A pretreatment method for trace impurity analysis in magnesium bis(oxocero)

Abstract

A pretreatment method for the analysis of trace impurities in magnesium pyrocene involves placing a precisely weighed, dried sampling bottle and sampling device into an inert atmosphere chamber. Magnesium pyrocene is then placed into the sampling bottle using the sampling device, the bottle cap is tightened, and the inert atmosphere chamber is removed. The total weight of the sampling bottle and the magnesium pyrocene contained therein is accurately weighed. A 5% (w / w) dilute acid solution is then added dropwise to a Class 100 cleaning table to allow the reaction to proceed. After the reaction slows down, a small amount of the 5% (w / w) dilute acid solution is added to fully dissolve the sample. The solution is first heated at a low temperature, and the sample on the inner wall of the bottle is rinsed clean with the 5% (w / w) dilute acid solution. The temperature is then increased to allow for a complete reaction, and the acid is removed until nearly dry. The substance in the sampling bottle is then dissolved with the 5% (w / w) dilute acid solution to prepare the corresponding test solution for subsequent detection. This invention solves the problems of complex processes and the easy introduction of other trace impurities in existing technologies.

Description

Technical Field

[0001] This invention relates to the field of chemical analysis technology, and in particular to a pretreatment method for the analysis of trace impurities in magnesium dicerocene. Background Technology

[0002] Organometallic compounds are crucial raw materials for epitaxial growth. Magnesium thiocene, a commonly used organometallic compound, is a key auxiliary material in the semiconductor and MOCVD industries, widely used in light-emitting diodes, laser diodes, transistors, and high-performance, high-efficiency solar cells. Magnesium thiocene is chemically highly reactive, exploding upon contact with water and burning upon contact with oxygen. Therefore, it must be decomposed into mild inorganic compounds in a specific atmosphere before it can be introduced into the instrument for impurity element determination.

[0003] Chinese invention patent CN102103049A discloses a trimethylaluminum HCl decomposition device for the analysis of trace impurities in trimethylaluminum, and provides a method for the elemental analysis of trace impurities in trimethylaluminum by decomposing it with HCl. Using hydrogen chloride gas for decomposition solves the problems of long decomposition reaction time and incomplete dissolution of different crystals, which can lead to deviations in analytical results. However, the preparation process of hydrogen chloride gas is complex, and the prepared hydrogen chloride gas may also contain other trace impurities, which can easily cause deviations in the analysis of organometallic compound products requiring a purity greater than 99.9995%. Summary of the Invention

[0004] In view of the above, the present invention provides a pretreatment method for the analysis of trace impurities in magnesium thiocene, in order to solve the problems of complex processes and easy introduction of other trace impurities in the prior art.

[0005] A pretreatment method for the analysis of trace impurities in magnesium dicerocene includes:

[0006] The accurately weighed dry sampling bottle and sampling device are placed into the inert atmosphere operating box. The sampling device is used to take magnesium pyrocene and place it in the sampling bottle. Then the bottle cap is tightened and the inert atmosphere operating box is taken out.

[0007] Accurately weigh the total weight of the sampling bottle and the magnesium thiocene contained therein. Then, add a 5% dilute acid solution dropwise to the sample on a Class 100 cleaning table to allow the reaction to proceed. After the reaction slows down, add a predetermined amount of 5% dilute acid solution to fully dissolve the sample. The solution is first heated to a first temperature. The sample on the inner wall of the bottle is then rinsed clean with the 5% dilute acid solution. The solution is then heated to a second temperature to allow the reaction to proceed fully. After the acid is removed to near dryness, the substance in the sampling bottle is dissolved with the 5% dilute acid solution to prepare the corresponding test solution for subsequent detection. The second temperature is higher than the first temperature.

[0008] The above-described pretreatment method for trace impurity analysis in magnesium pyrocene includes a stainless steel sampling spoon as the sampling device. Magnesium pyrocene is solid at room temperature and is placed into a sampling bottle using the stainless steel sampling spoon.

[0009] The above-mentioned pretreatment method for the analysis of trace impurities in magnesium thiocene, wherein the water content and oxygen content are maintained at less than 1 ppm in the inert atmosphere operating chamber; the inert atmosphere operating chamber is filled with inert gas.

[0010] In the above-mentioned pretreatment method for the analysis of trace impurities in magnesium thiocene, the inert gas is nitrogen or helium.

