CN102978596A - Method for measuring coating amount of galvanized sheet surface trivalent chromium passivator - Google Patents
Method for measuring coating amount of galvanized sheet surface trivalent chromium passivator Download PDFInfo
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- CN102978596A CN102978596A CN2012105675396A CN201210567539A CN102978596A CN 102978596 A CN102978596 A CN 102978596A CN 2012105675396 A CN2012105675396 A CN 2012105675396A CN 201210567539 A CN201210567539 A CN 201210567539A CN 102978596 A CN102978596 A CN 102978596A
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- galvanized sheet
- passivator
- trivalent chromium
- measurement
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Abstract
The invention discloses a method for measuring coating amount of a galvanized sheet surface trivalent chromium passivator, which comprises the following steps: preparing a sulfuric acid-phosphoric acid mixture, a potassium permanganate solution, a sodium azide water solution and a diphenylsemicarbazide solution; preparing a blank solution, a sample solution and a chromium standard solution; determining and reading the absorbance of the chromium standard solution and the sample solution; and calculating the coating amount of the galvanized sheet surface passivator. The method disclosed by the invention solves the problems of small area of X-ray fluorescence spectrometer base and measurement, and has wide measuring range; and the spectrometer used for detection reduces the errors caused by visual measurement, so that the measurement is more accurate. The method has the advantages of fewer sample solution interference factors, high accuracy, simple test instruments and common test reagents, and is simple to operate.
Description
Technical field
The invention belongs to the analytical chemistry field, relate to a kind of measuring method, be specifically related to a kind of method of measuring galvanized sheet surface trivalent chromium passivator coated weight.
Background technology
Carry out Passivation Treatment on band steel thermal treatment heat zinc coating plate surface, can improve corrosion resisting property and the work-ing life of zinc coating, prevent that effectively heat zinc coating plate from corrosion occurring in storing, use procedure.The traditional passivation technology of galvanized sheet is to adopt Cr
6+Passivation, Cr
6+Zn reacts at stable, the fine and close ZnCrO of galvanized sheet Surface Creation with the galvanized sheet surface
4And Cr (OH) CrO
4Passive film, play antiseptic property.And Cr
6+In a single day passive film goes to pot, and the sexavalent chrome in the film can ooze out with the zinc surface effect and again generate passive film, and namely this film has self-repair function, and etch resistant properties is good.But Cr
6+Belong to violent in toxicity, very big to environment and harm, various countries have put into effect a series of restriction Cr in succession in recent years
6+The mandatory rules of law of using, and some clients of Europe explicitly call for the galvanized sheet employing not contain Cr
6+Passivator process.For satisfying world market and China's household electric appliances to the urgent needs of nuisanceless galvanized sheet, simultaneously in order to reduce Cr
6+To the harm of environment and human body, present domestic galvanized sheet adopts Cr more
3+Passivation and without two kinds of Cr passivation.Because passivator passivation effect Cr
6+Passivator＞Cr
3+Passivator＞without Cr passivator, present domestic most employing Cr
3+Passivator, Cr
3+Passivator and the Zn reaction of galvanized sheet surface finally generate ZnCrF2PO
4Passive film has increased the corrosion resistance nature of galvanized sheet.And chromic toxicity only has 1% of sexavalent chrome toxicity, belongs to low toxicity, and similar at many aspect of performances and sexavalent chrome, uses at present trivalent chromium to substitute the sexavalent chrome passivation.
The coated weight of passivator directly affects corrosion resistance, so the coated weight of Measurement accuracy passivator is significant.Present measuring method mainly contains following several:
1.X fluorescence spectrophotometer
Method: the galvanized sheet standard jig that used passivator must be provided by the supplier before using; This model in advance at the passivator (organizing test piece) of the known coated weight of galvanized sheet coating, uses the content of X-fluorescence spectrometer measurement Cr element by the supplier more, and Criterion contains discharge curve in instrument.Measure galvanized sheet surface C r constituent content in the actual measurement process to convert galvanized sheet passivator coated weight to.
