Method and device for measuring content of trace boron in metal calcium

Abstract

The invention belongs to the technical field of chemical element analysis, and particularly relates to a method and device for measuring the content of trace boron in metal calcium. The method comprises the following steps: dissolving a to-be-detected sample to obtain to-be-detected liquid; measuring the intensity of emitted light to be measured of the liquid to be measured under a preset analysis wavelength by using an inductively coupled plasma atomic emission spectrometer; determining the content of the boron element in the to-be-detected sample based on a pre-determined standard curve and the to-be-detected emitted light intensity, the standard curve is obtained by fitting emission light intensity of a plurality of calcium-containing matrix boron standard solutions with different boron element contents under the preset analysis wavelength. According to the embodiment of the invention, the calcium matrix does not need to be separated, the inductively coupled plasma atomic emission spectrometer is directly used for determination, and the use of a toxic reagent methanol is avoided, so that the harm of the methanol reagent to a human body and the pollution to the environment are avoided, and the labor intensity of operators is reduced.

Description

Technical Field

[0001] The present application belongs to the technical field of chemical element analysis, and specifically relates to a method and device for determining trace boron content in metallic calcium. Background Art

[0002] Metallic calcium has the characteristics of high electronegativity and active chemical properties. It is a reducing agent for the preparation of many high-purity metals and rare earth materials. It is widely used in metallurgy, petrochemicals, battery energy, national defense and military industries. In the preparation process of metallic calcium, impurity elements such as boron, aluminum, iron, nickel, manganese, silicon, and copper will be introduced. The content of these impurity elements directly affects the purity, toughness, stability and other properties of the materials obtained by calcium reduction. Therefore, the accurate determination of impurity elements in metallic calcium is of positive significance for improving product quality, studying product physical and chemical properties, and promoting product performance upgrades.

[0003] At present, the only method for determining the boron element in metallic calcium is the curcumin spectrophotometry. This method has a complex operation process, is time-consuming (e.g., one analysis takes about 12 hours), and requires the use of a large amount of toxic reagent methanol. In recent years, the state and the company have attached great importance to environmental protection and occupational health issues, requiring the use of toxic and hazardous substances to be minimized. Methanol is toxic and has certain hazards to the human body and the environment. In addition, with the retirement of some employees and the needs of company development, the number of on-the-job testing personnel has decreased instead of increased. In order to ensure the timely reporting of sample test results, it is urgent to explore new methods for the determination of boron content in metallic calcium, improve sample testing efficiency and reduce the use of toxic reagent methanol while meeting the test requirements. Summary of the invention

[0004] The purpose of the present application is to provide a method and device for determining the trace boron content in metallic calcium, so as to solve the problem that the prior art is time-consuming and uses toxic reagents for detection.

[0005] Technical solution to achieve the purpose of this application:

[0006] The first aspect of the embodiment of the present application provides a method for determining the trace boron content in metallic calcium, the method comprising:

[0007] After dissolving the sample to be tested, a liquid to be tested is obtained;

[0008] Using an inductively coupled plasma atomic emission spectrometer, the intensity of the emission light to be measured of the liquid to be measured at a preset analysis wavelength;

[0009] The boron content in the sample to be tested is determined based on a pre-determined standard curve and the intensity of the emission light to be tested; the standard curve is obtained by fitting the emission light intensity of multiple calcium-containing matrix boron standard solutions with different boron content at the preset analysis wavelength.

[0010] Optionally, dissolving the sample to be tested to obtain a liquid to be tested specifically includes:

[0011] The sample to be tested is placed in a cold water bath, water is added to dissolve it, and then concentrated nitric acid is added to obtain the solution to be tested.

[0012] Optionally, the preset analysis wavelength is 249.772 nm.

[0013] Optionally, the standard curve is obtained by the following steps:

[0014] Putting the plurality of calcium-containing matrix boron standard solutions with different boron content into an inductively coupled plasma atomic emission spectrometer, and measuring the standard emission light intensity of each calcium-containing matrix boron standard solution at the preset analysis wavelength;

[0015] The standard curve is obtained by fitting according to the measured multiple standard emission light intensities and the content of boron element in the corresponding calcium-containing matrix boron standard solution.

