CN112611831A - Method for testing sulfur content in welding flux - Google Patents
Method for testing sulfur content in welding flux Download PDFInfo
- Publication number
- CN112611831A CN112611831A CN202010760048.8A CN202010760048A CN112611831A CN 112611831 A CN112611831 A CN 112611831A CN 202010760048 A CN202010760048 A CN 202010760048A CN 112611831 A CN112611831 A CN 112611831A
- Authority
- CN
- China
- Prior art keywords
- flux
- powder
- sulfur content
- absorption liquid
- glass plate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 230000004907 flux Effects 0.000 title claims abstract description 111
- 238000003466 welding Methods 0.000 title claims abstract description 51
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 48
- 239000011593 sulfur Substances 0.000 title claims abstract description 48
- 238000012360 testing method Methods 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000010521 absorption reaction Methods 0.000 claims abstract description 108
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims abstract description 78
- 239000000843 powder Substances 0.000 claims abstract description 72
- 239000007788 liquid Substances 0.000 claims abstract description 64
- 238000002485 combustion reaction Methods 0.000 claims abstract description 42
- 238000000227 grinding Methods 0.000 claims abstract description 40
- 229910000679 solder Inorganic materials 0.000 claims abstract description 22
- 238000004255 ion exchange chromatography Methods 0.000 claims abstract description 18
- 230000008014 freezing Effects 0.000 claims abstract description 8
- 238000007710 freezing Methods 0.000 claims abstract description 8
- 238000010998 test method Methods 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 48
- 239000005373 porous glass Substances 0.000 claims description 38
- GALOTNBSUVEISR-UHFFFAOYSA-N molybdenum;silicon Chemical compound [Mo]#[Si] GALOTNBSUVEISR-UHFFFAOYSA-N 0.000 claims description 29
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 28
- 239000000203 mixture Substances 0.000 claims description 28
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 27
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 24
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 21
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 20
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 17
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 12
- 150000001447 alkali salts Chemical class 0.000 claims description 11
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 10
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 238000010891 electric arc Methods 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000000243 solution Substances 0.000 description 12
- 239000002245 particle Substances 0.000 description 5
- 230000002745 absorbent Effects 0.000 description 4
- 239000002250 absorbent Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003480 eluent Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- NELHEDJEYYCDBN-UHFFFAOYSA-L OO.C([O-])(O)=O.[Na+].C([O-])(O)=O.[Na+] Chemical compound OO.C([O-])(O)=O.[Na+].C([O-])(O)=O.[Na+] NELHEDJEYYCDBN-UHFFFAOYSA-L 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000000105 evaporative light scattering detection Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/12—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Combustion & Propulsion (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides a method for testing the sulfur content in a welding flux. The test method comprises the following steps: providing a welding flux; freezing the flux; grinding the frozen flux to obtain flux powder; placing the solder powder in a combustion furnace, and combusting the solder powder to obtain sulfur dioxide gas; absorbing the sulfur dioxide gas by adopting absorption liquid; and carrying out ion chromatography test on the absorption liquid absorbing the sulfur dioxide gas, and calculating to obtain the sulfur content in the absorption liquid so as to obtain the sulfur content of the welding flux. The method for testing the sulfur content in the welding flux has higher accuracy.
Description
Technical Field
The invention relates to the technical field of detection, in particular to a method for testing sulfur content in a welding flux.
Background
Currently, in the process of measuring the sulfur content in a flux, it is necessary to grind the flux at room temperature so that the ground flux can be sufficiently burned. However, in the above-mentioned grinding process, frictional collision occurs between fluxes and between the fluxes and the grinding balls, and further frictional heat is generated, resulting in loss of sulfur in the fluxes, and further leading to inaccurate test results.
Disclosure of Invention
The invention mainly aims to provide a method for testing the sulfur content in a welding flux, aiming at improving the accuracy of testing the sulfur content in the welding flux.