The problem that this method exists: at first, because the penetration thickness of X ray is 70 μ m, and galvanized sheet single face zinc coating thickness is all less than 70 μ m, can say that the zinc layer is all punctured by X ray, and the Cr of different manufacturers or different heats is not identical, Cr content in the matrix is very large on the impact of the Cr content of passivator film like this, thereby has caused the inaccuracy of measuring result.Secondly, the coating of passivator can not be very even, and the survey area of X-fluorescence spectrograph is all very little, is generally the area of diameter 3.5mm, and so little area is not representative yet, and these two kinds of reasons cause the X-fluorescence spectrograph can not Measurement accuracy Cr
3+The passivator coated weight.
2.Cr
3+Colorimetric cylinder
Method: this colorimetric cylinder is a kind ofly to measure the instrument of trivalent chromium content by visual colorimetry, and characteristics are without preparing standard solution, simple and fast.
The problem that this method exists: this way is to measure the Cr of liquid pool
3+The method of content, judge according to the depth of color Cr content how much, and be ready visual contrast, although simple, quick, owing to material specification can not be unified, so the pressure of passivation squeezing roller changes, and every passivation squeezing roller hardness is also different, cause the coating rate of passivator different, and range estimation also have an error, only by the Cr of measurement liquid pool
3+Content is not enough to illustrate how many practical coating amounts is on the galvanized sheet.
3. by controlling the total acid point control coated weight of liquid pool passivating solution
Method: the coated weight of passive film, can be by adjusting the concentration (in the total acid point of passivating solution) of passivating solution, the parameters such as the pressure of passivation squeezing roller, hardness are controlled, for the ease of stablizing thickness, in actual production, think that control squeezing roller pressure and squeezing roller material hardness are constant, control coated weight by adjusting passivating solution total acid point.
The problem that this method exists: the coated weight of controlling passivator with the method for the total acid point of measuring the liquid pool passivating solution is inaccurate.The total acid point is that passivating solution enters the index that factory inspection is received, and is that the passivator of getting a certain amount of volume uses the method for titration to consume OH
-A numerical value, although passivating solution is pressed the proportioning of certain volume, the acid point changes, but because material specification can not be unified, so the pressure of passivation squeezing roller changes, and every passivation squeezing roller hardness also is different, causes the coating rate of passivator different, by the total acid point of measuring liquid pool passivator Cr on the galvanized sheet can not be described
3+How many practical coating amounts is.
4. use the coated weight of the pressure-controlling passive film of squeezing roller
Method: the control of passive film is mainly by up and down the winding-up angle of two nozzles and the pressure of the squeezing roller behind orientation and the deactivation slot are controlled in the deactivation slot.Topmost or the thickness of the pressure-controlling passive film of squeezing roller.Usually 0.5MPa pressure produces (22～30) mg/m in theory
2Passive film, 0.6MPa produces (14～20) mg/m
2Passive film.Best squeezing roller pressure awaits setting in the actual production.
The problem that this method exists: adopt the coated weight of the pressure-controlling passive film of control squeezing roller just to manage calculated value, and the Cr of liquid pool
3+Content does not detect, and because material specification is not unified, so the pressure of passivation squeezing roller also is vicissitudinous, and every passivation squeezing roller hardness also is different, judges that by the theoretical value of squeezing roller pressure the coated weight of passive film more can not truly illustrate the problem of practical coating amount.
Summary of the invention
The technical problem that (one) will solve
The technical problem to be solved in the present invention is Measurement accuracy galvanized sheet surface trivalent chromium passivator coated weight how.
(2) technical scheme
For solving the problems of the technologies described above, the invention provides a kind of method of measuring galvanized sheet surface trivalent chromium passivator coated weight, comprising:
Step 1, according to volume ratio (1.5～2.0): (1.5～2.0): (6～7) are configured to mixture of sulfuric phosphoric acid with sulfuric acid, phosphoric acid and water, the preparation mass concentration is the potassium permanganate solution of (20～25) g/L, mass concentration is the sodiumazide aqueous solution of (0.3～0.6) %, and mass concentration is two Urea,amino-solution of (1～2) %;
Step 2, with mixture of sulfuric phosphoric acid and two the Urea,amino-solution preparation blank solutions in the step 1, the preparation chromium standard solution also adds mixture of sulfuric phosphoric acid and two Urea,amino-solution therein;
Step 3 take the galvanized sheet that is coated with trivalent chromium passivator as sample, is gone out circular test piece, produces sample solution;
Step 4 adds two Urea,amino-solution in the sample solution that step 3 obtains, use distilled water diluting;
The absorbancy of chromium standard solution and sample solution is measured and read to step 5 under visible spectrophotometer wavelength 550nm, with the blank solution zeroing, with cuvette;
Step 6, the chromium standard solution that obtains according to mensuration and the absorbancy of sample solution are calculated galvanized sheet surface passivation agent coated weight.