[0016] Optionally, the contents of the boron element in the multiple calcium-containing matrix boron standard solutions are 0 μg / mL, 0.005 μg / mL, 0.05 μg / mL, 0.5 μg / mL and 1 μg / mL, respectively.

[0017] Optionally, the plurality of calcium-containing matrix boron standard solutions are obtained by the following steps:

[0018] 1 mL of a boron standard transition solution with a boron content of 100 μg / mL was mixed with 20 mL of a calcium matrix solution, and then diluted to 100 mL to obtain a calcium-based boron standard solution with a boron content of 1 μg / mL;

[0019] 50 mL of a calcium-based boron standard solution having a boron content of 1 μg / mL was mixed with 20 mL of the calcium-based solution, and then diluted to 100 mL to obtain a calcium-based boron standard solution having a boron content of 0.5 μg / mL;

[0020] 5 mL of a calcium-based boron standard solution having a boron content of 1 μg / mL was mixed with 20 mL of the calcium-based solution, and then diluted to 100 mL to obtain a calcium-based boron standard solution having a boron content of 0.05 μg / mL;

[0021] 0.5 mL of a calcium-based boron standard solution having a boron content of 1 μg / mL was mixed with 20 mL of the calcium-based solution, and then diluted to 100 mL to obtain a calcium-based boron standard solution having a boron content of 0.005 μg / mL;

[0022] 20 mL of the calcium matrix solution was diluted to 100 mL to obtain a calcium matrix boron standard solution with a boron content of 0 μg / mL.

[0023] Optionally, the content of boron in the sample to be tested is determined based on a pre-determined standard curve and the intensity of the emission light to be tested, and then further includes:

[0024] Eliminate the error of the boron content in the sample to be tested according to the intensity of the interfering emission light;

[0025] Wherein, the interfering emission light intensity is the emission light intensity of the blank solution at the preset analysis wavelength measured by inductively coupled plasma atomic emission spectrometer.

[0026] Optionally, eliminating the error of the boron content in the sample to be tested according to the intensity of the interfering emission light specifically includes:

[0027] Determine the content of boron element C0 in the blank solution according to the interfering emission light intensity and the standard curve;

[0028] The error of the boron content in the sample to be tested is eliminated according to the following formula (1):

[0029]

[0030] Wherein, ω is the content of boron in the sample to be tested after removing the error, C1 is the content of boron in the sample to be tested before removing the error, C0 is the content of boron in the blank solution; V is the volume of the liquid to be tested, and m is the mass of the sample to be tested.

[0031] A second aspect of the embodiment of the present application provides a device for determining the trace boron content in metallic calcium, the device comprising:

[0032] A dissolving module is used to dissolve the sample to be tested to obtain a liquid to be tested;

[0033] A measuring module, used for measuring the intensity of the emission light to be measured of the liquid to be measured at a preset analysis wavelength by using an inductively coupled plasma atomic emission spectrometer;

[0034] A determination module is used to determine the content of boron in the sample to be tested based on a pre-determined standard curve and the emission light intensity to be tested; the standard curve is obtained by fitting the emission light intensity of multiple calcium-containing matrix boron standard solutions with different boron content at the preset analysis wavelength.

[0035] The beneficial technical effects of this application are:

[0036] The embodiment of the present application provides a method and device for determining the trace boron content in metallic calcium, the method comprising: dissolving the sample to be tested to obtain a liquid to be tested; using an inductively coupled plasma atomic emission spectrometer to determine the emission light intensity to be tested of the liquid to be tested at a preset analysis wavelength; based on a pre-determined standard curve and the emission light intensity to be tested, determining the content of the boron element in the sample to be tested; the standard curve is obtained by fitting the emission light intensity of multiple calcium-containing matrix boron standard solutions with different boron content at the preset analysis wavelength. The embodiment of the present application only needs to add water and then concentrated nitric acid in a cold water bath to dissolve the metallic calcium sample, without separating the calcium matrix, and directly using an inductively coupled plasma atomic emission spectrometer for determination, avoiding the use of the toxic reagent methanol, thereby avoiding the damage of the methanol reagent to the human body and the pollution to the environment, and reducing the labor intensity of the operator. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] Figure 1 A schematic flow chart of a method for determining trace boron content in metallic calcium provided in an embodiment of the present application. DETAILED DESCRIPTION

[0038] In order to make those skilled in the art better understand the present application, the technical scheme in the embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. Obviously, the embodiments described below are only a part of the embodiments of the present application, not all. Based on the embodiments recorded in the present application, all other embodiments obtained by those skilled in the art without paying creative work are within the scope of protection of the present application.

