CN111678912B - Method for measuring residual carbon content on surface of cold-rolled sheet - Google Patents
Method for measuring residual carbon content on surface of cold-rolled sheet Download PDFInfo
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- CN111678912B CN111678912B CN202010556965.4A CN202010556965A CN111678912B CN 111678912 B CN111678912 B CN 111678912B CN 202010556965 A CN202010556965 A CN 202010556965A CN 111678912 B CN111678912 B CN 111678912B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 50
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 36
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 114
- 239000002390 adhesive tape Substances 0.000 claims abstract description 69
- 230000003595 spectral effect Effects 0.000 claims abstract description 21
- 239000002253 acid Substances 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 32
- 238000001514 detection method Methods 0.000 claims description 16
- 238000009616 inductively coupled plasma Methods 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000012224 working solution Substances 0.000 claims description 10
- 230000001070 adhesive effect Effects 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000012295 chemical reaction liquid Substances 0.000 claims description 8
- 229910021536 Zeolite Inorganic materials 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 7
- 239000010457 zeolite Substances 0.000 claims description 7
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 description 19
- 229910052742 iron Inorganic materials 0.000 description 19
- 239000010959 steel Substances 0.000 description 19
- 230000003749 cleanliness Effects 0.000 description 12
- 239000003921 oil Substances 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 239000010731 rolling oil Substances 0.000 description 9
- 238000004458 analytical method Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 238000004821 distillation Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000002250 absorbent Substances 0.000 description 4
- 230000002745 absorbent Effects 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000002310 reflectometry Methods 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 3
- 239000010960 cold rolled steel Substances 0.000 description 3
- 230000008878 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000007865 diluting Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 230000001939 inductive effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005096 rolling process Methods 0.000 description 3
- 239000012086 standard solution Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
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Abstract
The application discloses a method for measuring the residual carbon content on the surface of a cold-rolled sheet, which comprises the following steps: obtain an area S and a weight M 1 The first adhesive tape is used for completely adhering residues on the surface of the cold-rolled sheet to be tested to obtain the adhesive tape with the weight of M 2 Obtaining the weight M of the residue on the surface of the cold-rolled sheet in unit area; obtaining a standard working curve of Fe; the second adhesive tape is completely reacted with acid liquor, and then solid-liquid separation is carried out to obtain the Fe-containing adhesive tape 2+ A solution; the Fe content is measured 2+ Spectral line intensity of the solution; the Fe-containing material 2+ Substituting the spectral line intensity of the solution into the standard working curve of Fe to obtain the Fe-containing material 2+ Concentration C of the solution; obtaining the weight M of the iron powder in the surface residues of the cold-rolled sheet in unit area according to the concentration C Fe The method comprises the steps of carrying out a first treatment on the surface of the According to the weight M and the weight M Fe Obtaining the residual carbon content of the surface of the cold-rolled sheet in a unit area; the method can accurately measure the content of residual carbon on the surface of the cold-rolled sheet, and is simple to operate and short in time consumption.
Description
Technical Field
The application relates to the field of cold-rolled steel sheet surface chemical analysis, in particular to a method for measuring residual carbon content on the surface of a cold-rolled steel sheet.
Background
With the increasing competition of steel market, for cold-rolled products, users have put forward higher requirements on the performance and the shape of the cold-rolled steel plate, and also put forward higher requirements on the surface cleanliness of the steel plate. Because the cleanliness of the surface of the cold-rolled sheet can directly influence the subsequent process, if the surface residues of the cold-rolled sheet are too high, coating defects can be caused, and great trouble is brought to downstream users; on the other hand, the surface cleanliness of the cold-rolled sheet has a great influence on the corrosion resistance of the cold-rolled sheet. Xu and the like find that the surface residues obviously influence the uniformity of the corrosion resistance distribution of the rolled steel plate, and the corrosion resistance of the cleaned steel plate is better; the corrosion resistance of the annealed steel plate surface is poor in uniformity, and the corrosion resistance of the cleaned steel plate is better than that of the unwashed steel plate. Therefore, enterprises at home and abroad take the surface cleanliness of the cold-rolled sheet as an important basis for evaluating the quality of the product.