Preferably, in described step 6, utilize following formula to calculate galvanized sheet surface trivalent chromium passivator dual coating amount:
ρ(Cr)＝(c(Cr)×20×A×10
6)/(A
0×S)
Wherein: A
0Absorbancy for chromium standard solution;
A is the absorbancy of sample solution;
S is the area of test piece, unit: mm
2
C (Cr) is the chromium concn in the chromium standard solution, unit: mg/mL;
ρ (Cr) is galvanized sheet surface trivalent chromium passivator dual coating amount, unit: mg/m
2
Preferably, in step 3, in order to the below legal system solution of materialsing:
Step 3.1 is put into beaker with circular test piece and is added mixture of sulfuric phosphoric acid and shake, and when treating that white point appears in test piece test piece is taken out;
Step 3.2 drips nitric acid, heated and boiled in solution;
Step 3.3 adds potassium permanganate solution, heated and boiled in the solution that obtains to step 3.2 again;
Step 3.4 adds the sodiumazide aqueous solution to solution and becomes colourless rear stopped heating, and the cooling beaker gets final product to get sample solution to room temperature.
Preferably, the method for calculation of the chromium concn c (Cr) in the chromium standard solution are:
Wherein, M is the quality of potassiumchromate, and unit is g.
Preferably, the volume ratio of sulfuric acid, phosphoric acid and water is 1.5: 1.5: 7 in the described mixture of sulfuric phosphoric acid.
Preferably, the mass concentration of described potassium permanganate solution is 25g/L.
Preferably, the mass concentration of the described sodiumazide aqueous solution is 0.5%.
Preferably, the mass concentration of described two Urea,amino-solution is 1%.
Preferably, described two Urea,amino-solution are two Urea,amino-ethanolic solns or two Urea,amino-acetone solns.
(3) beneficial effect
The method of measurement galvanized sheet of the present invention surface trivalent chromium passivator coated weight, do not detect the value of Cr and total acid point in the liquid pool, do not consider the problem of passivator coating rate, directly with mixture of sulfuric phosphoric acid the passivator film on the certain area of galvanized sheet is dissolved, measure the Cr content in the solution, thereby detect galvanized sheet surface passivation agent Cr content, be not subjected to material specification on the impact of passivation squeezing roller pressure with different passivation squeezing roller hardness.The method has solved X-fluorescence spectrograph matrix and the little problem of survey area, and useful range is wide in range; Detect with spectrophotometer, reduce the error that range estimation brings, so that measurement is more accurate.Present method sample solution interfering factors is few, accurately; Simple to operate, test apparatus is simple and easy, and test drug is common.Can produce line according to detected result value feedback, according to material specification passivation squeezing roller pressure, galvanized sheet temperature be adjusted, reach and satisfy the salt-fog test time greater than under 96 hours the prerequisite, use minimum passivator.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is done into a detailed description.Following examples are used for explanation the present invention, but are not used for limiting the scope of the invention.
