Detection method for boron trifluoride complex

Abstract

The invention discloses a boron trifluoride complex detection method, which comprises: S1, equally dividing a sample to be detected into a plurality of parts, placing in the same container with scales, setting a blank control group, numbering the remaining parts according to a sequence, and metering the sample volume to H1, S2, weighing a plurality of parts of an adsorbent with the weight of M1 according to the sample part number, according to the method, the sample is equally divided, meanwhile, a blank control group is set for detection, the adsorbent is firstly put in, the sample is adsorbed, redundant volatile boron trifluoride complexes are removed, personnel inhalation is avoided, safety is improved, and the method is suitable for large-scale popularization and application. Then a sodium hydroxide solution is introduced for a reaction, and solid impurities are weighed, so that the concentration of the boron trifluoride complex is analyzed, and subsequent precise treatment on the boron trifluoride complex can be facilitated.

Description

Technical Field

[0001] The invention relates to the technical field of chemical detection, in particular to a detection method for boron trifluoride complex. Background Art

[0002] Boron trifluoride is an inorganic compound with the chemical formula BF3. It is a colorless gas that is soluble in cold water, concentrated sulfuric acid and most organic solvents. It is mainly used as a catalyst in organic synthesis and is also used to make high-energy fuel for rockets. Boron trifluoride has a molecular mass of 67.81. It is a colorless, non-flammable and non-combustible gas with asphyxiation. Boron trifluoride can form molecular compounds with many different types of compounds, such as alcohols, ethers, anhydrides, ketones, aldehydes, amines, etc. In addition, it can also form a 1:1 molecular complex with hydrogen sulfide, sulfur dioxide, and mercaptans. Boron trifluoride and its complexes are often used as catalysts. When treating boron trifluoride complexes;

[0003] However, currently when testing boron trifluoride complexes, it is not possible to handle the volatile components, and the risk of inhalation for testers is relatively high. Summary of the invention

[0004] The present invention provides a method for detecting a boron trifluoride complex, which can effectively solve the problem raised in the above background technology that, when detecting a boron trifluoride complex, volatile components cannot be processed, resulting in a high risk of inhalation by detection personnel.

[0005] To achieve the above object, the present invention provides the following technical solution: a method for detecting a boron trifluoride complex, comprising the following detection steps:

[0006] S1. First, divide the sample to be tested into several equal parts and place them in the same graduated container. Set up a blank control group and number the remaining parts in sequence. Measure the sample volume as H1.

[0007] S2. According to the number of samples, weigh several portions of adsorbent with a weight of M1, suspend the weighed adsorbent in the sample, heat the sample and stir the sample continuously;

[0008] S3, then take out the adsorbent from the container, measure the sample volume after adsorption and record it as H2, and weigh the weight of the adsorbent after use M2;

[0009] S4, drying the taken out adsorbent, and weighing the dried adsorbent again, recorded as M3;

[0010] S5, passing sodium hydroxide solution into the control group and the sample, stirring, and generating solid impurities after reaction;

[0011] S6, filtering the sample solution to obtain solid impurities, and drying the sample solution. The weight of the solid impurities is weighed and recorded as M4, and the volume of the remaining solution in the container is recorded as H3;

[0012] S7. Analyze the content of the boron trifluoride complex in the sample based on the sample volume, the weight of the adsorbent before use, the weight of the adsorbent after use, and the weight of solid impurities.

[0013] According to the above technical solution, in S1, the number of equal parts of the sample is greater than or equal to 4, and the container for holding the sample has a sealing cover and is in a normally closed state;

[0014] The blank control group consisted of the same volume of water in the same container;

[0015] The sample numbers are recorded as 1, 2, 3...N, and the blank control group number is recorded as 0;

[0016] The sample volumes were recorded as H1-1, H1-2, H1-3...H1-N, and the blank control group was recorded as H1-0.

[0017] According to the above technical solution, in S2, the adsorbent is a mixture of ion exchange resin, aluminum silicate particles and activated carbon, and the ratio of ion exchange resin, aluminum silicate and activated carbon is (1-2):1:(1-2);

[0018] Set the heating temperature to 10-30°C and the time to 0.5-5h.

