CN103645274B - Measure the method for chloride ion content in cold-rolling emulsion - Google Patents
Measure the method for chloride ion content in cold-rolling emulsion Download PDFInfo
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- CN103645274B CN103645274B CN201310637835.3A CN201310637835A CN103645274B CN 103645274 B CN103645274 B CN 103645274B CN 201310637835 A CN201310637835 A CN 201310637835A CN 103645274 B CN103645274 B CN 103645274B
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Abstract
The invention discloses a kind of method measuring chloride ion content in cold-rolling emulsion, its using after the mixed solvent of cold-rolling emulsion and acetic acid and isopropyl alcohol mixes as titrated dose, take silver nitrate standard solution as titrant, adopt automatical potentiometric titrimeter to measure.The chlorion that this method utilizes automatic potential titrator tests to determine in cold-rolling emulsion, solve chlorion in cold-rolling emulsion cannot accurately, the difficult problem of Fast Measurement, can determine the content of chlorion in cold-rolling emulsion accurately and rapidly, the control of rolling production line emulsion for cold rolling mill acid provides strong Data support; And be conducive to sour rolling line and take effective method to carry out best organization of production, guarantee the cold-strip steel of production high-quality, thus greatly improve the economic benefit of cold rolling mill.This method utilizes existing instrument and equipment to carry out, simple to operate, be easy to realize, accuracy is high, favorable reproducibility.
Description
Technical field
The present invention relates to a kind of chemical analysis method, especially a kind of method measuring chloride ion content in cold-rolling emulsion.
Background technology
The desalted water that chlorion in cold-rolling emulsion remains chlorion and preparation emulsion primarily of belt steel surface after pickling is introduced.In emulsion, the existence of chlorion is extremely harmful to steel rolling, when chlorine ion concentration reaches 50mg/L, can destroy the passivating film of belt steel surface and cause belt steel surface local corrosion, the annealed process of steel plate after rolling simultaneously can produce spot, affects plate surface quality.Therefore accurately detect the content of chlorion in emulsion, and strictly controlled, for raising cold-strip steel quality, there is very large effect.
In emulsion, chloride ion conductor is our difficult problem always, originally adopts Cl always
-+ Ag
+the principle of=AgCl precipitation, although this method is feasible in theory, but the selection of indicator is not easy very much, potassium chromate with 5% and superfluous silver ion react and generate henna siliver chromate and precipitate, this applicable chlorion measured in clarification water sample, it is obvious that color from yellow becomes Chinese red, but with the emulsion crossed originally as grey, it is not obvious that yellow becomes Chinese red, and relative error can reach 50%.Adopted the mercuric nitrate complexometry when pH=3 afterwards, in emulsion, chlorion generates stable complex compound, and when arriving titration end-point, excessive mercury ion and diphenyl carbazone react and generate purple blue complex compound, to indicate titration end-point.Adopt distilled water to do blank titration simultaneously, reduce relative error, but drip nitric acid when regulating pH value, easily adjusted, make variable color inaccurate, pH value often adjusted 0.2, and institute surveys chloride ion content will higher about 30mg/L, was in this way also unsuitable for production testing.At present domestic there is no a kind of can accurately, fast and titration end-point significantly measures the analytical approach of chlorion in emulsion.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method measuring chloride ion content in cold-rolling emulsion accurately and rapidly.
For solving the problems of the technologies described above, the technical solution used in the present invention is: its using after the mixed solvent of cold-rolling emulsion and acetic acid and isopropyl alcohol mixes as titrated dose, take silver nitrate standard solution as titrant, adopt automatical potentiometric titrimeter to measure.
The volume ratio of cold-rolling emulsion of the present invention and mixed solvent is 2 ~ 4:5.
In mixed solvent of the present invention, the volume ratio of acetic acid and isopropyl alcohol is 1:9.
Automatical potentiometric titrimeter of the present invention impose a condition as speed of agitator 30%; 60s consuming time; Titrant concentration 0.01mol/L; Titrant adds pattern for dynamically to add pattern; DE(setting value) 9.0mL; DV(is minimum) 0.006mL; DV(is maximum) 0.4mL; Receive measured value for balance control model; Stop maximum volume 20mL; The number of EQP point is 1.