The invention provides a kind of method of measuring galvanized sheet surface trivalent chromium passivator coated weight, measuring principle is: sample solution dissolves with mixture of sulfuric phosphoric acid, in micro acid medium, and Cr
3+(KMnO4) is oxidized to Cr by potassium permanganate
6+, Cr
6+Generate violet complex with two Urea,amino-reactions, under spectrophotometer wavelength 550nm, measure absorbancy, thereby calculate galvanized sheet surface passivation agent coated weight according to absorbancy.The concrete steps of measuring are as follows:
At first, prepare following reagent and solution:
1, with sulfuric acid (H
2SO
4) and phosphoric acid (H
3PO
4) and water be mixed with mixture of sulfuric phosphoric acid at 1.5: 1.5: 7 according to volume ratio;
2, get analytical pure potassium permanganate (KMnO
4) 25g, use first a small amount of dissolved in distilled water redilution to 1000 milliliter, compound concentration is the potassium permanganate solution of 25g/L;
3, get analytical pure sodiumazide (NaN
3) 5g, use first a small amount of dissolved in distilled water redilution to 1000 milliliter, compound concentration is 0.5% the sodiumazide aqueous solution;
4, get two Urea,amino-(C of standard reagent
13H
14N
4O) 10g with a small amount of ethanol or acetone solution redilution to 1000 milliliter, produces concentration and is two Urea,amino-dehydrated alcohols or two Urea,amino-acetone solns of 1%;
5, accurately take by weighing standard reagent potassiumchromate (K
2CrO
4) about 1.86g, accurately behind the radix point 4, use first a small amount of distilled water diluting, be settled to again 1000mL, get mentioned solution 10mL, be settled to 1000mL, this solution is chromium standard solution.Calculate chromium standard solution Cr concentration (mg/mL) according to following formula:
Wherein M is the potassiumchromate quality, and unit is g.
6, produce by the following method sample solution
6.1 with the circular test piece that punch press is gone out diameter 75mm, put into the 1000mL beaker and add 20 milliliters of mixture of sulfuric phosphoric acid and shake a moment, treat when white point appears in the test piece surface test piece to be taken out with distilled water flushing clean, solution for later use;
6.2 in solution, drip 5mL nitric acid, about two minutes of heated and boiled;
6.3 in solution, add 5mL potassium permanganate again, again boil;
Add sodiumazide to solution after 2 minutes and become colourless rear stopped heating 6.4 boil, take off beaker and be cooled to room temperature, be sample solution.
Secondly, get the steel measuring bottle of the sky of three 100ml.With the mixture of sulfuric phosphoric acid of 10ml and two Urea,amino-ethanolic solns configurations of 1ml blank solution, put into first steel measuring bottle, with distilled water diluting to scale; Preparation 20ml chromium standard solution also adds 10ml mixture of sulfuric phosphoric acid and two Urea,amino-solution of 1ml therein, second the steel measuring bottle of packing into, with distilled water diluting to scale; The sample solution that obtains in the step 6.4 is put into the 3rd steel measuring bottle, with distilled water diluting to scale.
Again, test solution is shaken up, use the cuvette of 1cm under visible spectrophotometer wavelength 550nm, with the blank solution zeroing, measure the absorbancy of chromium standard solution and sample solution.
At last, calculate result (mg/m according to following formula
2).
ρ(Cr)＝(c(Cr)×20×A×10
6)/(A
0×S)
Wherein: A
0: the absorbancy of chromium standard solution;
A: the absorbancy of sample solution;
S: the area of test piece;
C (Cr): the chromium concn in the chromium standard solution (mg/mL);
Illustrate: 1, ρ (Cr) is galvanized sheet surface C r
3+Passivator dual coating amount.
2, useful range: (15～100) mg/m
2
In implementation process of the present invention, except the concentration of listing in above-described embodiment, the concentration of all ingredients also can be: sulfuric acid, phosphoric acid and water are configured to mixture of sulfuric phosphoric acid according to volume ratio (2.0: 2.0: 6), the mass concentration of potassium permanganate solution is 20g/L or 22g/L, the mass concentration of the sodiumazide aqueous solution is 0.3% or 0.6%, the mass concentration of two Urea,amino-solution is 1.5% or 2%, all can realize goal of the invention.
The method of measurement galvanized sheet surface passivation agent coated weight of the present invention, do not detect the value of Cr and total acid point in the liquid pool, do not consider the problem of passivator coating rate, directly with mixture of sulfuric phosphoric acid the passivator film on the certain area of galvanized sheet is dissolved, measure the Cr content in the solution, thereby detect galvanized sheet surface passivation agent Cr content, be not subjected to material specification on the impact of passivation squeezing roller pressure with different passivation squeezing roller hardness.The method has solved X-fluorescence spectrograph matrix and the little problem of survey area, and useful range is wide in range; Detect with spectrophotometer, reduce the error that range estimation brings, so that measurement is more accurate.Present method sample solution interfering factors is few, accurately; Simple to operate, test apparatus is simple and easy, and test drug is common.Can produce line according to detected result value feedback, according to material specification passivation squeezing roller pressure, galvanized sheet temperature be adjusted, reach and satisfy the salt-fog test time greater than under 96 hours the prerequisite, use minimum passivator.
