CN112730402A - Method suitable for rapidly identifying sulfur content in wet ammonium paratungstate material in production process - Google Patents
Method suitable for rapidly identifying sulfur content in wet ammonium paratungstate material in production process Download PDFInfo
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- CN112730402A CN112730402A CN202011545200.7A CN202011545200A CN112730402A CN 112730402 A CN112730402 A CN 112730402A CN 202011545200 A CN202011545200 A CN 202011545200A CN 112730402 A CN112730402 A CN 112730402A
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 55
- 239000011593 sulfur Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 51
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 title claims abstract description 29
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 title claims abstract description 13
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 66
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 39
- 238000003756 stirring Methods 0.000 claims description 39
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims description 25
- 229910001626 barium chloride Inorganic materials 0.000 claims description 25
- 239000000243 solution Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000000706 filtrate Substances 0.000 claims description 18
- 239000012153 distilled water Substances 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000013558 reference substance Substances 0.000 claims description 9
- 239000003153 chemical reaction reagent Substances 0.000 claims description 6
- 239000012086 standard solution Substances 0.000 claims description 5
- 239000012085 test solution Substances 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 2
- 239000012088 reference solution Substances 0.000 claims description 2
- 239000000523 sample Substances 0.000 description 43
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 12
- 239000000047 product Substances 0.000 description 12
- 239000002244 precipitate Substances 0.000 description 9
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 4
- 238000004879 turbidimetry Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000012488 sample solution Substances 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000012716 precipitator Substances 0.000 description 2
- 238000003908 quality control method Methods 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
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
- G01N21/82—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 precipitate or turbidity
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a method for rapidly identifying the sulfur content of an ammonium paratungstate wet material in a production process, which is rapid and simple and has high accuracy.
Description
Technical Field
The invention relates to a method for measuring sulfur content, in particular to a method for detecting the sulfur content of wet ammonium paratungstate materials by using a turbidimetry method.
Technical Field
The ammonium paratungstate is mainly used for manufacturing metal tungsten powder made of tungsten trioxide or blue tungsten oxide. In the production of ammonium paratungstate, a vulcanizing agent is required to be added for removing impurities, the content of sulfur and sulfides in various forms in the product liquid is up to more than 2g/L, and the quality control of the sulfur in the product end is realized by implementing a sulfur removal process in the production. Before the drying procedure of the product section in the production process, the washing of sulfur attached to the wet material of the crystallized product and the residual amount identification of the sulfur are required to be realized so as to achieve the quality control standard that the sulfur of the product is lower than 7 PPM.
The existing method adopts a special sulfur determination instrument, has long determination time and can not meet the requirement of safety control and analysis on the product quality in the production process. And a combustion conductive method is adopted, the method burns a sample in oxygen flow at high temperature, sulfur generates sulfur dioxide, the sulfur is absorbed by iodine solution, and the method is measured by a conductive method, and is complex in operation and long in time consumption. CN201310497734 discloses an analysis method of sulfur in ammonium paratungstate, which adopts high-temperature calcination to oxidize sulfur into SO2、SO3By H2O2The solution was taken up and then the sulphur content was determined by ICP. The method still has the requirements of complex and fussy operation, need of precise instrument identification, unsuitability for the real-time control stage in the production procedure of the production line and quick detection of flow.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for rapidly detecting the sulfur content in ammonium paratungstate in a production process. The method is rapid and simple, and has high accuracy.
The invention is realized by the following technical scheme:
the invention provides a method for detecting the sulfur content in ammonium paratungstate in a production process, which comprises the following steps:
and (3) sequentially adding hydrogen peroxide, a citric acid solution and a barium chloride solution into an ammonium paratungstate sample, uniformly stirring for reaction, and then determining the sulfur content by a turbidimetric method.
Further, the method comprises the following steps:
(1) preparing a test solution: putting an ammonium paratungstate sample in a beaker, adding distilled water and hydrogen peroxide, shaking and standing, filtering, and heating the filtrate to be clear; adding citric acid solution, and stirring uniformly; adding barium chloride solution, and stirring well to obtain the final product;
(2) preparation of standard control solutions:
(3) the determination method comprises the following steps: the turbidity was observed and the sulfur content was determined.
