CN108445148A - The detection method of bromine trifluoride product purity - Google Patents
The detection method of bromine trifluoride product purity Download PDFInfo
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- CN108445148A CN108445148A CN201810250513.6A CN201810250513A CN108445148A CN 108445148 A CN108445148 A CN 108445148A CN 201810250513 A CN201810250513 A CN 201810250513A CN 108445148 A CN108445148 A CN 108445148A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
- G01N31/162—Determining the equivalent point by means of a discontinuity
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- G—PHYSICS
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N21/79—Photometric titration
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Abstract
The invention discloses a kind of detection methods of bromine trifluoride product purity, include the following steps：（Ⅰ）The pre-treatment of product；（Ⅱ）The extraction of product hydrolysis liquid；（Ⅲ）Bromine trifluoride product purity is analyzed；（Ⅳ）Calculate bromine trifluoride product purity.Simple and practicable, easy to operation, at low cost, safe, high certainty of measurement of the invention directly reacts preparation with bromine especially suitable for fluorine, and by the analysis of the low bromine trifluoride product of brominated bromide content in fully distillation impurity.
Description
Technical field
The invention belongs to the detection methods of compound purity between halogen, and in particular to a kind of inspection of bromine trifluoride product purity
Survey method.
Background technology
Bromine trifluoride is compound or a kind of good solvent between most widely used halogen, many inorganic fluoride energy
It is enough to be dissolved in bromine trifluoride well, it can also make the fluorization agent of inorganic matter and organic matter, be a kind of good fluorization agent.
Bromine trifluoride product has following special chemical property：Bromine trifluoride is a kind of very strong oxidant, has strong oxygen
The property changed and strong reactivity, exposure can occur dense smoke, combustible or organic matter can be made to catch fire, can be encouraged in the scene of a fire in air
The intensity of a fire；Being contacted with water or organic compound can explode, and meet water and fiercely react, and release hypertoxic smog.
Due to the special chemical property of bromine trifluoride, to sampling, sample treatment, experimental enviroment and analysis and detection device
Apparatus proposes very high requirement, and analysis difficulty of test is very big.The country there is no the document about bromine trifluoride purity detecting at present
Report.
So far, the purity detecting of domestic and international bromine trifluoride establishes unified standard not yet, while also without corresponding enterprise
Standard, professional standard or other standards.Therefore, there is an urgent need to a kind of simple and practicable, safe and reliable detection trifluoros in this field
Change the analysis method of bromine product purity.
Invention content
The present invention proposes that the purpose is to provide a kind of bromine trifluoride in order to overcome disadvantage existing in the prior art
The detection method of product purity.
The technical scheme is that：
A kind of detection method of bromine trifluoride product purity, includes the following steps：
（Ⅰ）The pre-treatment of product
（ⅰ）By a certain amount of bromine trifluoride and deionized water be respectively put into sample cell and hydrolysis bottle in, be then placed in refrigerator into
Row freezing processing；
（ⅱ）After the deionized water in the bromine trifluoride and hydrolysis bottle in sample cell solidifies, sample cell pipe lid and hydrolysis are unscrewed
Sample cell equipped with bromine trifluoride is thrown into the hydrolysis bottle equipped with deionized water, and tightens hydrolysis bottle cap rapidly by bottle cap,
Wait for that it melts, reacts；
（ⅲ）By step（ⅱ）Acquired solution is transferred in volumetric flask with deionized water constant volume to get product hydrolysis liquid；
（Ⅱ）The extraction of product hydrolysis liquid
It takes a certain amount of product hydrolysis liquid in separatory funnel, adds a certain amount of dimethylbenzene, it is quiet after being sufficiently mixed uniformly
It sets, then discards organic layer, the dimethylbenzene for adding same volume repeats extraction process, until inorganic layer color fade or holding
Stablize, retains inorganic layer solution；
（Ⅲ）Bromine trifluoride product purity is analyzed
A certain amount of step is accurately pipetted with pipette（Ⅱ）A certain amount of sulfuric acid solution is added in iodine flask in gained inorganic layer solution
And liquor kalii iodide, it is placed on after shaking up and is protected from light place, after standing, titrated with sodium thiosulfate standard solution, wait for that solution shoals in bottle
When, starch indicator is added, solution is become colorless by blue, and solution 30s is non-discolouring, reaches titration end-point, records titration used
The volume of liquid；
（Ⅳ）Calculate bromine trifluoride product purity
Each data are substituted into formula, calculate bromine trifluoride product purity；
In formula：ωBrF3--- the purity of bromine trifluoride, unit %；γ --- test solution point takes ratio；C --- sodium thiosulfate standard
The molar concentration of solution, unit mol/L；V --- the volume of titration sodium thiosulfate standard solution, unit mL；
V0--- titration is in company with the volume of sample blank test solution consumption sodium thiosulfate standard solution, unit mL；M --- bromine trifluoride
Molal weight 136.90, g/mol；The sampling amount of m --- bromine trifluoride, unit g.