In order to solve the technical problem, the method for testing the sulfur content in the welding flux provided by the invention comprises the following steps:
providing a welding flux;
freezing the flux;
grinding the frozen flux to obtain flux powder;
placing the solder powder in a combustion furnace, and combusting the solder powder to obtain sulfur dioxide gas;
absorbing the sulfur dioxide gas by adopting absorption liquid; and
and (4) carrying out ion chromatography test on the absorption liquid absorbing the sulfur dioxide gas, and calculating to obtain the sulfur content in the absorption liquid so as to obtain the sulfur content of the welding flux.
In some embodiments, the step of freezing the flux comprises:
filling the welding flux and the grinding balls into a grinding tank; and
the grind pot was cooled by immersing it in liquid nitrogen so that the temperature of the flux was below-10 ℃.
In some embodiments, the step of grinding the frozen flux to obtain the flux powder comprises:
and fixing the frozen grinding tank on an adapter of a grinding machine, and grinding the welding flux in the grinding tank, wherein the grinding time is 20-40 s, and the grinding frequency is 40-80 Hz.
In some embodiments, the testing method further comprises:
providing silicon-molybdenum powder, tin powder and iron powder, and mixing the solder powder, the silicon-molybdenum powder, the tin powder and the iron powder to obtain a mixture, wherein the mass ratio of the solder powder to the silicon-molybdenum powder to the tin powder to the iron powder is 1: 2-4: 2-4: 4-6; and
and putting the mixture into a combustion furnace, and combusting the mixture to obtain sulfur dioxide gas.
In some embodiments, the step of mixing the solder powder, the silicon molybdenum powder, the tin powder, and the iron powder comprises: sequentially placing silicon-molybdenum powder, tin powder, welding flux powder and iron powder in a crucible;
the step of placing the mixture in a furnace comprises: the crucible containing the mixture is placed in a furnace.
In some embodiments, the testing method further comprises the step of passing the flux powder through a 100 mesh screen after the flux is ground; and/or
The testing method also comprises the step of sieving at least one of silicon molybdenum powder, tin powder and iron powder through a 100-mesh sieve; and/or
The combustion furnace is an electric arc combustion furnace, the flow rate of a flow meter of the electric arc combustion furnace is 80-120 liters/hour, the combustion time is 1-4 s, the pressurization time is 0.1-0.5 s, and the oxygen purity is 99.9%.
In some embodiments, the absorption liquid is a mixture of an alkali solution and a hydrogen peroxide solution, the alkali salt concentration in the absorption liquid is 0.4-10 g/L, and the hydrogen peroxide solution contains 20-40% of hydrogen peroxide.
In some embodiments, the base salt is at least one of potassium hydroxide, sodium hydroxide, and a mixture of sodium carbonate and sodium bicarbonate.
In some embodiments, the step of absorbing the sulfur dioxide gas with an absorption liquid comprises:
providing a first porous glass plate absorption tube and a second porous glass plate absorption tube;
the absorption liquid is contained in the first porous glass plate absorption tube and the second porous glass plate absorption tube;
connecting the air outlet of the first porous glass plate absorption pipe to the air inlet of the second porous glass plate absorption pipe in series to form an absorption device;
connecting a gas inlet of the first porous glass plate absorption tube to a gas outlet of the combustion furnace, so that sulfur dioxide gas in the combustion furnace enters the first porous glass plate absorption tube and the second porous glass plate absorption tube through the gas outlet of the combustion furnace, wherein the time for absorbing the sulfur dioxide gas by adopting absorption liquid is 20-50 s; and
and mixing the absorption liquid in the first porous glass plate absorption tube and the second porous glass plate absorption tube.
In some embodiments, the step of performing an ion chromatography test on the absorption liquid absorbing the sulfur dioxide gas comprises the steps of:
drawing a standard curve of sulfate ions;
carrying out a plurality of ion chromatography tests on the absorption liquid absorbing the sulfur dioxide gas, and taking an average value;
bringing the average value into a standard curve of the sulfate ions to measure the concentration of the sulfate ions;
the sulfur content of the flux was calculated according to the following formula:
wherein W is the sulfur content of the flux, C is the concentration of sulfate ions in the absorption liquid, V is the volume of the absorption liquid, and m is the mass of the flux.
