CN112986165A - Enameled wire and method for measuring silicon content in auxiliary materials for production of enameled wire and application of enameled wire - Google Patents
Enameled wire and method for measuring silicon content in auxiliary materials for production of enameled wire and application of enameled wire Download PDFInfo
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 102
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- 239000010703 silicon Substances 0.000 title claims abstract description 102
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- 239000000463 material Substances 0.000 title claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 66
- 239000000243 solution Substances 0.000 claims abstract description 45
- 239000003960 organic solvent Substances 0.000 claims abstract description 34
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000012153 distilled water Substances 0.000 claims abstract description 27
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 230000010355 oscillation Effects 0.000 claims abstract description 21
- 238000001514 detection method Methods 0.000 claims abstract description 18
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- 239000012895 dilution Substances 0.000 claims abstract description 12
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 51
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- 238000012545 processing Methods 0.000 claims description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
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- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
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- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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Abstract
The invention relates to a method for measuring silicon content in enameled wires and production auxiliary materials thereof and application thereof, wherein the method comprises the following steps: s1, mixing a sample to be detected with an organic solvent, and then performing ultrasonic oscillation to obtain a sample treatment solution; s2, evaporating and concentrating the sample treatment solution, and then adding distilled water for dilution to obtain a first diluent; s3, mixing the first diluent with a mixed solution of hydrofluoric acid liquid and distilled water, heating and then developing the color of the mixed solution to obtain a solution to be detected; s4, carrying out absorbance detection on the solution to be detected to obtain an OD valueLiquid to be testedOD value of standard liquid for controlling silicon contentStandard liquidAnd comparing to judge whether the silicon content in the sample to be detected exceeds the standard or not. The method has the advantages of high sample applicability, simple operation, environmental protection and low detection cost, and solves the problem that the silicon content in the enameled wire and the production auxiliary materials thereof measured by enterprises is not standard and can be relied on.
Description
Technical Field
The invention belongs to the technical field of silicon content determination, and particularly relates to an enameled wire and a determination method and application of silicon content in production auxiliary materials of the enameled wire.
Background
The enameled wire industry is at the front end of the industrial chains of motor and electric appliances, household appliances, electronic information, communication and the like, and is a basic material for developing terminal products of machinery, electric appliances, communication and the like. Since the total silicon content in the enameled wire affects the reliability of downstream products, especially the higher silicon content causes the relay contact to fail. The downstream markets therefore impose strict requirements on the silicon content of the enamelled wires.
While the requirements for enameled wires in the field of relays are increasing day by day, enameled wire manufacturers cannot master corresponding silicon content testing methods, so that internal evaluation is greatly limited. The silicon content includes both inorganic and organosilicon contents. The enameled wire is a composite material of metal copper attached with a polymer insulating material, and no standard can be relied on at present. The production auxiliary materials of the enameled wire are various in types and complex in material quality. GB/T5121.23-2008 application scope is copper and copper alloy, and the sample processing process needs to use a large amount of sulphuric acid, nitric acid, and the rich sour gas of rich nitrogen that preliminary treatment process produced needs a large amount of water to dilute very not environmental protection, and the strong acid belongs to control chemicals, and purchasing cost is higher, still need prepare the silicon standard solution of gradient content in the test procedure, and whole preliminary treatment and experimental process operation steps are complicated and loaded down with trivial details, require high to the inspection personnel. The method is not suitable for measuring the silicon content in the enameled wire and production auxiliary materials thereof. The requirements of production, operation and use units cannot be met. Therefore, a determination method which has high sample applicability, simple operation, environmental protection and low detection cost, is particularly suitable for the enameled wire with the silicon content of more than or equal to 0.3mg/kg and the production auxiliary materials thereof needs to be developed, so as to adapt to the urgent requirements of modern enameled wire manufacturers on quality, performance and development, and have important practical production significance.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the method for measuring the silicon content in the enameled wire and the production auxiliary materials thereof, the method has the advantages of high sample applicability, simple operation, environmental protection and low detection cost, and solves the problem that the silicon content in the enameled wire and the production auxiliary materials thereof measured by enterprises is not standard and can be relied on.
