CN110057896A - The analysis method of content of fluoride in a kind of hazardous waste - Google Patents
The analysis method of content of fluoride in a kind of hazardous waste Download PDFInfo
- Publication number
- CN110057896A CN110057896A CN201910442446.2A CN201910442446A CN110057896A CN 110057896 A CN110057896 A CN 110057896A CN 201910442446 A CN201910442446 A CN 201910442446A CN 110057896 A CN110057896 A CN 110057896A
- Authority
- CN
- China
- Prior art keywords
- fluoride
- solution
- oxygen bomb
- content
- deionized water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- 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
- G01N27/333—Ion-selective electrodes or membranes
-
- 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
- G01N27/38—Cleaning of electrodes
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention provides a kind of analysis method of content of fluoride in hazardous waste.Pretreated sample completely burned in confined space is made using Oxygen Bomb Combustion technology, fluorine element a part in oxygen bomb is absorbed by the absorbing liquid in oxygen bomb, another part is actually taken up by gas the absorbing liquid in station by way of gas and absorbed, merge absorbing liquid and obtain fluoride extracting solution, extracting solution obtains testing sample solution after reprocessing.Fluorine ion series standard solution is prepared, and with potential value E to negative logarithm (E(mV)-log c of fluorinion concentrationF ‑(mg/L)) standard curve is drawn.The content of fluoride is calculated by standard curve according to the potential value measured using ion chromatograph-fluoride ion selective electrode measurement testing sample solution potential value.The accuracy of this method test result is higher.The testing time can be greatlyd save simultaneously.
Description
Technical field
The invention belongs to chemical analysis test fields, and in particular to a kind of Oxygen Bomb Combustion-gas absorption-ion-selective electrode
The method that method measures content of fluoride in hazardous waste.
Background technique
High temperature incineration is the common processing mode of hazardous waste, and the yield of hydrogen fluoride depends on being burned in incineration tail gas
Fluorine content and burning condition in hazardous waste.On the one hand, GB 18484-2001 " dangerous waste incineration contamination control standard " is right
The discharge finite quantity of hydrogen fluoride provides that on the other hand, fluoride can corrode burning facility, influence the service life of burning facility,
Therefore in hazardous waste processing disposition industry, it is necessary to analyze the content of fluoride in waste, be controlled after compatibility
Hydrogen fluoride content in material is burned, emission is made to achieve the purpose that rules and regulations and protection burning facility.GB/T
15555.11-1995 " the measurement fluorescence spectrophotometric method of solid waste fluoride " only defines solid waste leachate
Content of fluoride analysis method is not suitable for the total amount measurement of fluoride in hazardous waste.There has been no in hazardous waste at present
The analytical standard of fluoride total amount, some existing literatures use Oxygen Bomb Combustion-chromatography of ions, have used in pretreatment process super
It is shaken in sound wave or water-bath about 1 hour, it is cumbersome and take a long time, and not to the fluoride in gas after Oxygen Bomb Combustion
Recycling test is carried out, so as to cause test result deviation.
Summary of the invention
In view of the above deficiencies, the present invention provides a kind of Oxygen Bomb Combustion-gas absorption-ion selective electrode method measurement is dangerous
The method of content of fluoride in waste.The process that this method carries out the extraction of fluoride in sample to Oxygen Bomb Combustion technology changes
Into using gas absorbs station and absorbs to the gas in oxygen bomb, and automatical potentiometric titrimeter and fluoride ion selective electrode carry out sample
Product test, guarantees the timeliness and accuracy of sample test.
