CN108020546B - Quality tester for chemical cleaning passivation film, testing solution and using method - Google Patents
Quality tester for chemical cleaning passivation film, testing solution and using method Download PDFInfo
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- CN108020546B CN108020546B CN201711455102.2A CN201711455102A CN108020546B CN 108020546 B CN108020546 B CN 108020546B CN 201711455102 A CN201711455102 A CN 201711455102A CN 108020546 B CN108020546 B CN 108020546B
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- 238000004140 cleaning Methods 0.000 title claims abstract description 39
- 238000002161 passivation Methods 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 13
- 238000012360 testing method Methods 0.000 title claims description 10
- 239000007788 liquid Substances 0.000 claims abstract description 44
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000007689 inspection Methods 0.000 claims abstract description 22
- 229910052751 metal Inorganic materials 0.000 claims abstract description 22
- 239000002184 metal Substances 0.000 claims abstract description 22
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 20
- 238000010926 purge Methods 0.000 claims abstract description 11
- 238000003860 storage Methods 0.000 claims abstract description 11
- 238000007789 sealing Methods 0.000 claims abstract description 10
- 239000012085 test solution Substances 0.000 claims abstract description 5
- 238000004448 titration Methods 0.000 claims description 38
- 239000000243 solution Substances 0.000 claims description 26
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 claims description 24
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 22
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- 229910000975 Carbon steel Inorganic materials 0.000 claims description 13
- 239000010962 carbon steel Substances 0.000 claims description 13
- 239000010935 stainless steel Substances 0.000 claims description 13
- 229910001220 stainless steel Inorganic materials 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 11
- 235000019253 formic acid Nutrition 0.000 claims description 11
- 239000005639 Lauric acid Substances 0.000 claims description 10
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 10
- 230000007797 corrosion Effects 0.000 claims description 10
- 238000005260 corrosion Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000003112 inhibitor Substances 0.000 claims description 8
- 239000011780 sodium chloride Substances 0.000 claims description 8
- WUWHFEHKUQVYLF-UHFFFAOYSA-M sodium;2-aminoacetate Chemical compound [Na+].NCC([O-])=O WUWHFEHKUQVYLF-UHFFFAOYSA-M 0.000 claims description 6
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 230000003321 amplification Effects 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 238000003199 nucleic acid amplification method Methods 0.000 claims description 3
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims 1
- 239000004973 liquid crystal related substance Substances 0.000 claims 1
- 239000012528 membrane Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 12
- 229910052742 iron Inorganic materials 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 150000002739 metals Chemical class 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 10
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- 239000000203 mixture Substances 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 238000012372 quality testing Methods 0.000 description 4
- 238000002845 discoloration Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000003889 chemical engineering Methods 0.000 description 2
- 229910000365 copper sulfate Inorganic materials 0.000 description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 2
- 230000003111 delayed effect Effects 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- -1 potassium ferricyanide Chemical compound 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000000080 wetting agent Substances 0.000 description 2
- 241000238097 Callinectes sapidus Species 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 241000530268 Lycaena heteronea Species 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Images
Classifications
-
- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N2021/775—Indicator and selective membrane
Abstract
The invention discloses a chemical cleaning passivation film quality tester, a test solution and a using method, belongs to the technical field of industrial instruments and meters, and particularly relates to a chemical cleaning passivation film tester. The device comprises a liquid drop system, a nitrogen sealing and purging system, a color identification and comparison system, a light source system, a data acquisition system and a display and storage system. The method is used for identifying the quality inspection of the chemical cleaning passive film of various devices such as condensers, heat exchangers, boiler heating surfaces, chemical equipment and the like containing iron materials, and can also be used for inspecting the uniformity of metal coatings on the inner surfaces of metals.
Description
Technical Field
The invention belongs to the technical field of industrial instruments and meters, and particularly relates to a chemical cleaning passivation film tester.