Therefore, the invention provides a method for measuring the silicon content in the enameled wire and the production auxiliary materials thereof in a first aspect, which comprises the following steps:
s1, mixing a sample to be detected with an organic solvent, and then performing ultrasonic oscillation to obtain a sample treatment solution;
s2, evaporating and concentrating the sample treatment solution, and then adding distilled water for dilution to obtain a first diluent;
s3, mixing the first diluent with a mixed solution of hydrofluoric acid liquid and distilled water, heating and then developing the color of the mixed solution to obtain a solution to be detected;
s4, carrying out absorbance detection on the solution to be detected to obtain an OD valueLiquid to be testedOD value of standard liquid for controlling silicon contentStandard liquidAnd comparing to judge whether the silicon content in the sample to be detected exceeds the standard or not.
In some embodiments of the invention, the OD value is determined asLiquid to be testedOD value > ODStandard liquidThen, the silicon content in the sample to be detected exceeds the standard; when the OD value isLiquid to be testedNo more than OD valueStandard liquidIn time, the silicon content in the sample to be tested conforms to the management and controlAnd (4) standard.
In other embodiments of the present invention, under the same absorbance detection condition as the solution to be detected, the absorbance detection is performed on the silicon content control standard solution, so as to obtain the OD value of the silicon content control standard solutionStandard liquid。
In some embodiments of the present invention, the method for preparing the silicon content control standard solution comprises the steps of:
t1, preparing a silicon standard solution containing 0.9-1.1 mu g of silicon per milliliter;
t2, mixing the silicon standard solution with an organic solvent, evaporating and concentrating, and then adding distilled water for dilution to obtain a second diluent;
and T3, mixing the second diluent with a mixed solution of hydrofluoric acid liquid and distilled water, heating and then developing the color to obtain the silicon content control standard solution.
In other embodiments of the present invention, in step S1, the mass of the sample to be tested is 10-40 g; and/or the dosage of the organic solvent is 100-400 mL.
In some embodiments of the present invention, the organic solvent used in step S1 is the same as the organic solvent used in step T2; preferably, the organic solvent is selected from one or more of methanol, petroleum ether, xylene, n-hexane and cyclohexane.
In other embodiments of the present invention, in step S1, the ultrasonic oscillation is performed at a temperature of 50 to 60 ℃; and/or the time of the ultrasonic oscillation is 60-90 min.
In some embodiments of the present invention, in step S2, 9-10 mL of the sample treatment solution is evaporated and concentrated.
In other embodiments of the present invention, the evaporation concentration is performed at a temperature of 50 to 80 ℃ in steps S2 and T2.
In some embodiments of the present invention, in the step S3 and the step T3, the heating temperature is 50 to 60 ℃, and the heating time is 30 to 60 min.
In some preferred embodiments of the invention, the method further comprises the steps of:
and S5, distilling the sample processing liquid left after the completion of the measurement in the step S2, and recovering the organic solvent therein.
In some embodiments of the invention, the sample to be tested is selected from one or more of polyurethane enamelled wire, polyester enamelled wire, industrial felt, sweatband, thread gloves, waist paper packaging, pearl wool packaging, polyethylene packaging, moisture-proof packaging and carton.
In a second aspect of the invention, there is provided the use of a method according to the first aspect of the invention in the production of enamelled wire.
The invention has the beneficial effects that: the method can be used for processing and detecting the samples of polyurethane enameled wires, polyester enameled wires, industrial felts, sweat shirt fabrics, thread gloves, packaging waist paper, packaging pearl cotton, packaging polyethylene bags, moisture-proof bags and paper boxes of enameled wire manufacturers, and the samples to be detected have wide range, thereby being beneficial to the operation of detection personnel and further carrying out batch experiments efficiently. Sulfuric acid and nitric acid are not used in the detection process, the step of using professional equipment to absorb gas is omitted, the purchase cost is reduced, and the operation difficulty is reduced. The used organic solvent can be recycled, so that the purposes of environmental protection and saving are achieved. Meanwhile, the method optimizes the preparation process of the silicon standard solution and the analysis steps, and is beneficial to enhancing the finished product management and control of enameled wire manufacturers and the management and control of the production process.
Drawings
The invention will be further explained with reference to the drawings.
FIG. 1 is a flow chart of a method for measuring the silicon content in the enameled wire and the auxiliary materials for production thereof.
Detailed Description
The present application will be described in detail below.
As mentioned above, the enameled wire and the auxiliary materials for its production are complex materials and are mostly composite materials, and there is no standard for measuring the silicon content of the enameled wire and the auxiliary materials for its production.