At present, cold-rolled sheet factories at home and abroad search for the surface cleanliness of steel plates, and mainly study on rolling procedures and annealing procedures. The results show that the residue composition of the surface is different in different processes of the cold-rolled sheet. After rolling, the cold-rolled sheet is heated to a certain temperature and maintained for a certain period of time by a subsequent heat treatment, with the main residues of lubricating oil and iron powder, so as to obtain a uniform structure and desired mechanical properties. In the heat treatment process, the residual rolling oil on the surface of the cold-rolled sheet volatilizes, but carbon with different forms is left to adhere to the surface of the cold-rolled sheet, and iron powder, residual carbon and partial oil adhering to the surface of the cold-rolled sheet are residues on the surface of the cold-rolled strip steel when leaving the factory, and if the residual content left on the surface of the cold-rolled sheet is higher, the cleanliness of the surface of the cold-rolled sheet is lower, otherwise, if the residual content of the surface of the cold-rolled sheet is lower, the cleanliness of the surface of the cold-rolled sheet is higher. Therefore, many steel enterprises have great care in selecting rolling oil, and by selecting rolling oil with better quality, the content of residues on the surface of the cold-rolled sheet is better controlled, and the better cleanliness is very important.
Currently, the most common evaluation method is to judge the content of residues on the surface of the steel plate after rolling by adopting the reflectivity of the surface of the steel plate. In general, the higher the reflectivity, the lower the residual content of the cold-rolled surface, the better the cleanliness of the cold-rolled sheet surface; conversely, the lower the reflectivity, the higher the content of residues on the surface of the cold-rolled sheet, the poorer the surface cleanliness of the cold-rolled sheet; because the reflectivity of the surface of the steel plate and the residual oil and iron powder content of the surface of the steel plate are not in a complete linear relation, the method can make macroscopic judgment on the general trend, but can not directly measure the residual content of the surface of the cold-rolled plate; some researchers also adopt a direct weight method to detect residual oil and iron powder on the surface of the steel plate, but the residual rolling oil and iron powder on the surface of the steel plate after the cold-rolled plate is rolled have very low content, and the error of the direct weight method is very large, so that the surface quality of the steel plate cannot be accurately reflected; the method for measuring the residual oil and residual iron content on the surface of the cold-rolled sheet is formulated in the existing industry standard YB/T4302-2012' measuring method for residual oil and residual iron content on the surface of the cold-rolled sheet, wherein a distillation separation method is adopted in the standard, residual oil on absorbent gauze for wiping the sheet thickness of the steel sheet is separated and extracted, then the absorbent gauze is weighed, and finally the residual oil content in unit area is calculated; in addition, the residual iron in the detected area is repeatedly wiped by using absorbent gauze dipped with petroleum ether until no oil stain is visually observed on the gauze, the iron powder adhered on the absorbent gauze is dissolved by using hydrochloric acid, and the iron content in the solution is finally converted into the residual iron content in unit area by using a photometry method. In the process of measuring the residual oil content, distillation and extraction are needed, the operation is complicated, and the whole experiment process is time-consuming.
Therefore, how to develop a method for measuring the residual carbon content on the surface of the cold-rolled sheet, which is simple to operate and short in time consumption, can accurately measure the residual carbon content on the surface of the cold-rolled sheet, and becomes a key problem for research of metallurgical workers.
Disclosure of Invention
The application aims to provide a method for measuring the content of residual carbon on the surface of a cold-rolled sheet, which can accurately measure the content of residual carbon on the surface of the cold-rolled sheet, and is simple to operate and short in time consumption.
In order to achieve the above purpose, the application provides a method for measuring the residual carbon content on the surface of a cold-rolled sheet, which comprises the following steps:
obtain an area S and a weight M 1 The first adhesive tape is used for completely adhering residues on the surface of the cold-rolled sheet to be tested to obtain the adhesive tape with the weight of M 2 According to the area S, the weight M 1 And weight M 2 Obtaining the weight M of the surface residues of the cold-rolled sheet in unit area;
obtaining a standard working curve of Fe;
the second adhesive tape and the acid liquor are subjected to complete reaction to obtain a reaction liquid, and then the reaction liquid is subjected to solid-liquid separation to obtain a liquid containing Fe 2+ A solution;
the Fe content is measured 2+ Spectral line intensity of the solution;
by mixing the Fe-containing material with 2+ Substituting the spectral line intensity of the solution into the standard working curve of Fe to obtain the Fe-containing material 2+ Concentration C of the solution; obtaining the weight M of the iron powder in the surface residues of the cold-rolled sheet in unit area according to the concentration C Fe ；
According to the weight M and the weight M Fe Obtaining the residual carbon content of the surface of the cold-rolled sheet in unit area.
