Method for determining content of Si in organic matter by adopting ICP-OES
By dissolving the silicon-containing organic matter in the aqueous sodium hydroxide solution and heating and digesting it in the ICP-OES method, the problems of high sample pretreatment requirements and low measurement results in the prior art are solved, and the Si content measurement with simple operation and high accuracy is achieved.
Patent Information
- Application Number
- CN202411923483.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-25
- Publication Date
- 2025-03-28
AI Technical Summary
In the prior art, sample pretreatment requirements are high and measurement results are low.
The Si content in organic matter was determined by ICP-OES method, and the silicon-containing organic matter was dissolved in aqueous sodium hydroxide solution, and then digested by heating and digestion.
This method is simple to operate and has high accuracy, which can effectively solve the problems of high sample preprocessing requirements and low measurement results.
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Abstract
Description
Technical Field
[0001] The invention relates to a method for measuring Si content in organic matter by adopting ICP-OES. Background Art
[0002] At present, the methods for testing Si content in China include: gravimetric method, spectrophotometer method, atomic absorption spectrometry, atomic emission spectrometry and inductively coupled plasma spectrometer method. Each method has its own advantages and disadvantages. The gravimetric method is simple to operate but is easily affected by impurities; the spectrophotometer method is simple to operate and highly sensitive but is easily interfered by coexisting ions; the atomic absorption spectrometry method is highly sensitive but complex to operate; the atomic emission spectrometry method can test multiple elements at the same time, but the equipment cost is high and the operation is complex; the inductively coupled plasma spectrometer method can test multiple elements at the same time, has high sensitivity and low detection limit, but has high requirements for sample pretreatment. Summary of the invention
[0003] The technical problem to be solved by the present invention is to overcome the defects of the prior art that the sample pretreatment requirements are high and the measurement result accuracy is low, and a method for determining the Si content in organic matter by using ICP-OES is provided. The method for determining the Si content in organic matter by using ICP-OES provided by the present invention is simple to operate and has high accuracy.
[0004] The present invention solves the above technical problems through the following technical solutions:
[0005] The invention provides a method for measuring Si content in organic matter by using ICP-OES, which comprises the following steps: dissolving silicon-containing organic matter in a sodium hydroxide aqueous solution, heating and digesting it, and then detecting it by using ICP-OES to read the Si content.
[0006] In some embodiments, the silicon-containing organic compound is , R1, R2, R3 and R4 are independently C 1-12 Alkyl, C 1-12 Alkenyl, C 1-12 Alkoxy, C 1-12 Alkylamino, C 1-12 Alkylhydroxyl or -R 1-1 -XR 1-2 , R 1-1 C 1-6 Alkylene, R 1-2 C 1-12 Alkyl, C 1-12 Alkenyl, C 1-12 Alkynyl or C 1-12 Alkoxy; X is .
[0007] In some embodiments, R1, R2, R3, R4 and R 1-2In the 1-12 Alkyl", "C 1-12 Alkenyl", "C 1-12 Alkoxy", "C 1-12 Alkylamino", "C 1-12 Alkyl hydroxyl" and "C 1-12 "C" in "alkynyl" 1-12 "Independently for "C 1-6 ”, preferably “C 1-4 ”.
[0008] In some embodiments, R1, R2, and R3 are the same.
[0009] In some embodiments, R1, R2 and R3 are C 1-4 Alkoxy; for example, methoxy.
[0010] In some embodiments, R4 is C 1-4 Alkylamino or -R 1-1 -XR 1-2 ; R 1-1 C 1-4 Alkylene, R 1-2 C 1-4 Alkenyl.
[0011] In some embodiments, R4 is C 1-4 Alkylamino or -R 1-1 -XR 1-2 ; R 1-1 is methylene or straight-chain propylene; for example, straight-chain propylene; R 1-2 It is a propenyl group.
[0012] In some embodiments, the silicon-containing organic compound is aminopropyltrimethoxysilane or methacryloxypropyltrimethoxysilane.
[0013] In some embodiments, the mass of the silicon-containing organic matter used in a single test of the method is 0.1-2 g; for example, 0.5 g.
[0014] In some embodiments, the silicon content (mass percentage of Si element) of the silicon-containing organic matter is 0.1-30%, preferably 5-20%; for example, 15.62% or 11.95%.
[0015] In some embodiments, the concentration of the sodium hydroxide solution is 0.8-1.2 mol / L; preferably 1-1.2 mol / L; for example 1 mol / L.
[0016] In some embodiments, the mass-to-volume ratio of the silicon-containing organic matter to the sodium hydroxide solution is 5-100 g / L; preferably 20-30 g / L; for example 25 g / L.