The present invention is achieved by the following technical programs:
1) sample pretreatment: if it is solid sample, being crushed to partial size is 200 μm, if it is semisolid sample and liquid sample,
Sample is uniformly mixed by stirring;
2) it the extraction of sample fluoride: weighs 0.1 ~ 0.3 g(and is accurate to 0.0001 g) dangerous waste sample after pretreatment, be placed in
In oxygen bomb crucible, 0 ~ 0.5 g combustion adjuvant is added;Crucible is fixed in oxygen bomb, ignition wire is filled;10 are poured on oxygen bomb terminal
ML absorbing liquid, operation calorimeter make automatic oxygenation and ignition;It after burning, absorbs and injects 20 mL absorbing liquids in station, oxygen bomb connects
It connects gas and absorbs station, control outgassing rate, discharge gas in oxygen bomb in 20 ~ 30 minutes into gas absorption station;Gas is complete
After portion's discharge, collects oxygen bomb absorbing liquid and gas absorbs the absorbing liquid at station, be placed in 50 mL polyethylene volume bottles, use deionization
Water is respectively washed inside oxygen bomb and gas absorbs station, is transferred in volumetric flask, with deionized water constant volume, is obtained fluoride extracting solution;
3) standard solution of 1000 mg/L standard curve: is diluted to the stock solution of 10 mg/L with deionized water;It takes certain
The stock solution of volume, with diluent be configured to concentration be respectively 0,0.2,0.6,1.0,2.0,4.0 mg/L series standard it is molten
Liquid;Series standard solution is injected separately into 6 100 mL polyethylene cups, rotor is put into, is from low to high sequence with concentration, point
It is not sequentially inserted into fluoride ion selective electrode, continuous stirring solution, after current potential is stablized, reading potential value E;It is being measured every time
Before, electrode will be rinsed with deionized water, and blotted with filter paper;Before every measurement, electrode will be rinsed with deionized water,
And it is blotted with filter paper;Draw E(mV)-log cF -(mg/L) standard curve;
4) it measures: taking the fluoride extracting solution of appropriate step 2, be placed in 50mL polyethylene volume bottle, with sodium acetate solution or salt
It is 5.0 ~ 8.0 that acid solution, which is adjusted to pH value, and 10 mL total ionic strengths are added and adjust buffer solution, are diluted to mark with deionized water
Line shakes up;It is injected into 100 mL polyethylene cups, is put into rotor, be inserted into fluoride ion selective electrode, continuous stirring solution, to
After current potential is stablized, reading potential value Ex;Before every measurement, electrode will be rinsed with deionized water, and is blotted with filter paper;Root
According to the millivolt number measured, the content of fluoride is calculated by standard curve.
Wherein, combustion adjuvant described in step 2 is benzoic acid or paraffin oil, and additional amount is 0 ~ 0.5g.Solid sample is preferred
Benzoic acid, semisolid and liquid sample preferred paraffinic oils.
Wherein, ignition wire described in step 2 is cotton thread ignition wire.
Wherein, absorbing liquid described in step 2 is 0.3mol/L NaOH solution.
Wherein, diluent described in step 3) is that total ionic strength adjusts buffer solution: deionized water is according to volume ratio 1:4
The mixture mixed.
Wherein, it is 0.2mol/L sodium citrate and 1mol/L nitric acid that total ionic strength described in step 4), which adjusts buffer solution,
The mixed solution that the pH value of sodium is 5.0 ~ 6.0.
Compared with prior art, the present invention has the advantage that
(1) pre-treatment is carried out to hazardous waste sample using the method that Oxygen Bomb Combustion-gas absorbs, it is ensured that fluoride is by oxygen bomb
Absorbing liquid and the absorbing liquid that absorbs in station of gas fully absorb and extract, avoid the loss of target to be measured.Meanwhile sample
Product pre-treating method greatly saves the testing time than prior art simplicity.
(2) fluoride is measured using fluoride ion selective electrode, and is adjusted by the way that total ionic strength is added in sample solution
Buffer solution can effectively prevent fluorine ion and cation complex, guarantee the accuracy of test result.
Specific embodiment
For the ease of the understanding of this technology personnel, the present invention is made further instructions below with reference to embodiment, is implemented
The content that mode refers to not is limitation of the invention.
Embodiment 1: sample is the content of fluoride that " National Hazard waste register " waste classification is in the used oil of HW08
Measurement
1) sample pretreatment: stirring is uniformly mixed sample.
2) extraction of sample fluoride: 0.3011 g sample is weighed, is placed in oxygen bomb crucible.Crucible is fixed in oxygen bomb, is filled
Ignition wire.10 mL absorbing liquids are poured on oxygen bomb terminal, operation calorimeter makes automatic oxygenation and ignition.After burning, absorb
20 mL absorbing liquids are injected in standing, oxygen bomb connects gas and absorbs station, controls outgassing rate, makes in oxygen bomb gas in 20 ~ 30 minutes
Release to gas absorbs in station.Gas all after discharge, collects oxygen bomb absorbing liquid and gas absorbs the absorbing liquid at station, be placed in 50
In mL polyethylene volume bottle, be respectively washed inside oxygen bomb with deionized water and gas absorb station, be transferred in volumetric flask, spend from
Sub- water constant volume, obtains fluoride extracting solution.