Background
Because raw water enters thermal equipment untreated due to leakage and seepage of cooling equipment and is limited by economy, the water for the thermal equipment contains trace impurities and the like, so that the thermal equipment in the industries of electric power, chemical engineering, thermal power and the like can form sediments (carbonate scale, silicate scale, sulfate scale, grease and the like) and metal oxide corrosion products in operation, and the sediments and the corrosion products on a heating surface can be rapidly solidified under the conditions of high temperature and high pressure to form an additional layer with different thicknesses. In addition, the expansion coefficient of the additional layer is greatly different from that of a metal substrate, the metal can bear great additional stress, and the stress can also aggravate the electrochemical corrosion of the metal. Therefore, each enterprise pays great attention to the fact that the enterprises regularly inspect and chemically clean the heated surface to eliminate deposits and ensure the cleanliness of the interior of the metal.
Therefore, the chemical cleaning quality standard of industrial equipment (HG/T2387) and the chemical cleaning guide of a boiler of a thermal power plant (DL/T794) play an important role in guaranteeing the long-term safe, economic, temperature and environment-friendly operation of equipment in the industries of electric power, chemical engineering, heat power and the like, so that the cleaning work of the thermal equipment is guided to obtain important economic and social benefits.
In the chemical cleaning quality standard of industrial equipment (HG/T2387-2007), relevant description is carried out on the quality inspection of the passivation film, and a method and a standard value are given, but the color development (color change) reaction depends on artificial subjective judgment, and the result of an artificial titration experiment is often far higher than a standard qualified value (5 seconds are qualified or 8 blue points.), so that the guiding significance and the actual effect are lost, and therefore, in the chemical cleaning guide rule of a boiler of a thermal power plant (DL/T794) with higher technical requirements, the inspection requirement of the passivation film is only that a good passivation protective film is formed on the surface of a metal after cleaning. The reason for the large error of the passivation film quality inspection in HG/T2387 is that: 1) the quality inspection structure is greatly influenced by artificial subjective consciousness; 2) human sensory differences to standard colors; 3) the titration solution and the metal surface are affected by other factors, such as organic substances, to cause a series of chemical reactions and a delayed color reaction, which results in a large amount of results. The three reasons lead the quality inspection method of the passivation film in HG/T2387 to be further improved and perfected. Therefore, there is a need in the art for a new solution to solve this problem.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the quality inspection instrument for the chemical cleaning passive film is used for inspecting the quality of the chemical cleaning passive film of equipment such as condensers, heat exchangers, boiler heating surfaces, chemical equipment and the like which are made of various iron-containing materials, and can also be used for inspecting the uniformity of metal coatings on the inner surfaces of metals.
A quality tester for a chemical cleaning passivation film comprises a liquid drop system, a nitrogen sealing and purging system, a color identification and comparison system, a light source system, a data acquisition system and a display and storage system;
the liquid drop system comprises a sealed titration liquid pool, a titration needle, a needle-shaped electromagnetic valve, a titration pipeline and a timer 11;
the nitrogen sealing and purging system comprises a high-elasticity nitrogen storage bag and a nitrogen pipeline, and is used for purging the liquid drop pipeline and the titration needle, replacing and sealing the titration liquid pool to ensure that the titration liquid is not deteriorated;
the color identification and comparison system is used for monitoring the color change of the liquid drop, automatically comparing the color change with a standard color and sending a signal when a terminal color is reached;
the light source system comprises a standard color module and a signal amplification output device, and under a carbon steel inspection mode: starting a fluorescent lamp with the emission wavelength of 450-700 nm; in stainless steel inspection mode: starting a fluorescent lamp with the emission wavelength of 450-595 nm;
the data acquisition system collects the electric signals sent by the color comparison system, processes and outputs data, and the data are displayed on the display screen 61;
the display and storage system comprises a display screen and a memory card.
Further, the tester also comprises a metal frame and four bases.
Furthermore, the specification of the titration needle is 1 drop of 0.1ml, and the inner diameter of the titration pipeline is 0.15 mm.
Still further, the specification of the timer is a range of 0-1000s, and the precision is 0.1 s.
Still further, the standard color module stores standard color wavelengths of red, yellow-green, yellow, blue and dark blue.
A carbon steel film quality testing liquid used by a chemical cleaning passivation film quality tester is prepared according to the following modes: 4.1-5.3 g of analytically pure copper sulfate pentahydrate, 3.5g of analytically pure sodium chloride, 2mL of corrosion inhibitor IS-129, 0.2mL of analytically pure 0.1mol/L hydrochloric acid, 0.5mL of analytically pure 70% formic acid, 0.2mL of 1% analytically pure phenolphthalein, 0.1g of analytically pure sodium dodecyl sulfate, 0.1g of analytically pure lauric acid and 0.1-0.2 mL of 70% medical alcohol solution, and the solutions are diluted to 100mL by first-stage experimental water.
