CN116298115A - Method for identifying industrial salt and edible salt based on total organic carbon content - Google Patents
Method for identifying industrial salt and edible salt based on total organic carbon content Download PDFInfo
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- CN116298115A CN116298115A CN202310260525.8A CN202310260525A CN116298115A CN 116298115 A CN116298115 A CN 116298115A CN 202310260525 A CN202310260525 A CN 202310260525A CN 116298115 A CN116298115 A CN 116298115A
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- 150000003839 salts Chemical class 0.000 title claims abstract description 92
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 88
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000011550 stock solution Substances 0.000 claims abstract description 13
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 8
- 239000008231 carbon dioxide-free water Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- IWZKICVEHNUQTL-UHFFFAOYSA-M potassium hydrogen phthalate Chemical compound [K+].OC(=O)C1=CC=CC=C1C([O-])=O IWZKICVEHNUQTL-UHFFFAOYSA-M 0.000 claims description 4
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 4
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000000741 silica gel Substances 0.000 claims description 3
- 229910002027 silica gel Inorganic materials 0.000 claims description 3
- 229910052665 sodalite Inorganic materials 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- 238000005303 weighing Methods 0.000 claims 1
- 235000002639 sodium chloride Nutrition 0.000 description 72
- 238000001514 detection method Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000011071 total organic carbon measurement Methods 0.000 description 2
- 229920000426 Microplastic Polymers 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052674 natrolite Inorganic materials 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000000447 pesticide residue Substances 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000013582 standard series solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
-
- 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
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for identifying industrial salt and edible salt based on total organic carbon content, which comprises the following steps: preparing an organic carbon standard stock solution and an inorganic carbon standard stock solution respectively; drawing a standard curve of total carbon and inorganic carbon; determining the total carbon and inorganic carbon content of the sample, calculating the total organic carbon content of the sample, and judging the sample as edible salt when the total organic carbon content is less than 10 mg/L; when the total organic carbon is more than 20mg/L, judging that the sample is industrial salt; when the total organic carbon is more than 10 and less than 20mg/L, the gas chromatography-time-of-flight mass spectrometer is used for further distinguishing industrial salt from edible salt. The invention can rapidly and effectively identify and distinguish industrial salt from edible salt.
Description
Technical Field
The invention belongs to the technical field of salt inspection, and particularly relates to a method for identifying industrial salt and edible salt based on total organic carbon content.
Background
The two-alkali industry taking industrial salt as a main raw material in China generally enters a high-speed growth period, so that the yield and the demand of the industrial salt are large, the great development of the salt industry is directly driven, and meanwhile, the problems of difficult supervision and the like caused by the large-scale circulation of the industrial salt in the market are also caused. Besides edible salt, the salt circulated in the market also comprises unrefined raw material salt such as well mineral salt, rock salt, sea salt, lake salt and the like, industrial salt which is processed and used in industrial production such as two-alkali industry, water treatment, leather, printing and dyeing industry and the like, and other salts such as byproduct industrial salt brought by industrial production and the like. The salt, especially the industrial salt, is not refined and purified, does not meet the relevant national mandatory standard of edible salt, however, some illegal merchants obtain more profits for saving cost, and the illegal mixed use of the industrial salt as the edible salt for sale, thereby causing great potential safety hazard.
The traditional industrial salt detection and identification are concentrated on nitrite components possibly contained in the industrial salt detection and identification are generally carried out by adopting the national standard method 'determination of nitrite and nitrate in GB5009.33-2016 food'. However, nitrite content of some industrial salts may be within a safe range, but excessive organic pollutants such as industrial auxiliary agents, medicines or pesticide residues with unknown components are introduced due to the reasons of flow channels, production processes and the like, and the substances have great potential safety hazards, but a corresponding effective detection and analysis method is still lacking. At present, the organic related detection of the salt is only concentrated on micro plastic particles, organic polymer particles and the like in the edible salt, and the problems of detection and identification of industrial salt and the edible salt cannot be fundamentally solved.
Disclosure of Invention
The technical problems to be solved are as follows: aiming at the technical problems, the invention provides a method for identifying industrial salt and edible salt based on total organic carbon content, which can rapidly and effectively identify and distinguish the industrial salt and the edible salt.
