CN103645274A - Method for determining content of chlorine ion in cold-rolled emulsified liquid - Google Patents
Method for determining content of chlorine ion in cold-rolled emulsified liquid Download PDFInfo
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- CN103645274A CN103645274A CN201310637835.3A CN201310637835A CN103645274A CN 103645274 A CN103645274 A CN 103645274A CN 201310637835 A CN201310637835 A CN 201310637835A CN 103645274 A CN103645274 A CN 103645274A
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Abstract
The invention discloses a method for determining the content of chlorine ions in a cold-rolled emulsified liquid. According to the method, the cold-rolled emulsified liquid is uniformly mixed with a mixed solvent of acetic acid and isopropanol to be used as a titrated solution and a silver nitrate standard solution is used as a titrating solution; an automatic potential titrator is used for determining. According to the method, the automatic potential titrator is used for determining the chlorine ions in the cold-rolled emulsified liquid and the difficulty that the chlorine ions in the cold-rolled emulsified liquid cannot be determined accurately and rapidly is overcome; the content of the chlorine ions in the cold-rolled emulsified liquid can be determined accurately and rapidly so as to provide a powerful data support for the control of the emulsified liquid in an acid rolling production line of a cold rolling mill; the method is good for carrying out optimal production organization through an acid rolling line by adopting an effective method so as to ensure that high-quality cold-rolled band steel is produced, and furthermore, the economic benefits of the cold rolling mill are improved. The method for determining the content of the chlorine ions in the cold-rolled emulsified liquid is carried out by adopting existing instruments and equipment, and is easy to operate, easy to realize, high in accuracy and good in repeatability.
Description
Technical field
The present invention relates to a kind of chemical analysis method, especially a kind of method of measuring chloride ion content in cold-rolling emulsion.
Background technology
Chlorion in cold-rolling emulsion is mainly introduced by the desalted water of the residual chlorion of belt steel surface after pickling and preparation emulsion.In emulsion, the existence of chlorion is extremely harmful to steel rolling, when chlorine ion concentration reaches 5 0mg/L, can destroy the passivating film of belt steel surface and cause belt steel surface local corrosion, the annealed processing of steel plate after rolling simultaneously can produce spot, affects plate surface quality.Therefore accurately detect the content of chlorion in emulsion, and strictly control, for improving cold-strip steel quality, there is very large effect.
In emulsion, the mensuration of chlorion 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% reacts with superfluous silver ion and generates henna siliver chromate precipitation, chlorion in this applicable mensuration clarification water sample, it is obvious that color becomes Chinese red from yellow, but by the emulsion basis of crossing as grey, it is not obvious that yellow becomes Chinese red, and relative error can reach 50%.Adopted afterwards mercuric nitrate complexometry when pH=3, in emulsion, chlorion generates stable complex compound, and while arriving titration end-point, excessive mercury ion reacts with diphenyl carbazone and generates purple blue complex compound, to indicate titration end-point.Adopt distilled water to do blank titration simultaneously, reduce relative error, but when dripping nitric acid and regulating pH value, easily adjusted, make variable color inaccurate, pH value is every adjusted 0.2, the chloride ion content of surveying will higher about 30mg/L, the production testing that is in this way also unsuitable for.At present domestic there is no a kind of can be accurately, quick 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 of measuring accurately and rapidly chloride ion content in cold-rolling emulsion.
For solving the problems of the technologies described above, the technical solution used in the present invention is: its mixed solvent using cold-rolling emulsion and acetic acid and isopropyl alcohol mixes rear as titrated dose, take silver nitrate standard solution as titrant, adopts 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.
Imposing a condition as speed of agitator 30% of automatical potentiometric titrimeter of the present invention; 60s consuming time; Titrant concentration 0.01mol/L; Titrant interpolation pattern is dynamic appending pattern; DE(setting value) 9.0mL; DV(is minimum) 0.006mL; DV(is maximum) 0.4mL; Receiving measured value is balance control model; Stop maximum volume 20mL; The number that EQP is ordered is 1.
The present invention also comprises blank analysis process: with mixed solvent blank solvent, 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 0.01 mol/L; Titrant interpolation pattern is dynamic appending pattern; DE(setting value) 9.0mL; DV(is minimum) 0.004mL; DV(is maximum) 0.4mL; Receiving measured value is balance control model; Stop maximum volume 2mL; The number that EQP is ordered is 1.