Preparing a standard sample reference solution in the step (2) of the invention: weighing an ammonium paratungstate sample with the sulfur content of 7ppm in a beaker, adding distilled water and hydrogen peroxide, shaking, standing, filtering, and heating the filtrate to be clear; adding citric acid solution, and stirring uniformly; adding barium chloride solution, and stirring.
In the method, the hydrogen peroxide is used as an oxidant and can oxidize low-valence sulfur in the ammonium paratungstate into sulfate radicals; citric acid is a complexing agent and can mask the tungsten of the main body so as to eliminate chemical interference of the tungsten; then barium chloride is added as a precipitator of sulfur to form sulfate precipitates.
The sulfur content detection method provided by the invention has the main chemical reaction formula:
S2-+H2O2→SO42-
SO42-+Ba2+→BaSO4↓
further, the ratio of the volume of the hydrogen peroxide solution to the mass of the sample is 0.5-1.5: 40-60(ml/g), excessive hydrogen peroxide is added, some impurities are oxidized, the solution turns into light green, and judgment of results is affected. Preferably, the ratio of hydrogen oxide volume to sample mass is 1: 50.
further, the concentration of the citric acid solution is 40-70%. The concentration is lower than 40%, the complexation is incomplete, and interference is generated. Preferably at a concentration of 40% complexing is complete and has good stability to tungsten mask.
Further, the preparation of the citric acid solution comprises the following steps: 40-70g of citric acid crystals are dissolved in a proper amount of water and diluted to 100 mL.
Further, the concentration of barium chloride is 20-40%, the concentration of a precipitator (barium chloride) is too low and lower than 20%, the precipitation reaction is incomplete, the turbidity is not well observed, and the judgment of the result is influenced. The concentration is higher than 40%, barium chloride is easy to crystallize, and the mixture in the white barium sulfate precipitate influences the result judgment, so that whether the white precipitate is barium sulfate or barium chloride cannot be judged. Therefore, a concentration of 20% is most suitable.
Further, the preparation of the barium chloride solution: dissolving 20-40g of barium chloride crystal in a proper amount of water, and diluting to 100 mL.
Further, the volume ratio of the hydrogen peroxide to the citric acid solution to the barium chloride solution is 0.5-1:3-5:0.5-1, preferably 1:5: 1.
Furthermore, the turbidimetry of the test solution and the standard sample control adopts visual turbidimetry. The precipitate generated by the method is white barium sulfate precipitate which is difficult to dissolve in water, and whether the sulfur content of the sample exceeds 7ppm can be judged by visually observing the turbidity of the sample solution and the turbidity of the standard sample.
Advantageous effects
1. The method is used for identifying and judging the sulfur content of wet materials at the process product end, and performing quality safety control on product process nodes of a production line, the method is implemented in an enterprise for more than two years, the accumulated yield exceeds 10000 tons, and the qualified rate of product sulfur reaches 100%.
2. The invention has simple operation, no need of calcining or burning means, less solvent reagent, simplicity and easy purchase, the whole process only needs a few minutes to be completed, and the invention can be used as a production line to sample in real time for monitoring in a flowing state. The method realizes that whether the sulfur content of the ammonium paratungstate product meets the product quality safety control standard or not at the product process control stage of the production line.
3. The turbidimetry provided by the invention is verified to have the sulfur content of ammonium paratungstate far lower than 7ppm and higher accuracy, and can be used as a monitoring means for production.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The following is a description of embodiments of the present invention. The following examples are given to illustrate the present invention, but not to limit the scope of the present invention.
Example 1
Preparing a test sample: weighing 50 samples into a 300mL beaker, adding 30mL of distilled water, adding 1mL of hydrogen peroxide for analytical purification (concentration 30%), shaking for 5 minutes, standing for 5 minutes, filtering in a 100mL beaker by using quantitative filter paper, heating the filtrate to be clear, adding 5mL of citric acid (40%), stirring uniformly, washing the inner wall of the beaker, stirring uniformly again, adding 1mL of barium chloride (20%), and stirring uniformly.
Preparation of a reference substance: weighing 50g of ammonium paratungstate sample with the sulfur content of 7ppm into a 300mL beaker, adding 30mL of distilled water, adding 1mL of hydrogen peroxide (30%), shaking for 5 minutes, standing for 5 minutes, filtering in a 100mL beaker with quantitative filter paper, heating the filtrate until the filtrate is clear, adding 5mL of citric acid (40%), stirring uniformly, washing the inner wall of the beaker, stirring uniformly again, adding 1mL of barium chloride (20%), and stirring uniformly. This standard solution was stored in a transparent reagent bottle.