The technical scheme is as follows: a method for identifying industrial salt and edible salt based on total organic carbon content, comprising the steps of:
step one, respectively preparing an organic carbon standard stock solution and an inorganic carbon standard stock solution;
drawing a standard curve of total carbon and inorganic carbon;
measuring the total carbon and inorganic carbon content of the sample, calculating the total organic carbon content of the sample, and judging the sample as edible salt when the total organic carbon content is less than or equal to 10 mg/L; when the total organic carbon is more than or equal to 20mg/L, judging that the sample is industrial salt; when the total organic carbon is more than 10 and less than 20mg/L, the gas chromatography-time-of-flight mass spectrometer is used for further distinguishing industrial salt from edible salt.
Preferably, the preparation method of the organic carbon standard stock solution comprises the following steps: 2.1254g of potassium hydrogen phthalate is weighed, dried for 2 hours at 120 ℃, dissolved by carbon dioxide-free water, and then fixed in a 1000mL volumetric flask, wherein the organic carbon concentration of the solution is 1000mg/L.
Preferably, the preparation method of the inorganic carbon standard stock solution comprises the following steps: 1.750g and 2.208g of sodium bicarbonate and anhydrous sodium carbonate dried by silica gel are respectively weighed, dissolved by anhydrous carbon dioxide water and then fixed in a 1000mL volumetric flask, and the inorganic carbon concentration of the solution is 1000mg/L.
Further, the preparation method of the carbon dioxide-free water comprises the following steps: water was poured into the flask, boiled for 10min, immediately stoppered with a plug fitted with a sodalite tube, and cooled.
The beneficial effects are that: according to the method, salt to be detected and industrial salt samples are fully dissolved by using quantitative carbon dioxide-free water, qualitative filter paper is used for filtering, the filtered solution is used for measuring the content of inorganic carbon and total carbon by using an organic carbon tester, and the inorganic carbon and total carbon standard curves are compared and quantified, so that the total organic carbon content of the test samples is obtained. The total organic carbon measurement result shows that the total organic carbon residue in the industrial salt is one to two orders of magnitude higher than that of the edible salt, and the types of the industrial salt and the edible salt can be rapidly and effectively distinguished according to the characteristic.
Drawings
FIG. 1 is a graph showing peak shapes of inorganic carbon and total carbon content in industrial salt 1;
FIG. 2 is a graph showing peak shapes of inorganic carbon and total carbon content in industrial salt 2;
FIG. 3 is a graph showing peak shapes of inorganic carbon and total carbon content in edible salt 1;
FIG. 4 is a graph showing peak shapes of inorganic carbon and total carbon content in edible salt 2;
FIG. 5 is a graph showing peak shapes of inorganic carbon and total carbon content in edible salt 3;
FIG. 6 is a graph showing peak shapes of inorganic carbon and total carbon content in edible salt 4;
FIG. 7 is a graph showing peak shapes of inorganic carbon and total carbon content in edible salt 5;
FIG. 8 is a graph showing peak shapes of inorganic carbon and total carbon content in the edible salt 6.
Detailed Description
The invention is further described below with reference to the drawings and specific embodiments. The reagents used in the present invention are all commercially available and are specifically as follows: ultrapure water, potassium hydrogen phthalate (KHC 8H4O 4) (superior purity), anhydrous sodium carbonate (superior purity), sodium bicarbonate (superior purity).
Example 1
A method for identifying industrial salt and edible salt based on total organic carbon content, comprising the steps of:
step one, preparing a standard stock solution: organic carbon standard stock solution (c=1000 mg/L): 2.1254g of potassium hydrogen phthalate is weighed, dried for 2 hours at 120 ℃, dissolved by carbon dioxide-free water (preparation method: water is injected into a flask, boiled for 10 minutes, immediately plugged by a rubber plug with a natrolite ash tube, cooled) and then fixed in a 1000mL volumetric flask, and the organic carbon concentration of the solution is 1000mg/L. Inorganic carbon standard stock solution (c=1000 mg/L): 1.750g and 2.208g of sodium bicarbonate and anhydrous sodium carbonate are respectively weighed, dried by silica gel, dissolved by anhydrous carbon dioxide water and then fixed in a 1000mL volumetric flask, and the inorganic carbon concentration of the solution is 1000mg/L.
Drawing a standard curve: standard series solutions with total carbon mass concentration of 0.0mg/L, 4.0mg/L, 10.0mg/L, 20.0mg/L, 50.0mg/L, 100.0mg/L and 200.0mg/L are prepared, response values are measured, and calibration curves of Total Carbon (TC) and Inorganic Carbon (IC) are drawn and stored in an instrument for later use.
