CN102978596B - Measure the method for galvanized sheet surface trivalent chromium coated weight - Google Patents
Measure the method for galvanized sheet surface trivalent chromium coated weight Download PDFInfo
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Abstract
The invention discloses a kind of method measuring galvanized sheet surface trivalent chromium coated weight, comprise step: preparation mixture of sulfuric phosphoric acid, potassium permanganate solution, aqueous sodium azide and two Urea,amino-solution; Produce blank solution, sample solution and chromium standard solution; Measure and read the absorbancy of chromium standard solution and sample solution; Calculate galvanized sheet surface passivator coated weight.The method of measurement galvanized sheet surface trivalent chromium coated weight of the present invention, this method solve X fluorescence spectrometer matrix and the little problem of survey area, useful range is wide in range; Detect with spectrophotometer, reduce the error estimated and bring, make measurement 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.
Description
Technical field
The invention belongs to analytical chemistry field, relate to a kind of measuring method, be specifically related to a kind of method measuring galvanized sheet surface trivalent chromium coated weight.
Background technology
Carry out Passivation Treatment on band steel heat treatment heat zinc coating plate surface, corrosion resisting property and the work-ing life of zinc coating can be improved, effectively prevent heat zinc coating plate from storing, use procedure, occurring corrosion.The traditional passivation technology of galvanized sheet adopts Cr
6+passivation, Cr
6+with galvanized sheet surface Zn react stablize at galvanized sheet Surface Creation, densification ZnCrO
4with Cr (OH) CrO
4passive film, play antiseptic property.And Cr
6+passive film is once go to pot, and the sexavalent chrome in film can ooze out and again generate passive film with zinc surface effect, 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 used, and some clients of Europe explicitly call for galvanized sheet to adopt not containing Cr
6+passivator process.For meeting 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, current domestic galvanized sheet many employings Cr
3+passivation and without Cr passivation two kinds.Due to passivator passivation effect Cr
6+passivator > Cr
3+passivator > without Cr passivator, current domestic most employing Cr
3+passivator, Cr
3+passivator and galvanized sheet surface Zn react, and finally generate ZnCrF2PO
4passive film, adds the corrosion resistance nature of galvanized sheet.And chromic toxicity only has 1% of sexavalent chrome toxicity, belong to low toxicity, and similar at many aspect of performances and sexavalent chrome, and use trivalent chromium substitutes sexavalent chrome passivation at present.
The coated weight of passivator directly affects corrosion resistance, so the coated weight of Measurement accuracy passivator is significant.Current measuring method mainly contains following several:
1.X fluorescence spectrophotometer
Method: the galvanized sheet standard jig that passivator used must be provided by supplier before use; This model applies the passivator (organizing test piece) of known coated weight by supplier in advance on galvanized sheet, and use X fluorescence spectrometer to measure the content of Cr element, in instrument, Criterion is containing discharge curve.Galvanized sheet surface C r constituent content is measured to convert galvanized sheet passivator coated weight in actual measurement process.
This method Problems existing: first, penetration thickness due to X-ray is 70 μm, and galvanized sheet one side zinc coating thickness is all less than 70 μm, can say that zinc layers is all punctured by X-ray, and the Cr of different manufacturers or different heat is not identical, Cr content in such matrix is very large on the impact of the Cr content of passivator film, thus result in the inaccuracy of measuring result.Secondly, the coating of passivator can not be very even, and the survey area of X fluorescence spectrometer is all very little, is generally the area of diameter 3.5mm, and area little is like this not representative yet, and these two kinds of reasons cause X fluorescence spectrometer can not Measurement accuracy Cr
3+passivator coated weight.
2.Cr
3+colorimetric cylinder
A kind of method: this colorimetric cylinder is instrument carrying out measuring trivalent chromium content by visual colorimetry, and feature is without preparing standard solution, simple and fast.
This method Problems existing: this way measures the Cr of liquid pool
3+the method of content, judge that Cr content is how many according to the depth of color, and be ready visual contrast, although simple, quick, because 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 error, only by measuring the Cr of liquid pool
3+content is not enough to illustrate that on galvanized sheet, practical coating amount is how many.