The below discusses Measurement accuracy galvanized sheet surface C r
3+The meaning of passivator coated weight:
1. the passivator coated weight is on the impact of salt-fog test
The coated weight of passivator directly affects corrosion resistance, at present galvanized sheet acceleration corrosion resistance represented with the salt-fog test time, when galvanized sheet put into stop after 5% oxidation appears in the salt-spray cabinet rear surface test, be designated as the salt-fog test time, galvanized sheet surface passivation agent coated weight is to the corresponding relation of salt-fog test time as can be seen from Table 1.
Annotate: passivator producer is different, and measuring result is different, carries out the testing data contrast according to actual result.
Table 1 is for using metric measurement same specification galvanized sheet DIFFERENT Cr content and salt-fog test time
Mean value and uncertainty with the steel plate of the same content of metric measurement see Table 2
Table 2 mean value and the uncertainty of the same coated weight of metric measurement
2. salt-fog test and coated weight are to the guidance of matched proportion density
Table 3 is different galvanized sheet material specification passivator coated weights under the different passivator proportionings
According to table 3 as can be known, in the situation that matched proportion density increases, chromium content on the galvanized sheet raises, but the variation owing to passivation squeezing roller pressure under the identical proportioning causes galvanized sheet surface passivation agent coated weight different with every passivation squeezing roller hardness not equal a series of reasons of difference, material specification different and the galvanized sheet temperature, is irrational so be issued to control galvanized sheet surface passivation agent coated weight in the means of controlling passivator groove proportioning.
3. determine the benefit that matched proportion density brings
Advise that according to the supplier passivating solution was according to 1: 1 proportioning, the salt-fog test time all can reach 108 hours, reach individually 120 hours, even longer, satisfy salt-fog test time requirement (96 hours) fully, but reduce the cost when meeting customer need, according to 1: 1 proportioning passivating solution excessive concentration, according to actual proportioning adjustment, find that proportioning was 1: 1.2 (passivating solution stoste: in the time of de-salted water), satisfy the salt-fog test time fully more than 96 hours, satisfy client's requirement, according to when galvanized sheet thickness (0.8～1.0) the mm specification, according in 1: 1 proportioning situation, loss per ton steel passivator (0.5～0.6) Kg; But according to satisfying 1: 1.2 proportioning of customer demand more than 96 hours, loss per ton steel is (0.4～0.5) Kg, such loss per ton steel about 0.1Kg that descends, according to 45000 yuan/tons of calculating of passivator, the ton steel is saved 4.5 yuan of passivator, calculates according to 15000 tons of galvanized sheets of monthly output, and a month reduction cost is about 67500 yuan, when producing the galvanized sheet thickness reduction, month reduction cost is larger.
The above only is preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.
Claims (9)
1. a method of measuring galvanized sheet surface trivalent chromium passivator coated weight is characterized in that, comprising:
Step 1, according to volume ratio (1.5～2.0): (1.5～2.0): (6～7) are configured to mixture of sulfuric phosphoric acid with sulfuric acid, phosphoric acid and water, the preparation mass concentration is the potassium permanganate solution of (20～25) g/L, mass concentration is the sodiumazide aqueous solution of (0.3～0.6) %, and mass concentration is two Urea,amino-solution of (1～2) %;
Step 2, with mixture of sulfuric phosphoric acid and two the Urea,amino-solution preparation blank solutions in the step 1, the preparation chromium standard solution also adds mixture of sulfuric phosphoric acid and two Urea,amino-solution therein;
Step 3 take the galvanized sheet that is coated with trivalent chromium passivator as sample, is gone out circular test piece, produces sample solution;
Step 4 adds two Urea,amino-solution in the sample solution that step 3 obtains, use distilled water diluting;
The absorbancy of chromium standard solution and sample solution is measured and read to step 5 under visible spectrophotometer wavelength 550nm, with the blank solution zeroing, with cuvette;
Step 6, the chromium standard solution that obtains according to mensuration and the absorbancy of sample solution are calculated galvanized sheet surface passivation agent coated weight.