The step（ⅰ）Middle bromine trifluoride and the mass volume ratio of deionized water are calculated as 0.375 ~ 0.675 by g/mL：
10。
The step（Ⅱ）The volume ratio of middle product hydrolysis liquid and dimethylbenzene is 2：1.
The step（Ⅲ）The volume ratio of middle inorganic layer solution, sulfuric acid solution and liquor kalii iodide is 5：2：2.
The step（Ⅲ）The mass fraction of middle sulfuric acid solution is 20%, and the mass fraction of liquor kalii iodide is 10%, thio
The molar concentration of sulfuric acid sodium standard solution is 0.1 mol/L, and the mass fraction of starch indicator is 0.5%.
The step（Ⅳ）Titration consumes the volume V of sodium thiosulfate standard solution in company with sample blank test solution0Experiment
Method is：It pipettes and step（Ⅲ）The deionized water of taken inorganic layer solution same volume, is separately added into and step（Ⅲ）Trifluoro
Sulfuric acid solution, the liquor kalii iodide for changing same volume same concentrations in the analysis of bromine product purity, carry out same treatment, with identical dense
The sodium thiosulfate standard solution of degree titrates, when solution shoals in bottle, addition and step（Ⅲ）Bromine trifluoride product purity point
The starch indicator of same volume same concentrations, solution are become colorless by blue in analysis, and solution 30s is non-discolouring, reach titration eventually
Point records the volume of titrating solution used, and as titration consumes the volume of sodium thiosulfate standard solution in company with sample blank test solution
V0。
The testing principle of the present invention：
The present invention provides a kind of detection methods of the bromine trifluoride product purity suitable for laboratory, utilize indirect iodometric processes pair
Bromine trifluoride product sample carries out titrimetry.It specifically includes：Sample and deionized water are freezed respectively, the sample of freezing is thrown
Enter into the closed container equipped with chilled water.With bromine simple substance in xylene extraction hydrolyzate, the bromic acid in aqueous phase solution and excess
Potassium iodide reacts under acidic environment, generates elemental iodine.It is molten with sodium thiosulfate standard using starch solution as indicator
Liquid titrates above-mentioned solution, and the purity of bromine trifluoride is finally calculated with formula.
The beneficial effects of the invention are as follows：
The present invention provides a kind of detection methods of bromine trifluoride product purity, are suitable for direct as raw material using fluorine gas and simple substance bromine
Prepared by reaction, and by fully distilling, the detection of the low bromine trifluoride product of brominated bromide content in impurity.The present invention is simply easy
It is capable, easy to operation, at low cost, safe, high certainty of measurement.