[0011] The above-described pretreatment method for analyzing trace impurities in magnesium thiocene involves adding 0.1–0.3 g of the organometallic compound to the sampling bottle. Magnesium thiocene reacts violently with water, generating high heat and releasing flammable gases, which can ignite and explode upon contact with oxygen. In contrast, this invention uses a smaller sample size of 0.1–0.3 g, adding dropwise a 5% (w / w) dilute acid solution to allow the reaction to proceed, thus reducing the degree of reaction.

[0012] The above-mentioned pretreatment method for the analysis of trace impurities in magnesium thiocene, wherein the dilute acid solution with a solute mass percentage of 5% is prepared by diluting one or more of the following acids: nitric acid, hydrochloric acid, sulfuric acid, perchloric acid, hydrobromic acid, hydroiodic acid, perbromic acid, chloric acid, bromic acid, metaphosphoric acid, hydrofluoric acid, selenic acid, fluoroboric acid, fluorosulfonic acid, cyanic acid, thiocyanic acid, phosphoric acid, sulfurous acid, oxalic acid, formic acid, acetic acid, pyrophosphoric acid, trifluoroacetic acid, phosphorous acid, periodic acid, maleic acid, nitrous acid, benzoic acid, salicylic acid, tartaric acid, methanesulfonic acid, benzenesulfonic acid, and citric acid.

[0013] In the above-mentioned pretreatment method for the analysis of trace impurities in magnesium thiocene, the heating process is carried out in a Class 100 clean bench. All the gases emitted during heating are discharged by the exhaust fan and enter the waste gas treatment device through pipelines, so as not to cause waste gas pollution to the laboratory and outdoor environment.

[0014] The above-mentioned pretreatment method for the analysis of trace impurities in magnesium thiocene, wherein the first temperature is 50℃-70℃ and the holding time is 15-20 min; the second temperature is 150℃ and the holding time is no more than 40 min.

[0015] The above-mentioned pretreatment method for the analysis of trace impurities in magnesium bis(oxoceramium) has a total operation time of no more than 1 hour from the preparation of the sampling device to the completion of the decomposition of magnesium bis(oxoceramium).

[0016] The pretreatment method for the analysis of trace impurities in magnesium thiocene provided by the present invention uses a 5% dilute acid solution to decompose the organometallic compound magnesium thiocene dropwise to form soluble magnesium thiocene. It has the advantages of simple operation, good safety, short detection time, no environmental pollution, no introduction of other trace impurities, good repeatability of analytical results, and wide applicability. Detailed Implementation

[0017] To facilitate understanding of the present invention, a more complete description will be given below with reference to various embodiments. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.

[0018] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0019] This invention provides a pretreatment method for the analysis of trace impurities in magnesium dicerocene, comprising:

[0020] The accurately weighed dry sampling bottle and sampling device are placed into the inert atmosphere operating box. The sampling device is used to take magnesium pyrocene and place it in the sampling bottle. Then the bottle cap is tightened and the inert atmosphere operating box is taken out.

[0021] Accurately weigh the total weight of the sampling bottle and the magnesium thiocene contained therein. Then, add a 5% dilute acid solution dropwise to the sample on a Class 100 cleaning table to allow the reaction to proceed. After the reaction slows down, add a predetermined amount of 5% dilute acid solution to fully dissolve the sample. The solution is first heated to a first temperature. The sample on the inner wall of the bottle is then rinsed clean with the 5% dilute acid solution. The solution is then heated to a second temperature to allow the reaction to proceed fully. After the acid is removed to near dryness, the substance in the sampling bottle is dissolved with the 5% dilute acid solution to prepare the corresponding test solution for subsequent detection. The second temperature is higher than the first temperature.

[0022] In the above-mentioned pretreatment method for the analysis of trace impurities in magnesium dicerocene, the sampling device is a stainless steel sampling spoon.

[0023] The above-mentioned pretreatment method for the analysis of trace impurities in magnesium thiocene, wherein the water content and oxygen content are maintained at less than 1 ppm in the inert atmosphere operating chamber; the inert atmosphere operating chamber is filled with inert gas.

[0024] In the above-mentioned pretreatment method for the analysis of trace impurities in magnesium thiocene, the inert gas is nitrogen or helium.

[0025] In the above-mentioned pretreatment method for the analysis of trace impurities in magnesium thiocene, the weight of the organometallic compound added to the sampling bottle is 0.1 to 0.3 g.