[0017] In some embodiments, the digestion temperature is 160-200°C; preferably 180-200°C; for example 180°C.
[0018] In some embodiments, the time for dissolving the silicon-containing organic matter in the sodium hydroxide aqueous solution is 0.5-2 hours.
[0019] In some embodiments, the heating digestion time is 3-7 hours; for example, 5 hours.
[0020] In some embodiments, the silicon-containing organic matter and the sodium hydroxide aqueous solution are sealed in a polytetrafluoroethylene tank in an autoclave.
[0021] In some embodiments, the heating digestion is performed by placing the polytetrafluoroethylene tank in the autoclave in an oven for heating digestion.
[0022] In some embodiments, the method further comprises diluting the product after heating digestion, wherein the dilution is to dilute the solution to a silicon-containing organic matter concentration of 0.01 μg / mL-2 μg / mL; preferably 0.5-2 μg / mL; for example 1 μg / mL.
[0023] In some embodiments, among the parameters of the ICP-OES, the plasma gas flow rate may be 8-20 L / min, the purge gas flow rate may be 2-5 L / min, the nebulizer gas flow rate may be 0.2-1 L / min, and the auxiliary gas flow rate may be 0.2-1 L / min; for example, the plasma gas flow rate is 12.5 L / min, the purge gas flow rate is 3.4 L / min, the nebulizer flow rate is 0.5 L / min, and the auxiliary gas flow rate is 0.5 L / min.
[0024] In some embodiments, the method for determining the Si content in an organic matter using ICP-OES comprises the following specific steps: adding the silicon-containing organic matter and the sodium hydroxide aqueous solution into a polytetrafluoroethylene tank in a stainless steel micro-autoclave, heating and digesting in an oven after sealing, diluting after cooling, detecting with ICP-OES, and reading the Si content.
[0025] The positive improvement effect of the present invention is that the method for determining the Si content in organic matter by using ICP-OES provided by the present invention is simple to operate and has high accuracy. DETAILED DESCRIPTION
[0026] The present invention is further described below by way of examples, but the present invention is not limited to the scope of the examples.
[0027] ICP-OES parameters and instrument calibration:
[0028] Pipette 20mL of 1mol / L sodium hydroxide aqueous solution into a polytetrafluoroethylene tank in a 50mL stainless steel micro autoclave, weigh 0.5g of sample in the sodium hydroxide solution, shake thoroughly, cover with a lid to seal, and tighten the autoclave. Heat in a 180℃ oven for 5 hours, transfer to a 50mL centrifuge tube after cooling, and make up to 50mL with water. Weigh another 0.5g of sample solution and dilute with water to the corresponding concentration. Use ICP-OES to detect the standard solution and calibrate the instrument; the concentrations of the standard solution are: 0.01μg / mL, 0.1μg / mL, 0.5μg / mL, 1μg / mL and 2μg / mL. Finally, use ICP-OES for testing.
[0029] The parameters of ICP-OES were plasma gas flow rate of 12.5 L / min, purge gas flow rate of 3.4 L / min, nebulizer flow rate of 0.5 L / min, and auxiliary gas flow rate of 0.5 L / min.
[0030] Example 1
[0031] Sample to be tested: Pipette 20mL of 1mol / L sodium hydroxide aqueous solution into a polytetrafluoroethylene tank in a 50mL stainless steel micro autoclave, weigh 0.05g of aminopropyltrimethoxysilane in the sodium hydroxide solution, shake well, cover and seal, and tighten the autoclave. Heat in an oven at 180℃ for 5 hours, transfer to a 50mL centrifuge tube after cooling, and dilute to 50g with ultrapure water. Weigh 0.5g of the sample solution and dilute to 500g with ultrapure water.
[0032] Blank sample: Pipette 20mL of 1mol / L sodium hydroxide aqueous solution into a polytetrafluoroethylene tank in a 50mL stainless steel micro autoclave, shake well, seal with a lid, and tighten the autoclave. Heat in an oven at 180℃ for 5 hours, transfer to a 50mL centrifuge tube after cooling, and dilute to 50g with ultrapure water. Weigh 0.5g of sample solution and dilute to 500g with ultrapure water.
[0033] ICP-OES was used to test the samples and blank samples respectively, and the results are as follows:
[0034] .
[0035] Example 2
[0036] Sample to be tested: Pipette 20mL of 1mol / L sodium hydroxide aqueous solution into a polytetrafluoroethylene tank in a 50mL stainless steel micro autoclave, weigh 0.05g of methacryloxypropyltrimethoxysilane in the sodium hydroxide solution, shake well, cover and seal, and tighten the autoclave. Heat in an oven at 180℃ for 5 hours, transfer to a 50mL centrifuge tube after cooling, and dilute to 50g with ultrapure water. Weigh 0.5g of the sample solution and dilute to 500g with ultrapure water.