Specific implementation mode
The detection method of bromine trifluoride product purity of the present invention is described in detail with reference to embodiment：
A kind of detection method of bromine trifluoride product purity, includes the following steps：
（Ⅰ）The pre-treatment of product
（ⅰ）By 1.5~2.5 g bromine trifluorides from being poured into sample bottle in polytetrafluoro sample cell；By the polytetrafluoro sample equipped with sample
Quality control and 500mL polytetrafluoros hydrolysis bottle equipped with 40 mL deionized waters are put into refrigerator and carry out freezing processing；
（ⅱ）After sample in polytetrafluoro dress sample tubule and the water in polytetrafluoro hydrolysis bottle solidify, polytetrafluoro hydrolysis bottle bottle is unscrewed
Lid and polytetrafluoro fill sample tubule lid, and polytetrafluoro dress sample tubule is thrown into polytetrafluoro hydrolysis bottle, hydrolysis bottle cap is tightened rapidly, waits for
It melts, reacts；
（ⅲ）By step（ⅱ）Acquired solution is transferred in volumetric flask is settled to 250mL to get product hydrolysis liquid with deionized water；
（Ⅱ）The extraction of product hydrolysis liquid
Take step（Ⅰ）100 mL of gained sample hydrolyzate adds 50 mL dimethylbenzene in separatory funnel, is sufficiently mixed uniformly
Afterwards, it places 5 minutes, discards organic layer, then pour into 50 mL dimethylbenzene and repeat extraction process, until inorganic layer color fade or guarantor
It is fixed to keep steady, and retains inorganic layer solution；
（Ⅲ）Bromine trifluoride product purity is analyzed
25 mL steps are accurately pipetted with pipette（ii）It is molten that 10 mL, 20% sulfuric acid is added in iodine flask in gained inorganic layer solution
Liquid, 10 mL, 10% liquor kalii iodides are placed on after shaking up and are protected from light place, stand after ten minutes, with 0.1 mol/L sodium thiosulfate marks
3 mL, 0.5% starch indicators are added when solution shoals in bottle in quasi- solution titration, and solution is become colorless by blue, solution
30s is non-discolouring, reaches titration end-point.The volume of record titrating solution used.
（Ⅳ）Calculate bromine trifluoride product purity
Each data are substituted into formula, calculate bromine trifluoride product purity；
In formula：ωBrF3--- the purity of bromine trifluoride, unit %；γ --- test solution point takes ratio；C --- sodium thiosulfate standard
The molar concentration of solution, unit mol/L；V --- the volume of titration sodium thiosulfate standard solution, unit mL；
V0--- titration is in company with the volume of sample blank test solution consumption sodium thiosulfate standard solution, unit mL；M --- bromine trifluoride
Molal weight 136.90, g/mol；The sampling amount of m --- bromine trifluoride, unit g.
Embodiment 1
A kind of detection method of bromine trifluoride product purity, includes the following steps：
（Ⅰ）The pre-treatment of product
（ⅰ）By 2.3747 g bromine trifluorides from being poured into sample bottle in polytetrafluoro sample cell；By the polytetrafluoro sample equipped with sample
It manages and the 500mL polytetrafluoros hydrolysis bottle equipped with 40 mL deionized waters is put into refrigerator and carries out freezing processing；
（ⅱ）After sample in polytetrafluoro sample cell and the water in polytetrafluoro hydrolysis bottle solidify, polytetrafluoro hydrolysis bottle cap is unscrewed
And polytetrafluoro sample cell pipe lid, polytetrafluoro sample cell is thrown into polytetrafluoro hydrolysis bottle, hydrolysis bottle cap is tightened rapidly, waits for that it melts
Change, reaction；