[0026] The above-mentioned pretreatment method for the analysis of trace impurities in magnesium thiocene, wherein the dilute acid solution with a solute mass percentage of 5% is prepared by diluting one or more of the following acids: nitric acid, hydrochloric acid, sulfuric acid, perchloric acid, hydrobromic acid, hydroiodic acid, perbromic acid, chloric acid, bromic acid, metaphosphoric acid, hydrofluoric acid, selenic acid, fluoroboric acid, fluorosulfonic acid, cyanic acid, thiocyanic acid, phosphoric acid, sulfurous acid, oxalic acid, formic acid, acetic acid, pyrophosphoric acid, trifluoroacetic acid, phosphorous acid, periodic acid, maleic acid, nitrous acid, benzoic acid, salicylic acid, tartaric acid, methanesulfonic acid, benzenesulfonic acid, and citric acid.

[0027] In the above-mentioned pretreatment method for the analysis of trace impurities in magnesium thiocene, the heating process is carried out in a Class 100 clean bench, and all the gases emitted during heating are discharged by an exhaust fan and enter the waste gas treatment device through pipelines.

[0028] The above-mentioned pretreatment method for the analysis of trace impurities in magnesium thiocene, wherein the first temperature is 50℃-70℃ and the holding time is 15-20 min; the second temperature is 150℃ and the holding time is no more than 40 min.

[0029] The above-mentioned pretreatment method for the analysis of trace impurities in magnesium bis(oxoceramium) has a total operation time of no more than 1 hour from the preparation of the sampling device to the completion of the decomposition of magnesium bis(oxoceramium).

[0030] The embodiments of the present invention will be further described below with reference to several examples. The embodiments of the present invention are not limited to the specific embodiments described below. Appropriate modifications can be made within the scope of unchanged main claims.

[0031] Example 1

[0032] The precisely weighed, dried sampling bottle and stainless steel sampling spoon were placed in an inert atmosphere chamber, where the oxygen content was maintained between 0.3 and 0.6 ppm. Magnesium dicerocene was transferred into the sampling bottle using the stainless steel sampling spoon, and the bottle cap was tightened. The inert atmosphere chamber was then removed. The total weight of the sampling bottle and the magnesium dicerocene contained therein was accurately measured on an analytical balance, ensuring that the magnesium dicerocene in the bottle weighed approximately 0.1 g. Then, 5% nitric acid solution was added dropwise to a Class 100 cleaning table to allow the reaction to proceed. After the reaction slowed down, a small amount of 5% nitric acid solution was added to fully dissolve the sample. The solution was first heated at a low temperature, and the sample was rinsed clean from the inner wall of the bottle with 5% nitric acid solution. The temperature was then increased to allow the reaction to proceed fully, and the acid was removed until the bottle was nearly dry.

[0033] The substance in the sampling vial was dissolved in a 5% (w / w) nitric acid solution to prepare the corresponding test solution for detection. The ratio of the substance in the sampling vial to the nitric acid solution was 10 mg / mL. Inductively coupled plasma mass spectrometry (ICP-MS) was used.

[0034] Inject the sample using a mass spectrometry standard solution containing a metal element. Record the signal intensity of the analyte in the standard solution. Each standard solution should be measured at least three times until the relative standard deviation of the intensity values ​​from the three parallel measurements is no greater than 3%. Take the average value and plot a standard curve with the signal intensity of the analyte as the ordinate and the concentration of the analyte as the abscissa.

[0035] Inject the blank solution (without adding magnesium dicerocene sample to the sample vial, and the remaining steps are the same as for the sample solution) and the test sample solution under the same measurement conditions as for the standard solution. Record the signal intensity of different test elements. Repeat the measurement at least three times until the relative deviation of the three parallel intensity measurements is no greater than 3%, and take the average value.

[0036] The content of the analyte in the test solution was determined by analyzing the signal intensity of the analyte in the test solution against the corresponding metal element standard curve. The content of the corresponding analyte in the blank solution was calculated using the same method. The content of the corresponding analyte in magnesium dicerocene was then calculated using the following formula, and the results are shown in Table 1. The calculation formula is:

[0037]

[0038] In the formula:

[0039] w represents the content of the element to be measured in magnesium dicerocene, in micrograms per gram (μg / g);

[0040] w1 represents the content of the element to be tested in the solution, in micrograms per milliliter (μg / ml);

[0041] w0 represents the concentration of the element to be tested in the blank solution, in micrograms per milliliter (μg / ml);

[0042] V represents the volume of the solution to be tested, in milliliters (mL);

[0043] m represents the sample mass of magnesium dicerocene, in grams (g).