Step three, a sample preparation method: 100.0mg of each salt sample is accurately weighed into a 250mL beaker, 100.0mL of carbon dioxide-free water is accurately added, the soluble substances are fully stirred and dissolved, and after being filtered by 90mm qualitative filter paper, the Total Carbon (TC) and Inorganic Carbon (IC) contents are determined by machine analysis.
Specifically, in this example, 100.0mg of any 2 commercial salt samples and 6 edible salt samples on the market were weighed into 250mL beakers, 100.0mL of carbon dioxide-free water was accurately added to each sample, and the soluble substances were dissolved by stirring thoroughly, filtered with a 90mm qualitative filter paper, and the filtrates were quantitatively analyzed with an organic carbon analyzer, respectively.
The total organic carbon content measurement results are shown in table 1:
TABLE 1 Total organic carbon content in Industrial salt and edible salt
The specific peak shape patterns are shown in figures 1-8.
From the above total organic carbon measurement results, it can be seen that there is a significant difference in total organic carbon residues of edible salt and industrial salt: the total organic carbon content of 6 kinds of edible salt is between 0 and 10mg/L, and the total organic carbon content of 2 kinds of industrial salt is higher than 20mg/L. The obvious difference can be used as a preliminary basis for judging and distinguishing the industrial salt from the edible salt: when the total organic carbon content is less than or equal to 10mg/L, judging that the sample is edible salt; when the total organic carbon is more than or equal to 20mg/L, judging that the sample is industrial salt; when the total organic carbon is more than 10 and less than 20mg/L, the gas chromatography-time-of-flight mass spectrometer can be utilized to further identify and distinguish industrial salt and edible salt, thereby greatly shortening the identification time and improving the identification efficiency.
Claims (4)
1. A method for identifying industrial salt and edible salt based on total organic carbon content, comprising the steps of:
step one, respectively preparing an organic carbon standard stock solution and an inorganic carbon standard stock solution;
drawing a standard curve of total carbon and inorganic carbon;
measuring the total carbon and inorganic carbon content of the sample, calculating the total organic carbon content of the sample, and judging the sample as edible salt when the total organic carbon content is less than or equal to 10 mg/L; when the total organic carbon is more than or equal to 20mg/L, judging that the sample is industrial salt; when the total organic carbon is more than 10 and less than 20mg/L, the gas chromatography-time-of-flight mass spectrometer is used for further distinguishing industrial salt from edible salt.
2. The method for identifying industrial salts and edible salts based on total organic carbon content according to claim 1, wherein the method for preparing the standard stock solution of organic carbon is as follows: weighing 2.1254g potassium hydrogen phthalate, drying at 120 ℃ for 2h, dissolving with carbon dioxide-free water, and then fixing the volume in a volumetric flask of 1000mL, wherein the organic carbon concentration of the solution is 1000mg/L.
3. The method for identifying industrial salts and edible salts based on total organic carbon content according to claim 1, wherein the method for preparing the standard stock solution of inorganic carbon is as follows: 1.750g and 2.208g g of sodium bicarbonate and anhydrous sodium carbonate dried by silica gel are respectively weighed, dissolved by anhydrous carbon dioxide water and then fixed in a volumetric flask of 1000mL, and the inorganic carbon concentration of the solution is 1000mg/L.
4. A method for identifying industrial salts from edible salts based on total organic carbon content according to claim 2 or 3, characterized in that the method for preparing carbon dioxide free water is as follows: water was poured into the flask, boiled for 10min, immediately stoppered with a plug fitted with a sodalite tube, and cooled.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310260525.8A CN116298115A (en) | 2023-03-17 | 2023-03-17 | Method for identifying industrial salt and edible salt based on total organic carbon content |
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| CN202310260525.8A CN116298115A (en) | 2023-03-17 | 2023-03-17 | Method for identifying industrial salt and edible salt based on total organic carbon content |
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| CN116298115A true CN116298115A (en) | 2023-06-23 |
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| CN202310260525.8A Pending CN116298115A (en) | 2023-03-17 | 2023-03-17 | Method for identifying industrial salt and edible salt based on total organic carbon content |
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- 2023-03-17 CN CN202310260525.8A patent/CN116298115A/en active Pending
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