[0037] Blank sample: Pipette 20mL of 1mol / L sodium hydroxide aqueous solution into a polytetrafluoroethylene tank in a 50mL stainless steel micro autoclave, shake well, seal with a lid, and tighten the autoclave. Heat in an oven at 180℃ for 5 hours, transfer to a 50mL centrifuge tube after cooling, and dilute to 50g with ultrapure water. Weigh 0.5g of sample solution and dilute to 500g with ultrapure water.
[0038] ICP-OES was used to test the samples and blank samples respectively, and the results are as follows:
[0039] .
[0040] Example 3
[0041] Sample to be tested: Pipette 20mL of 1mol / L sodium hydroxide aqueous solution into a polytetrafluoroethylene tank in a 50mL stainless steel micro autoclave, weigh 0.05g of aminopropyltrimethoxysilane in the sodium hydroxide solution, shake well, cover and seal, and tighten the autoclave. Heat in a 160℃ / 200℃ oven for 5 hours, transfer to a 50mL centrifuge tube after cooling, and dilute to 50g with ultrapure water. Weigh 0.5g of the sample solution and dilute to 500g with ultrapure water.
[0042] Blank sample: Pipette 20mL of 1mol / L sodium hydroxide aqueous solution into a polytetrafluoroethylene tank in a 50mL stainless steel micro autoclave, shake well, seal with a lid, and tighten the autoclave. Heat in a 160℃ / 200℃ oven for 5 hours, transfer to a 50mL centrifuge tube after cooling, and dilute to 50g with ultrapure water. Weigh 0.5g of sample solution and dilute to 500g with ultrapure water.
[0043] ICP-OES was used to test the samples and blank samples respectively, and the results are as follows:
[0044] .
[0045] Example 4
[0046] Sample to be tested: Pipette 20mL of 1mol / L sodium hydroxide aqueous solution into a polytetrafluoroethylene tank in a 50mL stainless steel micro autoclave, weigh 0.05g of methacryloxypropyltrimethoxysilane in the sodium hydroxide solution, shake well, cover and seal, and tighten the autoclave. Heat in a 160℃ / 200℃ oven for 5 hours, transfer to a 50mL centrifuge tube after cooling, and dilute to 50g with ultrapure water. Weigh 0.5g of the sample solution and dilute to 500g with ultrapure water.
[0047] Blank sample: Pipette 20mL of 1mol / L sodium hydroxide aqueous solution into a polytetrafluoroethylene tank in a 50mL stainless steel micro autoclave, shake well, seal with a lid, and tighten the autoclave. Heat in a 160℃ / 200℃ oven for 5 hours, transfer to a 50mL centrifuge tube after cooling, and dilute to 50g with ultrapure water. Weigh 0.5g of sample solution and dilute to 500g with ultrapure water.
[0048] ICP-OES was used to test the samples and blank samples respectively, and the results are as follows:
[0049] .
[0050] Example 5
[0051] Sample to be tested: Pipette 20mL of 0.8 / 1.2mol / L sodium hydroxide aqueous solution into a polytetrafluoroethylene tank in a 50mL stainless steel micro autoclave, weigh 0.05g of aminopropyltrimethoxysilane in the sodium hydroxide solution, shake well, cover and seal, and tighten the autoclave. Heat in a 180℃ oven for 5 hours, transfer to a 50mL centrifuge tube after cooling, and dilute to 50g with ultrapure water. Weigh 0.5g of the sample solution and dilute to 500g with ultrapure water.
[0052] Blank sample: Pipette 20mL of 0.8 / 1.2mol / L sodium hydroxide aqueous solution into a polytetrafluoroethylene tank in a 50mL stainless steel micro autoclave, shake well, seal with a lid, and tighten the autoclave. Heat in an oven at 180℃ for 5 hours, transfer to a 50mL centrifuge tube after cooling, and dilute to 50g with ultrapure water. Weigh 0.5g of sample solution and dilute to 500g with ultrapure water.
[0053] Finally, ICP-OES was used to test the samples and blank samples respectively, and the results are as follows:
[0054] .