[0039] See also Figure 1 , which is a schematic flow chart of a method for determining trace boron content in metallic calcium provided in an embodiment of the present application.

[0040] The present invention provides a method for determining the content of trace boron in metallic calcium, comprising:

[0041] Step S101: dissolving the sample to be tested to obtain a liquid to be tested;

[0042] Step S102: using an inductively coupled plasma atomic emission spectrometer to measure the intensity of the emission light to be measured of the liquid to be measured at a preset analysis wavelength;

[0043] Step S103: Determine the content of boron in the sample to be tested based on a pre-determined standard curve and the intensity of the emission light to be tested; the standard curve is obtained by fitting the emission light intensity of multiple calcium-containing matrix boron standard solutions with different boron content at the preset analysis wavelength.

[0044] The embodiment of the present application aims at the problems of the current boron content determination technology in metallic calcium, such as the complicated operation process, long time consumption, and the need to use a large amount of toxic reagent methanol, and provides a method for determining the boron content in metallic calcium by inductively coupled plasma atomic emission spectrometry. According to the pre-determined standard curve and the use of an inductively coupled plasma atomic emission spectrometer, the intensity of the emission light to be measured at the preset analysis wavelength of the liquid to be measured is measured to determine the content of the boron element in the sample to be measured. The trace boron content in metallic calcium can be accurately determined, and it is not interfered by coexisting impurity elements such as aluminum, iron, nickel, manganese, silicon, and copper. There is no need to use toxic reagent methanol and additional chemical reagents, which not only saves energy and reduces consumption, but also saves analysis costs.

[0045] In a specific implementation, the preset analysis wavelength may be 249.772 nm. It is understandable that 249.772 nm is the best analysis wavelength for determining the amount of boron.

[0046] In some possible implementations of the embodiments of the present application, step S101 may specifically include:

[0047] The sample to be tested is placed in a cold water bath, water is added to dissolve it, and then concentrated nitric acid is added to obtain the solution to be tested.

[0048] In a specific example, 0.5 g of the sample to be tested can be weighed and transferred to a clean 50 mL polyethylene plastic beaker, and the beaker is placed in a cold water bath. Slowly add 10 mL of ultrapure water to the plastic beaker, and slowly shake while adding water. After the reaction is complete, slowly add 2.5 mL of concentrated nitric acid, put it in water, and after cooling to room temperature, transfer it to a 25 mL volumetric flask and dilute it to the scale with ultrapure water for testing.

[0049] In one example, in order to reduce the error caused by the added reagents, a blank solution can be prepared as a reagent blank using the same steps and reagents while preparing the test solution.

[0050] In the embodiment of the present application, it is only necessary to first add water and then concentrated nitric acid in a cold water bath to dissolve the metallic calcium sample. There is no need to separate the calcium matrix and the sample can be directly measured using an inductively coupled plasma atomic emission spectrometer. The entire measurement process is simple and reduces the labor intensity of the operator.

[0051] In some possible implementations of the embodiments of the present application, the standard curve can be obtained by the following steps:

[0052] Putting the plurality of calcium-containing matrix boron standard solutions with different boron content into an inductively coupled plasma atomic emission spectrometer, and measuring the standard emission light intensity of each calcium-containing matrix boron standard solution at the preset analysis wavelength;

[0053] The standard curve is obtained by fitting according to the measured multiple standard emission light intensities and the content of boron element in the corresponding calcium-containing matrix boron standard solution.

[0054] In one example, the contents of the boron element in the plurality of calcium-containing matrix boron standard solutions may be 0 μg / mL, 0.005 μg / mL, 0.05 μg / mL, 0.5 μg / mL and 1 μg / mL, respectively.