A stainless steel film quality testing liquid used by a chemical cleaning passive film quality tester is configured according to the following modes: 4.6-5.2 g analytically pure K3[Fe(CN)6]3.5g of analytically pure sodium chloride, 1mL of analytically pure 36% hydrochloric acid; 0.5mL of 0.5mol/L analytically pure sodium glycine, 0.1g of analytically pure sodium dodecyl sulfate, 0.2mL of 1% analytically pure phenolphthalein, 2mL of corrosion inhibitor XD-255, 0.2g of analytically pure lauric acid, 0.1mL of 70% medical alcohol solution, 0.2mL of analytically pure 98% sulfuric acid, and 1mL of analytically pure 70% formic acid, and the mixture is diluted to 100mL by distilled water.
The use method of the chemical cleaning passivation film quality tester is characterized by comprising the following steps:
fixing a chemical cleaning passivation film quality tester on the surface of metal, and selecting a carbon steel mode or a stainless steel mode according to the requirement;
step two, the quality inspection instrument for the chemical cleaning passivation film automatically selects 5 points on the metal surface, and solution is applied to each spot;
step three, the quality inspection instrument for the chemical cleaning passivation film automatically records the time from the first drop titration to the solution change from blue or yellow green to red or blue, and automatically compares the color of the drop with the standard color;
and in the carbon steel mode, the quality of the film is checked by depending on the time when the liquid drops are completely changed from blue to red, and when the time when the blue color of each point disappears and the time when the liquid drops are completely changed into red is more than 5s, the integrity and the uniformity of the quality of the passivation film are automatically evaluated according to the relation of the color change time of each point. After the test is finished, the pipeline and the titration needle are automatically purged by nitrogen;
in the stainless steel mode, when the number of blue dots of the yellow-green liquid drops in 10 minutes at each point is not less than 8, the product is qualified. And evaluating the integrity and uniformity of the quality of the passivation film according to the number of blue dots of the yellow-green liquid drop in 10 minutes at each point. After the test was completed, the tubing and titration needle were automatically purged with nitrogen.
Through the design scheme, the invention can bring the following beneficial effects: and the passivated film, wherein the metal matrix exposed after being damaged respectively reacts with blue copper sulfate solution and yellow potassium ferricyanide solution to form red elemental copper (blue color changes into red) or blue Fe3 [ Fe (CN)6 ] 2 (blue dots appear in yellow), the quality of the passivated film is checked according to the length of the color change time (the number of blue dots appear in yellow-green liquid drops within 10 minutes), and the integrity and uniformity of the passivated film are automatically checked according to a program according to the color change time difference and the blue dot number difference.
Drawings
The invention is further described with reference to the following figures and detailed description:
FIG. 1 is a schematic structural diagram of a chemical cleaning passivation film quality tester of the present invention.
FIG. 2 is a schematic top view of a chemical cleaning passivation film quality tester according to the present invention.
FIG. 3 is a schematic bottom view of a chemical cleaning passivation film quality tester according to the present invention.
Fig. 4 is a cross-sectional view of a chemical cleaning passivation film quality tester of the present invention.
In the figure, 1-liquid drop system, 2-nitrogen sealed purging system, 3-color identification and comparison system, 4-light source system, 5-data acquisition system, 6-display and storage system, 11-timer and 61-display screen.
Detailed Description
A chemical cleaning passivation film quality tester is shown in figures 1-4 and comprises a liquid drop system 1, a nitrogen sealing and purging system 2, a color identification and comparison system 3, a light source system 4, a data acquisition system 5 and a display and storage system 6;
the liquid drop system 1 comprises a sealed titration liquid pool, a titration needle, a needle-shaped electromagnetic valve, a titration pipeline and a timer 11;
the nitrogen sealing and purging system 2 comprises a high-elasticity nitrogen storage bag and a nitrogen pipeline, and is used for purging a liquid drop pipeline and a titration needle, replacing and sealing a titration liquid pool and ensuring that the titration liquid is not deteriorated;
the color identification and comparison system 3 is used for monitoring the color change of the liquid drop, automatically comparing the color change with a standard color and sending a signal when the end color is reached;
the light source system 4 comprises a standard color module and a signal amplification output device, and in a carbon steel inspection mode: starting a fluorescent lamp with the emission wavelength of 450-700 nm; in stainless steel inspection mode: starting a fluorescent lamp with the emission wavelength of 450-595 nm;
the data acquisition system 5 collects the electric signals sent by the color comparison system, processes and outputs data, and displays the data on the display screen 61;
the display and storage system 6 includes a display screen 61 and a memory card.
