CN109540875A - A kind of detection method of cold rolling tin plate surface chromium content - Google Patents
A kind of detection method of cold rolling tin plate surface chromium content Download PDFInfo
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Abstract
The present invention relates to a kind of detection methods of cold rolling tin plate surface chromium content, it the described method comprises the following steps: continuously intercepting the sample of two pieces of certain sizes on pollution-free, non-corroding cold rolling tin plate to be measured, respectively with the side surface and four sides of a kind of resin-blocked sample of high temperature-resistant acid-resistant alkali, one piece of sample is submerged with sulfuric acid solution, heating is kept the temperature after boiling, and prepares solution 1 to be measured；Another piece of sample is submerged with sodium hydroxide and sodium metasilicate mixed solution, is kept the temperature after heating, solution 2 to be measured is prepared；The content for measuring chromium in solution 1,2 to be measured respectively with inductive coupling plasma emission spectrograph, calculates specimen surface chromium hydroxide and chromic oxide content with this.The method of the present invention realizes the accurate detection of the total content of chromium, chromium hydroxide content and chromic oxide content in cold rolling tin plate surface passivation layer, control accurate for cold rolling tin plate passivation technology provides condition, facilitates the promotion of cold rolling tin plate surface quality.
Description
Technical field
The invention belongs to cold rolling coating surface of steel plate chemical analysis technology fields, and in particular to a kind of cold rolling tin plate table
The detection method of face chromium content.
Background technique
Tin plate refers to that surface is coated with the steel plate of one layer of very thin pure stannum layer, has good corrosion resistance, is mainly used as
The packaging material of canned food industry, medicine etc..To improve tin plate corrosion resistance, the generation of surface SnO, life are effectively controlled
Processing must be passivated during production.In tin plating production technology, there is two class of chromating and chromium-free deactivation, chromium-free deactivation is still
It can not up to compare favourably with chromating.Correlative study shows the passivation layer of electrolytic passivation method formation mainly by aoxidizing
Chromium and chromium hydroxide composition, with the difference of passivation parameter, the composition of the two is also variant, and passivation effect is anti-corrosion for tin plate
Property, the key technical index such as sulfur resistive, adhesive force exist and significantly affect.Chromium hydroxide can be improved the wellability of coating but reduce resistance to
The isolation capacity of coating but bad with the binding force of coating can be improved in high-temperature behavior, chromium oxide.When the total chromium of tin plate sheet surface contains
One timing of amount, the optimal allocation ratio for controlling tin plate sheet surface chromium hydroxide and chromium oxide can be such that every surface quality parameter reaches
More satisfactory level, therefore need accurately to detect chromium hydroxide content in tin plate surface passivation layer and chromic oxide content.
The prior art has the text using chromium hydroxide and chromium oxide in XPS (x-ray photoelectron spectroscopy) method measurement passivation layer
Report is offered, but due to the spectral peak high superposed of chromium hydroxide and chromium oxide, is only capable of being confirmed whether there are chromium hydroxide and chromium oxide,
Quantitative detection can not be carried out respectively to the two.
The rapid assay methods of Chinese patent application publication No. CN 102411011 A, entitled tin plate sheet surface chromium content
Patent application discloses a kind of rapid assay methods of tin plate sheet surface chromium content, and this method measures template using X fluorescence spectrum method
Surface dissolution front and back chromium content, acquired results are total chromium, cannot distinguish between chromium hydroxide and chromium oxide.
The inspection of 106872445 A of Chinese patent application publication No. CN, a kind of entitled cold rolling tin plate surface chromium content
Survey method discloses a kind of method based on inductively-coupled plasma spectrometer measurement surface chromium, the device acquired results energy
Chromium hydroxide and chromium oxide are distinguished, but sample preparation operation is not stained with and applies four sides, leads to the measurement of bare area in calculation formula
There is error；Adhesive tape is limited to the sealing of tin plate, the inevitable adhesive face surface chromium dissolution of soda acid dissolved samples process, into
Solution is surveyed, measurement result is influenced；Sample course of dissolution simultaneously, addition amount of liquid is excessive, inevitably has in subsequent constant volume process beaker
Liquid residue influences the accuracy of surveyed chromium.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of detection methods of cold rolling tin plate surface chromium content.