According to the technical scheme, the welding flux is frozen, then the frozen welding flux is ground, the ground welding flux is placed in a combustion furnace to be combusted, sulfur dioxide gas is absorbed through absorption liquid, and the sulfur content in the absorption liquid is tested by adopting ion chromatography, so that the sulfur content of the welding flux is obtained. Since the flux is frozen, the heat generated by the friction during grinding is not sufficient to allow sulfur to be lost and thus does not affect the accuracy of the test.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The description relating to "first", "second", etc. in this disclosure is for descriptive purposes only and is not to be construed as indicating or implying relative importance or implicit to the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
The invention provides a method for testing the sulfur content in a welding flux, which comprises the following steps:
providing a welding flux;
freezing the flux;
grinding the frozen flux to obtain flux powder;
placing the solder powder in a combustion furnace, and combusting the solder powder to obtain sulfur dioxide gas;
absorbing the sulfur dioxide gas by adopting absorption liquid; and
and (4) carrying out ion chromatography test on the absorption liquid absorbing the sulfur dioxide gas, and calculating to obtain the sulfur content in the absorption liquid so as to obtain the sulfur content of the welding flux.
According to the technical scheme, the welding flux is frozen, then the frozen welding flux is ground, the ground welding flux is placed in a combustion furnace to be combusted, sulfur dioxide gas is absorbed through absorption liquid, and the sulfur content in the absorption liquid is tested by adopting ion chromatography, so that the sulfur content of the welding flux is obtained. Since the flux is frozen, the heat generated by the friction during grinding is not sufficient to allow sulfur to be lost and thus does not affect the accuracy of the test. The test method has high accuracy, so that the test method has good repeatability.
In addition, the method for detecting the sulfur content in the welding flux has the advantages of simple operation, time saving and labor saving.
In some embodiments, the step of freezing the flux comprises:
filling the welding flux and the grinding balls into a grinding tank; and
the grind pot was cooled by immersing it in liquid nitrogen so that the temperature of the flux was below-10 ℃.
Preferably, the temperature of the frozen flux is below-20 ℃.
In one embodiment, the freezing process may be performed for 1-5 min. Preferably for 3 min.
In one embodiment, the grinding pot may be a screw-cap stainless steel grinding pot.
The step of grinding the frozen flux to obtain flux powder comprises the following steps:
and fixing the frozen grinding tank on an adapter of a grinding machine, and grinding the welding flux in the grinding tank, wherein the grinding time is 20-40 s, and the grinding frequency is 40-80 Hz.
It will be appreciated that the particle size of the solder powder obtained may be adjusted by setting the milling time and/or frequency.
According to the technical scheme, after the grinding tank is fixed on the adapter of the grinding machine, the grinding balls can grind the welding agent, and the proper particle size can be obtained. Because the temperature of the welding flux is lower than-10 ℃, the welding flux does not need to worry about sulfur loss caused by friction heat generation, and the welding flux can be finely ground, so that the specific surface area is increased, the subsequent combustion is more sufficient, and the test accuracy is increased.
In some embodiments, the testing method further comprises: and (3) sieving the solder powder by a 100-mesh sieve, and drying at the temperature of 90-120 ℃ for 50-70 min.
According to the technical scheme, after the solder powder passes through a 100-mesh sieve, the solder powder is dried for 50-70 min at the temperature of 90-120 ℃ so as to remove the moisture on the surface of the solder powder.
In some embodiments, the testing method further comprises:
providing silicon-molybdenum powder, tin powder and iron powder, and mixing the solder powder, the silicon-molybdenum powder, the tin powder and the iron powder to obtain a mixture, wherein the mass ratio of the solder powder to the silicon-molybdenum powder to the tin powder to the iron powder is 1: 2-4: 2-4: 4-6; and
and putting the mixture into a combustion furnace, and combusting the mixture to obtain sulfur dioxide gas.