The inventor of the application provides a method for measuring the silicon content in the enameled wire and production auxiliary materials thereof through research. The method is characterized in that a sample to be detected is mixed with an organic solvent and then subjected to ultrasonic oscillation under the heating condition so as to be pretreated, and further, polyurethane enameled wires, polyester enameled wires, industrial felts, sweat shirt fabrics, thread gloves, packaging waist paper, packaging pearl cotton, packaging polyethylene bags, moisture-proof bags and carton samples of enameled wire manufacturers can be subjected to treatment and detection. And then, by applying the sample pretreatment and final experimental test method, a detection method which is high in sample applicability, simple to operate, economical and environment-friendly is established, and the problem that the silicon content in the enameled wire and production auxiliary materials thereof measured by enterprises is not standard and can be relied on is solved.
Therefore, the invention relates to a method for measuring the silicon content in the enameled wire and the production auxiliary materials thereof, which comprises the following steps:
s1, mixing a sample to be detected with an organic solvent, and then performing ultrasonic oscillation to obtain a sample treatment solution;
s2, evaporating and concentrating the sample treatment solution, and then adding distilled water for dilution to obtain a first diluent;
s3, mixing the first diluent with a mixed solution of hydrofluoric acid liquid and distilled water, heating and then developing the color of the mixed solution to obtain a solution to be detected;
s4, carrying out absorbance detection on the solution to be detected to obtain an OD valueLiquid to be testedOD value of standard liquid for controlling silicon contentStandard liquidAnd comparing to judge whether the silicon content in the sample to be detected exceeds the standard or not.
In the invention, the step S1 is a pretreatment step of the sample to be detected, and compared with the existing GB/T5121.23-2008, the pretreatment process uses an organic solvent (such as methanol) to replace strong acid to treat the sample to be detected, so that the emission of nitrogen-rich gas is reduced, and the method is environment-friendly. Further, the color development of the acid-treated enamel wire was impossible, and the experiment was impossible because the treatment liquid contained a paint film which was not decomposed.
In some embodiments of the present invention, the mixture of the sample to be tested and the organic solvent is subjected to ultrasonic oscillation in a closed container.
In some embodiments of the invention, the OD value is determined asLiquid to be testedOD value > ODStandard liquidThen, the silicon content in the sample to be detected exceeds the standard; when the OD value isLiquid to be testedNo more than OD valueStandard liquidAnd then, the silicon content in the sample to be detected meets the control standard.
The silicon content in the silicon content control standard solution is determined by the control standard of a producer of the enameled wire on the silicon content in the product. That is, if the wire manufacturer requires that the silicon content in the product should not exceed a certain value (e.g., 0.5mg/kg), the silicon content in the silicon content control standard solution is the value (e.g., 0.5 mg/kg).
In other embodiments of the present invention, under the same absorbance detection condition as the solution to be detected, the absorbance detection is performed on the silicon content control standard solution, so as to obtain the OD value of the silicon content control standard solutionStandard liquid。
In some embodiments of the present invention, the method for preparing the silicon content control standard solution comprises the steps of:
t1, preparing a silicon standard solution containing 0.9-1.1 mu g of silicon per milliliter;
t2, mixing the silicon standard solution with an organic solvent, evaporating and concentrating, and then adding distilled water for dilution to obtain a second diluent;
and T3, mixing the second diluent with a mixed solution of hydrofluoric acid liquid and distilled water, heating and then developing the color to obtain the silicon content control standard solution.
In some embodiments of the present invention, a silicon standard solution containing 1 μ g of silicon per ml is prepared in step T1, which facilitates subsequent calculation. In other embodiments of the present invention, the operation of step T1 is: 1.0mL of the standard solution containing 100. mu.g of silicon per mL was transferred to a 100.0mL volumetric flask, diluted with distilled water to the marked line, and stored in a polyethylene bottle in a sealed state to obtain a silicon standard solution containing 1. mu.g of silicon per mL. Compared with GB/T5121.23-2008, the preparation process omits a complex standard liquid preparation process, and is simple and easy to operate.
In some embodiments of the invention, in step S1, the mass of the sample to be tested is 10-40 g; and/or the dosage of the organic solvent is 100-400 mL.
In the present invention, for convenience of subsequent calculation, the mass of the sample to be measured in step S1 is 10g, and the amount of the organic solvent is 100 mL.
In some embodiments of the present invention, the organic solvent used in step S1 is the same as the organic solvent used in step T2.