The invention mainly solves in existing cold rolling tin plate surface passivation layer that chromium hydroxide content and chromic oxide content can not be accurate
The technical issues of measurement.
In order to solve the above technical problems, the technical scheme adopted by the invention is that: a kind of cold rolling tin plate surface chromium member
The detection method of cellulose content, described detection method includes the following steps:
(1) it samples, it is 3.5cm × 3.5cm that two block sizes are continuously intercepted on pollution-free, non-corroding cold rolling tin plate to be measured
Sample, it is unclosed with a side surface and four sides, the sample other side for a kind of resin-blocked sample of high temperature-resistant acid-resistant alkali respectively
Surface is tested surface, and two pieces of samples are respectively labeled as sample 1 and sample 2；
(2) sample 1 is placed in 300mL beaker, it is the submergence examination of 6:5 dilution heat of sulfuric acid that 100 ± 5mL concentration is added into beaker
Sample, heating keep the temperature 2 ± 0.5min after boiling, sample 1 are taken out from solution, solution is transferred to 100mL capacity together with cleaning solution
In bottle, with deionized water constant volume, the solution to be measured 1 for measuring specimen surface chromium total content is obtained；
(3) sample 2 is placed in 300mL beaker, the hydroxide that 50 ± 5mL mass concentration is 300g ± 3/L is added into beaker
The sodium silicate solution that sodium solution and 50 ± 5mL mass concentration are 200 ± 2g/L submerges sample, keep the temperature 5 after being heated to 70 ± 5 DEG C ±
1min takes out sample 2 from solution, solution is transferred in 100mL volumetric flask together with cleaning solution, with deionized water constant volume, is obtained
To the solution to be measured 2 for measuring specimen surface chromium hydroxide content；
(4) establish the working curve of chromium content Yu its spectral intensity relationship: accurately pipette 0 respectively with pipette, 1,2,3,
4, for the chromium standard solution that 5mL mass concentration is 100 μ g/mL in 100mL volumetric flask, addition concentration is 1:11 dilution heat of sulfuric acid,
It with deionized water constant volume, shakes up, measures chromium at wavelength 283.563nm with inductive coupling plasma emission spectrograph
Spectral intensity calculates the unary linear regression equation of chromium content Yu its spectral intensity relationship working curve, determines C=a+b
×ICrThe value of middle a and b, in the equation: C is chromium content, unit is μ g, and a is background equivalent concentration, unit is μ g, and b is chromium
Spectral intensity be μ g/cps, I to the conversion coefficient of quality, unitCrSpectral intensity, unit cps for chromium；
(5) total with specimen surface chromium in inductive coupling plasma emission spectrograph difference determination step (2) solution 1 to be measured
Sample Surface Hydrogen chromic oxide content in content and step (3) solution 2 to be measured eliminates impurity element with from peak two point button background method
Interference, by regression equation C=a+b × I of working curve in step (4)CrCalculate chromium content in solution 1 to be measured and to be measured
Chromium content in solution 2；
(6) calculate specimen surface chromium hydroxide and chromic oxide content: specimen surface chromium hydroxide content presses formula CCr(OH)3=C2×
1.9813×10-3/ S is calculated, C in formulaCr(OH)3For specimen surface chromium hydroxide content, unit mg/m2；Specimen surface chromium oxide
Content presses formula CCr2O3=(C1-C2)×1.4616×10-3/ S is calculated, in formula: CCr2O3For specimen surface chromic oxide content, unit
For mg/m2, C1It is μ g, C for chromium content, unit in solution 1 to be measured2It is μ g for chromium content, unit in solution 2 to be measured,
S is the area of the exposed side surface of sample, unit m2。
High temperature-resistant acid-resistant alkali resin described in step (1) of the present invention is acrylic adhesive.
It is 20 ± 2mL of dilute sulfuric acid (1+11) solution that volumetric concentration is added in step (4) of the present invention.