[0055] Example 6
[0056] Sample to be tested: Pipette 20mL of 0.8 / 1.2mol / L sodium hydroxide aqueous solution into a polytetrafluoroethylene tank in a 50mL stainless steel micro autoclave, weigh 0.05g of methacryloxypropyltrimethoxysilane in the sodium hydroxide solution, shake well, cover and seal, and tighten the autoclave. Heat in a 180℃ oven for 5 hours, transfer to a 50mL centrifuge tube after cooling, and dilute to 50g with ultrapure water. Weigh 0.5g of the sample solution and dilute to 500g with ultrapure water.
[0057] Blank sample: Pipette 20mL of 0.8 / 1.2mol / L sodium hydroxide aqueous solution into a polytetrafluoroethylene tank in a 50mL stainless steel micro autoclave, shake well, seal with a lid, and tighten the autoclave. Heat in an oven at 180℃ for 5 hours, transfer to a 50mL centrifuge tube after cooling, and dilute to 50g with ultrapure water. Weigh 0.5g of sample solution and dilute to 500g with ultrapure water.
[0058] .
[0059] Comparative Example 1
[0060] Sample to be tested: weigh 0.05g of aminopropyltrimethoxysilane in a polytetrafluoroethylene digestion tank, add 5mL of 65% concentrated nitric acid and 1mL of 40% hydrofluoric acid, cover the lid and put it into a microwave digestion instrument for digestion. After digestion, after acid release and acid removal, pour out the remaining liquid in the digestion tank and dilute it to 50g with ultrapure water. Then weigh 0.5g of sample solution and dilute it to 500g with ultrapure water.
[0061] Blank sample: Add 5mL of 65% concentrated nitric acid and 1mL of 40% hydrofluoric acid to the digestion tank, cover it tightly and place it in the microwave digestion instrument for digestion. After digestion, after acid release and acid removal, pour out the remaining liquid in the digestion tank and dilute it to 50g with ultrapure water. Then weigh 0.5g of sample solution and dilute it to 500g with ultrapure water.
[0062] .
[0063] Comparative Example 2
[0064] Sample to be tested: Weigh 0.05g of methacryloxypropyltrimethoxysilane and put it into a polytetrafluoroethylene digestion tank, add 5mL of 65% concentrated nitric acid and 1mL of 40% hydrofluoric acid, cover the lid and put it into a microwave digestion instrument for digestion. After digestion, after acid release and acid removal, pour out the remaining liquid in the digestion tank and dilute it to 50g with ultrapure water. Then weigh 0.5g of sample solution and dilute it to 500g with ultrapure water.
[0065] Blank sample: Add 5mL of 65% concentrated nitric acid and 1mL of 40% hydrofluoric acid to the digestion tank, cover it tightly and place it in the microwave digestion instrument for digestion. After digestion, after acid release and acid removal, pour out the remaining liquid in the digestion tank and dilute it to 50g with ultrapure water. Then weigh 0.5g of sample solution and dilute it to 500g with ultrapure water.
[0066] .
[0067] Comparative Example 3
[0068] Sample to be tested: Sodium carbonate and boric acid are mixed in a mass ratio of 2:1. A small amount of sample is placed on a hot plate for carbonization, then placed in a platinum crucible, and 10 times the mass of the sodium carbonate-boric acid mixture is added (do not directly add the 10 times mixture to mix, but leave a small amount of the mixture, and spread the remaining mixture on the surface after the sample and the mixture are evenly mixed). Place the platinum crucible in a muffle furnace and melt at 900-1000℃ for 20 minutes. After taking it out, add excess hydrochloric acid to acidify, then dilute to constant volume, and finally test it with ICP-OES. The test result is only 50% of the theoretical value.
Claims
1. A method for determining Si content in organic matter by ICP-OES, characterized in that: It includes the following steps: The silicon-containing organic matter was dissolved in a sodium hydroxide aqueous solution, heated for digestion, and then detected by ICP-OES to read the Si content.
2. The method for determining Si content in organic matter by ICP-OES according to claim 1, characterized in that: The silicon-containing organic matter is , R1, R2, R3 and R4 are independently C 1-12 Alkyl, C 1-12 Alkenyl, C 1-12 Alkoxy, C 1-12 Alkylamino, C 1-12 Alkylhydroxyl or -R 1-1 -XR 1-2 , R 1-1 C 1-6 Alkylene, R 1-2 C 1-12 Alkyl, C 1-12 Alkenyl, C 1-12 Alkynyl or C 1-12 Alkoxy; X is .
3. The method for measuring Si content in organic matter by ICP-OES according to claim 2, characterized in that: It meets one or both of the following conditions: (1) R1, R2, R3, R4 and R 1-2 In the above, the "C 1-12 Alkyl", "C 1-12 "Alkenyl", "C 1-12 Alkoxy", "C 1-12 Alkylamino", "C 1-12 Alkyl hydroxyl" and "C 1-12 "Alkynyl" in "C 1-12 "Independently"C 1-6 "; preferably "C 1-4 ”; (2) R1, R2 and R3 are the same.