3) standard solution of 1000 mg/L standard curve: is diluted to the stock solution of 10 mg/L with deionized water.It takes
The stock solution of certain volume is configured to the series that concentration is respectively 0,0.2,0.6,1.0,2.0,4.0 mg/L with diluent and marks
Quasi- solution.Series standard solution is injected separately into 6 100 mL polyethylene cups, rotor is put into, is from low to high suitable with concentration
Sequence, is sequentially inserted into fluoride ion selective electrode respectively, continuous stirring solution, after current potential is stablized, reading potential value E.It is surveying every time
Before amount, electrode will be rinsed with deionized water, and blotted with filter paper.Before every measurement, it will be rinsed with deionized water
Electrode, and blotted with filter paper.Draw E(mV)-log cF -(mg/L) standard curve.
4) it measures: taking the fluoride extracting solution of appropriate step 2, be placed in 50mL polyethylene volume bottle, use sodium acetate solution
Or it is 5.0 ~ 8.0 that hydrochloric acid solution, which is adjusted to pH value, and 10 mL total ionic strengths are added and adjust buffer solution, are diluted with deionized water
To graticule, shake up.It is injected into 100 mL polyethylene cups, is put into rotor, be inserted into fluoride ion selective electrode, continuously stir molten
Liquid, after current potential is stablized, reading potential value Ex.Before every measurement, electrode will be rinsed with deionized water, and is inhaled with filter paper
It is dry.According to the millivolt number measured, the content of fluoride is calculated by standard curve.The fluoride of the used oil obtained through this embodiment
(with F-Meter) content be 0.007%.
Embodiment 2: sample is that " National Hazard waste register " waste classification is that fluoride in the bottoms of HW11 contains
The measurement of amount
1) sample pretreatment: being 200 μm by sample comminution to partial size.
2) extraction of sample fluoride: 0.2008 g sample is weighed, is placed in oxygen bomb crucible.Crucible is fixed on oxygen bomb
It is interior, fill ignition wire.10 mL absorbing liquids are poured on oxygen bomb terminal, operation calorimeter makes automatic oxygenation and ignition.Burning
Afterwards, absorb and inject 20 mL absorbing liquids in station, oxygen bomb connects gas and absorbs station, controls outgassing rate, make in oxygen bomb gas 20 ~
Release to gas absorbs in station in 30 minutes.Gas all after discharge, collects oxygen bomb absorbing liquid and gas absorbs the absorbing liquid at station,
It is placed in 50 mL polyethylene volume bottles, is respectively washed inside oxygen bomb with deionized water and gas absorbs station, be transferred to volumetric flask
In, with deionized water constant volume, obtain fluoride extracting solution.
3) standard solution of 1000 mg/L standard curve: is diluted to the stock solution of 10 mg/L with deionized water.It takes
The stock solution of certain volume is configured to the series that concentration is respectively 0,0.2,0.6,1.0,2.0,4.0 mg/L with diluent and marks
Quasi- solution.Series standard solution is injected separately into 6 100 mL polyethylene cups, rotor is put into, is from low to high suitable with concentration
Sequence, is sequentially inserted into fluoride ion selective electrode respectively, continuous stirring solution, after current potential is stablized, reading potential value E.It is surveying every time
Before amount, electrode will be rinsed with deionized water, and blotted with filter paper.Before every measurement, it will be rinsed with deionized water
Electrode, and blotted with filter paper.Draw E(mV)-log cF -(mg/L) standard curve.
4) it measures: taking the fluoride extracting solution of appropriate step 2, be placed in 50mL polyethylene volume bottle, use sodium acetate solution
Or it is 5.0 ~ 8.0 that hydrochloric acid solution, which is adjusted to pH value, and 10 mL total ionic strengths are added and adjust buffer solution, are diluted with deionized water
To graticule, shake up.It is injected into 100 mL polyethylene cups, is put into rotor, be inserted into fluoride ion selective electrode, continuously stir molten
Liquid, after current potential is stablized, reading potential value Ex.Before every measurement, electrode will be rinsed with deionized water, and is inhaled with filter paper
It is dry.According to the millivolt number measured, the content of fluoride is calculated by standard curve.The fluorination of the bottoms obtained through this embodiment
Object is (with F-Meter) content be 0.3%.