In one embodiment, the mass ratio of the solder powder, the silicon-molybdenum powder, the tin powder and the iron powder is 1: 3: 3: 5.
in one embodiment, the purity of the silicon-molybdenum powder is greater than 99.8%, the purity of the tin powder is not less than 99.95%, and the purity of the iron powder is not less than 99.98%.
In one embodiment, the step of mixing the solder powder, the silicon-molybdenum powder, the tin powder, and the iron powder includes: the silicon-molybdenum powder, the tin powder, the welding flux powder and the iron powder are sequentially placed in a crucible.
In one embodiment, the crucible may be a copper crucible.
In one embodiment, the step of placing the mixture in a furnace comprises: the crucible containing the mixture is placed in a furnace.
In the technical scheme of the invention, the welding flux powder, the silicon-molybdenum powder, the tin powder and the iron powder are mixed and ignited by electric arc, the silicon-molybdenum powder and the tin powder are used as combustion promoters, and the iron powder is used as a combustible substance, so that the combustion of the welding flux powder is facilitated. Moreover, the silicon-molybdenum powder is light and is firstly placed in the crucible to prevent the silicon-molybdenum powder from being blown away when oxygen is introduced, and the iron powder is used as combustible and is finally placed in the crucible, so that the adding sequence of the welding flux powder, the silicon-molybdenum powder, the tin powder and the iron powder is set to obtain a better combustion effect.
In some embodiments, the testing method further comprises the step of passing the flux through a 100 mesh screen after the flux has been ground.
In the technical scheme of the invention, after the welding flux is ground, the welding flux powder is sieved by a 100-mesh sieve, so that the welding flux powder with the particle size smaller than 100 meshes is screened out, and the welding flux powder with the smaller particle size can be fully combusted.
In some embodiments, the testing method further comprises the step of sieving at least one of silicon molybdenum powder, tin powder, and iron powder through a 100 mesh sieve.
In the technical scheme of the invention, at least one of silicon molybdenum powder, tin powder and iron powder is sieved by a 100-mesh sieve, so that the silicon molybdenum powder, tin powder or iron powder with the particle size smaller than 100 meshes is obtained, and the silicon molybdenum powder, tin powder or iron powder has larger specific surface area, thereby playing respective roles and being beneficial to combustion of the welding flux powder.
In some embodiments, the combustion furnace is an arc combustion furnace, the flow rate of a flow meter of the arc combustion furnace is 80-120L/h, the combustion time is 1-4 s, the pressurization time is 0.1-0.5 s, and the oxygen purity is 99.9%.
In one embodiment, the copper crucible containing the mixture to be measured is placed in an arc furnace, oxygen is introduced, an arc is ignited, and the obtained sulfur dioxide gas is combusted.
In the technical scheme of the invention, an electric arc combustion furnace is adopted to combust the welding flux powder. Because high-temperature heating is not needed, compared with the danger caused by oxygen combustion at 1250-1300 ℃ by using a high-temperature furnace in the prior art, the testing method has the advantage of small danger coefficient.
In some embodiments, the absorption liquid is a mixture of an alkaline solution and a hydrogen peroxide solution. The alkali salt in the alkali solution is at least one of potassium hydroxide, sodium hydroxide and a mixture of sodium carbonate and sodium bicarbonate. The concentration of alkali salt in the absorption liquid is 0.4-10 g/L. The content of the hydrogen peroxide in the hydrogen peroxide solution is 20-40%.
The alkali salt is at least one of potassium hydroxide, sodium hydroxide and a mixture of sodium carbonate and sodium bicarbonate.
In one embodiment, the alkali salt is potassium hydroxide, and the concentration of potassium hydroxide in the absorption liquid is 2-10 g/L, preferably 4-6 g/L, and more preferably 5 g/L.
In one embodiment, the alkali salt is sodium hydroxide, and the concentration of the sodium hydroxide in the absorption liquid is 2-10 g/L, preferably 4-6 g/L, and more preferably 5 g/L.