（ⅲ）By step（ⅱ）Acquired solution is transferred in volumetric flask, and be settled to 250 mL with deionized water hydrolyzes to get sample
Liquid；
（Ⅱ）The extraction of product hydrolysis liquid
Take step（Ⅰ）100 mL of gained sample hydrolyzate adds 50 mL dimethylbenzene in separatory funnel, is sufficiently mixed uniformly
Afterwards, it places 5 minutes, discards organic layer, then pour into 50 mL dimethylbenzene and repeat extraction process, until inorganic layer color fade or guarantor
It is fixed to keep steady, and retains inorganic layer solution；
（Ⅲ）Bromine trifluoride product purity is analyzed
25 mL steps are accurately pipetted with pipette（Ⅱ）It is molten that 10 mL, 20% sulfuric acid is added in iodine flask in gained inorganic layer solution
Liquid, 10 mL, 10% liquor kalii iodides are placed on after shaking up and are protected from light place, stand after ten minutes, with 0.1011 mol/L sodium thiosulfate
Standard solution titrates, and when solution shoals in bottle, 3 mL, 0.5% starch indicators is added, solution is become colorless by blue, solution
30s is non-discolouring, reaches titration end-point, and the volume for consuming sodium thiosulfate standard solution is 33.25 mL, and blank test consumes sulphur
The volume of sodium thiosulfate standard solution is 0.15 mL, and test solution point takes than being 1/10, and the purity using formula calculating bromine trifluoride is
96.46%。
Embodiment 2
A kind of detection method of bromine trifluoride product purity, includes the following steps：
（Ⅰ）The pre-treatment of product
（ⅰ）By 1.8243 g bromine trifluorides from being poured into sample bottle in polytetrafluoro sample cell；By the polytetrafluoro sample equipped with sample
It manages and the 500mL polytetrafluoros hydrolysis bottle equipped with 40 mL deionized waters is put into refrigerator and carries out freezing processing；
（ⅱ）After sample in polytetrafluoro sample cell and the water in polytetrafluoro hydrolysis bottle solidify, polytetrafluoro hydrolysis bottle cap is unscrewed
And polytetrafluoro sample cell pipe lid, polytetrafluoro sample cell is thrown into polytetrafluoro hydrolysis bottle, hydrolysis bottle cap is tightened rapidly, waits for that it melts
Change, reaction；
（ⅲ）By step（ⅱ）Acquired solution is transferred in volumetric flask, and be settled to 250 mL with deionized water hydrolyzes to get sample
Liquid；
（Ⅱ）The extraction of product hydrolysis liquid
Take step（Ⅰ）100 mL of gained sample hydrolyzate adds 50 mL dimethylbenzene in separatory funnel, is sufficiently mixed uniformly
Afterwards, it places 5 minutes, discards organic layer, then pour into 50 mL dimethylbenzene and repeat extraction process, until inorganic layer color fade or guarantor
It is fixed to keep steady, and retains inorganic layer solution；
（Ⅲ）Bromine trifluoride product purity is analyzed
25 mL steps are accurately pipetted with pipette（Ⅱ）It is molten that 10 mL, 20% sulfuric acid is added in iodine flask in gained inorganic layer solution
Liquid, 10 mL, 10% liquor kalii iodides are placed on after shaking up and are protected from light place, stand after ten minutes, with 0.1011 mol/L sodium thiosulfate
Standard solution titrates, and when solution shoals in bottle, 3 ml, 0.5% starch indicators is added, solution is become colorless by blue, solution
30s is non-discolouring, reaches titration end-point, and the volume for consuming sodium thiosulfate standard solution is 25.55 mL, and blank test consumes sulphur
The volume of sodium thiosulfate standard solution is 0.15 mL, and test solution point takes than being 1/10, and the purity of bromine trifluoride is calculated using formula
It is 96.35%.