The tester also includes a metal frame 7 and four mounts.
The specification of the titration needle is 1 drop of 0.1ml, and the inner diameter of the titration pipeline is 0.15 mm.
The specification of the timer 11 is a range of 0-1000s, and the precision is 0.1 s.
The standard color module stores red, yellow-green, yellow, blue and dark blue standard color wavelengths.
A carbon steel film quality testing liquid used by a chemical cleaning passivation film quality tester is prepared according to the following modes: 4.1-5.3 g of analytically pure copper sulfate pentahydrate, 3.5g of analytically pure sodium chloride, 2mL of corrosion inhibitor IS-129, 0.2mL of analytically pure 0.1mol/L hydrochloric acid, 0.5mL of analytically pure 70% formic acid, 0.2mL of 1% analytically pure phenolphthalein, 0.1g of analytically pure sodium dodecyl sulfate, 0.1g of analytically pure lauric acid and 0.1-0.2 mL of 70% medical alcohol solution, and the solutions are diluted to 100mL by first-stage experimental water.
A stainless steel film quality testing liquid used by a chemical cleaning passive film quality tester is configured according to the following modes: 4.6-5.2 g analytically pure K3[Fe(CN)6]3.5g of analytically pure sodium chloride, 1mL of analytically pure 36% hydrochloric acid; 0.5mL of 0.5mol/L analytically pure sodium glycine, 0.1g of analytically pure sodium dodecyl sulfate, 0.2mL of 1% analytically pure phenolphthalein, 2mL of corrosion inhibitor XD-255, 0.2g of analytically pure lauric acid, 0.1mL of 70% medical alcohol solution, 0.2mL of analytically pure 98% sulfuric acid, and 1mL of analytically pure 70% formic acid, and the mixture is diluted to 100mL by distilled water.
A use method of a chemical cleaning passivation film quality tester comprises the following steps:
fixing a chemical cleaning passivation film quality tester on the surface of metal, and selecting a carbon steel mode or a stainless steel mode according to the requirement;
step two, the quality inspection instrument for the chemical cleaning passivation film automatically selects 5 points on the metal surface, and solution is applied to each spot;
step three, the quality inspection instrument for the chemical cleaning passivation film automatically records the time from the first drop titration to the solution change from blue or yellow green to red or blue, and automatically compares the color of the drop with the standard color;
and in the carbon steel mode, the quality of the film is checked by depending on the time when the liquid drops are completely changed from blue to red, and when the time when the blue color of each point disappears and the time when the liquid drops are completely changed into red is more than 5s, the integrity and the uniformity of the quality of the passivation film are automatically evaluated according to the relation of the color change time of each point. After the test is finished, the pipeline and the titration needle are automatically purged by nitrogen;
in the stainless steel mode, when the number of blue dots of the yellow-green liquid drops in 10 minutes at each point is not less than 8, the product is qualified. And evaluating the integrity and uniformity of the quality of the passivation film according to the number of blue dots of the yellow-green liquid drop in 10 minutes at each point. After the test was completed, the tubing and titration needle were automatically purged with nitrogen.
Examples
Suitable for carbon steel film quality test
The composition of the test solution was: the mass fraction is acid copper sulfate, formic acid and alcohol mixed solution. The preparation requirements are as follows: 4.1-5.3 g of analytically pure copper sulfate pentahydrate, 3.5g of analytically pure sodium chloride, 2mL of corrosion inhibitor IS-129, 0.2mL of analytically pure 0.1mol/L hydrochloric acid, 0.5mL of analytically pure 70% formic acid, 0.2mL of 1% analytically pure phenolphthalein, 0.1g of analytically pure sodium dodecyl sulfate, 0.1g of analytically pure lauric acid, and 0.1-0.2 mL of 70% medical alcohol solution, and the solution IS diluted to 100mL by first-stage experimental water.