Further, the adhesive properties of the tape were >18OZ/in.
Further, the first adhesive tape is used for completely adhering the residues on the surface of the cold-rolled sheet to be tested to obtain the cold-rolled sheet with the weight of M 2 Comprises:
the adhesive tape is tightly adhered to the surface of the cold-rolled sheet to be measured, the cold-rolled sheet is pressed for 1 to 15 minutes, and then the adhesive tape is torn off, so that the weight M is obtained 2 Is a second tape of the first tape.
Further, the step of completely reacting the second adhesive tape with an acid solution to obtain a reaction solution includes:
and adding the second adhesive tape into acid liquor, adding zeolite, and performing complete reaction to obtain reaction liquid.
Further, the acid liquid is hydrochloric acid or sulfuric acid.
Further, the acid liquor is dilute hydrochloric acid with the concentration of 1 mol/L-3 mol/L or dilute sulfuric acid with the concentration of 1 mol/L-3 mol/L.
Further, the obtaining a standard working curve of Fe includes:
preparing N parts of standard working solutions with different Fe concentrations; wherein N is an integer > 1; and measuring the spectral line intensity of the N standard working solutions, and drawing a standard working curve of Fe according to the spectral line intensity and the concentration of the iron element.
Still further, the N is an integer > 5.
Further, the measured line intensity of the N parts of standard working solution, and the measured Fe-containing 2+ Spectral line intensity of the solution, both comprising:
the method comprises the steps of measuring by adopting an inductively coupled plasma emission spectrometer, wherein the detection conditions of the inductively coupled plasma emission spectrometer are as follows: the RF power is 1145-1155W, the pump speed is 45-55 rpm, the auxiliary air flow is 0.3-0.7L/min, the atomizer air flow is 0.5-0.9L/min, the atomizer pressure is 0.1-0.3 MPa, and the flushing time is 40-50 s.
Further, the detection wavelength is 234.3nm.
Further, the spectral line intensity of the N parts of standard working solution is equal to that of the Fe-containing solution 2+ The detection conditions of the line intensity of the solution are the same.
One or more technical solutions in the embodiments of the present application at least have the following technical effects or advantages:
the method for measuring the residual carbon content on the surface of the cold-rolled sheet provided by the application firstly selects the adhesive tape to extract the residual carbon content on the surface of the cold-rolled sheet, the extraction method better measures the weight M of the residual carbon content on the surface of the cold-rolled sheet, and the weight M of the iron powder in the residual carbon content on the surface of the cold-rolled sheet in unit area is obtained Fe Based on the weight M and the weight M Fe Obtaining the residual carbon content of the surface of the cold-rolled sheet in a unit area; the prior art has no method for measuring the content of residual carbon, only the method for measuring the weight of the iron powder in the residues is adopted, and the weight of the iron powder in the residues is also obtained by a distillation method,according to the method disclosed by the application, for the cold-rolled sheet, cutting is not needed, a sample is not damaged, in-situ detection and analysis can be performed on the sample, distillation separation is not needed, an organic reagent is not needed to touch, and the method is environment-friendly. The method can accurately measure the content of residual carbon on the surface of the cold-rolled sheet, and is simple to operate and short in time consumption. The RSD value of the detection method is 5.93%, and the precision is high. The value of the residual carbon content on the surface of the cold-rolled sheet provides objective basis for judging the quality of the rolling oil and the heat treatment process, and can also be used as objective basis for judging the surface cleanliness of the sample.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present application, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a method for measuring the residual carbon content on the surface of a cold-rolled sheet;
FIG. 2 is a standard working graph of iron element in example 1 of the present application;
fig. 3 is a standard working graph of iron element in example 2 of the present application.
Detailed Description
The advantages and various effects of the present application will be more clearly apparent from the following detailed description and examples. It will be understood by those skilled in the art that these specific embodiments and examples are intended to illustrate the application, not to limit the application.
Throughout the specification, unless specifically indicated otherwise, the terms used herein should be understood as meaning as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. In case of conflict, the present specification will control.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present application are commercially available or may be prepared by existing methods.