3. by controlling the total acid point control coated weight of liquid pool passivating solution
Method: the coated weight of passive film, by adjusting the concentration (in the total acid of passivating solution point) of passivating solution, the parameter such as pressure, hardness of passivation squeezing roller controls, for the ease of stable thickness, in actual production, think control squeezing roller pressure and squeezing roller material hardness constant, control coated weight by adjustment passivating solution total acid point.
This method Problems existing: the coated weight controlling passivator by the method for the total acid point measuring liquid pool passivating solution is inaccurate.Total acid point is the index that passivating solution enters factory inspection receipts, is that the method for the passivator titration of getting a certain amount of volume consumes OH
-a numerical value, although passivating solution presses the proportioning of certain volume, acid point is change, but because material specification can not be unified, so the pressure of passivation squeezing roller changes, and every passivation squeezing roller hardness is also different, causes the coating rate of passivator different, by the total acid point measuring liquid pool, passivator Cr on galvanized sheet can not be described
3+practical coating amount is how many.
4. with the coated weight of the pressure-controlling passive film of squeezing roller
Method: the control of passive film controls mainly through the pressure of the squeezing roller after the winding-up angle of two nozzles upper and lower in deactivation slot and orientation and 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 actual production.
This method Problems existing: adopt the coated weight of the pressure-controlling passive film controlling 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 is also vicissitudinous, and every passivation squeezing roller hardness is also different, the theoretical value by squeezing roller pressure judges that the coated weight of passive film more truly can not illustrate the problem of practical coating amount.
Summary of the invention
(1) technical problem that will solve
The technical problem to be solved in the present invention is how Measurement accuracy galvanized sheet surface trivalent chromium coated weight.
(2) technical scheme
For solving the problems of the technologies described above, the invention provides a kind of method measuring galvanized sheet surface trivalent chromium coated weight, comprising:
Step 1, according to volume ratio (1.5 ~ 2.0): (1.5 ~ 2.0): sulfuric acid, phosphoric acid and water are configured to mixture of sulfuric phosphoric acid by (6 ~ 7), preparation mass concentration is the potassium permanganate solution of (20 ~ 25) g/L, mass concentration is the aqueous sodium azide of (0.3 ~ 0.6) %, and mass concentration is two Urea,amino-solution of (1 ~ 2) %;
Step 2, with the mixture of sulfuric phosphoric acid in step 1 and two Urea,amino-solution preparation blank solutions, preparation chromium standard solution also adds mixture of sulfuric phosphoric acid and two Urea,amino-solution wherein;
Step 3, to be coated with the galvanized sheet of trivalent chromium passivator for sample, to go out circular test piece, produces sample solution;
Step 4, adds two Urea,amino-solution, with distilled water diluting in the sample solution that step 3 obtains;
Step 5, with cuvette under visible spectrophotometer wavelength 550nm, with blank solution zeroing, measures and reads the absorbancy of chromium standard solution and sample solution;
Step 6, calculates galvanized sheet surface passivator coated weight according to the absorbancy measuring chromium standard solution and the sample solution obtained.
Preferably, in described step 6, following formula is utilized to calculate galvanized sheet surface trivalent chromium dual coating amount:
ρ(Cr)＝(c(Cr)×20×A×10
6)/(A
0×S)
Wherein: A
0for the absorbancy of 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 chromium standard solution, unit: mg/mL;
ρ (Cr) is galvanized sheet surface trivalent chromium dual coating amount, unit: mg/m
2.
Preferably, in step 3, to materials solution in order to below legal system:
Step 3.1, puts into beaker and adds mixture of sulfuric phosphoric acid shake, test piece taken out when white point appears in test piece by circular test piece;
Step 3.2, drips nitric acid, heated and boiled in solution;
Step 3.3, then add potassium permanganate solution, heated and boiled in the solution obtained to step 3.2;
Step 3.4, adds aqueous sodium azide to solution and becomes colourless rear stopping heating, cooling beaker to room temperature, sample solution.