The determination method comprises the following steps: and (4) taking a sample, observing the turbidity, comparing with a standard sample reference substance, and judging whether the sulfur content of the sample exceeds 7ppm or not, wherein the sample with the sulfur content of 7ppm is taken as a standard sample. The precipitate generated by the method is white barium sulfate precipitate which is difficult to dissolve in water, and whether the sulfur content of the sample exceeds 7ppm can be judged by visually observing the turbidity of the sample solution and the turbidity of the standard sample.
Example 2
Preparing a test sample: weighing 50 samples into a 300mL beaker, adding 30mL of distilled water, adding 0.5mL of hydrogen peroxide for analytical purification (concentration of 30%), shaking for 5 minutes, standing for 5 minutes, filtering in a 100mL beaker by using quantitative filter paper, heating the filtrate to be clear, adding 5mL of citric acid (50% concentration), stirring uniformly, washing the inner wall of the beaker, stirring uniformly again, adding 1mL of barium chloride (30% concentration), and stirring uniformly.
Preparation of a reference substance: weighing 50g of ammonium paratungstate sample with the sulfur content of 7ppm into a 300mL beaker, adding 30mL of distilled water, adding 1mL of hydrogen peroxide (30%), shaking for 5 minutes, standing for 5 minutes, filtering in a 100mL beaker with quantitative filter paper, heating the filtrate until the filtrate is clear, adding 5mL of citric acid (50%), stirring uniformly, washing the inner wall of the beaker, stirring uniformly again, adding 1mL of barium chloride (30%), and stirring uniformly. This standard solution was stored in a transparent reagent bottle.
The determination method comprises the following steps: and (4) taking a sample, observing the turbidity, comparing with a standard sample reference substance, and judging whether the sulfur content of the sample exceeds 7ppm or not, wherein the sample with the sulfur content of 7ppm is taken as a standard sample.
Example 3
Preparing a test sample: weighing 50 samples into a 300mL beaker, adding 30mL of distilled water, adding 1mL of hydrogen peroxide for analytical purification (concentration of 30%), shaking for 5 minutes, standing for 5 minutes, filtering in a 100mL beaker by using quantitative filter paper, heating the filtrate to be clear, adding 5mL of citric acid (70% concentration), stirring uniformly, washing the inner wall of the beaker, stirring uniformly again, adding 1mL of barium chloride (40% concentration), and stirring uniformly.
Preparation of a reference substance: weighing 50g of ammonium paratungstate sample with the sulfur content of 7ppm into a 300mL beaker, adding 30mL of distilled water, adding 1mL of hydrogen peroxide (30%), shaking for 5 minutes, standing for 5 minutes, filtering in a 100mL beaker with quantitative filter paper, heating the filtrate until the filtrate is clear, adding 5mL of citric acid (70%), stirring uniformly, washing the inner wall of the beaker, stirring uniformly again, adding 1mL of barium chloride (40%), and stirring uniformly. This standard solution was stored in a transparent reagent bottle.
The determination method comprises the following steps: and (4) taking a sample, observing the turbidity, comparing with a standard sample reference substance, and judging whether the sulfur content of the sample exceeds 7ppm or not, wherein the sample with the sulfur content of 7ppm is taken as a standard sample.
Example 4
Preparing a test sample: weighing 50 samples into a 300mL beaker, adding 30mL of distilled water, adding 0.3mL of hydrogen peroxide for analytical purification (concentration 30%), shaking for 5 minutes, standing for 5 minutes, filtering in a 100mL beaker with quantitative filter paper, heating the filtrate to be clear, adding 3mL of citric acid (40%), stirring uniformly, washing the inner wall of the beaker, stirring uniformly again, adding 1mL of barium chloride (20%), and stirring uniformly.
Preparation of a reference substance: weighing 50g of ammonium paratungstate sample with the sulfur content of 7ppm into a 300mL beaker, adding 30mL of distilled water, adding 1mL of hydrogen peroxide (30%), shaking for 5 minutes, standing for 5 minutes, filtering in a 100mL beaker with quantitative filter paper, heating the filtrate until the filtrate is clear, adding 5mL of citric acid (40%), stirring uniformly, washing the inner wall of the beaker, stirring uniformly again, adding 0.5mL of barium chloride (20%), and stirring uniformly. This standard solution was stored in a transparent reagent bottle.