The technical scheme provided by the embodiment of the application aims to solve the technical problems, and the overall thought is as follows:
in order to achieve the above object, this embodiment provides a method for determining the residual carbon content on the surface of a cold-rolled sheet, including:
s1, obtaining an adhesive tape, and weighing the weight M of the adhesive tape 1 Measuring the length and width of the adhesive tape to obtain the area S of the adhesive tape; adhering the cold-rolled sheet surface residues through the adhesive tape to obtain an adhesive tape adhered with the cold-rolled sheet surface residues, and weighing the weight M of the adhesive tape adhered with the cold-rolled sheet surface residues 2 Obtaining the weight M= (M) of the surface residues of the cold-rolled sheet in unit area 2 -M 1 )/S；
When the adhesive tape is used, the adhesive tape is tightly adhered to the surface of the cold-rolled sheet, the adhesive tape is tightly pressed back and forth by hands for 1-15 min, and then the adhesive tape is torn off, so that the adhesive tape with residues on the surface of the cold-rolled sheet is obtained.
After the residues on the surface of the cold-rolled sheet are adhered by the adhesive tape, the cold-rolled sheet can be directly subjected to subsequent operation or placed in a sample bag for standby, the residues adhered on the adhesive tape are not easy to fall off, and the sample is better preserved than the gauze and the defatted cotton.
Preferably, the adhesive properties of the tape are >18OZ/in. The inventor found through practice that the adhesive tape with the adhesive property of >18OZ/in can well adhere residues on the surface of the cold-rolled sheet. The adhesive tape has the main components of polyvinyl chloride organic matters, has the advantages of high temperature resistance, acid and alkali resistance, flame retardance and the like, has strong adhesive force, the adhesive property of the adhesive tape to a steel belt is more than 18OZ/in, the adhesive tape is used for adhering residues on the surface of a cold-rolled sheet in a certain area by using the strong adhesive force of the adhesive tape, because iron powder and carbon powder are adhered to the surface of the cold-rolled sheet, the iron powder and the carbon powder can be adhered from the surface of the cold-rolled sheet through the adhesive tape with strong adhesive force, and due to the good adhesive force of the adhesive tape, the adhered samples can be well stored on the adhesive tape and are not easy to fall off in a sample bag, and the total quality of the residues on the surface of the cold-rolled sheet can be obtained by measuring the poor quality of the adhesive tape before and after adhering the residues on the surface of the cold-rolled sheet, and then the total quality of the residues in unit area can be converted.
S2, obtaining a standard working curve of Fe;
preparing N parts of standard working solutions with different iron element concentrations; wherein N is an integer > 1; measuring the spectral line intensity of the N standard working solutions, and drawing a standard working curve of the iron element according to the spectral line intensity and the iron element concentration;
specifically, the iron standard operating curve is plotted by computer software through a unitary linear regression equation (equation 1). The working curve is determined according to the residual iron amount on the surface of the cold-rolled sheet. Generally, the residual iron content of industrial production surfaces is a relatively fixed range value. If the instrument is replaced by a working curve which is built every time, if the instrument is stable, a working curve can be used in the measuring range without repeatedly measuring the working curve.
S3, completely reacting the second adhesive tape with acid liquor to obtain a reaction liquid, and then carrying out solid-liquid separation on the reaction liquid to obtain a liquid containing Fe 2+ A solution;
s4, removing the volume V 1 Is not less than Fe 2+ The volume of the solution is fixed to the volume V 2 After that, the Fe content was measured 2+ Spectral line intensity of the solution;
s5, by mixing the Fe-containing alloy with 2+ Substituting the spectral line intensity of the solution into the standard working curve of Fe to obtain the Fe-containing material 2+ Concentration C of the solution; obtaining the weight M of the iron powder in the surface residues of the cold-rolled sheet in unit area according to the concentration C Fe ，M Fe ＝C×(V 2 /V 1 )/S；
S6, according to the weight M and the weight M Fe Obtaining the residual carbon content M of the surface of the cold-rolled sheet in unit area c ＝M-M Fe ；
According to the method for measuring the residual carbon content on the surface of the cold-rolled sheet, disclosed by the application, the adhesive tape is selected for extracting the residual carbon content on the surface of the cold-rolled sheet, the quality of an extract is better controlled by the extraction method, and the method is free from cutting, damaging a sample, carrying out in-situ detection and analysis on the sample, and is free from distillation separation, free from touching an organic reagent, and environment-friendly. The method can accurately measure the content of residual carbon on the surface of the cold-rolled sheet, and is simple to operate and short in time consumption. The value provides objective basis for judging the quality of the rolling oil and the heat treatment process, and can also be used as objective basis for judging the surface cleanliness of the sample.