Preferably, the method for calculation of the chromium concn c (Cr) in chromium standard solution are:
Wherein, M is the quality of potassiumchromate, and unit is g.
Preferably, in described mixture of sulfuric phosphoric acid, the volume ratio of sulfuric acid, phosphoric acid and water is 1.5: 1.5: 7.
Preferably, the mass concentration of described potassium permanganate solution is 25g/L.
Preferably, the mass concentration of described aqueous sodium azide 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 surface trivalent chromium coated weight of the present invention, do not detect the value of Cr and total acid point in liquid pool, do not consider the problem of passivator coating rate, passivator film on certain for galvanized sheet area dissolves by direct mixture of sulfuric phosphoric acid, measure the Cr content in solution, thus detect galvanized sheet surface passivator Cr content, by the impact of material specification on passivation squeezing roller pressure and different passivation squeezing roller hardness.This method solve X fluorescence spectrometer matrix and the little problem of survey area, useful range is wide in range; Detect with spectrophotometer, reduce the error estimated and bring, make measurement 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.Line can be produced according to detected result value feedback, according to material specification, passivation squeezing roller pressure, galvanized sheet temperature be adjusted, reach and meet under the salt-fog test time is greater than the prerequisite of 96 hours, use minimum passivator.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is done into a detailed description.Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
The invention provides a kind of method measuring galvanized sheet surface trivalent chromium coated weight, measuring principle is: sample solution mixture of sulfuric phosphoric acid dissolves, in micro acid medium, and Cr
3+cr is oxidized to by potassium permanganate (KMnO4)
6+, Cr
6+react with two Urea,amino-and generate violet complex, under spectrophotometer wavelength 550nm, measure absorbancy, thus calculate galvanized sheet surface passivator coated weight according to absorbancy.The concrete steps measured are as follows:
First, following reagent and solution is prepared:
1, by sulfuric acid (H
2sO
4) and phosphoric acid (H
3pO
4) and water be mixed with mixture of sulfuric phosphoric acid according to volume ratio 1.5: 1.5: 7;
2, analytical pure potassium permanganate (KMnO is got
4) 25g, first dissolve redilution to 1000 milliliter with a small amount of distilled water, compound concentration is the potassium permanganate solution of 25g/L;
3, analytical pure sodiumazide (NaN is got
3) 5g, first dissolve redilution to 1000 milliliter with a small amount of distilled water, compound concentration is the aqueous sodium azide of 0.5%;
4, standard reagent two Urea,amino-(C are got
13h
14n
4o) 10g, with a small amount of ethanol or acetone solution redilution to 1000 milliliter, produces two Urea,amino-dehydrated alcohols or two Urea,amino-acetone solns that concentration is 1%;
5, standard reagent potassiumchromate (K is accurately taken
2crO
4) about 1.86g, after accurate radix point 4, first use a small amount of distilled water diluting, then be settled to 1000mL, get above-mentioned solution 10mL, be settled to 1000mL, this solution is chromium standard solution.Chromium standard solution Cr concentration (mg/mL) is calculated according to following formula:
Wherein M is potassiumchromate quality, and unit is g.
6, sample solution is produced by the following method
6.1 go out the circular test piece of diameter 75mm with punch press, put into 1000mL beaker and add 20 milliliters of mixture of sulfuric phosphoric acid shakes for a moment, when white point appears in strip, test piece is taken out with distilled water flushing clean, solution for later use;
6.2 drip 5mL nitric acid in solution, heated and boiled about two minutes;
6.3 add 5mL potassium permanganate again in solution, again boil;
6.4 boil and to add sodiumazide to solution after 2 minutes and become colourless rear stoppings and heating, and take off beaker and are cooled to room temperature, be sample solution.