The present invention also comprises blank analysis process: with mixed solvent blank solvent, and silver nitrate standard solution is titrant, adopts automatical potentiometric titrimeter to measure.Automatical potentiometric titrimeter imposes a condition as speed of agitator 30% in described blank analysis process; 10s consuming time; Titrant concentration 0.01mol/L; Titrant adds pattern for dynamically to add pattern; DE(setting value) 9.0mL; DV(is minimum) 0.004mL; DV(is maximum) 0.4mL; Receive measured value for balance control model; Stop maximum volume 2mL; The number of EQP point is 1.
The beneficial effect that produces of technique scheme is adopted to be: the chlorion that the present invention utilizes automatic potential titrator tests to determine in cold-rolling emulsion, solve chlorion in cold-rolling emulsion cannot accurately, the difficult problem of Fast Measurement, can determine the content of chlorion in cold-rolling emulsion accurately and rapidly, the control of rolling production line emulsion for cold rolling mill acid provides strong Data support; And be conducive to sour rolling line and take effective method to carry out best organization of production, guarantee the cold-strip steel of production high-quality, thus greatly improve the economic benefit of cold rolling mill.The inventive method utilizes existing instrument and equipment to carry out, simple to operate, be easy to realize, accuracy is high, favorable reproducibility.
Embodiment
Below in conjunction with specific embodiment, the present invention is further detailed explanation.
In this mensuration cold-rolling emulsion, the method for chloride ion content utilizes automatic potential titrator tests to determine the content of chlorion in cold-rolling emulsion.First the routine analyzer that automatic potential titrator tests determines chlorion in emulsion is created, setting titrator speed of agitator: 30%; Consuming time: 60s; Titrant concentration: 0.01mol/L; Titrant adds pattern: dynamically add pattern; DE(setting value): 9.0mL; DV (minimum): 0.006mL; DV (maximum): 0.4mL; Receive measured value: balance control model; Stop maximum volume: 20mL; The number of EQP point: 1.
Find the cold-rolling emulsion sample of direct titration not solubilizer process when measuring sample, titration end-point not easily occurs, occurs terminal once in a while, and titration value is also unstable.After through repeatedly repeatedly testing, in cold-rolling emulsion sample, add isopropyl alcohol and acetic acid mixed solvent, acetic acid in mixed solvent: isopropyl alcohol=1:9(volume), cold-rolling emulsion: mixed solvent=2 ~ 4:5(volume); Mixed solvent can dissolve the medium oil composition of emulsion, ensures to keep constant pH in titration process, reduces the solubleness of silver chloride simultaneously thus makes titration end-point more easy to identify and more stable.After adding isopropyl alcohol and acetic acid mixed solvent, measurement result introduces blank value, and the blank value that the production batch difference because of medicine measures is different, so preferably before mensuration cold-rolling emulsion sample or Simultaneously test blank value.
Create the blank value routine analyzer that automatic potential titrator tests determines chlorion in cold-rolling emulsion, setting titrator speed of agitator: 30%; Consuming time: 10s; Titrant concentration: 0.01mol/L; Titrant adds pattern: dynamically add pattern; DE(setting value): 9.0mL; DV (minimum): 0.004mL; DV (maximum): 0.4mL; Receive measured value: balance control model; Stop maximum volume: 2mL; The number of EQP point: 1.
Before measuring emulsion sample, first getting 50mL blank solvent uses the blank value routine analyzer of chlorion in cold-rolling emulsion to measure blank value, get 20 ~ 40mL cold-rolling emulsion again, add 50mL blank solvent, use chloride ion conductor program in cold-rolling emulsion to measure, when there is titration end-point, routine analyzer deducts the analysis result that blank value calculates chlorion in emulsion automatically.
Embodiment 1: this assay method adopts following concrete technology step.
One, automatical potentiometric titrimeter creates the routine analyzer measuring chlorion in cold-rolling emulsion: setting titrator speed of agitator: 30%; Consuming time: 60s; Titrant concentration: 0.01mol/L; Titrant adds pattern: dynamically add pattern; DE(setting value): 9.0mL; DV (minimum): 0.006mL; DV (maximum): 0.4mL; Receive measured value: balance control model; Stop maximum volume: 20mL; The number of EQP point: 1.
