are cleared up：The phosphorus being collected into step 1 and its compound 15ml are taken, is added
0.2M salpeter solution 5ml, 0.5M sulfuric acid solution 10ml, clear up 30min under acidic environment.
3. ammonium molybdate is added in the solution after resolution, ammonium phosphomolybdate is generated：50g/L ammonium molybdate solutions are added in digestion solution,
Ammonium phosphomolybdate is generated, with NaOH solution tune PH to 7.
4. the preparation of standard solution：Dried 0.1389 g of potassium dihydrogen phosphate is accurately weighed, is quantitatively shifted after being dissolved in water
Enter in 100 mL volumetric flasks, be settled to scale, be configured to the phosphate standard storing solution of a concentration of 1.0mol/L, dilutes as needed
At various concentration.
5. using composite modified electrode to be detected for current potential from -0.6 ~ 0.8 V cyclic voltammetry scans, carry out later micro-
Sectors rushes voltammetric determination, and record current-potential curve establishes standard curve according to the correspondence of electric current and total phosphorus concentration,
Measurement for phosphorus content in sample to be tested.
（1）Glass-carbon electrode is placed in acetonitrile, pyrroles, LiClO is added4, cerous nitrate, zirconium nitrate, using cyclic voltammetry
It prepares；
（2）It is 1 ~ 3 in mass ratio by graphene, Platinum Nanoparticles:2 ~ 5 ratio is dissolved in acetone soln, magnetic agitation 1 ~ 2 hour,
Form uniform dispersion liquid；
（3）Modified electrode prepared by step (1) is placed in the solution of step (2) preparation, in the case of magnetic agitation, slowly
Dropwise addition aqueous slkali adjust pH=8 ~ 10,10 ~ 20h of time of repose；
（4）By prepared by step (3) modified electrode drying, and under indifferent gas nitrogen protection in 300 ~ 500 DEG C calcine 1h ~
3h obtains composite modified electrode.
Step（1）Pyrrole concentrations are 2mol/L in the mixed solution；The LiClO4A concentration of 2mol/L；The nitric acid
Cerium is 10g/L；The zirconium nitrate is 30g/L.
The actual conditions of the cyclic voltammetry are：In 1.0V voltage ranges, speed cycle volt is swept with 100 mV/s
8 circle of peace scanning, by treated, electrode is fully eluted with ultra-pure water.
6. selectivity：
It is control with 0.05mmol/L phosphate radical solution, investigates same concentrations, the sulfate radical of 10 times of concentration, nitrate anion situation.
The results show that the response current that phosphate radical after above-mentioned interfering substance is added shows the total phosphorus inspection that the present invention establishes without significant change
Survey method has good selectivity phosphorus.
7. the range of linearity and detection limit：It uses composite modified electrode to be detected and recycles volt from -0.6 ~ 0.8 V for current potential
Peace scanning, carries out Differential Pulse Voltammetry, record current-potential curve is corresponding with total phosphorus concentration according to electric current later
Relationship establishes standard curve, electric current（I, μ A）With the concentration of phosphorus（C, mmol/L）4.5 × 10-7~1.2×10-5 Mol/L ranges
Interior in a linear relationship, equation of linear regression is：I = 64.7c + 4.563（R2=0.9999, n=5）.Letter based on three times
It makes an uproar ratio（S/N = 3）, obtain the modified electrode and 2.5 × 10 be limited to the detection of phosphorus-8mol/L。
8. measuring the phosphorus content in air using this method, the rate of recovery is 97.0% ~ 103.0%, and relative standard deviation is：
2.6%。
Claims (10)
1. the detection method of phosphorus and its compound in a kind of detection workplace air, which is characterized in that the detection method includes
Following steps：
（1）Collect the phosphorus and its compound in air；
（2）The phosphorus being collected into and compound are cleared up；
（4）Ammonium molybdate is added in solution after resolution, ammonium phosphomolybdate is generated, with alkali tune PH to 5 ~ 7；
（5）It is detected using composite modified electrode, obtains testing result.
2. detection method according to claim 1, which is characterized in that described to use composite modified electrode to be detected for electricity
Position carries out Differential Pulse Voltammetry, record current-potential curve, root later from -0.6 ~ 0.8 V cyclic voltammetry scans
According to the correspondence of electric current and total phosphorus concentration, standard curve is established, for the measurement of phosphorus content in sample to be tested, electric current（I, μ A）
With the concentration of phosphorus（C, mmol/L）1.9 × 10-8~0.7×10-2In a linear relationship within the scope of mol/L, equation of linear regression is：
I = 30.49c + 2.74（R=0.999, n=13）.
3. detection method according to claim 1, which is characterized in that collect phosphorus and its change in air in the step 1
Close object method be：The sampling folder of filter membrane will be installed, it, then will filter with 0.5 ~ 4L/min flow collection 0.1 ~ 8h air samples
Film is put into small beaker, and is added 5 ~ 15 mL of ultra-pure water and impregnated 10 ~ 30 min.
4. according to the detection method in claim 3, which is characterized in that the filter membrane is：Glass fiber filter paper, miillpore filter and
One kind of Vinylidene Chloride filter membrane, a diameter of 20 ~ 30mm.
5. according to the detection method in claim 3, which is characterized in that the filter membrane is：Glass fiber filter paper.
6. detection method according to claim 1, which is characterized in that the resolution step is：It takes and is collected into step 1
0.05 ~ 0.5M salpeter solutions, 5 ~ 10ml, 0.01 ~ 0.8M, 1 ~ 10ml of sulfuric acid solution is added, in acid in 5 ~ 15ml of phosphorus and its compound
Property environment under clear up 10 ~ 30min.
7. detection method according to claim 1, which is characterized in that the composite modified electrode is made by the steps
And it obtains：
（1）By pyrroles, LiClO4, cerous nitrate, zirconium nitrate be added acetonitrile in, stir evenly, glass-carbon electrode be placed in the mixed solution
In, it is prepared using cyclic voltammetry；
（2）It is 1 ~ 3 in mass ratio by graphene, Platinum Nanoparticles:2 ~ 5 ratio is dissolved in acetone soln, magnetic agitation 1 ~ 2 hour,
Form uniform dispersion liquid；
(3) modified electrode prepared by step (1) is placed in the solution of step (2) preparation, in the case of magnetic agitation, slowly
Dropwise addition aqueous slkali adjust pH=8 ~ 10,10 ~ 20h of time of repose；
(4) by prepared by step (3) modified electrode dry, and under indifferent gas nitrogen protection in 300 ~ 500 DEG C calcine 1h ~
3h obtains composite modified electrode.
8. detection method according to claim 7, which is characterized in that the actual conditions of the cyclic voltammetry are：-
In 1.5 ~ 1.0V voltage ranges, enclosed with the fast cyclic voltammetry scan 3 ~ 8 of sweeping of 50 ~ 100 mV/s, will treated electrode with super
Pure water fully elutes.
9. detection method according to claim 7, which is characterized in that step（1）The concentration of pyrroles in the mixed solution
For 0.05 ~ 2mol/L；The LiClO4A concentration of 0.05 ~ 2mol/L；A concentration of 5 ~ 10g/L of the cerous nitrate；The nitre
A concentration of 20 ~ 30g/L of sour zirconium.
10. according to detection method described in claim 1, which is characterized in that a concentration of 30 ~ 50g/L of the ammonium molybdate.
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