Inductive coupling plasma emission spectrometer measures to be measured in wavelength 283.563nm in step (4) of the present invention
Chromium spectral intensity I in solution 1 and solution to be measured 2Cr
A kind of mentality of designing of the detection method of cold rolling tin plate of the invention surface chromium content:
Composition distribution of the method for the present invention based on chromium in tin plate surface passivation layer, exists in conjunction with chromium oxide and chromium hydroxide
The difference of dissolution characteristics in different medium, with sulfuric acid solution dissolve tin plate sheet surface sour solvable chromium, that is, total chromium, with sodium hydroxide with
Sodium metasilicate mixed solution dissolves the solvable chromium, that is, chromium hydroxide of tin plate sheet surface alkali, is contained using the chromium for dissolving measured alkaline medium
Amount is scaled chromium hydroxide, obtains chromium hydroxide content in the chromium of surface；Alkaline medium is subtracted with the chromium content that sulfuric acid boils dissolution
The chromium content of dissolution, then it is scaled chromium oxide, obtain chromic oxide content in the chromium of surface.
The beneficial effects of adopting the technical scheme are that 1, the method for the present invention realizes cold rolling tin plate table
The accurate detection of the total content of chromium, chromium hydroxide content and chromic oxide content in the passivation layer of face is passivated work for cold rolling tin plate
The control accurate of skill provides condition, facilitates the promotion of cold rolling tin plate surface quality.2, the present invention is resistance to using high temperature resistant
One side surface of the resin-blocked sample of soda acid and four sides avoid the measurement error of bare area generation；It also avoids simultaneously
During soda acid dissolved samples, solution to be measured is entered using the adhesive face surface chromium dissolution of the sealing surfaces such as adhesive tape, is influenced
Measurement result.3, the method for the present invention is simple and easy to do, and detection can be completed in 30min.
Specific embodiment
Present invention will be explained in further detail combined with specific embodiments below.
Detection method includes the following steps for a kind of cold rolling tin plate surface chromium content:
It (1) is respectively 2.33,2.46,2.57 g/m using 3 kinds of quality of coating2Tin plate be sample to be tested, sampling, in no dirt
Contaminating, continuously intercepting two block sizes on the cold rolling tin plate to be measured of non-corroding is 3.5cm × 3.5cm sample, uses acrylic acid respectively
Ester gum closes a side surface and four sides for sample, and the unclosed surface in the sample other side is tested surface, and two pieces of samples are distinguished
It is labeled as sample 1 and sample 2；The step 2 time is repeated, that is, takes 3 parallel samples；
(2) sample 1 is placed in 300mL beaker, it is the submergence examination of 6:5 dilution heat of sulfuric acid that 100 ± 5mL concentration is added into beaker
Sample, heating keep the temperature 2 ± 0.5min after boiling, sample 1 are taken out from solution, solution is transferred to 100mL capacity together with cleaning solution
In bottle, with deionized water constant volume, the solution to be measured 1 for measuring specimen surface chromium total content is obtained；
(3) sample 2 is placed in 300mL beaker, the hydroxide that 50 ± 5mL mass concentration is 300 ± 3g/L is added into beaker
The sodium silicate solution that sodium solution and 50 ± 5mL mass concentration are 200 ± 2g/L submerges sample, keep the temperature 5 after being heated to 70 ± 5 DEG C ±
1min takes out sample 2 from solution, solution is transferred in 100mL volumetric flask together with cleaning solution, with deionized water constant volume, is obtained
To the solution to be measured 2 for measuring specimen surface chromium hydroxide content；
(4) establish the working curve of chromium content Yu its spectral intensity relationship: accurately pipette 0 respectively with pipette, 1,2,3,
4, for the chromium standard solution that 5mL mass concentration is 10 μ g/mL in 100mL volumetric flask, addition concentration is 1:11 dilution heat of sulfuric acid 20
± 2ml is shaken up with deionized water constant volume, is measured at 283.563 nm of wavelength with inductive coupling plasma emission spectrograph
The spectral intensity of chromium calculates the unary linear regression equation of chromium content Yu its spectral intensity relationship working curve,
Determine C=a+b × ICr(related coefficient: a is 142.2, b 4145.8 in 0.999916), in the equation: C be chromium content,
Unit is μ g, and a is background equivalent concentration, unit is μ g, and b is conversion coefficient of the spectral intensity to quality of chromium, unit is μ g/
Cps, ICrSpectral intensity, unit cps for chromium；
(5) total with specimen surface chromium in inductive coupling plasma emission spectrograph difference determination step (2) solution 1 to be measured
Sample Surface Hydrogen chromic oxide content in content and step (3) solution 2 to be measured eliminates impurity element with from peak two point button background method
Interference, by regression equation C=142.2+4145.8I of working curve in step (4)CrCalculate the chromium content in solution 1 to be measured