Embodiment 3
A kind of detection method of bromine trifluoride product purity, includes the following steps：
（Ⅰ）The pre-treatment of product
（ⅰ）By 1.7397 g bromine trifluorides from being poured into sample bottle in polytetrafluoro sample cell；By the polytetrafluoro sample equipped with sample
It manages and the 500mL polytetrafluoros hydrolysis bottle equipped with 40 mL deionized waters is put into refrigerator and carries out freezing processing；
（ⅱ）After sample in polytetrafluoro sample cell and the water in polytetrafluoro hydrolysis bottle solidify, polytetrafluoro hydrolysis bottle cap is unscrewed
And polytetrafluoro sample cell pipe lid, polytetrafluoro sample cell is thrown into polytetrafluoro hydrolysis bottle, hydrolysis bottle cap is tightened rapidly, waits for that it melts
Change, reaction；
（ⅲ）By step（ⅱ）Acquired solution is transferred in volumetric flask, and be settled to 250 mL with deionized water hydrolyzes to get sample
Liquid；
（Ⅱ）The extraction of product hydrolysis liquid
Take step（Ⅰ）100 ml of gained sample hydrolyzate adds 50 mL dimethylbenzene in separatory funnel, is sufficiently mixed uniformly
Afterwards, it places 5 minutes, discards organic layer, then pour into 50 mL dimethylbenzene and repeat extraction process, until inorganic layer color fade or guarantor
It is fixed to keep steady, and retains inorganic layer solution；
（Ⅲ）Bromine trifluoride product purity is analyzed
25 mL steps are accurately pipetted with pipette（Ⅱ）It is molten that 10 mL, 20% sulfuric acid is added in iodine flask in gained inorganic layer solution
Liquid, 10 mL, 10% liquor kalii iodides are placed on after shaking up and are protected from light place, stand after ten minutes, with 0.1011 mol/L sodium thiosulfate
Standard solution titrates, and when solution shoals in bottle, 3 mL, 0.5% starch indicators is added, solution is become colorless by blue, solution
30s is non-discolouring, reaches titration end-point, and the volume for consuming sodium thiosulfate standard solution is 24.30 mL, and blank test consumes sulphur
The volume of sodium thiosulfate standard solution is 0.15 mL, and test solution point takes than being 1/10, and the purity of bromine trifluoride is calculated using formula
It is 96.07%.
Bromine trifluoride is contacted with inflammable combustible to catch fire, and hydrolysis is very violent, generate a large amount of toxic and harmful gas,
Product danger is very big, and hydrolysis vessels must be closed, and sampling amount can not be excessive.In view of the accuracy and peace of lab analysis
Quan Xing, by calculating the voltage endurance capability of bottle, which selects 500ml polytetrafluoroethylene (PTFE) bottle as hydrolysis vessels, takes
Sample amount is set to 1.5 ~ 2.5g.If hydrolyzing bottle very little, the voltage endurance capability of bottle is considered, sampling amount is with regard to very little, and consumption titrating solution is just
Can be seldom, analytical error and titration error can all increase, and in addition very little sampling amount is not easy to sampling operation；If sampling amount increases
Greatly, sampling operation danger increases, and hydrolyzing the volume of bottle must also increase, can be many with hydrolyzate out, and it is unnecessary to cause
Waste.Consider, lab analysis selects 500ml polytetrafluoroethylene (PTFE) bottle as hydrolysis bottle, and sampling amount is set to 1.5 ~ 2.5g.
When needing to expand sampling amount range, it may be selected that other resistance to pressures are good and corrosion resistant container makees hydrolysis vessels, it can
The detection for realizing wider sampling amount makes the method for the present invention using broader.With the amount of the deionized water of bromine trifluoride reaction
On the basis of ensureing bromine trifluoride complete hydrolysis, appropriate increase is being applied with ensureing to come into full contact with bromine trifluoride
In test in laboratory, when sampling amount is set to 1.5 ~ 2.5g and the amount of deionized water of bromine trifluoride reaction may be set to 40ml.
Sulfuric acid solution and liquor kalii iodide need to be excessively to ensure that bromate reacts completely in hydrolyzate, hydrolyzate bromate
Amount determines the amount of sulfuric acid solution and liquor kalii iodide.
The present invention provides a kind of detection methods of bromine trifluoride product purity, are suitable for using fluorine gas and simple substance bromine as raw material
Directly prepared by reaction, and by fully distilling, the detection of the low bromine trifluoride product of brominated bromide content in impurity.Letter of the invention
Single easy, easy to operation, at low cost, safe, high certainty of measurement, is particularly suitable for the small-scale safety test in laboratory.