In some preferred embodiments of the present invention, the organic solvent is selected from one or more of methanol, petroleum ether, xylene, n-hexane and cyclohexane.
In some embodiments of the present invention, in step S1, the ultrasonic vibration is performed at a temperature of 50 to 60 ℃. In some embodiments of the present invention, the ultrasonic vibration may be performed at a temperature of 50 ℃, 55 ℃, or 60 ℃. If the ultrasonic oscillation is carried out at the temperature of more than 60 ℃, the organic solvent (such as methanol) can volatilize more quickly in the ultrasonic oscillation process, and because the extraction container is in a sealed state, the pressure in the container is increased due to the large volatilization of the organic solvent (such as methanol), and the risk of explosion exists, the temperature can not exceed 60 ℃. When the ultrasonic oscillation is performed at a temperature of 50 ℃ or lower, the extraction is insufficient due to an excessively low temperature, and the final measurement result is affected.
In other embodiments of the present invention, the time of the ultrasonic oscillation is 60 to 90 min.
In some embodiments of the present invention, in step S2, 9-10 mL of the sample treatment solution is evaporated and concentrated. In some embodiments of the present invention, 10mL of the sample processing solution is evaporated and concentrated in step S2 for the convenience of calculation. The remaining sample processing solution may be subjected to distillation to recover the organic solvent therein.
In other embodiments of the present invention, the evaporation concentration in step S2 and step T2 is performed at the same temperature, preferably at 50 to 80 ℃. In some embodiments of the invention, the evaporative concentration is performed at a temperature of 70 ℃ in both step S2 and step T2.
In the present invention, the volume ratio of the hydrofluoric acid liquid to the distilled water in the mixed liquid of the hydrofluoric acid liquid and the distilled water used in steps S3 and T3 is 1:1, and the content of hydrofluoric acid in the hydrofluoric acid liquid is 40 wt%.
In some embodiments of the invention, the temperature and time conditions of the heating are the same in step S3 and step T3; preferably, the heating temperature is 50-60 ℃, and the heating time is 30-60 min.
In the present invention, the color development steps in step S3 and step T3 coincide, and are substantially the same as GB/T5121.23-2008.
In some preferred embodiments of the invention, the method further comprises the steps of:
and S5, distilling the sample processing liquid left after the completion of the measurement in the step S2, and recovering the organic solvent therein. The recovered organic solvent can be used for the next experiment. The step is favorable for reducing the discharge of waste liquid and reducing the cost.
In some embodiments of the invention, the sample to be tested is selected from one or more of polyurethane enamelled wire, polyester enamelled wire, industrial felt, sweatband, thread gloves, waist paper packaging, pearl wool packaging, polyethylene packaging, moisture-proof packaging and carton.
In some embodiments of the present invention, the method for determining the silicon content in the enameled wire and the auxiliary materials for manufacturing the enameled wire specifically includes the following steps (the flow chart is shown in fig. 1):
(1) weighing 10-40 g of a sample to be detected, soaking the sample in 100-400 mL of an organic solvent, sealing the container, and carrying out ultrasonic oscillation for 60-90 min under the heating condition of 50-60 ℃ to obtain a sample treatment solution;
(2) taking 9-10 mL of the sample treatment solution, evaporating and concentrating to 0.5-1 mL under the heating condition of 50-80 ℃, and then adding 9-10 mL of distilled water for dilution to obtain a first dilution solution;
(3) mixing the first diluent with 0.4-0.5 ml of mixed solution formed by mixing 40 wt% of hydrofluoric acid liquid and distilled water according to the volume ratio of 1:1, uniformly stirring by using a stirring rod, standing for 25-30 min, heating at 50-60 ℃ for 30-60 min, and then developing (the developing step is basically the same as GB/T5121.23-2008) to obtain a liquid to be detected;
(4) taking 1.0mL of the standard solution containing 100 micrograms of silicon per milliliter, transferring the standard solution into a 100.0mL volumetric flask, diluting the standard solution to a marked line by using distilled water, and sealing and storing the standard solution by using a polyethylene bottle to obtain the silicon standard solution containing 1 micrograms of silicon per milliliter;
(5) mixing the silicon standard solution with 9-10 mL of organic solvent, evaporating and concentrating to 0.5-1 mL under the heating condition of 50-80 ℃, and then adding 9-10 mL of distilled water for dilution to obtain a second diluent;
(6) mixing the second diluent with 0.4-0.5 ml of mixed solution formed by mixing 40 wt% of hydrofluoric acid liquid and distilled water according to the volume ratio of 1:1, uniformly stirring by using a stirring rod, standing for 25-30 min, heating at 50-60 ℃ for 30-60 min, and then developing (the developing step is basically the same as GB/T5121.23-2008) to obtain silicon content control standard solution;
(7) respectively carrying out absorbance detection on the solution to be detected and the silicon content control standard solution under the same condition to obtain the OD value of the solution to be detectedLiquid to be testedOD value of standard liquid for controlling silicon contentStandard liquid(ii) a For OD valueLiquid to be testedAnd OD valueStandard liquidComparing to judge whether the silicon content in the sample to be detected exceeds the standard or not;
(8) and (3) distilling the sample treatment solution which is left after the measurement in the step (2) is completed, and recovering the organic solvent in the sample treatment solution.