[0055] In another example, the plurality of calcium-containing matrix boron standard solutions are obtained by the following steps:

[0056] 1 mL of a boron standard transition solution with a boron content of 100 μg / mL was mixed with 20 mL of a calcium matrix solution, and then diluted to 100 mL to obtain a calcium-based boron standard solution with a boron content of 1 μg / mL;

[0057] 50 mL of a calcium-based boron standard solution having a boron content of 1 μg / mL was mixed with 20 mL of the calcium-based solution, and then diluted to 100 mL to obtain a calcium-based boron standard solution having a boron content of 0.5 μg / mL;

[0058] 5 mL of a calcium-based boron standard solution having a boron content of 1 μg / mL was mixed with 20 mL of the calcium-based solution, and then diluted to 100 mL to obtain a calcium-based boron standard solution having a boron content of 0.05 μg / mL;

[0059] 0.5 mL of a calcium-based boron standard solution having a boron content of 1 μg / mL was mixed with 20 mL of the calcium-based solution, and then diluted to 100 mL to obtain a calcium-based boron standard solution having a boron content of 0.005 μg / mL;

[0060] 20 mL of the calcium matrix solution was diluted to 100 mL to obtain a calcium matrix boron standard solution with a boron content of 0 μg / mL.

[0061] The method for obtaining the standard curve in the embodiment of the present application is described in detail below with reference to a specific example.

[0062] Step 3.1 Preparation of calcium matrix solution:

[0063] Accurately weigh 25 g of spectrally pure calcium carbonate into a beaker, add an appropriate amount of water, then add 50 mL of concentrated nitric acid, make up to 100 mL with ultrapure water to prepare a 10% calcium matrix solution, and transfer to a plastic bottle for storage.

[0064] Step 3.2 Preparation of boron standard transition solution N5:

[0065] Accurately transfer 10 mL of 1000 μg / mL boron standard stock solution into a 100 mL volumetric flask, dilute to the mark with ultrapure water to obtain a boron standard transition solution N5 with a concentration of 100 μg / mL, and transfer to a polyethylene plastic bottle for later use.

[0066] Step 3.3 Preparation of calcium-based boron standard solution:

[0067] Accurately pipette 1 mL of N5 and 20 mL of calcium matrix solution into the same 100 mL volumetric flask, dilute to scale with ultrapure water, shake well, and obtain a standard solution N4 with a boron content of 1 μg / mL;

[0068] Accurately pipette 50 mL of N4 and 20 mL of calcium matrix solution into the same 100 mL volumetric flask, dilute to scale with ultrapure water, shake well, and obtain a standard solution N3 with a boron content of 0.5 μg / mL;

[0069] Accurately pipette 5 mL of N4 and 20 mL of calcium matrix solution into the same 100 mL volumetric flask, dilute to scale with ultrapure water, shake well, and obtain a standard solution N2 with a boron content of 0.05 μg / mL;

[0070] Accurately pipette 0.5 mL of N4 and 20 mL of calcium matrix solution into the same 100 mL volumetric flask, dilute to the scale with ultrapure water, shake well, and obtain a standard solution N1 with a boron content of 0.005 μg / mL.

[0071] Finally, the obtained N1-N4 boron standard solution was introduced into the inductively coupled plasma atomic emission spectrometer through the injection system, the emission light intensity of the boron element at the optimal analysis wavelength of 249.772 nm was measured, and a standard curve was drawn.

[0072] In some possible implementations of the embodiments of the present application, in order to eliminate the interference of the boron element that may exist in the added reagent on the measurement result, step S103 may further include:

[0073] Eliminate the error of the boron content in the sample to be tested according to the intensity of the interfering emission light;

[0074] Wherein, the interfering emission light intensity is the emission light intensity of the blank solution at the preset analysis wavelength measured by inductively coupled plasma atomic emission spectrometer.

[0075] In one example, eliminating the error of the boron content in the sample to be tested according to the intensity of the interfering emission light may specifically include:

[0076] Determine the content of boron element C0 in the blank solution according to the interfering emission light intensity and the standard curve;

[0077] The error of the boron content in the sample to be tested is eliminated according to the following formula (1):

[0078]

[0079] Wherein, ω is the content of boron in the sample to be tested after removing the error, C1 is the content of boron in the sample to be tested before removing the error, C0 is the content of boron in the blank solution; V is the volume of the liquid to be tested, and m is the mass of the sample to be tested.