[0019] According to the above technical solution, in S2, the adsorbent is placed in the middle of the sample, and the sample is stirred around the adsorbent. The frequency of the sample stirring is (1-3) r / s.

[0020] According to the above technical solution, in S3, the same mass of adsorbent is placed in the blank control group, and the same heating and stirring are performed. When the adsorbent in the sample is taken out, the adsorbent in the blank control group is taken out, and the weight of the adsorbent in the blank control group is weighed, which is recorded as M2-0;

[0021] The weight of the adsorbent after use in the sample is recorded as M2-1, M2-2, M2-3...M2-N;

[0022] The volume of the blank control group after adsorption was recorded as H2-0, and the volumes of the samples after adsorption were recorded as H2-1, H2-2, H2-3...H2-N.

[0023] According to the above technical solution, in S4, the weight of the used adsorbent in the sample after drying is recorded as M3-1, M3-2, M3-3...M3-N;

[0024] The weight of the adsorbent in the blank control group after drying was recorded as M3-0;

[0025] The drying time in S4 and S6 is 30-60 minutes, and the drying temperature is 45-60°C.

[0026] According to the above technical solution, in S5, the volume of the sodium hydroxide solution introduced is (0.1-1)H2;

[0027] The solid impurities generated by the reaction in the sample are sodium fluoride and sodium metaborate.

[0028] According to the above technical solution, in S6, the sample solution is first allowed to stand, the upper clear liquid is poured out, and then the lower mixed solution is filtered, and the filtered solution and the upper clear liquid are poured back into the container, which is H3.

[0029] According to the above technical solution, in S6, the weight of the solid impurities filtered out from each sample is recorded as M4-1, M4-2, M4-3...M4-N respectively;

[0030] The weight of solid impurities in the control group was recorded as M4-0;

[0031] The volumes of the remaining solutions in the sample containers are recorded as H3-1, H3-2, H3-3, ... H3-N;

[0032] The remaining solution volume in the control group container was recorded as H3-0.

[0033] According to the above technical solution, in S7, the difference between M2 and M1 in each container is calculated in turn, and recorded as M21;

[0034] Calculate the difference between M3 and M1 in each container in turn, and record it as M31;

[0035] Calculate the difference between H1 and H2 in each container in turn, and record it as H12;

[0036] Calculate the difference between H1 and H3 in each container in turn, and record it as H13;

[0037] Calculate the difference between H2 and H3 in each container in turn, and record it as H23;

[0038] Calculate the ratio of the volume of sodium hydroxide solution introduced to the weight of solid impurities M4, and record it as R4.

[0039] According to the above technical solution, in S7, the calculated difference and ratio are respectively plotted as curves;

[0040] The abscissa of the graph is the sample container number, and the ordinates of the graph are M21, M31, H12, H13, H23 and R4, respectively.

[0041] Compared with the prior art, the present invention has the following beneficial effects:

[0042] 1. By placing an adsorbent made of a mixture of ion exchange resin, aluminum silicate and activated carbon into the sample, the boron trifluoride in the sample is absorbed, the adsorbent before and after absorption is weighed, and the weight difference before and after the adsorbent is used is calculated, the adsorption amount of the boron trifluoride complex in the sample solution can be detected, the volume of the sample solution before and after absorption is measured, the solution difference is calculated, and the absorption amount of the sample solution is calculated, which helps to detect the boron trifluoride complex in the sample solution. The adsorption operation can adsorb the gas volatilized in the solution, reduce the risk of inhalation by the test personnel, and is safer and more efficient.

[0043] 2. By passing sodium hydroxide solution into the sample solution, the generated sodium fluoride and sodium metaborate solid impurities are filtered, and then dried and weighed, so as to react with the boron trifluoride complex in the solution, facilitate the conversion of the boron trifluoride in the solution remaining after adsorption, and help extract fluorine and boron elements, so that the solution can be treated, and the concentration of the boron trifluoride complex in the solution can be detected according to the amount of solid impurities generated.

[0044] 3. By setting up blank controls and multiple groups of samples, external interference can be eliminated through the control group to make the data more accurate. By testing multiple groups of samples, more data can be obtained, thereby reducing the impact of errors and making the test results closer to reality, thereby improving the success rate of the test and improving the detection efficiency of boron trifluoride.