[0044] Table 1

[0045] impurity elements Cu(μg / g) Fe(μg / g) Mn(μg / g) Si (μg / g) Zn(μg / g) First test results ≤0.001 0.008 0.002 0.011 ≤0.001 Second test results ≤0.001 0.008 0.002 0.010 ≤0.001 Third test results ≤0.001 0.009 0.003 0.010 ≤0.001

[0046] As shown in the table above, the method described in this embodiment yields good repeatability and stable results for the determination of trace impurities in magnesium dicerocene.

[0047] Example 2

[0048] Precisely weighed, dried sampling bottles and stainless steel sampling spoons were placed in an inert atmosphere chamber, where the oxygen content was maintained between 0.3 and 0.6 ppm. Magnesium dicerocene was transferred into the sampling bottle using the stainless steel sampling spoon, and the bottle cap was tightened before removing the chamber. The total weight of the sampling bottle and the magnesium dicerocene contained therein was precisely measured on an analytical balance, ensuring the magnesium dicerocene in the bottle weighed approximately 0.1 g. Then, 5% hydrochloric acid solution was added dropwise to a Class 100 cleaning table to allow the reaction to proceed. After the reaction slowed, a small amount of 5% hydrochloric acid solution was added to fully dissolve the sample. The solution was first heated at a low temperature, and the sample was rinsed clean from the inner wall of the bottle with 5% hydrochloric acid solution. The temperature was then increased to allow for a complete reaction, and the acid was removed until nearly dry. The substance in the sampling bottle was then dissolved in 5% hydrochloric acid solution to prepare the corresponding test solution for analysis.

[0049] The instrument used was inductively coupled plasma mass spectrometry (ICP-MS). The testing and calculation methods were the same as in Example 1. The results of three determinations of the magnesium dicerocene sample are shown in Table 2.

[0050] Table 2

[0051] impurity elements Cu(μg / g) Fe(μg / g) Mn(μg / g) Si (μg / g) Zn(μg / g) First test results ≤0.001 0.007 ≤0.001 0.009 ≤0.001 Second test results ≤0.001 0.008 ≤0.001 0.010 ≤0.001 Third test results ≤0.001 0.007 ≤0.001 0.010 ≤0.001

[0052] As shown in the table above, the method described in this embodiment yields good repeatability and stable results for the determination of trace impurities in magnesium dicerocene.

[0053] Example 3

[0054] Precisely weighed, dried sampling bottles and stainless steel sampling spoons were placed in an inert atmosphere chamber, where the oxygen content was maintained between 0.3 and 0.6 ppm. Magnesium dicerocene was transferred into the sampling bottle using the stainless steel sampling spoon, and the bottle cap was tightened before removing the chamber. The total weight of the sampling bottle and the magnesium dicerocene contained therein was precisely measured on an analytical balance, ensuring the magnesium dicerocene in the bottle weighed approximately 0.1 g. Then, 5% sulfuric acid solution was added dropwise to a Class 100 cleaning table to allow the reaction to proceed. After the reaction slowed, a small amount of 5% sulfuric acid solution was added to fully dissolve the sample. The solution was first heated at a low temperature, and the sample was rinsed clean from the bottle's inner wall using 5% sulfuric acid solution. The bottle was then heated to allow the reaction to proceed fully, and the acid was removed until nearly dry. The substance in the sampling bottle was then dissolved using 5% sulfuric acid solution to prepare the corresponding test solution for analysis.

[0055] The instrument used was inductively coupled plasma mass spectrometry (ICP-MS). The testing and calculation methods were the same as in Example 1. The results of three determinations of the magnesium dicerocene sample are shown in Table 3.

[0056] Table 3

[0057] impurity elements Cu(μg / g) Fe(μg / g) Mn(μg / g) Si (μg / g) Zn(μg / g) First test results ≤0.001 0.009 ≤0.001 0.013 ≤0.001 Second test results ≤0.001 0.010 ≤0.001 0.012 ≤0.001 Third test results ≤0.001 0.010 ≤0.001 0.013 ≤0.001

[0058] As shown in the table above, the method described in this embodiment yields good repeatability and stable results for the determination of trace impurities in magnesium dicerocene.