Wherein, the sodium dodecyl sulfate is a wetting agent which reduces the surface tension of the liquid drop; the phenolphthalein has the function of eliminating the difference between the color of the iron liquid drop and the standard color; the medical alcohol eliminates the delayed phenomena of the point drop reaction and the color development reaction caused by metal adsorbed protein, oil and the like, and the lauric acid is used for relieving the optical reaction of the medicine and reducing the deterioration rate of the medicine.
The test method comprises the following steps: the 5-point discoloration time (Sn) is shown.
And (4) uniformity inspection basis: the root mean square average value of the 5-point discoloration time (Sn) is taken as a reference (Sj), and the average value of the 5-point discoloration time (Sn) is taken as Ss.
When the | Sj-Ss | is less than or equal to 0.5, the quality of the passive film is complete and uniform.
When the agent Sj-SsI is more than or equal to 0.5 and less than or equal to 1, the quality of the passive film is complete and uniform.
When the weight of the agent Sj-SsI is more than or equal to 1.5, the quality of the passive film is more complete and more uniform.
When the weight of the agent Sj-Ssj is less than or equal to 1.5 and less than or equal to 2, the incomplete and uneven quality of the passive film is shown.
When the | Sj-Ss | 3, the quality of the passive film is very incomplete and uneven.
Is suitable for the quality test of the stainless steel film
The composition of the test solution was: the mass fraction is the mixed solution of acid potassium ferricyanide, formic acid, sodium aminoacetate, phenolphthalein and alcohol. The preparation requirements are as follows: 4.6-5.2 g analytically pure K3〖Fe(CN)63.5g of analytically pure sodium chloride, 1mL of analytically pure 36% hydrochloric acid; 0.5mL of 0.5mol/L analytically pure sodium glycine, 0.1g of analytically pure sodium dodecyl sulfate, 0.2mL of 1% analytically pure phenolphthalein, 2mL of corrosion inhibitor XD-255, 0.2g of analytically pure lauric acid, 0.1mL of 70% medical alcohol solution, 0.2mL of analytically pure 98% sulfuric acid, and 1mL of analytically pure 70% formic acid, and the mixture is diluted to 100mL by distilled water.
Wherein, the sodium dodecyl sulfate is a wetting agent which reduces the surface tension of the liquid drop; the sodium aminoacetate is used for shielding the interference of ferric iron on the reaction of color development (yellow green → blue dot); the phenolphthalein has the function of eliminating the difference between the color of the iron liquid drop and the standard color; the medical alcohol is used for ensuring the dissolution of phenolphthalein and eliminating the delay phenomenon of point drop reaction and color development reaction caused by metal adsorbed protein, oil and the like, the formic acid is a buffer solution of pH value, and the lauric acid is used for relieving the optical reaction of the medicine and reducing the deterioration rate of the medicine.
The test method comprises the following steps: as the number of blue dots appearing in 10 minutes per 5 dots.
And (4) uniformity inspection basis: the root mean square average of the number of blue dots (Sn) appearing at 5 dots in 10 minutes was taken as a reference (Sj), and the average of the number of blue dots (Sn) appearing at 5 dots in 10 minutes was taken as Ss.
When the | Sj-Ss | is less than or equal to 1, the quality of the passive film is complete and uniform.
When the weight of the agent Sj-SsI is more than or equal to 1 and less than or equal to 2, the quality of the passive film is complete and uniform.
When the weight of the agent Sj-SsI is more than or equal to 2 and less than or equal to 3, the quality of the passive film is complete and uniform.
When the | Sj-Ss | is more than or equal to 3, incomplete and uneven quality of the passive film is shown.
When the | Sj-Ss | 4, the quality of the passive film is very incomplete and uneven.