[0045] In summary, by dividing the sample into equal parts and setting up a blank control group for testing, the adsorbent is first put in to adsorb the sample to remove excess volatile boron trifluoride complex to avoid inhalation by personnel and improve safety, and then sodium hydroxide solution is introduced to react, the solid impurities are weighed to help analyze the concentration of the boron trifluoride complex, which can help with the subsequent precise treatment of the boron trifluoride complex. BRIEF DESCRIPTION OF THE DRAWINGS

[0046] The accompanying drawings are used to provide further understanding of the present invention and constitute a part of the specification. They are used to explain the present invention together with the embodiments of the present invention and do not constitute a limitation of the present invention.

[0047] In the attached picture:

[0048] Figure 1 It is a flow chart of the detection steps of the present invention. DETAILED DESCRIPTION

[0049] The preferred embodiments of the present invention are described below in conjunction with the accompanying drawings. It should be understood that the preferred embodiments described herein are only used to illustrate and explain the present invention, and are not used to limit the present invention.

[0050] Embodiment 1:

[0051] like Figure 1 As shown, the present invention provides a technical solution, a method for detecting a boron trifluoride complex, comprising the following detection steps:

[0052] S1. First, divide the sample to be tested into several equal parts and place them in the same graduated container. Set up a blank control group and number the remaining parts in sequence. Measure the sample volume as H1.

[0053] S2. According to the number of samples, weigh several portions of adsorbent with a weight of M1, suspend the weighed adsorbent in the sample, heat the sample and stir the sample continuously;

[0054] S3, then take out the adsorbent from the container, measure the sample volume after adsorption and record it as H2, and weigh the weight of the adsorbent after use M2;

[0055] S4, drying the taken out adsorbent, and weighing the dried adsorbent again, recorded as M3;

[0056] S5, passing sodium hydroxide solution into the control group and the sample, stirring, and generating solid impurities after reaction;

[0057] S6, filtering the sample solution to obtain solid impurities, and drying the sample solution. The weight of the solid impurities is weighed and recorded as M4, and the volume of the remaining solution in the container is recorded as H3;

[0058] S7. Analyze the content of the boron trifluoride complex in the sample based on the sample volume, the weight of the adsorbent before use, the weight of the adsorbent after use, and the weight of solid impurities.

[0059] In S1, the number of sample aliquots is greater than or equal to 4, and the container containing the sample has a sealed lid and is in a normally closed state;

[0060] The blank control group consisted of the same volume of water in the same container;

[0061] The sample numbers are recorded as 1, 2, 3...N, and the blank control group number is recorded as 0;

[0062] The sample volumes were recorded as H1-1, H1-2, H1-3...H1-N, and the blank control group was recorded as H1-0.

[0063] In S2, the adsorbent is a mixture of ion exchange resin, aluminum silicate particles and activated carbon, and the ratio of ion exchange resin, aluminum silicate and activated carbon is 1:1:1;

[0064] Set the heating temperature to 30°C and the heating time to 1 h.

[0065] In S2, the adsorbent is placed in the middle of the sample, and the sample is stirred around the adsorbent, and the frequency of sample stirring is 3r / s.

[0066] In S3, the same mass of adsorbent is placed in the blank control group, and the same heating and stirring are performed. When the adsorbent in the sample is taken out, the adsorbent in the blank control group is taken out, and the weight of the adsorbent in the blank control group is weighed, which is recorded as M2-0;

[0067] The weight of the adsorbent after use in the sample is recorded as M2-1, M2-2, M2-3...M2-N;

[0068] The volume of the blank control group after adsorption was recorded as H2-0, and the volumes of the samples after adsorption were recorded as H2-1, H2-2, H2-3...H2-N.

[0069] In S4, the weight of the adsorbent after use and drying in the sample is recorded as M3-1, M3-2, M3-3...M3-N;

[0070] The weight of the adsorbent in the blank control group after drying was recorded as M3-0;

[0071] The drying time in S4 and S6 was 45 min and the drying temperature was 5°C.