Secondly, the steel measuring bottle of the sky of three 100ml is got.With mixture of sulfuric phosphoric acid and 1ml bis-Urea,amino-ethanolic soln configuration blank solutions of 10ml, 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 1ml bis-Urea,amino-solution wherein, loads second steel measuring bottle, with distilled water diluting to scale; The sample solution obtained in step 6.4 is put into the 3rd steel measuring bottle, with distilled water diluting to scale.
Again, test solution is shaken up, with the cuvette of 1cm under visible spectrophotometer wavelength 550nm, with blank solution zeroing, measure the absorbancy of chromium standard solution and sample solution.
Finally, result (mg/m is calculated 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 (mg/mL) in chromium standard solution;
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 listed 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 aqueous sodium azide 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 passivator coated weight of the present invention, do not detect the value of Cr and total acid point in liquid pool, do not consider the problem of passivator coating rate, passivator film on certain for galvanized sheet area dissolves by direct mixture of sulfuric phosphoric acid, measure the Cr content in solution, thus detect galvanized sheet surface passivator Cr content, by the impact of material specification on passivation squeezing roller pressure and different passivation squeezing roller hardness.This method solve X fluorescence spectrometer matrix and the little problem of survey area, useful range is wide in range; Detect with spectrophotometer, reduce the error estimated and bring, make measurement 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.Line can be produced according to detected result value feedback, according to material specification, passivation squeezing roller pressure, galvanized sheet temperature be adjusted, reach and meet under the salt-fog test time is greater than the prerequisite of 96 hours, use minimum passivator.
Measurement accuracy galvanized sheet surface C r is discussed below
3+the meaning of passivator coated weight:
1. passivator coated weight is on the impact of salt-fog test
The coated weight of passivator directly affects corrosion resistance, current galvanized sheet accelerates corrosion resistance and represents with the salt-fog test time, put into after 5% oxidation appears in salt-spray cabinet rear surface when galvanized sheet and stop test, be designated as the salt-fog test time, galvanized sheet surface passivator coated weight is to the corresponding relation of salt-fog test time as can be seen from Table 1.
Note: passivator producer is different, and measuring result is different, carries out 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
By the mean value of the steel plate of the same content of metric measurement and uncertainty in 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 weight under different passivator proportioning
Known according to table 3, when matched proportion density increases, chromium content on galvanized sheet raises, but the difference of and galvanized sheet temperature different with every passivation squeezing roller hardness due to the change of passivation squeezing roller pressure, the not equal a series of reason of material specification cause galvanized sheet surface passivator coated weight different under identical proportioning, so be issued in the means controlling passivator groove proportioning, to control galvanized sheet surface passivator coated weight be irrational.
3. determine the benefit that matched proportion density brings
Advise that passivating solution is according to 1: 1 proportioning according to supplier, the salt-fog test time all can reach 108 hours, reach individually 120 hours, even longer, meet salt-fog test time requirement (96 hours) completely, but reduce the cost while meeting customer need, according to 1: 1 proportioning passivating solution excessive concentration, adjust according to actual proportioning, find that proportioning is when 1: 1.2 (passivating solution stoste: de-salted water), meet the salt-fog test time completely more than 96 hours, meet the requirement of client, according to when galvanized sheet thickness (0.8 ~ 1.0) mm specification, according in 1: 1 proportioning situation, loss per ton steel passivator (0.5 ~ 0.6) Kg, but according to meeting 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 declines about 0.1Kg, according to passivator 45000 yuan/ton calculating, passivator 4.5 yuan saved by ton steel, calculates, reduce costs by the moon and be about 67500 yuan according to monthly output 15000 tons of galvanized sheets, when producing galvanized sheet thickness and reducing, the moon reduces costs larger.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing 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 (7)