A second aspect of the invention relates to the use of a method according to the first aspect of the invention in the production of enamelled wire.
Examples
In order that the present invention may be more readily understood, the following detailed description will proceed with reference being made to examples, which are intended to be illustrative only and are not intended to limit the scope of the invention. The starting materials or components used in the present invention may be commercially or conventionally prepared unless otherwise specified.
Example 1
(1) The polyurethane enameled wire of a certain enameled wire manufacturer in the Zhuhai is sampled by using tools such as tweezers, scissors and the like, is numbered as Z1, is put into a plastic self-sealing bag and is brought back to a laboratory. 10.0g of the sample No. Z1 was weighed and immersed in 100.0mL of methanol solvent, the container was closed, and the sample treatment liquid a1 was obtained by ultrasonic oscillation for 60min under a heating condition of 60 ℃.
(2) Accurately measuring 10.0mL of sample treatment liquid a1 into a polytetrafluoroethylene beaker, heating at 70.0 ℃, evaporating and concentrating to 0.5mL, adding 10.0mL of distilled water for dilution, slowly adding 0.5mL (12 drops) of mixed liquid formed by mixing 40 wt% of hydrofluoric acid liquid and distilled water in a volume ratio of 1:1, stirring uniformly by using a stirring rod, standing for 30min, heating at 55 ℃ for 30min, and then developing (the developing step is basically the same as GB/T5121.23-2008), thus obtaining a liquid T1 to be detected after the development is finished.
(3) Preparing a silicon standard solution: 1.0mL of the standard solution containing 100. mu.g of silicon per mL was transferred to a 100.0mL volumetric flask, diluted with distilled water to the marked line, and stored in a polyethylene bottle in a sealed state to obtain a silicon standard solution containing 1. mu.g of silicon per mL.
(4) Preparing a silicon content control standard solution: as the silicon content control standard of a certain manufacturer of the Zhuhai enameled wire is not higher than 0.5mg/kg, only 0.5mg/kg of silicon content control standard solution needs to be prepared in the step. Accurately measuring 0.5mL of the silicon standard solution prepared in the step (3) into a polytetrafluoroethylene beaker, accurately adding 10.0mL of methanol solvent, heating at 70.0 ℃, evaporating and concentrating to 0.5mL, adding 10.0mL of distilled water for dilution, slowly adding 0.5mL (12 drops) of mixed solution formed by mixing 40 wt% of hydrofluoric acid liquid and distilled water in a volume ratio of 1:1, uniformly stirring by using a stirring rod, standing for 30min, heating at 55 ℃ for 30min, and then developing (the developing step is basically the same as GB/T5121.23-2008), thus obtaining the silicon content control standard solution of 0.5mg/kg to be prepared after the developing is finished.
(5) The solution to be measured and the silicon content control standard solution were transferred to a 10mm cuvette, respectively, and absorbance measurement was performed at a wavelength of 800nm using a UV-visible spectrophotometer model Shimadzu, Japan, and the reading was recorded (see Table 1). The silicon content of the polyurethane enameled wire is less than 0.5mg/kg by comparing the reading, and the control standard is met.
TABLE 1
(6) And (3) distilling and recovering the residual 90mL of sample treatment solution obtained after the measurement in the step (2) at the temperature of 80 ℃ twice by using a conventional distilling device, wherein the obtained secondary recovered solution can be continuously used.