[0059] Example 4

[0060] Precisely weighed, dried sampling bottles and stainless steel sampling spoons were placed in an inert atmosphere chamber, where the oxygen content was maintained between 0.3 and 0.6 ppm. Magnesium thiocene was transferred into the sampling bottle using the stainless steel sampling spoon, and the bottle cap was tightened before removing the chamber. The total weight of the sampling bottle and the magnesium thiocene contained therein was precisely measured on an analytical balance, ensuring the magnesium thiocene in the bottle weighed approximately 0.1 g. Then, a 5% perchloric acid solution was added dropwise to a Class 100 cleaning table to allow the reaction to proceed. After the reaction slowed, a small amount of the 5% perchloric acid solution was added to fully dissolve the sample. The solution was first heated at a low temperature, and the sample was rinsed clean from the bottle's inner wall with the 5% perchloric acid solution. The bottle was then heated to allow the reaction to proceed fully, and the acid was removed until nearly dry. The substance in the sampling bottle was then dissolved in the 5% perchloric acid solution to prepare the corresponding test solution for analysis.

[0061] The instrument used was inductively coupled plasma mass spectrometry (ICP-MS). The testing and calculation methods were the same as in Example 1. The results of three determinations of the magnesium dicerocene sample are shown in Table 4.

[0062] Table 4

[0063] impurity elements Cu(μg / g) Fe(μg / g) Mn(μg / g) Si (μg / g) Zn(μg / g) First test results ≤0.001 0.012 ≤0.001 0.010 ≤0.001 Second test results ≤0.001 0.013 ≤0.001 0.011 ≤0.001 Third test results ≤0.001 0.012 ≤0.001 0.011 ≤0.001

[0064] As shown in the table above, the method described in this embodiment yields good repeatability and stable results for the determination of trace impurities in magnesium dicerocene.

[0065] Example 5

[0066] Precisely weighed, dried sampling bottles and stainless steel sampling spoons were placed in an inert atmosphere chamber, where the oxygen content was maintained between 0.3 and 0.6 ppm. Magnesium dicerocene was transferred into the sampling bottle using the stainless steel sampling spoon, and the bottle cap was tightened before removing the chamber. The total weight of the sampling bottle and the magnesium dicerocene contained therein was precisely weighed on an analytical balance, ensuring the magnesium dicerocene in the bottle weighed approximately 0.1 g. Then, 5% chloric acid solution was added dropwise to a Class 100 cleaning table to allow the reaction to proceed. After the reaction slowed, a small amount of 5% chloric acid solution was added to fully dissolve the sample. The solution was first heated at a low temperature, and the sample was rinsed clean from the bottle's inner wall with 5% chloric acid solution. The bottle was then heated to allow for a complete reaction, and the acid was removed until nearly dry. The substance in the sampling bottle was then dissolved in 5% chloric acid solution to prepare the corresponding test solution for analysis.

[0067] The instrument used was inductively coupled plasma mass spectrometry (ICP-MS). The testing and calculation methods were exactly the same as in Example 1. The results of three determinations of the magnesium dicerocene sample are shown in Table 5.

[0068] Table 5

[0069] impurity elements Cu(μg / g) Fe(μg / g) Mn(μg / g) Si (μg / g) Zn(μg / g) First test results ≤0.001 0.012 0.003 0.012 ≤0.001 Second test results ≤0.001 0.013 0.004 0.011 ≤0.001 Third test results ≤0.001 0.012 0.003 0.011 ≤0.001

[0070] As shown in the table above, the method described in this embodiment yields good repeatability and stable results for the determination of trace impurities in magnesium dicerocene.

[0071] In addition, in the implementation cases where magnesium cerene was digested using one or more of the following acids—nitric acid, hydrochloric acid, sulfuric acid, perchloric acid, chloric acid, hydrobromic acid, hydroiodic acid, perbromic acid, bromic acid, metaphosphoric acid, hydrofluoric acid, selenic acid, fluoroboric acid, fluorosulfonic acid, cyanic acid, thiocyanic acid, phosphoric acid, sulfurous acid, oxalic acid, formic acid, acetic acid, pyrophosphoric acid, trifluoroacetic acid, phosphorous acid, periodic acid, maleic acid, nitrous acid, benzoic acid, salicylic acid, tartaric acid, methanesulfonic acid, benzenesulfonic acid, and citric acid—in a dilute acid solution with a solute mass percentage of 5%, the measured trace impurity content in magnesium cerene all met the requirements and showed good repeatability.