In one embodiment, the alkali salt is a mixture of sodium carbonate and sodium bicarbonate, and the mass percent of the sodium carbonate in the absorption liquid is 0.39-0.7 g/L, preferably 0.5-0.6 g/L, and the mass percent of the sodium bicarbonate in the absorption liquid is 0.01-0.05 g/L, preferably 0.015-0.02 g/L.
In one embodiment, the preparation method of the absorption liquid is that the absorption liquid absorption is: accurately weighing 0.530g of sodium carbonate and 0.017g of sodium bicarbonate, placing the sodium carbonate and the sodium bicarbonate into a beaker, dissolving the sodium carbonate and the sodium bicarbonate with a small amount of water, adding 100mL of 30% hydrogen peroxide solution, stirring the mixture evenly, and transferring the mixture into a 1L volumetric flask to obtain an absorption solution.
In the technical scheme of the invention, the absorption liquid is a mixed solution of an alkali solution and a hydrogen peroxide solution. The alkali salt in the alkali solution is at least one of potassium hydroxide, sodium hydroxide and a mixture of sodium carbonate and sodium bicarbonate. The concentration of alkali salt in the absorption liquid is 0.4-10 g/L. The content of the hydrogen peroxide in the hydrogen peroxide solution is 20-40%. After the sulfur dioxide is introduced into the absorption liquid, sulfate ions are generated. The content of sulfate ions can be detected by ion chromatography to obtain the sulfur content in the flux.
In some embodiments, the step of absorbing the sulfur dioxide gas with an absorption liquid comprises:
providing a first porous glass plate absorption tube and a second porous glass plate absorption tube;
the absorption liquid is contained in the first porous glass plate absorption tube and the second porous glass plate absorption tube;
connecting the air outlet of the first porous glass plate absorption pipe to the air inlet of the second porous glass plate absorption pipe in series to form an absorption device;
connecting a gas inlet of the first porous glass plate absorption tube to a gas outlet of the combustion furnace, so that sulfur dioxide gas in the combustion furnace enters the first porous glass plate absorption tube and the second porous glass plate absorption tube through the gas outlet of the combustion furnace, wherein the time for absorbing the sulfur dioxide gas by adopting absorption liquid is 20-50 s; and
and mixing the absorption liquid in the first porous glass plate absorption tube and the second porous glass plate absorption tube.
In one embodiment, the absorption time is preferably 30-40 s, and more preferably 35 s.
In one embodiment, the first fritted absorbent tube and the second fritted absorbent tube have a capacity of 25 mL.
In one embodiment, the first and second fritted absorbent tubes contain 10mL of the absorbent solution.
In the technical scheme of the invention, the gas outlet of the first porous glass plate absorption tube is connected in series to the gas inlet of the second porous glass plate absorption tube to form the absorption device, the gas inlet of the first porous glass plate absorption tube is connected to the gas outlet of the combustion furnace, and sulfur dioxide gas produced by combustion flux can enter the first porous glass plate absorption tube and the second porous glass plate absorption tube through the gas outlet of the combustion furnace, so that the sulfur dioxide can be absorbed by the absorption liquid to generate sulfate ions.
In some embodiments, the step of performing an ion chromatography test on the absorption liquid absorbing the sulfur dioxide gas comprises the steps of:
drawing a standard curve of sulfate ions;
carrying out a plurality of ion chromatography tests on the absorption liquid absorbing the sulfur dioxide gas, and taking an average value;
bringing the average value into a standard curve of the sulfate ions to measure the concentration of the sulfate ions;
the sulfur content of the flux was calculated according to the following formula:
wherein W is the sulfur content of the flux, C is the concentration of sulfate ions in the absorption liquid, V is the volume of the absorption liquid, m is the mass of the flux, and 3 is the coefficient of conversion of sulfate ions to sulfur.