1. measure a method for galvanized sheet surface trivalent chromium coated weight, it is characterized in that, comprising:
Step 1, according to volume ratio (1.5 ~ 2.0): (1.5 ~ 2.0): sulfuric acid, phosphoric acid and water are configured to mixture of sulfuric phosphoric acid by (6 ~ 7), preparation mass concentration is the potassium permanganate solution of (20 ~ 25) g/L, mass concentration is the aqueous sodium azide of (0.3 ~ 0.6) %, and mass concentration is the diphenylamino urea solution of (1 ~ 2) %;
Step 2, with the mixture of sulfuric phosphoric acid in step 1 and phenylaniline urea solution preparation blank solution, preparation chromium standard solution also adds mixture of sulfuric phosphoric acid and diphenylamino urea solution wherein;
Step 3, to be coated with the galvanized sheet of trivalent chromium passivator for sample, to go out circular test piece, produces sample solution;
Step 4, adds diphenylamino urea solution, with distilled water diluting in the sample solution that step 3 obtains;
Step 5, with cuvette under visible spectrophotometer wavelength 550nm, with blank solution zeroing, measures and reads the absorbancy of chromium standard solution and sample solution;
Step 6, calculates galvanized sheet surface passivator coated weight according to the absorbancy measuring chromium standard solution and the sample solution obtained;
In step 3, to materials solution in order to below legal system:
Step 3.1, puts into beaker and adds mixture of sulfuric phosphoric acid shake, test piece taken out when white point appears in test piece by circular test piece;
Step 3.2, drips nitric acid, heated and boiled in solution;
Step 3.3, then add potassium permanganate solution, heated and boiled in the solution obtained to step 3.2;
Step 3.4, adds aqueous sodium azide to solution and becomes colourless rear stopping heating, cooling beaker to room temperature, sample solution;
In described step 6, following formula is utilized to calculate galvanized sheet surface trivalent chromium dual coating amount:
ρ(Cr)＝(c(Cr)×20×A×10
6)/(A
0×S)
Wherein: A
0for the absorbancy of 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 chromium standard solution, unit: mg/mL;
ρ (Cr) is galvanized sheet surface trivalent chromium dual coating amount, unit: mg/m
2.
2. the method measuring galvanized sheet surface trivalent chromium coated weight as claimed in claim 1, it is characterized in that, the method for calculation of the chromium concn c (Cr) in chromium standard solution are:
Wherein, M is the quality of potassiumchromate, and unit is g.
3. the method measuring galvanized sheet surface trivalent chromium coated weight as claimed in claim 1, it is characterized in that, in described mixture of sulfuric phosphoric acid, the volume ratio of sulfuric acid, phosphoric acid and water is 1.5: 1.5: 7.
4. the method measuring galvanized sheet surface trivalent chromium coated weight as claimed in claim 1, it is characterized in that, the mass concentration of described potassium permanganate solution is 25g/L.
5. the method measuring galvanized sheet surface trivalent chromium coated weight as claimed in claim 1, it is characterized in that, the mass concentration of described aqueous sodium azide is 0.5%.
6. the method measuring galvanized sheet surface trivalent chromium coated weight as claimed in claim 1, it is characterized in that, the mass concentration of described diphenylamino urea solution is 1%.
7. the method measuring galvanized sheet surface trivalent chromium coated weight as claimed in claim 1, it is characterized in that, described diphenylamino urea solution is phenylaniline urea ethanolic soln or phenylaniline urea acetone soln.
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| [日]无机应用比色分析编辑委员会.吸收光度法.《元素实用光度分析》.辽宁科学技术出版社,1988,第228-232页. * |
| 热镀锌钢板表面铬的分光光度计法测试及研究;单凯军等;《第二届薄钢板质量研讨会论文集》;20040422;第156页-第158页 * |
| 胡之德等.合金钢中铬的测定—二苯基卡巴肼光度法.《分光光度分析法》.宁夏人民出版社,1987,第455-456页. * |
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Address after: No. 396, Chaoxia Road, Dagang Economic and Technological Development Zone, Binhai New Area, Tianjin 300270 Patentee after: Tianjin Xintian steel cold rolled plate Co.,Ltd. Address before: 300270 middle section of Wanquan Road, Dagang Economic Development Zone, Binhai New Area, Tianjin Patentee before: TIANJIN ROLLING-ONE STEEL Co.,Ltd. |