Two, automatical potentiometric titrimeter creates and measures blank value routine analyzer: setting titrator speed of agitator: 30%; Consuming time: 10s; Titrant concentration: 0.01mol/L; Titrant adds pattern: dynamically add pattern; DE(setting value): 9.0mL; DV (minimum): 0.004mL; DV (maximum): 0.4mL; Receive measured value: balance control model; Stop maximum volume: 2mL; The number of EQP point: 1.
Three, the preparation of silver nitrate standard solution (0.01mol/L) and demarcation:
The preparation of a, silver nitrate standard solution (0.1mol/L): take 17.5 grams of silver nitrates, be dissolved in 1000ml water, shake up.Solution is stored in brown volumetric flask.
B, chlorion standard solution (CL
-: 1mg/mL) preparation: take 1.6485 grams and be dissolved in the water in 500 ~ 600 DEG C of little benchmark sodium chloride up to constant weight of calcination 2, move in 1000ml volumetric flask, be diluted with water to scale, shake up.
The preparation of c, potassium chromate (50g/L): take 5.0 grams of potassium chromates and be dissolved in 100mL water.
The demarcation of d, silver nitrate standard solution (0.1mol/L): draw chlorion standard solution (CL
-: 1mg/mL) 25ml is in 150ml beaker, add water 50ml, add 1, phenolphthalein, red just disappearance is adjusted to NaOH and nitric acid, add potassium chromate indicator 10, be titrated to bolarious siliver chromate precipitation with 0.1mol/L silver nitrate standard solution and appear as terminal, record the volume of the silver nitrate standard solution consumed.Blank value synchronous operation.
E, silver nitrate standard solution (mol/L), calculate by following formula (I):
In formula (I),
V
1: 0.1mol/L silver nitrate (AgNO during titration
3) consumption (mL) of standard solution;
V
0: 0.1mol/L silver nitrate (AgNO when titration is blank
3) consumption (mL) of standard solution;
Wherein: 1.6485 for taking the quality (g) of benchmark sodium chloride; 58.443 is the molal weight (g/mol) of sodium chloride; 25 for drawing the volume (mL) of chlorion standard solution; 1 is the constant volume 1000mL of chlorion standard solution.
Calculate silver nitrate standard solution to obtain concentration and be: 0.1006mol/L.
The preparation of f, silver nitrate standard solution (0.01mol/L): accurately pipette 0.1mol/L silver nitrate standard solution 100mL in 1000mL volumetric flask, be diluted with water to scale, shake up.Silver nitrate concentration after dilution is 0.0100mol/L.
Four, blank solvent (mixed solvent) measure blank value is prepared: measure 100mL acetic acid and 900mL isopropyl alcohol in 1000mL reagent bottle, mixing.Pipette 50mL blank solvent in sample cup for liquid, the silver nitrate standard solution of 0.01mol/L is as titrant, and use automatical potentiometric titrimeter blank determination program to carry out titration, after arriving titration end-point, instrument records blank value automatically, and blank value is 0.001mmol.
Five, produce emulsion sample and measure its chloride ion content: pipetting cold-rolling emulsion subnatant 20mL in sample cup for liquid, add 50mL mixed solvent as titrated dose, the silver nitrate standard solution of 0.01mol/L is as titrant, use automatical potentiometric titrimeter cold-rolling emulsion to measure program and carry out titration, after arriving titration end-point, instrument uses cold-rolling emulsion sample drop definite value to connect with the formula of blank solvent titration value and calculates, and in display cold-rolling emulsion, determination of chloride ion value is 28.356ppm.
Embodiment 2: this assay method adopts following concrete technology step.
Step one to step 3 with embodiment 1.
Four, blank solvent (mixed solvent) measure blank value is prepared: measure 100mL acetic acid and 900mL isopropyl alcohol in 1000mL reagent bottle, mixing.Pipette 50mL blank solvent in sample cup for liquid, the silver nitrate standard solution of 0.01mol/L is as titrant, and use automatical potentiometric titrimeter blank determination program to carry out titration, after arriving titration end-point, instrument records blank value automatically, and blank value is 0.002mmol.
Five, produce emulsion sample and measure its chloride ion content: pipetting cold-rolling emulsion subnatant 25mL in sample cup for liquid, add 50mL blank solvent, the silver nitrate standard solution of 0.01mol/L is as titrant, use automatical potentiometric titrimeter cold-rolling emulsion to measure program and carry out titration, after arriving titration end-point, instrument uses rolled samples titration value to connect with the formula of blank solvent titration value and calculates, and showing cold rolling middle chlorine ion content determination value is 16.735ppm.