Preferably, the acid liquor is diluted hydrochloric acid with the concentration of 1 mol/L-3 mol/L or diluted sulfuric acid with the concentration of 1 mol/L-3 mol/L. The dilute acid was used for good atomization during the post inductively coupled plasma test.
Preferably, a small amount of zeolite may be added during the reaction, and due to the porous silicate nature of zeolite, a certain amount of air is present in the pores to prevent bumping.
In the step S2 and the step S3, the spectrum detection method adopts an inductively coupled plasma emission spectrometer, and the detection conditions of the inductively coupled plasma emission spectrometer are as follows: RF power is 1145-1155W (best 1150W), pump speed is 45-55 rpm (best 50 rpm), auxiliary air flow is 0.3-0.7L/min (best 0.5L/min), atomizer air flow is 0.5-0.9L/min (best 0.7L/min), atomizer pressure is 0.1-0.3 MPa (best 0.2 MPa), and flushing time is 40-50 s (best 45 s). Under the detection conditions, the peak type is good, and the detection limit is low.
Wherein the optimal detection wavelength of the iron element is 234.3nm. According to the method, a plurality of characteristic spectral lines are selected as analysis spectral lines aiming at iron elements, the spectral line intensities corresponding to different wavelengths are different, and the anti-interference capability is also different.
From the above, the method for measuring the residual carbon content on the surface of the cold-rolled sheet provided by the application can accurately measure the residual carbon content on the surface of the cold-rolled sheet.
The method for measuring the residual carbon content on the surface of a cold-rolled sheet according to the present application will be described in detail with reference to examples, comparative examples and experimental data.
The instrument is used: ICAP6300 full spectrum direct-reading inductively coupled plasma emission spectrometer (Siemens, inc. of Siemens, U.S.A.). The detection conditions of the inductively coupled plasma emission spectrometer are as follows: RF power 1150W, pump speed 50rpm, auxiliary air flow 0.5L/min, atomizer gas flow 0.7L/min, atomizer pressure 0.2MPa, rinse time 45s.
The reagents used in the application are all of high-grade pure, and the experimental water is primary water conforming to the specification in GB/T6682.
Example 1
The 1# and 2# tapes were weighed separately using an analytical balance, where m of 1# 1 2.0110g, m 2 1.9442g, weighing, placing the adhesive tape into a sample bag, sealing with a seal, removing the intermediate warehouse of the cold-rolled sheet, and respectively attaching the adhesive tape to the intermediate and right-side parts of the cold-rolled sheet, wherein the adhesive tape has a length of 200.00mm, a width of 50.00mm, and a width of 0.01m 3 The adhesive tape is tightly adhered to the surface of the cold-rolled sheet, and is tightly pressed back and forth by hands for 3min, the adhesive tape is torn off, and the adhesive tape is put back into a sample bag and sealed by a seal. After returning to the laboratory, the adhesive tape was taken out, 2.2312g and 2.2231g of each of the 1# and 2# adhesive tapes were weighed by an analytical balance, then the adhesive tape was placed in a beaker containing 50mL of dilute hydrochloric acid, zeolite was added, heated until the volume of the solution was nearly dry, the beaker was removed to cool, deionized water was added to about 30mL, filtration was performed, the filtrate was removed, 50mL of filtrate was removed, and diluted and fixed in a 100mL volumetric flask.
Preparing a working curve by using 25mg/L iron standard solution, respectively transferring 0, 4,8, 16 and 24mL into a 50mL volumetric flask, diluting to constant volume, respectively measuring the content of iron element in the solution by using an inductively coupled plasma emission spectrometer in the range of 0,2,4,8 and 12mg/L in the working curve, and drawing the working curve, wherein the linear equation is I=1411.63793+9534.14655C and the linear correlation coefficient is 0.99917 as shown in figure 2.