[0072] In S5, the volume of the sodium hydroxide solution introduced is 0.5H2;

[0073] The solid impurities generated by the reaction in the sample are sodium fluoride and sodium metaborate.

[0074] In S6, the sample solution is first allowed to stand, the upper clear liquid is poured out, and then the lower mixed solution is filtered, and the filtered solution and the upper clear liquid are poured back into the container, which is H3.

[0075] In S6, the weight of the solid impurities filtered out of each sample is recorded as M4-1, M4-2, M4-3...M4-N;

[0076] The weight of the solid impurities in the control group is recorded as M4-0, and M4-0 is 0;

[0077] The volumes of the remaining solutions in the sample containers are recorded as H3-1, H3-2, H3-3, ... H3-N;

[0078] The remaining solution volume in the control group container is recorded as H3-0, and H3-0 is equal to H2-0.

[0079] In S7, the difference between M2 and M1 in each container is calculated in turn, and recorded as M21;

[0080] Calculate the difference between M3 and M1 in each container in turn, and record it as M31;

[0081] Calculate the difference between H1 and H2 in each container in turn, and record it as H12;

[0082] Calculate the difference between H1 and H3 in each container in turn, and record it as H13;

[0083] Calculate the difference between H2 and H3 in each container in turn, and record it as H23;

[0084] Calculate the ratio of the volume of sodium hydroxide solution introduced to the weight of solid impurities M4, and record it as R4.

[0085] In S7, the calculated difference and ratio are plotted in curve graphs respectively;

[0086] The abscissa of the graph is the sample container number, and the ordinates of the graph are M21, M31, H12, H13, H23 and R4, respectively.

[0087] Embodiment 2:

[0088] In S2, the adsorbent is a mixture of ion exchange resin, aluminum silicate particles and activated carbon, and the ratio of ion exchange resin, aluminum silicate and activated carbon is 1.5:1:1.5;

[0089] Set the heating temperature to 25°C and the heating time to 0.5h.

[0090] In S2, the adsorbent is placed in the middle of the sample, and the sample is stirred around the adsorbent, and the frequency of sample stirring is 1 r / s.

[0091] In S3, the same mass of adsorbent is placed in the blank control group, and the same heating and stirring are performed. When the adsorbent in the sample is taken out, the adsorbent in the blank control group is taken out, and the weight of the adsorbent in the blank control group is weighed, which is recorded as M2-0;

[0092] The weight of the adsorbent after use in the sample is recorded as M2-1, M2-2, M2-3...M2-N;

[0093] The volume of the blank control group after adsorption was recorded as H2-0, and the volumes of the samples after adsorption were recorded as H2-1, H2-2, H2-3...H2-N.

[0094] In S4, the weight of the adsorbent after use and drying in the sample is recorded as M3-1, M3-2, M3-3...M3-N;

[0095] The weight of the adsorbent in the blank control group after drying was recorded as M3-0;

[0096] The drying time in S4 and S6 was 45 min and the drying temperature was 10°C.

[0097] In S5, the volume of the sodium hydroxide solution introduced is 0.1H2.

[0098] The solid impurities generated by the reaction in the sample are sodium fluoride and sodium metaborate.

[0099] In S6, the sample solution is first allowed to stand, the upper clear liquid is poured out, and then the lower mixed solution is filtered, and the filtered solution and the upper clear liquid are poured back into the container, which is H3.

[0100] In S6, the weight of the solid impurities filtered out of each sample is recorded as M4-1, M4-2, M4-3...M4-N;

[0101] The weight of the solid impurities in the control group is recorded as M4-0, and M4-0 is 0;

[0102] The volumes of the remaining solutions in the sample containers are recorded as H3-1, H3-2, H3-3, ... H3-N;

[0103] The remaining solution volume in the control group container is recorded as H3-0, and H3-0 is equal to H2-0.

[0104] In S7, the difference between M2 and M1 in each container is calculated in turn, and recorded as M21;

[0105] Calculate the difference between M3 and M1 in each container in turn, and record it as M31;

[0106] Calculate the difference between H1 and H2 in each container in turn, and record it as H12;

[0107] Calculate the difference between H1 and H3 in each container in turn, and record it as H13;

[0108] Calculate the difference between H2 and H3 in each container in turn, and record it as H23;

[0109] Calculate the ratio of the volume of sodium hydroxide solution introduced to the weight of solid impurities M4, and record it as R4.