Embodiment 3: this assay method adopts following concrete technology step.
Step one to step 3 with embodiment 1.
Four, blank solvent (mixed solvent) measure blank value is prepared: measure 100mL acetic acid and 900mL isopropyl alcohol in 1000mL reagent bottle, mixing.Pipette 50mL blank solvent in sample cup for liquid, the silver nitrate standard solution of 0.01mol/L is as titrant, and use automatical potentiometric titrimeter blank determination program to carry out titration, after arriving titration end-point, instrument records blank value automatically, and blank value is 0.001mmol.
Five, produce emulsion sample and measure its chloride ion content: pipetting cold-rolling emulsion subnatant 30mL in sample cup for liquid, add 50mL blank solvent, use automatical potentiometric titrimeter cold-rolling emulsion to measure program and carry out titration, after arriving titration end-point, instrument uses cold-rolling emulsion sample drop definite value to connect with the formula of blank solvent titration value and calculates, and in display cold-rolling emulsion, chlorine ion content determination value is 8.893ppm.
For verifying feasibility of the present invention, do the inspection of precision test, accuracy test and measurement range at the conditions of the experiments described above.
Precision test: get 11 parts, same emulsion sample and use automatic potential titrator tests its chloride ion content fixed, calculate its relative standard deviation, experimental data is in table 1.
Table 1: Precision test result
Accuracy test: the chlorion standard substance adding inequality in emulsion sample, use automatic potential titrator tests to determine the recovery, experimental data is in table 2.
Table 2: accuracy test result
Show that the precision of this method, accuracy all can meet production analysis requirement by above data, be applicable to production testing completely.
Claims (4)
1. one kind measures the method for chloride ion content in cold-rolling emulsion, it is characterized in that: its using after the mixed solvent of cold-rolling emulsion and acetic acid and isopropyl alcohol mixes as titrated dose, take silver nitrate standard solution as titrant, adopt automatical potentiometric titrimeter to measure; Described cold-rolling emulsion: the volume ratio of mixed solvent is 2 ~ 4:5; Acetic acid in described mixed solvent: the volume ratio of isopropyl alcohol is 1:9.
2. the method for chloride ion content in mensuration cold-rolling emulsion according to claim 1, is characterized in that, described automatical potentiometric titrimeter impose a condition as speed of agitator 30%; 60s consuming time; Titrant concentration 0.01mol/L; Titrant adds pattern for dynamically to add pattern; DE setting value is 9.0mL; DV minimum value 0.006mL; DV maximal value is 0.4mL; Receive measured value for balance control model; Stop maximum volume 20mL; The number of EQP point is 1.
3. the method for chloride ion content in mensuration cold-rolling emulsion according to claim 1 and 2, it is characterized in that, it also comprises blank analysis process: using mixed solvent as blank solvent, and silver nitrate standard solution is titrant, adopts automatical potentiometric titrimeter to measure.
4. the method for chloride ion content in mensuration cold-rolling emulsion according to claim 3, is characterized in that, in described blank analysis process, automatical potentiometric titrimeter imposes a condition as speed of agitator 30%; 10s consuming time; Titrant concentration 0.01mol/L; Titrant adds pattern for dynamically to add pattern; DE setting value is 9.0mL; DV minimum value is 0.004mL; DV maximal value is 0.4mL; Receive measured value for balance control model; Stop maximum volume 2mL; The number of EQP point is 1.
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| CN104459020B (en) * | 2014-12-15 | 2016-06-01 | 山东鑫泉医药有限公司 | 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone detection method of content |
| CN105136894B (en) * | 2015-07-24 | 2017-10-17 | 铜陵有色金属集团股份有限公司金冠铜业分公司 | The assay method of chloride ion content in copper electrolyte |
| CN106908566A (en) * | 2015-12-23 | 2017-06-30 | 中国石油天然气股份有限公司 | Method for measuring chloride content in water |
| CN110618128B (en) * | 2019-10-15 | 2021-11-09 | 河海大学 | Test bar for rapidly testing concentration of chloride ions in concrete and preparation method and application thereof |
| CN113671111B (en) * | 2021-08-26 | 2024-04-19 | 金能化学(齐河)有限公司 | Method for quantitatively detecting chloride ions in potassium sorbate |
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