Example 2
10.0g of the sample No. Z1 was weighed and immersed in 100.0mL of methanol solvent, the container was closed, and the sample treatment liquid a2 was obtained by ultrasonic oscillation for 90min under a heating condition of 55 ℃.
30.0g of the sample No. Z1 was weighed and soaked in 300.0mL of methanol solvent, the container was closed, and the sample treatment liquid a3 was obtained by ultrasonic oscillation for 90min under a heating condition of 55 ℃.
The sample treatment liquids a2 and a3 were treated in the same manner as in example 1, respectively, to thereby obtain solutions to be tested T2 and T3, respectively.
A standard solution for controlling the silicon content at 0.5mg/kg was prepared in the same manner as in example 1.
The solutions to be measured, T2 and T3, and the silicon content controlling standard solution were transferred to a 10mm cuvette, respectively, and absorbance measurement was carried out at a wavelength of 800nm using a Nippon Shimadzu UVmini-1240 type ultraviolet-visible spectrophotometer, and the reading was recorded (see Table 2). The silicon content of the polyurethane enameled wire is less than 0.5mg/kg by comparing the reading, and the control standard is met.
TABLE 2
From the data in table 2, it can be seen that although the mass ratio of methanol addition volume to sample is 10:1, the readings of solutions to be tested T2 and T3 are not the same, possibly due to: firstly, the silicon element is unevenly distributed on the enameled wire, so that the content of a certain section of sample is too much or too little, and the data are inconsistent. Second, in the case of 30g of sample, the sample may be agglomerated or not fully contacted with methanol, resulting in less silicon being extracted, and thus a smaller value is shown in the data.
In addition, the test solution T1 of example 1 was subjected to ultrasonic oscillation for 60min under the heating condition of 60 ℃ in the pretreatment process, whereas the test solution T2 of example 2 was subjected to ultrasonic oscillation for 90min under the heating condition of 55 ℃ in the pretreatment process, since the object was achieved at a higher temperature for a shorter time. Meanwhile, by comparing the readings of the solution to be detected T1 and the solution to be detected T2, the extraction is found to be more thorough and better under the pretreatment condition of ultrasonic oscillation for 90min under the heating condition of 55 ℃.
Example 3
Industrial felts and waist papers of certain manufacturers of the Zhuhai enameled wires are sampled by means of tweezers, scissors and the like, are respectively numbered as Z2 and Z3, are put into a plastic self-sealing bag and are brought back to a laboratory. 10.0g of each of the above samples Z2 and Z3 was weighed, immersed in 100.0mL of methanol solvent, and the samples were treated with ultrasonic vibration at 55 ℃ for 60min in a closed container to obtain a4 and a5, respectively.
The sample treatment liquids a4 and a5 were treated in the same manner as in example 1, respectively, to thereby obtain solutions to be tested T4 and T5, respectively.
A standard solution for controlling the silicon content at 0.5mg/kg was prepared in the same manner as in example 1.
The solutions to be measured, T4 and T5, and the silicon content controlling standard solution were transferred to a 10mm cuvette, respectively, and absorbance measurement was carried out at a wavelength of 800nm using a Nippon Shimadzu UVmini-1240 type ultraviolet-visible spectrophotometer, and the reading was recorded (see Table 3). The silicon content of the industrial felt and the waist paper is less than 0.5mg/kg according to the comparison of the reading, and both the industrial felt and the waist paper meet the control standard.
TABLE 3
Comparative example 1
The experimental procedure was essentially the same as in example 1, except that: 10.0g of the sample No. Z1 was weighed and soaked in 90.0mL of methanol solvent, the container was closed, and ultrasonic vibration was performed at 60 ℃ for 60min to obtain a sample treatment solution a 6. And carrying out subsequent treatment on the sample treatment liquid a6 to obtain a test liquid T6.
A standard solution for controlling the silicon content at 0.5mg/kg was prepared in the same manner as in example 1.
The solution to be measured T6 and the silicon content control standard solution were transferred to a 10mm cuvette, respectively, and absorbance measurement was performed at a wavelength of 800nm using a uv-vis spectrophotometer model shimadzu UVmini-1240, japan, and the reading was recorded (see table 4).
TABLE 4
As can be seen from table 4, when the sample is extracted with 90mL of methanol solvent, the sample is insufficiently extracted due to insufficient coverage and soaking with the methanol solvent.