[0080] It can be understood that the reagents added to the blank solution and their contents are consistent with those in the liquid with the strip.

[0081] The embodiment of the present application provides a method for determining the trace boron content in metallic calcium, comprising: dissolving the sample to be tested to obtain a liquid to be tested; using an inductively coupled plasma atomic emission spectrometer to determine the emission light intensity of the liquid to be tested at a preset analysis wavelength; determining the content of the boron element in the sample to be tested based on a pre-determined standard curve and the emission light intensity to be tested; the standard curve is obtained by fitting the emission light intensity of multiple calcium-containing matrix boron standard solutions with different boron content at the preset analysis wavelength. The embodiment of the present application only needs to add water and then concentrated nitric acid in a cold water bath to dissolve the metallic calcium sample, without separating the calcium matrix, and directly using an inductively coupled plasma atomic emission spectrometer for determination, avoiding the use of the toxic reagent methanol, thereby avoiding the damage of the methanol reagent to the human body and the pollution to the environment, and reducing the labor intensity of the operator.

[0082] The actual effect of the method for determining the trace boron content in metallic calcium provided in the embodiment of the present application is described in detail below with reference to a specific example.

[0083] Metallic calcium is a product obtained by distillation of purchased crude calcium, which may contain impurity elements such as aluminum, beryllium, cobalt, chromium, iron, nickel, manganese, silicon, and copper. In order to explore the influence of the above coexisting elements on the determination results of boron, this experiment prepared three low, medium, and high concentrations of impurity interference samples with boron content of 0.005μg / mL, 0.05μg / mL, and 0.5μg / mL, respectively, six samples for each concentration, and the boron element and interfering elements and concentrations are shown in Table 1. The prepared impurity interference experimental samples were tested, and the results are shown in Table 2.

[0084] Table 1 Coexisting interfering elements and concentrations

[0085]

[0086] Table 2 Statistical table of coexistence interference element test results

[0087]

[0088]

[0089] The method for determining the trace boron content in metallic calcium provided in the embodiment of the present application can accurately determine the trace boron content in metallic calcium without being interfered by coexisting impurity elements such as aluminum, iron, nickel, manganese, silicon, and copper. The operation process is simple and time-saving, and there is no need to use toxic reagent methanol and additional chemical reagents, which not only saves energy and reduces consumption, but also saves analysis costs.

[0090] Table 3 below is the minimum detection limit of the experiment; Table 4 is the precision of the experiment; Table 5 is the spiked recovery rate of the experiment.

[0091] Table 3 Minimum detection limit of the experiment (2% calcium matrix concentration)

[0092]

[0093] Table 4 The precision of boron content determination of the same sample was determined 3 times / day for 3 consecutive days

[0094]

[0095]

[0096] Table 5 Recovery of spiked boron

[0097]

[0098] Based on the method for determining the trace boron content in metallic calcium provided in the above embodiment, the embodiment of the present application also provides a device for determining the trace boron content in metallic calcium.

[0099] The present invention provides a device for determining the content of trace boron in metallic calcium, comprising:

[0100] A dissolving module is used to dissolve the sample to be tested to obtain a liquid to be tested;

[0101] A measuring module, used for measuring the intensity of the emission light to be measured of the liquid to be measured at a preset analysis wavelength by using an inductively coupled plasma atomic emission spectrometer;

[0102] A determination module is used to determine the content of boron in the sample to be tested based on a pre-determined standard curve and the emission light intensity to be tested; the standard curve is obtained by fitting the emission light intensity of multiple calcium-containing matrix boron standard solutions with different boron content at the preset analysis wavelength.

[0103] In one example, the dissolution module can be specifically used to:

[0104] The sample to be tested is placed in a cold water bath, water is added to dissolve it, and then concentrated nitric acid is added to obtain the solution to be tested.

[0105] As an example, the preset analysis wavelength is 249.772 nm.

[0106] In some possible implementations of the embodiments of the present application, the standard curve is obtained by the following steps:

[0107] Putting the plurality of calcium-containing matrix boron standard solutions with different boron content into an inductively coupled plasma atomic emission spectrometer, and measuring the standard emission light intensity of each calcium-containing matrix boron standard solution at the preset analysis wavelength;

[0108] The standard curve is obtained by fitting according to the measured multiple standard emission light intensities and the content of boron element in the corresponding calcium-containing matrix boron standard solution.