[0072] Comparative Example

[0073] The precisely weighed dry sampling bottle and stainless steel sampling spoon were placed into the inert atmosphere operating chamber. Magnesium dicerocene was taken into the sampling bottle using the stainless steel sampling spoon, and then the bottle cap was tightened. The inert atmosphere operating chamber was then removed. The total weight of the sampling bottle and the magnesium dicerocene contained therein was accurately measured on the analytical balance, ensuring that the weight of the magnesium dicerocene in the sampling bottle was approximately 0.1 g.

[0074] Sampling rules and safety should comply with the provisions of the "General Rules for Sampling of Solid Chemical Products" (GB / T 6679) and the "General Safety Rules for Sampling of Industrial Chemical Products" (GB / T 3723). Loosen the bottle opening to allow the organometallic compounds in the bottle to oxidize naturally for 120 hours. Then, prepare the corresponding test solution using a 5% nitric acid solution for detection.

[0075] The experiment revealed three problems with this process:

[0076] 1. The decomposition reaction takes a long time, which is not conducive to the testing needs of multiple batches of production;

[0077] 2. Some organometallic sources tend to form different crystals during the slow oxidation process, which cannot be completely dissolved, causing deviations in the analytical results;

[0078] 3. The decomposition and natural oxidation of the metal-organic source in the sampling bottle may cause environmental pollution if directly discharged, requiring additional treatment of the exhaust gas.

[0079] In summary, the pretreatment method for the analysis of trace impurities in magnesium thiocene provided by this invention uses the stepwise addition of a 5% dilute acid solution to decompose the organometallic compound magnesium thiocene into soluble magnesium thiocene. This method has the advantages of simple operation, good safety, short detection time, no environmental pollution, no introduction of other trace impurities, good repeatability of analytical results, and wide applicability.

[0080] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these modifications and improvements all fall within the scope of protection of the present invention. Therefore, the scope of protection of this patent should be determined by the appended claims.

Claims

1. A pretreatment method for the analysis of trace impurities in bis-magnesocene, characterized by, The application relates to a method for preparing a sample solution of a metal organic compound, which comprises the following steps: The dry sample bottle and the sampling device are sent into an inert atmosphere operation box, the sample bottle is filled with the metal organic compound by using the sampling device, the bottle cap is screwed, the inert atmosphere operation box is taken out, and the whole operation from the sampling device to the decomposition of the metal organic compound is completed within 1 hour; The total weight of the sample bottle and the metal organic compound is accurately measured, then a 5% mass percentage acid solution is added drop by drop on a hundred-level clean bench to make the sample react, a preset amount of 5% mass percentage acid solution is added after the reaction is stable, the sample is fully dissolved, the solution is heated at a first temperature, the sample on the inner wall of the bottle is washed clean by using the 5% mass percentage acid solution, then the solution is heated at a second temperature to make the sample fully react, and the acid is removed to near dryness, the substances in the sample bottle are dissolved by using the 5% mass percentage acid solution, and the corresponding sample solution is prepared for subsequent detection, wherein the second temperature is higher than the first temperature, the acid solution is one of nitric acid, hydrochloric acid, sulfuric acid and perchloric acid, the first temperature is 50-70 DEG C, and the heating time is 15-20 min; the second temperature is 150 DEG C, and the heating time is not more than 40 min.

2. The pretreatment method for the analysis of trace impurities in bis-magnesium according to claim 1, characterized by, The sampling device is a stainless steel sampling spoon.

3. The pretreatment method for the analysis of trace impurities in bis-magnesium according to claim 1, characterized in that, The inert atmosphere operation box contains less than 1 ppm of water and less than 1 ppm of oxygen.

4. The pretreatment method for the analysis of trace impurities in dimethyl magnesium according to claim 3, characterized in that, The inert atmosphere operation box is filled with inert gas.

5. The pretreatment method for the analysis of trace impurities in bis-magnesium according to claim 1, characterized by, The inert gas is nitrogen or helium.

6. The pretreatment method for the analysis of trace impurities in bis-magnesium according to claim 1, characterized by, The weight of the metal organic compound added into the sample bottle is 0.1-0.3 g. The heating process is carried out in the hundred-level clean bench, and the gas generated during the heating process is discharged by an exhaust fan and then enters a waste gas treatment device through a pipeline.

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