The beneficial effect that adopts technique scheme to produce is: the present invention utilizes automatic potential titrator tests to determine the chlorion in cold-rolling emulsion, having solved chlorion in cold-rolling emulsion cannot be accurately, a difficult problem for Fast Measurement, can determine accurately and rapidly the content of chlorion in cold-rolling emulsion, 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, thereby 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, and 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 create automatic potential titrator tests and determine the routine analyzer of chlorion in emulsion, set titrator speed of agitator: 30%; Consuming time: 60s; Titrant concentration: 0.01 mol/L; Titrant adds pattern: dynamic appending pattern; DE(setting value): 9.0mL; DV (minimum): 0.006 mL; DV (maximum): 0.4 mL; Receive measured value: balance control model; Stop maximum volume: 20 mL; The number that EQP is ordered: 1.
When measuring sample, find the direct titration cold-rolling emulsion sample that solubilizer is not processed, titration end-point is not prone to, and occurs once in a while terminal, and titration value is also unstable.After through repeatedly repeatedly experiment, 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 oiliness composition in emulsion, guarantee to keep constant pH in titration process, thereby the solubleness that simultaneously reduces silver chloride makes titration end-point more easy to identify and more stable.After adding isopropyl alcohol and acetic acid mixed solvent, measurement result has been introduced blank value, because of the different blank values of measuring of the production batch of medicine different, so be preferably in measure cold-rolling emulsion sample before or measure blank value simultaneously.
Create automatic potential titrator tests and determine the blank value routine analyzer of chlorion in cold-rolling emulsion, set titrator speed of agitator: 30%; Consuming time: 10s; Titrant concentration: 0.01 mol/L; Titrant adds pattern: dynamic appending pattern; DE(setting value): 9.0mL; DV (minimum): 0.004 mL; DV (maximum): 0.4 mL; Receive measured value: balance control model; Stop maximum volume: 2 mL; The number that EQP is ordered: 1.
Measure before emulsion sample, first get the blank value routine analyzer mensuration blank value that 50mL blank solvent is used chlorion in cold-rolling emulsion, get again 20~40mL cold-rolling emulsion, add 50mL blank solvent, use the mensuration program of chlorion in cold-rolling emulsion to measure, while 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 of measuring chlorion in cold-rolling emulsion: set titrator speed of agitator: 30%; Consuming time: 60s; Titrant concentration: 0.01 mol/L; Titrant adds pattern: dynamic appending pattern; DE(setting value): 9.0mL; DV (minimum): 0.006 mL; DV (maximum): 0.4 mL; Receive measured value: balance control model; Stop maximum volume: 20 mL; The number that EQP is ordered: 1.
Two, automatical potentiometric titrimeter creates and measures blank value routine analyzer: set titrator speed of agitator: 30%; Consuming time: 10s; Titrant concentration: 0.01 mol/L; Titrant adds pattern: dynamic appending pattern; DE(setting value): 9.0mL; DV (minimum): 0.004 mL; DV (maximum): 0.4 mL; Receive measured value: balance control model; Stop maximum volume: 2mL; The number that EQP is ordered: 1.
Three, preparation and the demarcation of silver nitrate standard solution (0.01mol/L):
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
-: preparation 1mg/ mL): take 1.6485 grams and be dissolved in the water in the 2 hours benchmark sodium chloride to constant weight of 500~600 ℃ of calcinations, 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, with NaOH and nitric acid, be adjusted to red just disappearance, add 10 of potassium chromate indicator, with 0.1mol/L silver nitrate standard solution, be titrated to bolarious siliver chromate precipitation and appear as terminal, the volume of the silver nitrate standard solution that record consumes.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.
Calculating silver nitrate standard solution obtains concentration and is: 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, prepare blank solvent (mixed solvent) and measure blank value: measuring 100mL acetic acid and 900 mL isopropyl alcohols in 1000mL reagent bottle, mix.Pipette 50mL blank solvent in sample cup for liquid, the silver nitrate standard solution of 0.01mol/L, as titrant, is used automatical potentiometric titrimeter blank determination program to carry out titration, arrives after titration end-point, and 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 mensuration program to carry out titration, arrive after titration end-point, instrument uses cold-rolling emulsion sample drop definite value to connect and calculate with the formula of blank solvent titration value, shows that in cold-rolling emulsion, determination of chloride ion value is 28.356ppm.
Embodiment 2: this assay method adopts following concrete technology step.
Step 1 to step 3 with embodiment 1.
Four, prepare blank solvent (mixed solvent) and measure blank value: measuring 100mL acetic acid and 900 mL isopropyl alcohols in 1000mL reagent bottle, mix.Pipette 50mL blank solvent in sample cup for liquid, the silver nitrate standard solution of 0.01mol/L, as titrant, is used automatical potentiometric titrimeter blank determination program to carry out titration, arrives after titration end-point, and 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 mensuration program to carry out titration, arrive after titration end-point, instrument uses rolled samples titration value to connect and calculate with the formula of blank solvent titration value, shows that cold rolling middle chlorine ion content determination value is 16.735ppm.