In one embodiment, the method for drawing the standard curve comprises the following steps: transferring 0.00mL, 0.20mL, 0.40mL, 1.00mL and 2.00mL of the standard solution of sulfate ions at the concentration of 1000mg/L into a 100mL volumetric flask; diluting with ultrapure water, and fixing the volume to a scale; after shaking up, placing the mixture on an ion chromatograph for testing to obtain the peak area of a standard working curve of sulfate ions; and drawing a standard working curve of concentration-peak area to obtain a sulfate ion standard curve equation.
In one embodiment, the ion chromatography adopts a Metrosep Upp17-150/4.0 anion analysis column and a Metrosep Upp5 guard/4.0 protection column, and adopts an MSM-A anion suppressor and a conductivity detector, the temperature of the chromatography column is set to be 20-30 ℃, the sample injection amount is 20 mu L, the flow rate is 1mL/min, the eluent contains the same components and component contents as the alkali solution of the absorption solution, and the solvent of the eluent is water. The components of the leacheate and the absorption liquid can be kept consistent, and the content of each component is also kept consistent, so that the body effect is reduced, and the result of quantitative analysis is more accurate and reliable.
In one embodiment, the alkaline solution of the absorption solution contains sodium carbonate with a concentration of 0.530g/L and sodium bicarbonate with a concentration of 0.017 g/L. The leacheate also contained sodium carbonate at a concentration of 0.530g/L and sodium bicarbonate at a concentration of 0.017 g/L.
In one embodiment, the absorption liquid absorbing the sulfur dioxide gas is subjected to at least 7 ion chromatography tests, and the average value is taken.
In the technical scheme of the invention, the absorption liquid absorbing sulfur dioxide gas is subjected to ion chromatography test for a plurality of times, an average value is taken, the average value is brought into a standard curve of sulfate ions, the concentration of the sulfate ions is measured, and the sulfur content of the welding flux is calculated according to a formula. The ion chromatography test mode has the advantages of simple and convenient operation, short time consumption and convenient mass detection. The testing method provided by the invention has the advantages that the frozen welding flux is ground, then passes through a 100-mesh sieve, and then is combusted by adopting an arc combustion method, wherein the silicon-molybdenum powder, tin powder and iron powder are used for promoting the full combustion of the welding flux, sulfur dioxide gas generated by combustion can be absorbed by an absorption liquid (such as a sodium carbonate-sodium bicarbonate-hydrogen peroxide mixed solution), and the sulfur content is tested by ion chromatography, so that the testing method provided by the invention has the advantages of high accuracy, good repeatability, convenience and simplicity in operation, short time consumption and convenience in large-batch detection.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which can be directly or indirectly applied to other related technical fields without departing from the spirit of the present invention, are included in the scope of the present invention.
Claims (10)
1. A method for testing the sulfur content in a flux comprises the following steps:
providing a welding flux;
freezing the flux;
grinding the frozen flux to obtain flux powder;
placing the solder powder in a combustion furnace, and combusting the solder powder to obtain sulfur dioxide gas;
absorbing the sulfur dioxide gas by adopting absorption liquid; and
and (4) carrying out ion chromatography test on the absorption liquid absorbing the sulfur dioxide gas, and calculating to obtain the sulfur content in the absorption liquid so as to obtain the sulfur content of the welding flux.
2. The method for testing the sulfur content of flux according to claim 1, wherein said step of freezing said flux comprises:
filling the welding flux and the grinding balls into a grinding tank; and
the grind pot was cooled by immersing it in liquid nitrogen so that the temperature of the flux was below-10 ℃.
3. The method for testing the sulfur content in flux according to claim 2, wherein said step of grinding the frozen flux to obtain flux powder comprises:
and fixing the frozen grinding tank on an adapter of a grinding machine, and grinding the welding flux in the grinding tank, wherein the grinding time is 20-40 s, and the grinding frequency is 40-80 Hz.
4. The method for testing the sulfur content in flux according to any one of claims 1 to 3, further comprising:
providing silicon-molybdenum powder, tin powder and iron powder, and mixing the solder powder, the silicon-molybdenum powder, the tin powder and the iron powder to obtain a mixture, wherein the mass ratio of the solder powder to the silicon-molybdenum powder to the tin powder to the iron powder is 1: 2-4: 2-4: 4-6; and
and putting the mixture into a combustion furnace, and combusting the mixture to obtain sulfur dioxide gas.