Embodiment 3: sample is the content of fluoride in the paint slag that " National Hazard waste register " waste classification is HW12
Measurement
1) sample pretreatment: will be crushed to partial size is 200 μm.
2) extraction of sample fluoride: weighing 0.1998 g sample, be placed in oxygen bomb crucible, and 0.2 g benzoic acid is added.It will
Crucible is fixed in oxygen bomb, fills ignition wire.Pour into 10 mL absorbing liquids on oxygen bomb terminal, operation calorimeter make automatic oxygenation and
Ignition.It after burning, absorbs and injects 20 mL absorbing liquids in station, oxygen bomb connects gas and absorbs station, controls outgassing rate, makes oxygen
Gas is discharged to gas in 20 ~ 30 minutes and is absorbed in station in bullet.Gas all after discharge, collects oxygen bomb absorbing liquid and gas is inhaled
The absorbing liquid for receiving station, is placed in 50 mL polyethylene volume bottles, is respectively washed inside oxygen bomb with deionized water and gas absorbs station,
It is transferred in volumetric flask, with deionized water constant volume, obtains fluoride extracting solution.
3) standard solution of 1000 mg/L standard curve: is diluted to the stock solution of 10 mg/L with deionized water.It takes
The stock solution of certain volume is configured to the series that concentration is respectively 0,0.2,0.6,1.0,2.0,4.0 mg/L with diluent and marks
Quasi- solution.Series standard solution is injected separately into 6 100 mL polyethylene cups, rotor is put into, is from low to high suitable with concentration
Sequence, is sequentially inserted into fluoride ion selective electrode respectively, continuous stirring solution, after current potential is stablized, reading potential value E.It is surveying every time
Before amount, electrode will be rinsed with deionized water, and blotted with filter paper.Before every measurement, it will be rinsed with deionized water
Electrode, and blotted with filter paper.Draw E(mV)-log cF -(mg/L) standard curve.
4) it measures: taking the fluoride extracting solution of appropriate step 2, be placed in 50mL polyethylene volume bottle, use sodium acetate solution
Or it is 5.0 ~ 8.0 that hydrochloric acid solution, which is adjusted to pH value, and 10 mL total ionic strengths are added and adjust buffer solution, are diluted with deionized water
To graticule, shake up.It is injected into 100 mL polyethylene cups, is put into rotor, be inserted into fluoride ion selective electrode, continuously stir molten
Liquid, after current potential is stablized, reading potential value Ex.Before every measurement, electrode will be rinsed with deionized water, and is inhaled with filter paper
It is dry.According to the millivolt number measured, the content of fluoride is calculated by standard curve.The fluorination of the bottoms obtained through this embodiment
Object is (with F-Meter) content be 0.02%.
Embodiment 4: sample is the content of fluoride that " National Hazard waste register " waste classification is in the fixing solution of HW16
Measurement
1) sample pretreatment: it is uniformly mixed sample by stirring.
2) extraction of sample fluoride: weighing 0.2200 g sample, be placed in oxygen bomb crucible, and 0.5 g paraffin oil is added.It will
Crucible is fixed in oxygen bomb, fills ignition wire.Pour into 10 mL absorbing liquids on oxygen bomb terminal, operation calorimeter make automatic oxygenation and
Ignition.It after burning, absorbs and injects 20 mL absorbing liquids in station, oxygen bomb connects gas and absorbs station, controls outgassing rate, makes oxygen
Gas is discharged to gas in 20 ~ 30 minutes and is absorbed in station in bullet.Gas all after discharge, collects oxygen bomb absorbing liquid and gas is inhaled
The absorbing liquid for receiving station, is placed in 50 mL polyethylene volume bottles, is respectively washed inside oxygen bomb with deionized water and gas absorbs station,
It is transferred in volumetric flask, with deionized water constant volume, obtains fluoride extracting solution.
3) standard solution of 1000 mg/L standard curve: is diluted to the stock solution of 10 mg/L with deionized water.It takes
The stock solution of certain volume is configured to the series that concentration is respectively 0,0.2,0.6,1.0,2.0,4.0 mg/L with diluent and marks
Quasi- solution.Series standard solution is injected separately into 6 100 mL polyethylene cups, rotor is put into, is from low to high suitable with concentration
Sequence, is sequentially inserted into fluoride ion selective electrode respectively, continuous stirring solution, after current potential is stablized, reading potential value E.It is surveying every time
Before amount, electrode will be rinsed with deionized water, and blotted with filter paper.Before every measurement, it will be rinsed with deionized water
Electrode, and blotted with filter paper.Draw E(mV)-log cF -(mg/L) standard curve.