The Fe content in the corresponding volumetric flask of 1# is 4.75mg/L, the Fe content in the corresponding volumetric flask of 2# is 6.6mg/L, the residual iron content converted to the surface of the 1# sample is 9.5mg/L, and the residual iron content on the surface of the 2# sample is 13.2mg/L. The data of the specific measurements and calculations are shown in table 1.
TABLE 1 carbon residue on cold rolled sheet surfaces
As is clear from Table 1, the residual carbon amounts in the middle and right portions of the cold-rolled sheet were 125g/m, respectively 2 And 158g/m 2 As shown by the measurement result, the average value of the carbon residue on the surface of the cold-rolled sheet is 141.5g/m 2 。
Example 2
Different rolling oils were selected, three rolling oils were used in three identical production lines, and after heat treatment under the same conditions, 1#, 2#, 3# samples were obtained, and the tape (the tape mass before adhesion was denoted as M 1 ) Respectively adhering to the surface of the sample, measuring the carbon residue on the surface of the sample, and measuring the carbon residue at different positions of the same sample at each time, wherein the samples are sequentially recorded as 1# -1, 1# -2#, 2# -1, 3# -1 and 3# -2. The quality of the adhesive tape before use is shown in Table 2, the length of the adhesive tape is 200.00mm, the width of the adhesive tape is 50.00mm, the adhesive tape is also pressed on the surface of a sample for 4min, the adhesive tape is torn off and put into a sample bag for storage, and the quality of the adhesive tape is measured and recorded as M 2 The total amount of the residue of the cold-rolled sheet was obtained by calculating the difference in mass before and after the measurement of the adhesive tape, and the calculation results are shown in Table 1. Then the adhesive tape is dissolved in 50mL (1+1) dilute hydrochloric acid, zeolite is added, the mixture is heated to be nearly dry, cooled to room temperature, deionized water is added, and the mixture is poured into a 100mL volumetric flask for constant volume.
Preparing a working curve by using 100mg/L iron standard solution, respectively transferring 0, 2.5, 5, 7.5 and 10mL into a 50mL volumetric flask, diluting to constant volume, respectively measuring the content of iron element in the solution by using an inductive coupling plasma emission spectrometer, wherein the content of iron element in the working curve is respectively 0,5, 10, 15 and 20mg/L, drawing the working curve, respectively making the content of iron element in the working curve be 0,5, 10, 15 and 20mg/L, drawing the working curve, and the linear equation of the working curve is I=2050.8+2971.54C, and the linear correlation coefficient of the working curve is 0.99947 as shown in figure 3. The iron content in the solution was measured by an inductively coupled plasma emission spectrometer, and the Fe content in the sample was calculated on a working curve, and the measurement results are shown in table 2.
TABLE 2 carbon residue on surfaces of different cold-rolled sheets
As is clear from Table 2, the average value of the carbon residue on the surface of sample # 1 was 211mg/m 2 The average value of the carbon residue on the surface of sample # 2 was 176mg/m 2 The average value of the carbon residue on the surface of sample # 3 was 101.5mg/m 2 The comparison of the total amount of residues and the amount of carbon residues shows that the residue content on the surface of the No. 3 sample is the greatest, but the carbon residues are smaller, mainly iron residues, and the total amount of residues on the surface of the No. 1 sample is the least, but the ratio of the carbon residues is higher, and the comparison analysis shows that the rolling oil used for the No. 3 sample has the least carbon residues, so that the production is most facilitated.
Experimental example 1 precision experiment
On the same production line, after heat treatment under the same conditions, precision tests were carried out at sample surface selection 5, designated as samples # 1, # 2, # 3, # 4 and # 5, respectively, and the tape (the tape mass before adhesion was designated as M 1 ) And respectively adhering to each surface of the sample, and measuring the carbon residue on the surface of the sample. The quality of the adhesive tape before use is shown in Table 3, the length of the adhesive tape is 200.00mm, the width of the adhesive tape is 50.00mm, the adhesive tape is also pressed on the surface of a sample for 4min, the adhesive tape is torn off and put into a sample bag for storage, and the quality of the adhesive tape is measured and recorded as M 2 The total amount of residues at different parts of the cold-rolled sheet was obtained by calculating the difference in mass before and after the measurement of the adhesive tape, and the calculation results are shown in table 3. Then the adhesive tape is dissolved in 50mL (1+1) dilute hydrochloric acid, zeolite is added, the mixture is heated to be nearly dry, cooled to room temperature, deionized water is added, and the mixture is poured into a 100mL volumetric flask for constant volume.