With the chromium content in solution 2 to be measured；
The chromium content detection result of the solution 1 to be measured of table 1 and solution to be measured 2
(6) calculate specimen surface chromium hydroxide and chromic oxide content: specimen surface chromium hydroxide content presses formula CCr(OH)3=C2×
1.9813×10-3/ S is calculated, C in formulaCr(OH)3For specimen surface chromium hydroxide content, unit mg/m2；Specimen surface chromium oxide
Content presses formula CCr2O3=(C1-C2)×1.4616×10-3/ S is calculated, in formula: CCr2O3For specimen surface chromic oxide content, unit
For mg/m2, C1It is μ g, C for chromium content, unit in solution 1 to be measured2It is μ g for chromium content, unit in solution 2 to be measured,
S is the area of the exposed side surface of sample, unit m2。
(7) implementation result of the invention
2 specimen surface chromium hydroxide of table and chromic oxide content testing result
As shown in Table 2, RSD shows that this method precision with higher, measurement result reproducibility are good less than 3%.
The above embodiments are only used to illustrate and not limit the technical solutions of the present invention, although referring to above-described embodiment to this hair
It is bright to be described in detail, those skilled in the art should understand that: still the present invention can be modified or be waited
With replacement, without departing from the spirit or scope of the invention, or any substitutions, should all cover in power of the invention
In sharp claimed range.
Claims (4)
1. a kind of detection method of cold rolling tin plate surface chromium content, which is characterized in that the detection method include with
Lower step:
(1) it samples, it is 3.5cm × 3.5cm that two block sizes are continuously intercepted on pollution-free, non-corroding cold rolling tin plate to be measured
Sample, it is unclosed with a side surface and four sides, the sample other side for a kind of resin-blocked sample of high temperature-resistant acid-resistant alkali respectively
Surface is tested surface, and two pieces of samples are respectively labeled as sample 1 and sample 2；
(2) sample 1 is placed in 300mL beaker, it is the submergence examination of 6:5 dilution heat of sulfuric acid that 100 ± 5mL concentration is added into beaker
Sample, heating keep the temperature 2 ± 0.5min after boiling, sample 1 are taken out from solution, solution is transferred to 100mL capacity together with cleaning solution
In bottle, with deionized water constant volume, the solution to be measured 1 for measuring specimen surface chromium total content is obtained；
(3) sample 2 is placed in 300mL beaker, the hydroxide that 50 ± 5mL mass concentration is 300 ± 3g/L is added into beaker
The sodium silicate solution that sodium solution and 50 ± 5mL mass concentration are 200 ± 2g/L submerges sample, keep the temperature 5 after being heated to 70 ± 5 DEG C ±
1min takes out sample 2 from solution, solution is transferred in 100mL volumetric flask together with cleaning solution, with deionized water constant volume, is obtained
To the solution to be measured 2 for measuring specimen surface chromium hydroxide content；
(4) establish the working curve of chromium content Yu its spectral intensity relationship: accurately pipette 0 respectively with pipette, 1,2,3,
4, for the chromium standard solution that 5mL mass concentration is 100 μ g/mL in 100mL volumetric flask, addition concentration is 1:11 dilution heat of sulfuric acid,
It with deionized water constant volume, shakes up, measures chromium respectively at 283.563 nm of wavelength with inductive coupling plasma emission spectrograph
The spectral intensity of element calculates the unary linear regression equation of chromium content Yu its spectral intensity relationship working curve, really
Determine C=a+b × ICrThe value of middle a and b, in the equation: C is chromium content, unit is μ g, and a is background equivalent concentration, unit μ
G, b are conversion coefficient of the spectral intensity to quality of chromium, unit is μ g/cps, ICrSpectral intensity, unit cps for chromium；
(5) total with specimen surface chromium in inductive coupling plasma emission spectrograph difference determination step (2) solution 1 to be measured
Sample Surface Hydrogen chromic oxide content in content and step (3) solution 2 to be measured eliminates impurity element with from peak two point button background method
Interference, by regression equation C=a+b × I of working curve in step (4)CrCalculate chromium content in solution 1 to be measured and to be measured
Chromium content in solution 2；
(6) calculate specimen surface chromium hydroxide and chromic oxide content: specimen surface chromium hydroxide content presses formula CCr(OH)3=C2×
1.9813×10-3/ S is calculated, C in formulaCr(OH)3For specimen surface chromium hydroxide content, unit mg/m2；Specimen surface chromium oxide
Content presses formula CCr2O3=(C1-C2)×1.4616×10-3/ S is calculated, in formula: CCr2O3For specimen surface chromic oxide content, unit
For mg/m2, C1It is μ g, C for chromium content, unit in solution 1 to be measured2It is μ g for chromium content, unit in solution 2 to be measured,
S is the area of the exposed side surface of sample, unit m2。
2. a kind of detection method of cold rolling tin plate surface according to claim 1 chromium content, which is characterized in that
High temperature-resistant acid-resistant alkali resin described in step (1) is acrylic adhesive.