4) it measures: taking the fluoride extracting solution of appropriate step 2, be placed in 50mL polyethylene volume bottle, use sodium acetate solution
Or it is 5.0 ~ 8.0 that hydrochloric acid solution, which is adjusted to pH value, and 10 mL total ionic strengths are added and adjust buffer solution, are diluted with deionized water
To graticule, shake up.It is injected into 100 mL polyethylene cups, is put into rotor, be inserted into fluoride ion selective electrode, continuously stir molten
Liquid, after current potential is stablized, reading potential value Ex.Before every measurement, electrode will be rinsed with deionized water, and is inhaled with filter paper
It is dry.According to the millivolt number measured, the content of fluoride is calculated by standard curve.The fluorination of the bottoms obtained through this embodiment
Object is (with F-Meter), as a result it is not detected.
Embodiment 5: sample is that " National Hazard waste register " waste classification is that fluoride in the biochemical sludge of HW17 contains
The measurement of amount
1) sample pretreatment: will be crushed to partial size is 200 μm.
2) extraction of sample fluoride: 0.1026 g dangerous waste sample after pretreatment is weighed, is placed in oxygen bomb crucible, adds
Enter 0.25 g benzoic acid.Crucible is fixed in oxygen bomb, ignition wire is filled.10 mL absorbing liquids, operating quantity are poured on oxygen bomb terminal
Hot instrument makes automatic oxygenation and ignition.It after burning, absorbs and injects 20 mL absorbing liquids in station, oxygen bomb connects gas and absorbs station, control
Outgassing rate processed discharges gas in oxygen bomb in 20 ~ 30 minutes into gas absorption station.Gas all after discharge, collects oxygen
It plays absorbing liquid and gas absorbs the absorbing liquid at station, be placed in 50 mL polyethylene volume bottles, be respectively washed in oxygen bomb with deionized water
Portion and gas absorb station, are transferred in volumetric flask, with deionized water constant volume, obtain fluoride extracting solution.
3) standard solution of 1000 mg/L standard curve: is diluted to the stock solution of 10 mg/L with deionized water.It takes
The stock solution of certain volume is configured to the series that concentration is respectively 0,0.2,0.6,1.0,2.0,4.0 mg/L with diluent and marks
Quasi- solution.Series standard solution is injected separately into 6 100 mL polyethylene cups, rotor is put into, is from low to high suitable with concentration
Sequence, is sequentially inserted into fluoride ion selective electrode respectively, continuous stirring solution, after current potential is stablized, reading potential value E.It is surveying every time
Before amount, electrode will be rinsed with deionized water, and blotted with filter paper.Before every measurement, it will be rinsed with deionized water
Electrode, and blotted with filter paper.Draw E(mV)-log cF -(mg/L) standard curve.
4) it measures: taking the fluoride extracting solution of appropriate step 2, be placed in 50mL polyethylene volume bottle, use sodium acetate solution
Or it is 5.0 ~ 8.0 that hydrochloric acid solution, which is adjusted to pH value, and 10 mL total ionic strengths are added and adjust buffer solution, are diluted with deionized water
To graticule, shake up.It is injected into 100 mL polyethylene cups, is put into rotor, be inserted into fluoride ion selective electrode, continuously stir molten
Liquid, after current potential is stablized, reading potential value Ex.Before every measurement, electrode will be rinsed with deionized water, and is inhaled with filter paper
It is dry.According to the millivolt number measured, the content of fluoride is calculated by standard curve.The fluorination of the bottoms obtained through this embodiment
Object is (with F-Meter) content be 0.2%.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (6)
1. the analysis method of content of fluoride in a kind of hazardous waste, it is characterised in that the following steps are included:
1) sample pretreatment: if it is solid sample, being crushed to partial size is 200 μm, if it is semisolid sample and liquid sample,
Sample is uniformly mixed by stirring;
2) it the extraction of sample fluoride: weighs 0.1 ~ 0.3 g(and is accurate to 0.0001 g) dangerous waste sample after pretreatment, be placed in
In oxygen bomb crucible, 0 ~ 0.5 g combustion adjuvant is added;Crucible is fixed in oxygen bomb, ignition wire is filled;10 are poured on oxygen bomb terminal