4. The method for measuring Si content in organic matter by ICP-OES according to claim 3, characterized in that: It meets one or both of the following conditions: (1) R1, R2 and R3 are C 1-4 Alkoxy; for example methoxy; (2) R4 is C 1-4 Alkylamino or -R 1-1 -XR 1-2 ; R 1-1 C 1-4 Alkylene, R 1-2 C 1-4 Alkenyl.
5. The method for measuring Si content in organic matter by ICP-OES according to claim 4, characterized in that: R4 is C 1-4 Alkylamino or -R 1-1 -XR 1-2 ; R 1-1 is methylene or straight-chain propylene; for example, straight-chain propylene; R 1-2 It is a propenyl group.
6. The method for determining Si content in organic matter by ICP-OES according to claim 1, characterized in that: The silicon-containing organic compound is aminopropyltrimethoxysilane or methacryloxypropyltrimethoxysilane.
7. The method for determining Si content in organic matter by ICP-OES according to claim 1, characterized in that: It meets one or more of the following conditions: (1) The mass of silicon-containing organic matter used in a single test of the method is 0.1~2g; (2) The silicon content of the silicon-containing organic matter is 0.1-30%; (3) The concentration of the sodium hydroxide solution is 0.8-1.2 mol / L; (4) The mass-to-volume ratio of the silicon-containing organic matter to the sodium hydroxide solution is 5-100 g / L; (5) The digestion temperature is 160-200°C; (6) The time for dissolving the silicon-containing organic matter in the sodium hydroxide aqueous solution is 0.5-2 hours; (7) The heating digestion time is 3-7 hours; (8) The silicon-containing organic matter and the sodium hydroxide aqueous solution are sealed in a polytetrafluoroethylene tank in an autoclave; (9) The method further comprises diluting the product after heating digestion, wherein the dilution is to dilute the solution to a concentration of silicon-containing organic matter of 0.01 μg / mL-2 μg / mL; (10) Among the parameters of the ICP-OES, the plasma gas flow rate is 8-20 L / min; (11) Among the parameters of the ICP-OES, the purge gas flow rate is 2-5 L / min; (12) Among the parameters of the ICP-OES, the nebulizer gas flow rate is 0.2-1 L / min; (13) Among the parameters of the ICP-OES, the auxiliary gas flow rate is 0.2-1 L / min.
8. The method for measuring Si content in organic matter by ICP-OES according to claim 7, characterized in that: It meets one or more of the following conditions: (1) The mass of silicon-containing organic matter used in a single test of the method is 0.5 g; (2) The silicon content of the silicon-containing organic matter is 5-20%; (3) The concentration of the sodium hydroxide solution is 1-1.2 mol / L; (4) The mass-to-volume ratio of the silicon-containing organic matter to the sodium hydroxide solution is 20-30 g / L; (5) The digestion temperature is 180-200°C; (6) The heating digestion time is 5 hours; (7) The heating digestion is to place the polytetrafluoroethylene tank in the autoclave in an oven for heating digestion; (8) The dilution is to dilute the solution to a concentration of silicon-containing organic matter of 0.5-2 μg / mL; (9) Among the parameters of the ICP-OES, the plasma gas flow rate is 12.5 L / min, (10) Among the parameters of the ICP-OES, the purge gas flow rate is 3.4 L / min, (11) Among the parameters of ICP-OES, the nebulizer gas flow rate is 0.5 L / min, (12) Among the parameters of the ICP-OES, the auxiliary gas flow rate is 0.5 L / min.
9. The method for measuring Si content in organic matter by ICP-OES according to claim 8, characterized in that: It meets one or more of the following conditions: (1) The silicon content of the silicon-containing organic matter is 15.62% or 11.95%; (2) The concentration of the sodium hydroxide solution is 1 mol / L; (3) The mass-to-volume ratio of the silicon-containing organic matter to the sodium hydroxide solution is 25 g / L; (4) The digestion temperature is 180°C; (5) The dilution is to dilute the solution to a concentration of silicon-containing organic matter of 1 μg / mL.
10. The method for determining Si content in organic matter by ICP-OES according to claim 1, characterized in that: The method for determining the Si content in organic matter by using ICP-OES comprises the following specific steps: adding the silicon-containing organic matter and the sodium hydroxide aqueous solution into a polytetrafluoroethylene tank in a stainless steel micro-autoclave, heating and digesting in an oven after sealing, diluting after cooling, detecting by ICP-OES, and reading the Si content.