[0109] In one example, the contents of the boron element in the plurality of calcium-containing matrix boron standard solutions are 0 μg / mL, 0.005 μg / mL, 0.05 μg / mL, 0.5 μg / mL and 1 μg / mL, respectively.

[0110] In another example, the plurality of calcium-containing matrix boron standard solutions are obtained by the following steps:

[0111] 1 mL of a boron standard transition solution with a boron content of 100 μg / mL was mixed with 20 mL of a calcium matrix solution, and then diluted to 100 mL to obtain a calcium-based boron standard solution with a boron content of 1 μg / mL;

[0112] 50 mL of a calcium-based boron standard solution having a boron content of 1 μg / mL was mixed with 20 mL of the calcium-based solution, and then diluted to 100 mL to obtain a calcium-based boron standard solution having a boron content of 0.5 μg / mL;

[0113] 5 mL of a calcium-based boron standard solution having a boron content of 1 μg / mL was mixed with 20 mL of the calcium-based solution, and then diluted to 100 mL to obtain a calcium-based boron standard solution having a boron content of 0.05 μg / mL;

[0114] 0.5 mL of a calcium-based boron standard solution having a boron content of 1 μg / mL was mixed with 20 mL of the calcium-based solution, and then diluted to 100 mL to obtain a calcium-based boron standard solution having a boron content of 0.005 μg / mL;

[0115] 20 mL of the calcium matrix solution was diluted to 100 mL to obtain a calcium matrix boron standard solution with a boron content of 0 μg / mL.

[0116] In some possible implementations of the embodiments of the present application, the device may further include:

[0117] An error removal module, used to eliminate the error of the boron content in the sample to be tested according to the intensity of the interfering emission light;

[0118] Wherein, the interfering emission light intensity is the emission light intensity of the blank solution at the preset analysis wavelength measured by inductively coupled plasma atomic emission spectrometer.

[0119] In one example, the error removal module is specifically used to:

[0120] Determine the content of boron element C0 in the blank solution according to the interfering emission light intensity and the standard curve;

[0121] The error of the boron content in the sample to be tested is eliminated according to the following formula (1):

[0122]

[0123] Wherein, ω is the content of boron in the sample to be tested after removing the error, C1 is the content of boron in the sample to be tested before removing the error, C0 is the content of boron in the blank solution; V is the volume of the liquid to be tested, and m is the mass of the sample to be tested.

[0124] The embodiment of the present application provides a device for determining the trace boron content in metallic calcium, comprising: a dissolution module for dissolving the sample to be tested to obtain a liquid to be tested; a determination module for determining the emission light intensity of the liquid to be tested at a preset analysis wavelength using an inductively coupled plasma atomic emission spectrometer; a determination module for determining the content of the boron element in the sample to be tested based on a pre-determined standard curve and the emission light intensity to be tested; the standard curve is obtained by fitting the emission light intensity of multiple calcium-containing matrix boron standard solutions with different boron content at the preset analysis wavelength. The embodiment of the present application only needs to add water and then concentrated nitric acid in a cold water bath to dissolve the metallic calcium sample, without separating the calcium matrix, and directly uses an inductively coupled plasma atomic emission spectrometer for determination, avoiding the use of the toxic reagent methanol, thereby avoiding the damage of the methanol reagent to the human body and the pollution to the environment, and reducing the labor intensity of the operator.

[0125] The present application is described in detail above in conjunction with the accompanying drawings and embodiments, but the present application is not limited to the above embodiments, and various changes can be made within the knowledge of ordinary technicians in the field without departing from the purpose of the present application. Any content not described in detail in the present application can adopt the existing technology.

Claims

1. A method for determining the trace boron content in metallic calcium, characterized in that: The method comprises: After dissolving the sample to be tested, a liquid to be tested is obtained; Using an inductively coupled plasma atomic emission spectrometer, the intensity of the emission light to be measured of the liquid to be measured at a preset analysis wavelength; The boron content in the sample to be tested is determined based on a pre-determined standard curve and the intensity of the emission light to be tested; the standard curve is obtained by fitting the emission light intensity of multiple calcium-containing matrix boron standard solutions with different boron content at the preset analysis wavelength.