[0110] In S7, the calculated difference and ratio are plotted in curve graphs respectively;

[0111] The abscissa of the graph is the sample container number, and the ordinates of the graph are M21, M31, H12, H13, H23 and R4, respectively.

[0112] Embodiment 3:

[0113] In S2, the adsorbent is a mixture of ion exchange resin, aluminum silicate particles and activated carbon, and the ratio of ion exchange resin, aluminum silicate and activated carbon is 2:1:2;

[0114] Set the heating temperature to 10°C and the heating time to 5h.

[0115] In S2, the adsorbent is placed in the middle of the sample, and the sample is stirred around the adsorbent, and the frequency of sample stirring is 2r / s.

[0116] In S3, the same mass of adsorbent is placed in the blank control group, and the same heating and stirring are performed. When the adsorbent in the sample is taken out, the adsorbent in the blank control group is taken out, and the weight of the adsorbent in the blank control group is weighed, which is recorded as M2-0;

[0117] The weight of the adsorbent after use in the sample is recorded as M2-1, M2-2, M2-3...M2-N;

[0118] The volume of the blank control group after adsorption was recorded as H2-0, and the volumes of the samples after adsorption were recorded as H2-1, H2-2, H2-3...H2-N.

[0119] In S4, the weight of the adsorbent after use and drying in the sample is recorded as M3-1, M3-2, M3-3...M3-N;

[0120] The weight of the adsorbent in the blank control group after drying was recorded as M3-0;

[0121] The drying time in S4 and S6 was 30 minutes and the drying temperature was 1°C.

[0122] In S5, the volume of the sodium hydroxide solution introduced is H2.

[0123] The solid impurities generated by the reaction in the sample are sodium fluoride and sodium metaborate.

[0124] In S6, the sample solution is first allowed to stand, the upper clear liquid is poured out, and then the lower mixed solution is filtered, and the filtered solution and the upper clear liquid are poured back into the container, which is H3.

[0125] In S6, the weight of the solid impurities filtered out of each sample is recorded as M4-1, M4-2, M4-3...M4-N;

[0126] The weight of the solid impurities in the control group is recorded as M4-0, and M4-0 is 0;

[0127] The remaining solution volumes in the sample containers are recorded as H3-1, H3-2, H3-3, ... H3-N;

[0128] The remaining solution volume in the control group container is recorded as H3-0, and H3-0 is equal to H2-0.

[0129] In S7, the difference between M2 and M1 in each container is calculated in turn, and recorded as M21;

[0130] Calculate the difference between M3 and M1 in each container in turn, and record it as M31;

[0131] Calculate the difference between H1 and H2 in each container in turn, and record it as H12;

[0132] Calculate the difference between H1 and H3 in each container in turn, and record it as H13;

[0133] Calculate the difference between H2 and H3 in each container in turn, and record it as H23;

[0134] Calculate the ratio of the volume of sodium hydroxide solution introduced to the weight of solid impurities M4, and record it as R4.

[0135] In S7, the calculated difference and ratio are plotted in curve graphs respectively;

[0136] The abscissa of the graph is the sample container number, and the ordinates of the graph are M21, M31, H12, H13, H23 and R4, respectively.

[0137] Finally, it should be noted that the above description is only a preferred example of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art can still modify the technical solutions described in the aforementioned embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for detecting a boron trifluoride complex, characterized in that: The detection steps include the following: S1. First, divide the sample to be tested into several equal parts and place them in the same graduated container. Set up a blank control group and number the remaining parts in sequence. Measure the sample volume as H1. S2. According to the number of samples, weigh several portions of adsorbent with a weight of M1, suspend the weighed adsorbent in the sample, heat the sample and stir the sample continuously; S3, then take out the adsorbent from the container, measure the sample volume after adsorption and record it as H2, and weigh the weight of the adsorbent after use M2; S4, drying the taken out adsorbent, and weighing the dried adsorbent again, recorded as M3; S5, passing sodium hydroxide solution into the control group and the sample, stirring, and generating solid impurities after reaction; S6, filtering the sample solution to obtain solid impurities, and drying the sample solution. The weight of the solid impurities is weighed and recorded as M4, and the volume of the remaining solution in the container is recorded as H3; S7. Analyze the content of the boron trifluoride complex in the sample based on the sample volume, the weight of the adsorbent before use, the weight of the adsorbent after use, and the weight of solid impurities.

