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 PDF

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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
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fluoride
solution
oxygen bomb
content
deionized water
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叶汝汉
杨宗兴
马凤珠
罗平
许晋
陈铭
彭学良
黎金盛
陈嘉庆
卢福伟
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YAMEN NEW FORTUNE ENVIRONMENTAL PROTECTION Inc
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28Electrolytic cell components
    • G01N27/30Electrodes, e.g. test electrodes; Half-cells
    • G01N27/333Ion-selective electrodes or membranes
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28Electrolytic cell components
    • G01N27/30Electrodes, e.g. test electrodes; Half-cells
    • G01N27/38Cleaning of electrodes
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/416Systems

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  • Health & Medical Sciences (AREA)
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  • 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

The analysis method of content of fluoride in a kind of hazardous waste
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.
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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

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Application publication date: 20190726