Preparing a working curve by using 100mg/L iron standard solution, respectively transferring 0, 2.5, 5, 7.5 and 10mL into a 50mL volumetric flask, diluting to a constant volume, respectively measuring the iron content in the solution by using an inductive coupling plasma emission spectrometer, respectively measuring the iron content in the solution by using the iron content ranges of 0,5, 10, 15 and 20mg/L in the working curve, drawing the working curve, respectively measuring the iron content in the solution by using the inductive coupling plasma emission spectrometer, calculating the Fe content in the sample by using the working curve, and measuring the Fe content in the sample by using the measuring result shown in Table 3.
TABLE 3 results of precision test of carbon residue on Cold rolled sheet surface
As can be seen from the data in Table 3, the RSD value of the detection method is 5.93%, which accords with the relevant regulations about the variation coefficient in the laboratory in GB/T27417-2017 "standard evaluation chemistry analysis method confirmation and verification guide", and the result shows that the precision is high.
In summary, the method for measuring the residual carbon content on the surface of the cold-rolled sheet provided by the application can accurately measure the residual carbon content on the surface of the cold-rolled sheet, and is simple to operate and short in time consumption; the precision is high.
Finally, it is also noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present application have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the application.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present application without departing from the spirit or scope of the application. Thus, it is intended that the present application also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (3)
1. The method for measuring the residual carbon content on the surface of the cold-rolled sheet is characterized by comprising the following steps of:
obtain an area S and a weight M 1 The first adhesive tape is tightly adhered to the surface of the cold-rolled sheet to be measured, the first adhesive tape is pressed for 1 to 15 minutes, and then the adhesive tape is torn off, so that the weight M is obtained 2 According to the area S, the weight M 1 And weight M 2 Obtaining the weight M of the residue on the surface of the cold-rolled sheet in unit area, and the adhesive property of the adhesive tape>18OZ/in；
Obtaining a standard working curve of Fe;
the second adhesive tape and the acid liquor are subjected to complete reaction to obtain a reaction liquid, and then the reaction liquid is subjected to solid-liquid separation to obtain a liquid containing Fe 2+ The acid liquor is dilute hydrochloric acid with the concentration of 1 mol/L-3 mol/L or dilute sulfuric acid with the concentration of 1 mol/L-3 mol/L;
the Fe content is measured 2+ Spectral line intensity of the solution;
by mixing the Fe-containing material with 2+ Substituting the spectral line intensity of the solution into the standard working curve of Fe to obtain the Fe-containing material 2+ Concentration C of the solution; obtaining the weight M of the iron powder in the surface residues of the cold-rolled sheet in unit area according to the concentration C Fe ；
According to the weight M and the weight M Fe Obtaining the residual carbon content of the surface of the cold-rolled sheet in a unit area;
the standard working curve of Fe is obtained, which comprises the following steps:
preparing N parts of standard working solutions with different Fe concentrations; wherein N is an integer > 5; measuring the spectral line intensity of the N standard working solutions, and drawing a standard working curve of Fe according to the spectral line intensity and the iron element concentration;
the measured line intensity of the N parts of standard working solution and the measured Fe content 2+ Spectral line intensity of the solution, both comprising:
the method comprises the steps of measuring by adopting an inductively coupled plasma emission spectrometer, wherein the detection conditions of the inductively coupled plasma emission spectrometer are as follows: the RF power is 1145-1155W, the pump speed is 45-55 rpm, the auxiliary air flow is 0.3-0.7L/min, the atomizer air flow is 0.5-0.9L/min, the atomizer pressure is 0.1-0.3 MPa, the flushing time is 40-50 s, and the detection wavelength is 234.3nm.
2. The method of claim 1, wherein the completely reacting the second tape with the acid solution to obtain a reaction solution comprises:
and adding the second adhesive tape into acid liquor, adding zeolite, and performing complete reaction to obtain reaction liquid.
3. The method according to claim 1, wherein the N parts of standard working solution have spectral line intensities with the Fe-containing solution 2+ The detection conditions of the line intensity of the solution are the same.
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