ML absorbing liquid, operation calorimeter make automatic oxygenation and ignition;It after burning, absorbs and injects 20 mL absorbing liquids in station, oxygen bomb connects
It connects gas and absorbs station, control outgassing rate, discharge gas in oxygen bomb in 20 ~ 30 minutes into gas absorption station;Gas is complete
After portion's discharge, collects oxygen bomb absorbing liquid and gas absorbs the absorbing liquid at station, be placed in 50 mL polyethylene volume bottles, use deionization
Water is respectively washed inside oxygen bomb and gas absorbs station, is transferred in volumetric flask, with deionized water constant volume, is obtained fluoride extracting solution;
3) standard solution of 1000 mg/L standard curve: is diluted to the stock solution of 10 mg/L with deionized water;It takes certain
The stock solution of volume, with diluent be configured to concentration be respectively 0,0.2,0.6,1.0,2.0,4.0 mg/L series standard it is molten
Liquid;Series standard solution is injected separately into 6 100 mL polyethylene cups, rotor is put into, is from low to high sequence with concentration, point
It is not sequentially inserted into fluoride ion selective electrode, continuous stirring solution, after current potential is stablized, reading potential value E;It is being measured every time
Before, electrode will be rinsed with deionized water, and blotted with filter paper;Before every measurement, electrode will be rinsed with deionized water,
And it is blotted with filter paper;Draw E(mV)-log cF -(mg/L) standard curve;
4) it measures: taking the fluoride extracting solution of appropriate step 2, be placed in 50mL polyethylene volume bottle, with sodium acetate solution or salt
It is 5.0 ~ 8.0 that acid solution, which is adjusted to pH value, and 10 mL total ionic strengths are added and adjust buffer solution, are diluted to mark with deionized water
Line shakes up;It is injected into 100 mL polyethylene cups, is put into rotor, be inserted into fluoride ion selective electrode, continuous stirring solution, to
After current potential is stablized, reading potential value Ex;Before every measurement, electrode will be rinsed with deionized water, and is blotted with filter paper;Root
According to the millivolt number measured, the content of fluoride is calculated by standard curve.
2. the analysis method of content of fluoride in a kind of hazardous waste according to claim 1, which is characterized in that step 2
The combustion adjuvant is benzoic acid or paraffin oil, and additional amount is 0 ~ 0.5g.
3. the analysis method of content of fluoride in a kind of hazardous waste according to claim 1, which is characterized in that step 2
The ignition wire is cotton thread ignition wire.
4. the analysis method of content of fluoride in a kind of hazardous waste according to claim 1, which is characterized in that step 2
The absorbing liquid is 0.3mol/L NaOH solution.
5. the analysis method of content of fluoride in a kind of hazardous waste according to claim 1, which is characterized in that step 3)
The diluent is that total ionic strength adjusts buffer solution: the mixture that deionized water is mixed according to volume ratio 1:4.
6. the analysis method of content of fluoride in a kind of hazardous waste according to claim 5, which is characterized in that step 4)
It is 5.0 ~ 6.0 that the total ionic strength, which adjusts the pH value that buffer solution is 0.2mol/L sodium citrate and 1mol/L sodium nitrate,
Mixed solution.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910442446.2A CN110057896A (en) | 2019-05-25 | 2019-05-25 | The analysis method of content of fluoride in a kind of hazardous waste |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910442446.2A CN110057896A (en) | 2019-05-25 | 2019-05-25 | The analysis method of content of fluoride in a kind of hazardous waste |
Publications (1)
Publication Number | Publication Date |
---|---|
CN110057896A true CN110057896A (en) | 2019-07-26 |
Family
ID=67324531
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201910442446.2A Pending CN110057896A (en) | 2019-05-25 | 2019-05-25 | The analysis method of content of fluoride in a kind of hazardous waste |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN110057896A (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109696517A (en) * | 2017-10-20 | 2019-04-30 | 广东东阳光药业有限公司 | In a kind of detection polymerization liquid in fluorine-containing alkylacrylate fluorine content method |