2. A method for detecting a boron trifluoride complex according to claim 1, characterized in that: In S1, the number of sample aliquots is greater than or equal to 4, and the container for holding the sample has a sealed cover and is in a normally closed state; The blank control group consisted of the same volume of water in the same container; The sample numbers are recorded as 1, 2, 3...N, and the blank control group number is recorded as 0; The sample volumes were recorded as H1-1, H1-2, H1-3...H1-N, and the blank control group was recorded as H1-0.

3. A method for detecting a boron trifluoride complex according to claim 1, characterized in that: In S2, the adsorbent is a mixture of ion exchange resin, aluminum silicate particles and activated carbon, and the ratio of ion exchange resin, aluminum silicate and activated carbon is (1-2):1:(1-2); Set the heating temperature to 10-30°C and the time to 0.5-5h.

4. A method for detecting a boron trifluoride complex according to claim 3, characterized in that: In S2, the adsorbent is placed in the middle of the sample, and the sample is stirred around the adsorbent. The frequency of the sample stirring is (1-3) r / s.

5. A method for detecting a boron trifluoride complex according to claim 1, characterized in that: In S3, the same mass of adsorbent is placed in the blank control group, and the same heating and stirring are performed. When the adsorbent in the sample is taken out, the adsorbent in the blank control group is taken out, and the weight of the adsorbent in the blank control group is weighed, which is recorded as M2-0; The weight of the adsorbent after use in the sample is recorded as M2-1, M2-2, M2-3...M2-N; The volume of the blank control group after adsorption was recorded as H2-0, and the volumes of the samples after adsorption were recorded as H2-1, H2-2, H2-3...H2-N.

6. A method for detecting a boron trifluoride complex according to claim 1, characterized in that: In said S4, the weight of the adsorbent after use in the sample after drying is recorded as M3-1, M3-2, M3-3...M3-N; The weight of the adsorbent in the blank control group after drying was recorded as M3-0; The drying time in S4 and S6 is 30-60 minutes, and the drying temperature is 1-10°C; In S5, the volume of the sodium hydroxide solution introduced is (0.1-1) H2; The solid impurities generated by the reaction in the sample are sodium fluoride and sodium metaborate.

7. A method for detecting a boron trifluoride complex according to claim 1, characterized in that: In the above S6, the sample solution is first allowed to stand, the upper clear liquid is poured out, and then the lower mixed solution is filtered, and the filtered solution and the upper clear liquid are poured back into the container, which is H3.

8. A method for detecting a boron trifluoride complex according to claim 7, characterized in that: In S6, the weight of the solid impurities filtered out from each sample is recorded as M4-1, M4-2, M4-3...M4-N respectively; The weight of solid impurities in the control group was recorded as M4-0; The volumes of the remaining solutions in the sample containers are recorded as H3-1, H3-2, H3-3, ... H3-N; The remaining solution volume in the control group container was recorded as H3-0.

9. A method for detecting a boron trifluoride complex according to claim 1, characterized in that: In S7, the difference between M2 and M1 in each container is calculated in turn, and recorded as M21; Calculate the difference between M3 and M1 in each container in turn, and record it as M31; Calculate the difference between H1 and H2 in each container in turn, and record it as H12; Calculate the difference between H1 and H3 in each container in turn, and record it as H13; Calculate the difference between H2 and H3 in each container in turn, and record it as H23; Calculate the ratio of the volume of sodium hydroxide solution introduced to the weight of solid impurities M4, and record it as R4.

10. A method for detecting a boron trifluoride complex according to claim 9, characterized in that: In S7, the calculated difference and ratio are respectively plotted as curves; The abscissa of the graph is the sample container number, and the ordinates of the graph are M21, M31, H12, H13, H23 and R4, respectively.

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