3. a kind of detection method of cold rolling tin plate surface according to claim 1 chromium content, which is characterized in that
It is 20 ± 2mL of dilute sulfuric acid (1+11) solution that volumetric concentration is added in the step (4).
4. a kind of detection method of cold rolling tin plate surface chromium content according to claim 1 to 3,
It is characterized in that, inductive coupling plasma emission spectrometer is in wavelength 283.563nm measurement solution to be measured in the step (4)
1 and solution to be measured 2 in chromium spectral intensity ICr。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110243810A (en) * | 2019-07-01 | 2019-09-17 | 中国第一汽车股份有限公司 | The test method of zirconium content in a kind of metal material surface conversion film |
| CN110261198A (en) * | 2019-07-01 | 2019-09-20 | 中国第一汽车股份有限公司 | The preparation method and its quantitative approach of the standard test panel containing zirconium in a kind of metal material surface conversion film |
| CN112782257A (en) * | 2019-11-07 | 2021-05-11 | 上海梅山钢铁股份有限公司 | Method for detecting passive film component content of cold-rolled electrolytic tin-plated steel plate |
| CN113281326A (en) * | 2021-05-21 | 2021-08-20 | 安泰科技股份有限公司 | Characterization method of thickness of galvanized passivation film |
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| CN105158105A (en) * | 2015-08-28 | 2015-12-16 | 浙江鑫宙竹基复合材料科技有限公司 | Method for detecting surface water absorptivity of bamboo composite pressure pipe |
| CN106872445A (en) * | 2015-12-11 | 2017-06-20 | 上海梅山钢铁股份有限公司 | A kind of detection method of cold rolling tin plate surface chromium content |
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Patent Citations (2)
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| CN105158105A (en) * | 2015-08-28 | 2015-12-16 | 浙江鑫宙竹基复合材料科技有限公司 | Method for detecting surface water absorptivity of bamboo composite pressure pipe |
| CN106872445A (en) * | 2015-12-11 | 2017-06-20 | 上海梅山钢铁股份有限公司 | A kind of detection method of cold rolling tin plate surface chromium content |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110243810A (en) * | 2019-07-01 | 2019-09-17 | 中国第一汽车股份有限公司 | The test method of zirconium content in a kind of metal material surface conversion film |
| CN110261198A (en) * | 2019-07-01 | 2019-09-20 | 中国第一汽车股份有限公司 | The preparation method and its quantitative approach of the standard test panel containing zirconium in a kind of metal material surface conversion film |
| CN112782257A (en) * | 2019-11-07 | 2021-05-11 | 上海梅山钢铁股份有限公司 | Method for detecting passive film component content of cold-rolled electrolytic tin-plated steel plate |
| CN112782257B (en) * | 2019-11-07 | 2023-08-11 | 上海梅山钢铁股份有限公司 | Method for detecting component content of passive film of cold-rolled electroplated tin steel plate |
| CN113281326A (en) * | 2021-05-21 | 2021-08-20 | 安泰科技股份有限公司 | Characterization method of thickness of galvanized passivation film |
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Application publication date: 20190329 |