CN113447605A (en) * | 2021-04-19 | 2021-09-28 | 湖南瀚洋环保科技有限公司 | Detection method for incineration type hazardous waste |
CN114935598A (en) * | 2022-04-06 | 2022-08-23 | 武汉大学 | Detection method for gas-liquid phase product after SF6 degradation |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104614416A (en) * | 2013-11-01 | 2015-05-13 | 深圳职业技术学院 | Detecting method of fluoride in soldering paste |
CN104729900A (en) * | 2015-03-13 | 2015-06-24 | 安徽皖仪科技股份有限公司 | Sample pre-treatment method for detecting lead element content in diesel oil by atomic absorption method |
CN108802149A (en) * | 2018-06-19 | 2018-11-13 | 湖南师范大学 | A kind of Oxygen Bomb Combustion quickly measures the detection method of PAHs in coal content |
-
2019
- 2019-05-25 CN CN201910442446.2A patent/CN110057896A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104614416A (en) * | 2013-11-01 | 2015-05-13 | 深圳职业技术学院 | Detecting method of fluoride in soldering paste |
CN104729900A (en) * | 2015-03-13 | 2015-06-24 | 安徽皖仪科技股份有限公司 | Sample pre-treatment method for detecting lead element content in diesel oil by atomic absorption method |
CN108802149A (en) * | 2018-06-19 | 2018-11-13 | 湖南师范大学 | A kind of Oxygen Bomb Combustion quickly measures the detection method of PAHs in coal content |
Non-Patent Citations (1)
Title |
---|
ASTM INTERNATIONAL: "《ASTM D 3761-96(reapproved 2002)》", 31 December 2002 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109696517A (en) * | 2017-10-20 | 2019-04-30 | 广东东阳光药业有限公司 | In a kind of detection polymerization liquid in fluorine-containing alkylacrylate fluorine content method |
CN113447605A (en) * | 2021-04-19 | 2021-09-28 | 湖南瀚洋环保科技有限公司 | Detection method for incineration type hazardous waste |
CN114935598A (en) * | 2022-04-06 | 2022-08-23 | 武汉大学 | Detection method for gas-liquid phase product after SF6 degradation |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN110057896A (en) | The analysis method of content of fluoride in a kind of hazardous waste | |
CN114235523B (en) | Method for detecting heavy metal element content of fly ash of household garbage power plant | |
CN103149073B (en) | X-ray fluorescence spectra analyzes the MTG YBCO bulk method of ferrosilicon, Si-Ca-Ba, silicomanganese, ferro-aluminum or ferro-titanium sample | |
CN103439213B (en) | The system detecting method of industry carborundum component | |
CN106018666A (en) | Oxygen bomb combustion method for testing content of halogens and content of sulphur in industrial solid waste | |
CN105449297B (en) | The quantitative analysis method of electrolyte consumption | |
CN103994994A (en) | Method for analyzing silicon in ferro-vanadium | |
CN108956815A (en) | The test method of chloride ion content in a kind of sea sand | |
WO2024077976A1 (en) | Method for simultaneously and rapidly determining chlorine, bromine and iodine by means of combination of high-temperature hydrolysis and icp-ms | |
CN106248609B (en) | A kind of method that ultraviolet specrophotometer measures hexafluorophosphoric acid lithium content in lithium-ion battery electrolytes | |
CN104991036A (en) | Determination method for soil alkali-hydrolyzable nitrogen | |
CN107765019A (en) | A kind of Continuous Flow Analysis instrument control system and method | |
CN109799226A (en) | A kind of method of chromic oxide content in measurement vessel slag | |
CN108414558A (en) | A kind of MTG YBCO bulk method measuring ferrochrome chemical composition for x-ray fluorescence spectrum analysis method | |
CN105067583B (en) | The measuring method of lead content in a kind of chrome ore | |
CN109507266A (en) | A kind of detection method of anode foils remained on surface chloride ion | |
CN105866326A (en) | Determining method for calcium fluoride content in ore | |
CN101482495A (en) | Method for rapidly measuring concentration of hexavalent chromium water solution | |
CN106198813A (en) | The analysis method of lithium battery electrolytes | |
Boniface et al. | The determination of carbon in steel by coulometric titration in partially aqueous medium | |
CN106248775A (en) | Quantitative detection method for reducing analysis errors of ICP-MS and ICP-AES whole process | |
Cain et al. | An Electrolytic Resistance Method for Determining Carbon in Steel. | |
ITTO20110605A1 (en) | PROCEDURE FOR THE QUANTITATIVE DETERMINATION OF TOTAL CHLORINE IN A MATRIX | |
CN106885799A (en) | A kind of method for determining content of magnesium in core level sponge zirconium particle | |
CN110412116A (en) | The test method and its application of sulfur content |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190726 |