5. The method of testing the sulfur content of flux of claim 4 wherein said step of mixing said flux powder, silicon molybdenum powder, tin powder, and iron powder comprises: sequentially placing silicon-molybdenum powder, tin powder, welding flux powder and iron powder in a crucible;
the step of placing the mixture in a furnace comprises: the crucible containing the mixture is placed in a furnace.
6. The method for testing the sulfur content in flux according to any one of claims 1 to 3, further comprising the step of sieving the flux powder through a 100-mesh sieve after the flux is ground; and/or
The testing method also comprises the step of sieving at least one of silicon molybdenum powder, tin powder and iron powder through a 100-mesh sieve; and/or
The combustion furnace is an electric arc combustion furnace, the flow rate of a flow meter of the electric arc combustion furnace is 80-120 liters/hour, the combustion time is 1-4 s, the pressurization time is 0.1-0.5 s, and the oxygen purity is 99.9%.
7. The method for measuring sulfur content in flux according to any one of claims 1 to 3, wherein said absorption liquid is a mixture of an alkali solution and a hydrogen peroxide solution, the concentration of the alkali salt in said absorption liquid is 0.4 to 10g/L, and the content of hydrogen peroxide in said hydrogen peroxide solution is 20 to 40%.
8. The method for testing the sulfur content of flux of claim 7 wherein said alkali salt is at least one of potassium hydroxide, sodium hydroxide, and a mixture of sodium carbonate and sodium bicarbonate.
9. The method for testing the sulfur content in flux according to any one of claims 1 to 3, wherein said step of absorbing said sulfur dioxide gas with an absorption liquid comprises:
providing a first porous glass plate absorption tube and a second porous glass plate absorption tube;
the absorption liquid is contained in the first porous glass plate absorption tube and the second porous glass plate absorption tube;
connecting the air outlet of the first porous glass plate absorption pipe to the air inlet of the second porous glass plate absorption pipe in series to form an absorption device;
connecting a gas inlet of the first porous glass plate absorption tube to a gas outlet of the combustion furnace, so that sulfur dioxide gas in the combustion furnace enters the first porous glass plate absorption tube and the second porous glass plate absorption tube through the gas outlet of the combustion furnace, wherein the time for absorbing the sulfur dioxide gas by adopting absorption liquid is 20-50 s; and
and mixing the absorption liquid in the first porous glass plate absorption tube and the second porous glass plate absorption tube.
10. The method for measuring the sulfur content in flux according to any one of claims 1 to 3, wherein said step of performing an ion chromatography test on an absorption liquid in which sulfur dioxide gas is absorbed and calculating the sulfur content in the absorption liquid comprises:
drawing a standard curve of sulfate ions;
carrying out a plurality of ion chromatography tests on the absorption liquid absorbing the sulfur dioxide gas, and taking an average value;
bringing the average value into a standard curve of the sulfate ions to measure the concentration of the sulfate ions;
the sulfur content of the flux was calculated according to the following formula:
wherein W is the sulfur content of the flux, C is the concentration of sulfate ions in the absorption liquid, V is the volume of the absorption liquid, and m is the mass of the flux.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010760048.8A CN112611831A (en) | 2020-07-31 | 2020-07-31 | Method for testing sulfur content in welding flux |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010760048.8A CN112611831A (en) | 2020-07-31 | 2020-07-31 | Method for testing sulfur content in welding flux |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112611831A true CN112611831A (en) | 2021-04-06 |
Family
ID=75224424