2. the method for the surperficial trivalent chromium passivator coated weight of measurement galvanized sheet as claimed in claim 1 is characterized in that, in described step 6, utilizes following formula to calculate galvanized sheet surface trivalent chromium passivator dual coating amount:
ρ(Cr)＝(c(Cr)×20×A×10
6)/(A
0×S)
Wherein: A
0Absorbancy for chromium standard solution;
A is the absorbancy of sample solution;
S is the area of test piece, unit: mm
2
C (Cr) is the chromium concn in the chromium standard solution, unit: mg/mL;
ρ (Cr) is galvanized sheet surface trivalent chromium passivator dual coating amount, unit: mg/m
2
3. the method for measurement galvanized sheet as claimed in claim 1 surface trivalent chromium passivator coated weight is characterized in that, in step 3, in order to the below legal system solution of materialsing:
Step 3.1 is put into beaker with circular test piece and is added mixture of sulfuric phosphoric acid and shake, and when treating that white point appears in test piece test piece is taken out;
Step 3.2 drips nitric acid, heated and boiled in solution;
Step 3.3 adds potassium permanganate solution, heated and boiled in the solution that obtains to step 3.2 again;
Step 3.4 adds the sodiumazide aqueous solution to solution and becomes colourless rear stopped heating, and the cooling beaker gets final product to get sample solution to room temperature.
4. the method for measurement galvanized sheet as claimed in claim 2 surface trivalent chromium passivator coated weight is characterized in that the method for calculation of the chromium concn c (Cr) in the chromium standard solution are:
Wherein, M is the quality of potassiumchromate, and unit is g.
5. the method for the surperficial trivalent chromium passivator coated weight of measurement galvanized sheet as claimed in claim 1 is characterized in that the volume ratio of sulfuric acid, phosphoric acid and water is 1.5: 1.5: 7 in the described mixture of sulfuric phosphoric acid.
6. the method for the surperficial trivalent chromium passivator coated weight of measurement galvanized sheet as claimed in claim 1 is characterized in that the mass concentration of described potassium permanganate solution is 25g/L.
7. the method for the surperficial trivalent chromium passivator coated weight of measurement galvanized sheet as claimed in claim 1 is characterized in that the mass concentration of the described sodiumazide aqueous solution is 0.5%.
8. the method for the surperficial trivalent chromium passivator coated weight of measurement galvanized sheet as claimed in claim 1 is characterized in that the mass concentration of described two Urea,amino-solution is 1%.
9. the method for the surperficial trivalent chromium passivator coated weight of measurement galvanized sheet as claimed in claim 1 is characterized in that described two Urea,amino-solution are two Urea,amino-ethanolic solns or two Urea,amino-acetone solns.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104878332A (en) * | 2015-06-03 | 2015-09-02 | 河北钢铁股份有限公司邯郸分公司 | Production method for improving corrosion resistance of heat-based galvanized sheet and strip products |
| CN109604336A (en) * | 2018-10-24 | 2019-04-12 | 首钢京唐钢铁联合有限责任公司 | A kind of preparation method and device of heat zinc coating plate |
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| JP2005274503A (en) * | 2004-03-26 | 2005-10-06 | Matsushita Electric Ind Co Ltd | Method and device for measuring hexavalent chromium |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS5044983A (en) * | 1973-08-24 | 1975-04-22 | ||
| JP2005274503A (en) * | 2004-03-26 | 2005-10-06 | Matsushita Electric Ind Co Ltd | Method and device for measuring hexavalent chromium |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104878332A (en) * | 2015-06-03 | 2015-09-02 | 河北钢铁股份有限公司邯郸分公司 | Production method for improving corrosion resistance of heat-based galvanized sheet and strip products |
| CN109604336A (en) * | 2018-10-24 | 2019-04-12 | 首钢京唐钢铁联合有限责任公司 | A kind of preparation method and device of heat zinc coating plate |
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| CN102978596B (en) | 2015-08-05 |
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