The determination method comprises the following steps: and (4) taking a sample, observing the turbidity, comparing with a standard sample reference substance, and judging whether the sulfur content of the sample exceeds 7ppm or not, wherein the sample with the sulfur content of 7ppm is taken as a standard sample. The precipitate generated by the method is white barium sulfate precipitate which is difficult to dissolve in water, and the sulfur content of the sample can be judged to be not more than 7ppm by visual inspection of the turbidity of the sample solution and the turbidity of the standard sample.
Claims (7)
1. A method for rapidly identifying the sulfur content of wet ammonium paratungstate materials in production procedures is characterized by comprising the following steps:
(1) preparing a test solution: putting an ammonium paratungstate sample in a beaker, adding distilled water and hydrogen peroxide, shaking and standing, filtering, and heating the filtrate to be clear; adding citric acid solution, and stirring uniformly; adding barium chloride solution, and stirring well to obtain the final product;
(2) preparation of standard control solutions:
(3) the determination method comprises the following steps: the turbidity was observed and the sulfur content was determined.
2. The method for rapidly identifying the sulfur content of the wet ammonium paratungstate material in the production process according to claim 1, wherein the method comprises the following steps: preparing the standard sample reference solution in the step (2): weighing an ammonium paratungstate sample with the sulfur content of 7ppm in a beaker, adding distilled water and hydrogen peroxide, shaking, standing, filtering, and heating the filtrate to be clear; adding citric acid solution, and stirring uniformly; adding barium chloride solution, and stirring.
3. The method for rapidly identifying the sulfur content of the wet ammonium paratungstate material in the production process according to claim 1 or 2, wherein the method comprises the following steps: the ratio of the volume of the hydrogen peroxide solution to the mass of the sample is 0.5-1.5: 40-60(ml/g), preferably, the ratio of hydrogen oxide volume to sample mass is 1: 50.
4. the method for rapidly identifying the sulfur content of the wet ammonium paratungstate material in the production process according to claim 1 or 2, wherein the method comprises the following steps: the concentration of the citric acid solution is 40-70%, and the preferred concentration is 40%.
5. The method for rapidly identifying the sulfur content of the wet ammonium paratungstate material in the production process according to claim 1 or 2, wherein the method comprises the following steps: the concentration of the barium chloride is 20-40%, and 20% is preferred.
6. The method for rapidly identifying the sulfur content of the wet ammonium paratungstate material in the production process according to claim 1 or 2, wherein the method comprises the following steps: the volume ratio of the hydrogen peroxide to the citric acid solution to the barium chloride solution is 0.5-1:3-5:0.5-1, preferably 1:5: 1.
7. The method for rapidly identifying the sulfur content of the wet ammonium paratungstate material in the production process according to claim 1, wherein the method comprises the following steps: the method comprises the following steps:
(1) preparing a test solution:
weighing 50g of sample, putting the sample in a 300mL beaker, adding 30mL of distilled water, adding 1mL of hydrogen peroxide for purity analysis, shaking for 5 minutes, standing for 5 minutes, filtering the sample in a 100mL beaker by using quantitative filter paper, heating the filtrate to be clear, adding 5mL of citric acid with the concentration of 40%, uniformly stirring, washing the inner wall of the beaker, uniformly stirring again, adding 1mL of barium chloride with the concentration of 20%, and uniformly stirring;
(2) preparation of standard control solutions: weighing 50g of ammonium paratungstate sample with the sulfur content of 7ppm into a 300mL beaker, adding 30mL of distilled water, adding 1mL of hydrogen peroxide, shaking for 5 minutes, standing for 5 minutes, filtering in a 100mL beaker by using quantitative filter paper, heating the filtrate to be clear, adding 5mL of 40% citric acid, stirring uniformly, washing the inner wall of the beaker, stirring uniformly again, adding 1mL of 20% barium chloride, and stirring uniformly; this standard solution was stored in a transparent reagent bottle.
(3) The determination method comprises the following steps: and (3) taking a test sample to observe turbidity, comparing the turbidity with a standard sample reference substance, and judging whether the sulfur content of the test sample exceeds 7ppm or not, wherein the sample with the sulfur content of 7ppm is taken as a standard sample.
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