Claims (6)
1. The utility model provides a chemistry washs passive film quality inspection appearance which characterized in that: the device comprises a liquid drop system (1), a nitrogen sealing and purging system (2), a color identification and comparison system (3), a light source system (4), a data acquisition system (5) and a display and storage system (6);
the liquid drop system (1) comprises a sealed titration liquid pool, a titration needle, a needle-shaped electromagnetic valve, a titration pipeline and a timer (11);
the nitrogen sealing and purging system (2) comprises a high-elasticity nitrogen storage bag and a nitrogen pipeline, and is used for purging the liquid drop pipeline and the titration needle, replacing and sealing the titration liquid pool and ensuring that the titration liquid is not deteriorated;
the color identification and comparison system (3) is used for monitoring the color change of the liquid drop, automatically comparing the color change with a standard color and sending a signal when a terminal color is reached;
the light source system (4) comprises a standard color module and a signal amplification output device, and in a carbon steel inspection mode: starting a fluorescent lamp with the emission wavelength of 450-700 nm; in stainless steel inspection mode: starting a fluorescent lamp with the emission wavelength of 450-595 nm;
the data acquisition system (5) collects the electric signals sent by the color comparison system, processes and outputs data, and the data is displayed on the liquid crystal display screen;
the display and storage system (6) comprises a display screen (61) and a memory card;
when the titration solution is carbon steel film quality test solution, the titration solution is prepared in the following way: 4.1-5.3 g of analytically pure copper sulfate pentahydrate, 3.5g of analytically pure sodium chloride, 2mL of corrosion inhibitor IS-129, 0.2mL of analytically pure 0.1mol/L hydrochloric acid, 0.5mL of analytically pure 70% formic acid, 0.2mL of 1% analytically pure phenolphthalein, 0.1g of analytically pure sodium dodecyl sulfate, 0.1g of analytically pure lauric acid and 0.1-0.2 mL of 70% medical alcohol solution, and the solutions are diluted to 100mL by first-stage experimental water;
the titration solution is prepared by the following method when adopting a stainless steel membrane quality test solution: 4.6-5.2 g analytically pure K3[Fe(CN)6]3.5g of analytically pure sodium chloride, 1mL of analytically pure 36% hydrochloric acid; 0.5mL of 0.5mol/L analytically pure sodium glycine, 0.1g of analytically pure sodium dodecyl sulfate, 0.2mL of 1% analytically pure phenolphthalein, 2mL of corrosion inhibitor XD-255, 0.2g of analytically pure lauric acid, 0.1mL of 70% medical alcohol solution, and 0.2mL of analytically pure sodium dodecyl sulfate98% sulfuric acid, 1mL of analytically pure 70% formic acid, diluted to 100mL with distilled water.
2. The quality tester for the chemical cleaning passivation film of claim 1, wherein: the tester also comprises a metal frame (7) and four bases.
3. The quality tester for the chemical cleaning passivation film of claim 1, wherein: the specification of the titration needle is 1 drop of 0.1ml, and the inner diameter of the titration pipeline is 0.15 mm.
4. The quality tester for the chemical cleaning passivation film of claim 1, wherein: the specification of the timer is 0-1000s of measuring range and 0.1s of precision.
5. The quality tester for the chemical cleaning passivation film of claim 1, wherein: the standard color module stores red, yellow-green, yellow, blue and dark blue standard color wavelengths.
6. The use method of the chemical cleaning passivation film quality tester as claimed in claim 1, characterized by comprising the following steps:
fixing the chemical cleaning passivation film quality tester of claim 1 on a metal surface, and selecting a carbon steel mode or a stainless steel mode according to requirements;
step two, the quality inspection instrument for the chemical cleaning passivation film automatically selects 5 points on the metal surface, and solution is applied to each point;
step three, the quality inspection instrument for the chemically cleaned passivation film automatically records the time from the titration of the first drop to the change of the solution from blue or yellow green to red or blue, and automatically compares the color of the drop with the standard color;
in the carbon steel mode, the quality of the film is checked by means of the time when the liquid drops are completely changed from blue to red, when the time that the blue color of each point disappears and the time that the liquid drops are completely changed into red is more than 5s, the completeness and the uniformity of the quality of the passive film are automatically evaluated according to the color change time relation of each point, and after the test is finished, a pipeline and a titration needle are automatically purged by nitrogen;
and under the stainless steel mode, when the number of blue dots of the yellow-green liquid drops in 10 minutes of each point is not less than 8, the quality integrity and uniformity of the passivation film are evaluated according to the number of blue dots of the yellow-green liquid drops in 10 minutes of each point, and after the test is finished, the pipeline and the titration needle are automatically purged by nitrogen.
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