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010760048.8A Pending CN112611831A (en) | 2020-07-31 | 2020-07-31 | Method for testing sulfur content in welding flux |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112611831A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102128797A (en) * | 2010-12-09 | 2011-07-20 | 湖北兴发化工集团股份有限公司 | Method for measuring total sulfur content in yellow phosphorus tail gas |
| CN106338551A (en) * | 2015-07-07 | 2017-01-18 | 中国石油化工股份有限公司 | Analytical method for content of elemental sulphur in different forms in reforming catalyst |
| CN107167552A (en) * | 2016-08-31 | 2017-09-15 | 北京彤程创展科技有限公司 | A kind of method for determining sulfur content in rubber and rubber product |
-
2020
- 2020-07-31 CN CN202010760048.8A patent/CN112611831A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102128797A (en) * | 2010-12-09 | 2011-07-20 | 湖北兴发化工集团股份有限公司 | Method for measuring total sulfur content in yellow phosphorus tail gas |
| CN106338551A (en) * | 2015-07-07 | 2017-01-18 | 中国石油化工股份有限公司 | Analytical method for content of elemental sulphur in different forms in reforming catalyst |
| CN107167552A (en) * | 2016-08-31 | 2017-09-15 | 北京彤程创展科技有限公司 | A kind of method for determining sulfur content in rubber and rubber product |
Non-Patent Citations (3)
| Title |
|---|
| 李青: "《平板显示基板玻璃技术概论 第1版》", 30 June 2017, 河北科技技术出版社 * |
| 熊文明等: ""管式炉燃烧-离子色谱法测定熔炼焊剂中硫"", 《理化检验-化学分册》 * |
| 苏珊 尼尔森: "《食品分析 第五版》", 31 May 2019, 北京：中国轻工业出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103196880B (en) | Method for determining content of arsenic in iron ore by using hydride generation-atomic fluorescence spectroscopy | |
| CN110398565A (en) | A comprehensive analysis device for combustion and fire extinguishing process of cup burner | |
| CN103471879A (en) | Flue gas trapping device and method for rapidly and accurately measuring 7 heavy metals in flue gas | |
| CN109030703A (en) | A kind of method of content of halogen in Oxygen Bomb Combustion-sulfate by ion chromatography cable nonmetallic materials | |
| CN100595567C (en) | A Method for Quantitatively Analyzing Metal Elements in Alloys | |
| CN116148243A (en) | A kind of detection method of total amount of inorganic carbon in organic decarburization solution | |
| CN112611831A (en) | Method for testing sulfur content in welding flux | |
| CN103543134B (en) | The method of lead content in Hg-afs Determination iron ore | |
| CN103499536A (en) | Method for measuring indium content in exhaust gas by utilizing flame atomic absorption spectrometry | |
| Boniface et al. | The determination of carbon in steel by coulometric titration in partially aqueous medium | |
| CN111257258A (en) | Method for detecting zinc in dust mud based on atomic absorption spectrum | |
| CN110672577A (en) | Method for measuring selenium content in rice | |
| CN206515230U (en) | It is a kind of at the same measure air in nitrous acid, ozone, the equipment of nitrogen dioxide | |
| CN114414539B (en) | Method for measuring content of bismuth and antimony elements in roasted molybdenum concentrate | |
| CN212228732U (en) | System for measuring effective sulfur content in ore | |
| CN111983062B (en) | A kind of detection method of trace DMAEA in air | |
| CN104597108B (en) | A kind of detection method of Hg element in cigarette mainstream smoke content | |
| CN101561409B (en) | Electrolyte analysis standard solution and preparation method thereof | |
| Cai et al. | Quantification of lithium in molten chlorides by optical emission spectrometry using a novel molten-salt-electrode microplasma source | |
| CN110118740A (en) | Measure the micro-wave digestion sampling Graphite Furnace Atomic Absorption analysis method of trace lead in white wine | |
| CN116165191A (en) | A method for detecting the concentration of HCO3- and CO32- in organic decarburization solution | |
| CN219694818U (en) | Measuring device for carbonation degree of alcohol amine solution | |
| CN110095556A (en) | Measure the thermal desorption-gas chromatograph and detection method of sulfide content in hydrogen | |
| CN222734142U (en) | Carbon dioxide gas generation amount measuring device | |
| CN118641529A (en) | A rapid determination method for gold, platinum and palladium in complex nickel-copper sulfide materials |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210406 |