Comparative example 2
The experimental procedure was essentially the same as in example 1, except that: 10.0g of the sample No. Z1 was weighed and soaked in 90.0mL of methanol solvent, the container was closed, and ultrasonic vibration was performed at 40 ℃ for 60min to obtain a sample treatment solution a 7. And carrying out subsequent treatment on the sample treatment liquid a7 to obtain a test liquid T7.
A standard solution for controlling the silicon content at 0.5mg/kg was prepared in the same manner as in example 1.
The solution to be measured T7 and the silicon content-controlling standard solution were transferred to a 10mm cuvette, respectively, and absorbance measurement was performed at a wavelength of 800nm using a uv-vis spectrophotometer model shimadzu UVmini-1240, japan, and the reading was recorded (see table 5).
TABLE 5
As can be seen from Table 5, when the ultrasonic vibration is carried out at an excessively low temperature (e.g., 40 ℃ C.), insufficient extraction is also caused.
It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not constitute any limitation to the present invention. The present invention has been described with reference to exemplary embodiments, but the words which have been used herein are words of description and illustration, rather than words of limitation. The invention can be modified, as prescribed, within the scope of the claims and without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.
Claims (10)
1. A method for measuring the silicon content in enameled wires and production auxiliary materials thereof comprises the following steps:
s1, mixing a sample to be detected with an organic solvent, and then performing ultrasonic oscillation to obtain a sample treatment solution;
s2, evaporating and concentrating the sample treatment solution, and then adding distilled water for dilution to obtain a first diluent;
s3, mixing the first diluent with a mixed solution of hydrofluoric acid liquid and distilled water, heating and then developing the color of the mixed solution to obtain a solution to be detected;
s4, carrying out absorbance detection on the solution to be detected to obtain an OD valueLiquid to be testedOD value of standard liquid for controlling silicon contentStandard liquidAnd comparing to judge whether the silicon content in the sample to be detected exceeds the standard or not.
2. The method of claim 1, wherein the OD value is determined asLiquid to be testedOD value > ODStandard liquidThen, the silicon content in the sample to be detected exceeds the standard; when the OD value isLiquid to be testedNo more than OD valueStandard liquidAnd then, the silicon content in the sample to be detected meets the control standard.
3. According to claimThe method of claim 1 or 2, characterized in that the absorbance detection is performed on the silicon content control standard solution under the same absorbance detection condition as the solution to be detected, and then the OD value of the silicon content control standard solution is obtainedStandard liquid。
4. The method according to any one of claims 1 to 3, wherein the method for preparing the silicon content control standard solution comprises the steps of:
t1, preparing a silicon standard solution containing 0.9-1.1 mu g of silicon per milliliter;
t2, mixing the silicon standard solution with an organic solvent, evaporating and concentrating, and then adding distilled water for dilution to obtain a second diluent;
and T3, mixing the second diluent with a mixed solution of hydrofluoric acid liquid and distilled water, heating and then developing the color to obtain the silicon content control standard solution.
5. The method according to any one of claims 1 to 4, wherein in step S1, the mass of the sample to be tested is 10-40 g; and/or the dosage of the organic solvent is 100-400 mL;
and/or the organic solvent used in step S1 is the same as the organic solvent used in step T2; preferably, the organic solvent is selected from one or more of methanol, petroleum ether, xylene, n-hexane and cyclohexane.
6. The method according to any one of claims 1 to 5, wherein in step S1, the ultrasonic oscillation is performed at a temperature of 50 to 60 ℃; and/or the time of the ultrasonic oscillation is 60-90 min;
and/or in step S2, evaporating and concentrating 9-10 mL of the sample treatment solution.
7. The method according to any one of claims 1 to 6, wherein the evaporative concentration is performed at a temperature of 50 to 80 ℃ in steps S2 and T2; and/or
In the step S3 and the step T3, the heating temperature is 50-60 ℃, and the heating time is 30-60 min.
8. The method according to any one of claims 1-7, characterized in that the method further comprises the steps of:
and S5, distilling the sample processing liquid left after the completion of the measurement in the step S2, and recovering the organic solvent therein.
9. The method according to any one of claims 1 to 8, wherein the sample to be tested is selected from one or more of polyurethane enamelled wire, polyester enamelled wire, industrial felt, sweat shirt fabric, thread gloves, waist paper packaging, pearl wool packaging, polyethylene packaging, moisture-proof bags and cartons.
10. Use of a method according to any of claims 1-9 in the production of enamelled wire.
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