Embodiment 3: this assay method adopts following concrete technology step.
Step 1 to step 3 with embodiment 1.
Four, prepare blank solvent (mixed solvent) and measure blank value: measuring 100mL acetic acid and 900 mL isopropyl alcohols in 1000mL reagent bottle, mix.Pipette 50mL blank solvent in sample cup for liquid, the silver nitrate standard solution of 0.01mol/L, as titrant, is used automatical potentiometric titrimeter blank determination program to carry out titration, arrives after titration end-point, and 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 mensuration program to carry out titration, arrive after titration end-point, instrument uses cold-rolling emulsion sample drop definite value to connect and calculate with the formula of blank solvent titration value, shows that in cold-rolling emulsion, chlorine ion content determination value is 8.893ppm.
For verifying feasibility of the present invention, precision test, accuracy test and measurement range check under above-mentioned test condition, have been done.
Precision test: get 11 parts, same emulsion sample and use fixed its chloride ion content of automatic potential titrator tests, calculate its relative standard deviation, experimental data is in Table 1.
Table 1: Precision test result
Accuracy test: add the chlorion standard substance of inequality in emulsion sample, use automatic potential titrator tests to determine the recovery, experimental data is in Table 2.
Table 2: accuracy test result
By above data, show that precision, the accuracy of this method all can meet production and analyze requirement, be applicable to production testing completely.
Claims (6)
1. a method of measuring chloride ion content in cold-rolling emulsion, it is characterized in that: its mixed solvent using cold-rolling emulsion and acetic acid and isopropyl alcohol mixes rear as titrated dose, take silver nitrate standard solution as titrant, adopt automatical potentiometric titrimeter to measure.
2. the method for chloride ion content in mensuration cold-rolling emulsion according to claim 1, is characterized in that: the volume ratio of described cold-rolling emulsion and mixed solvent is 2~4:5.
3. the method for chloride ion content in mensuration cold-rolling emulsion according to claim 1, is characterized in that: in described mixed solvent, the volume ratio of acetic acid and isopropyl alcohol is 1:9.
4. the method for chloride ion content in mensuration cold-rolling emulsion according to claim 1, is characterized in that, the imposing a condition as speed of agitator 30% of described automatical potentiometric titrimeter; 60s consuming time; Titrant concentration 0.01mol/L; Titrant interpolation pattern is dynamic appending pattern; DE(setting value) 9.0mL; DV(is minimum) 0.006mL; DV(is maximum) 0.4mL; Receiving measured value is balance control model; Stop maximum volume 20mL; The number that EQP is ordered is 1.
5. according to the method for chloride ion content in the mensuration cold-rolling emulsion described in claim 1-4 any one, it is characterized in that, it also comprises blank analysis process: with mixed solvent blank solvent, silver nitrate standard solution is titrant, adopts automatical potentiometric titrimeter to measure.
6. the method for chloride ion content in mensuration cold-rolling emulsion according to claim 5, 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 0.01 mol/L; Titrant interpolation pattern is dynamic appending pattern; DE(setting value) 9.0mL; DV(is minimum) 0.004mL; DV(is maximum) 0.4mL; Receiving measured value is balance control model; Stop maximum volume 2mL; The number that EQP is ordered is 1.
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CN110618128A (en) * | 2019-10-15 | 2019-12-27 | 河海大学 | Test bar for rapidly testing concentration of chloride ions in concrete and preparation method and application thereof |
CN113671111A (en) * | 2021-08-26 | 2021-11-19 | 金能科技股份有限公司 | Method for quantitatively detecting chloride ions in potassium sorbate |
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CN104459020A (en) * | 2014-12-15 | 2015-03-25 | 山东鑫泉医药有限公司 | Method for detecting content of 1-chloroformyl-3-mesyl-2-imidazolidone |
CN105136894A (en) * | 2015-07-24 | 2015-12-09 | 铜陵有色金属集团股份有限公司金冠铜业分公司 | Determination method of chloride ion content of copper electrolyte |
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 | The assay method of chloride content in water |
CN110618128A (en) * | 2019-10-15 | 2019-12-27 | 河海大学 | Test bar for rapidly testing concentration of chloride ions in concrete and preparation method and application thereof |
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 |
CN113671111A (en) * | 2021-08-26 | 2021-11-19 | 金能科技股份有限公司 | Method for quantitatively detecting chloride ions in potassium sorbate |
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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