Claims (6)
1. a kind of detection method of bromine trifluoride product purity, it is characterised in that：Include the following steps：
（Ⅰ）The pre-treatment of product
（ⅰ）By a certain amount of bromine trifluoride and deionized water be respectively put into sample cell and hydrolysis bottle in, be then placed in refrigerator into
Row freezing processing；
（ⅱ）After the deionized water in the bromine trifluoride and hydrolysis bottle in sample cell solidifies, sample cell pipe lid and hydrolysis are unscrewed
Sample cell equipped with bromine trifluoride is thrown into the hydrolysis bottle equipped with deionized water, and tightens hydrolysis bottle cap rapidly by bottle cap,
Wait for that it melts, reacts；
（ⅲ）By step（ⅱ）Acquired solution is transferred in volumetric flask with deionized water constant volume to get product hydrolysis liquid；
（Ⅱ）The extraction of product hydrolysis liquid
It takes a certain amount of product hydrolysis liquid in separatory funnel, adds a certain amount of dimethylbenzene, it is quiet after being sufficiently mixed uniformly
It sets, then discards organic layer, the dimethylbenzene for adding same volume repeats extraction process, until inorganic layer color fade or holding
Stablize, retains inorganic layer solution；
（Ⅲ）Bromine trifluoride product purity is analyzed
A certain amount of step is accurately pipetted with pipette（Ⅱ）A certain amount of sulfuric acid solution is added in iodine flask in gained inorganic layer solution
And liquor kalii iodide, it is placed on after shaking up and is protected from light place, after standing, titrated with sodium thiosulfate standard solution, wait for that solution shoals in bottle
When, starch indicator is added, solution is become colorless by blue, and solution 30s is non-discolouring, reaches titration end-point, records titration used
The volume of liquid；
（Ⅳ）Calculate bromine trifluoride product purity
Each data are substituted into formula, calculate bromine trifluoride product purity；
In formula：ωBrF3--- the purity of bromine trifluoride, unit %；γ --- test solution point takes ratio；C --- sodium thiosulfate standard
The molar concentration of solution, unit mol/L；V --- the volume of titration sodium thiosulfate standard solution, unit mL；
V0--- titration is in company with the volume of sample blank test solution consumption sodium thiosulfate standard solution, unit mL；M --- bromine trifluoride
Molal weight 136.90, g/mol；The sampling amount of m --- bromine trifluoride, unit g.
2. a kind of detection method of bromine trifluoride product purity according to claim 1, it is characterised in that：The step
（ⅰ）Middle bromine trifluoride and the mass volume ratio of deionized water are calculated as 0.375 ~ 0.675 by g/mL：10.
3. a kind of detection method of bromine trifluoride product purity according to claim 1, it is characterised in that：The step
（Ⅱ）The volume ratio of middle product hydrolysis liquid and dimethylbenzene is 2：1.
4. a kind of detection method of bromine trifluoride product purity according to claim 1, it is characterised in that：The step
（Ⅲ）The volume ratio of middle inorganic layer solution, sulfuric acid solution and liquor kalii iodide is 5：2：2.
5. a kind of detection method of bromine trifluoride product purity according to claim 1, it is characterised in that：The step
（Ⅲ）The mass fraction of middle sulfuric acid solution is 20%, and the mass fraction of liquor kalii iodide is 10%, sodium thiosulfate standard solution
Molar concentration is 0.1 mol/L, and the mass fraction of starch indicator is 0.5%.
6. a kind of detection method of bromine trifluoride product purity according to claim 1, it is characterised in that：The step
（Ⅳ）Titration consumes the volume V of sodium thiosulfate standard solution in company with sample blank test solution0Test method be：It pipettes and step
（Ⅲ）The deionized water of taken inorganic layer solution same volume, is separately added into and step（Ⅲ）In the analysis of bromine trifluoride product purity
Sulfuric acid solution, the liquor kalii iodide of same volume same concentrations carry out same treatment, with the sodium thiosulfate standard of same concentrations
Solution titrates, when solution shoals in bottle, addition and step（Ⅲ）Same volume is identical dense in the analysis of bromine trifluoride product purity
The starch indicator of degree, solution are become colorless by blue, and solution 30s is non-discolouring, reach titration end-point, record titrating solution used
Volume, as titration in company with sample blank test solution consumption sodium thiosulfate standard solution volume V0。
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