2. The method for determining the trace boron content in metallic calcium according to claim 1, characterized in that: After the sample to be tested is dissolved, the liquid to be tested is obtained, which specifically includes: The sample to be tested is placed in a cold water bath, water is added to dissolve it, and then concentrated nitric acid is added to obtain the solution to be tested.

3. The method for determining the trace boron content in metallic calcium according to claim 1, characterized in that: The preset analysis wavelength is 249.772 nm.

4. The method for determining the trace boron content in metallic calcium according to any one of claims 1 to 3, characterized in that: The standard curve is obtained by the following steps: Putting the plurality of calcium-containing matrix boron standard solutions with different boron content into an inductively coupled plasma atomic emission spectrometer, and measuring the standard emission light intensity of each calcium-containing matrix boron standard solution at the preset analysis wavelength; The standard curve is obtained by fitting according to the measured multiple standard emission light intensities and the content of boron element in the corresponding calcium-containing matrix boron standard solution.

5. The method for determining the trace boron content in metallic calcium according to claim 4, characterized in that: The contents of the boron element in the plurality of calcium-containing matrix boron standard solutions are 0 μg / mL, 0.005 μg / mL, 0.05 μg / mL, 0.5 μg / mL and 1 μg / mL respectively.

6. The method for determining the trace boron content in metallic calcium according to claim 5, characterized in that: The plurality of calcium-containing matrix boron standard solutions are obtained by the following steps: 1 mL of a boron standard transition solution with a boron content of 100 μg / mL was mixed with 20 mL of a calcium matrix solution, and then diluted to 100 mL to obtain a calcium-based boron standard solution with a boron content of 1 μg / mL; 50 mL of a calcium-based boron standard solution having a boron content of 1 μg / mL was mixed with 20 mL of the calcium-based solution, and then diluted to 100 mL to obtain a calcium-based boron standard solution having a boron content of 0.5 μg / mL; 5 mL of a calcium-based boron standard solution having a boron content of 1 μg / mL was mixed with 20 mL of the calcium-based solution, and then diluted to 100 mL to obtain a calcium-based boron standard solution having a boron content of 0.05 μg / mL; 0.5 mL of a calcium-based boron standard solution having a boron content of 1 μg / mL was mixed with 20 mL of the calcium-based solution, and then diluted to 100 mL to obtain a calcium-based boron standard solution having a boron content of 0.005 μg / mL; 20 mL of the calcium matrix solution was diluted to 100 mL to obtain a calcium matrix boron standard solution with a boron content of 0 μg / mL.

7. The method for determining the trace boron content in metallic calcium according to any one of claims 1 to 3, characterized in that: The method further comprises: determining the content of the boron element in the sample to be tested based on the pre-determined standard curve and the intensity of the emission light to be tested, and then: Eliminate the error of the boron content in the sample to be tested according to the intensity of the interfering emission light; Wherein, the interfering emission light intensity is the emission light intensity of the blank solution at the preset analysis wavelength measured by inductively coupled plasma atomic emission spectrometer.

8. The method for determining the trace boron content in metallic calcium according to claim 7, characterized in that: The method of eliminating the error of the boron content in the sample to be tested according to the intensity of the interfering emission light specifically includes: Determine the content of boron element C0 in the blank solution according to the interfering emission light intensity and the standard curve; The error of the boron content in the sample to be tested is eliminated according to the following formula (1): Wherein, ω is the content of boron in the sample to be tested after removing the error, C1 is the content of boron in the sample to be tested before removing the error, C0 is the content of boron in the blank solution; V is the volume of the liquid to be tested, and m is the mass of the sample to be tested.

9. A device for determining the trace boron content in metallic calcium, characterized in that: The device comprises: A dissolving module is used to dissolve the sample to be tested to obtain a liquid to be tested; A measuring module, used for measuring the intensity of the emission light to be measured of the liquid to be measured at a preset analysis wavelength by using an inductively coupled plasma atomic emission spectrometer; A determination module is used to determine the content of boron in the sample to be tested based on a pre-determined standard curve and the emission light intensity to be tested; the standard curve is obtained by fitting the emission light intensity of multiple calcium-containing matrix boron standard solutions with different boron content at the preset analysis wavelength.

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