A method and device for chemical analysis sample digestion without heating

Abstract

The present invention provides a method and device for digestion of chemical analysis samples without heating, and the method comprises: adding a chemical analysis sample into a container, adding a composite digestion solution into the container, and obtaining a sample mixed solution; digesting the sample mixed solution by ultrasonic wave, and then fixing the volume to obtain a sample digestion solution. The present invention causes the sample mixed solution to vibrate at a high frequency by ultrasonic wave, so that the collision frequency of the chemical analysis sample and the composite digestion solution is increased, and the reaction rate between the two is accelerated, and at the same time, the chemical analysis sample can be fully contacted with the composite digestion solution, and the digestion efficiency is improved; in addition, the sample digestion solution is digested by ultrasonic wave, and it does not need to be heated, but mechanical energy is used to digest the chemical analysis sample, and the digestion of the chemical analysis sample is realized by a heating-free method, avoiding the problem of excessive time consumption caused by heating and cooling, and the digestion time is short and the operation is simple.

Description

Technical Field

[0001] The present invention relates to the technical field of material analysis, and in particular to a method and a device for digesting a chemical analysis sample without heating. Background Art

[0002] In the process of chemical analysis of samples, sample digestion is an important part of chemical wet analysis. In the prior art, the sample needs to go through a multi-step chemical reaction to evenly dissolve the various components to be analyzed in the sample and disperse them in an acidic solution, and then use them for subsequent analysis and measurement. Among them, a part of the sample can be directly chemically hot acid digested under heating conditions in a dilute acid within a certain concentration range. The main technical process is: place the sample in a digestion container - add acidic digestion solution - heat digestion - add other reagents - complete digestion, and after digestion, further constant volume cooling is required, specifically: natural cooling or running water cooling - add other reagents - transfer to a constant volume container - transfer the container washing liquid to the constant volume container - use distilled water to make constant volume.

[0003] Common digestion methods include electric heating digestion, microwave digestion and graphite digestion. They have different heating sources, but they are all heating digestion methods. Due to the need for heating and cooling, it takes a long time and the operation is cumbersome. Heating the acid solution is also prone to reagent splashing, resulting in component contamination and even safety accidents. Summary of the invention

[0004] The problem solved by the invention is how to provide a heating-free digestion method which does not require heating, has a short digestion time and is simple to operate.

[0005] To solve at least one aspect of the above problems, the present invention provides a method for digesting a chemical analysis sample without heating, comprising the following steps:

[0006] Step S1, adding a chemical analysis sample into a container, and adding a composite digestion solution into the container to obtain a sample mixture;

[0007] Step S2, digesting the sample mixture by ultrasonic wave, and then fixing the volume to obtain a sample digestion solution.

[0008] Preferably, the chemical analysis sample includes non-ferrous metals and their alloys, steel materials, cement, metallurgical slag, metallic manganese, low-carbon ferromanganese or nickel.

[0009] Preferably, the composite digestion solution comprises at least one of hydrochloric acid, nitric acid, sulfuric acid, perchloric acid, hydrobromic acid, hydroiodic acid, citric acid, tartaric acid and hydrofluoric acid, and the composite digestion solution further comprises an organic solvent and / or water.

[0010] Preferably, in step S2, digesting the sample mixture by ultrasound includes: placing the sample mixture in an ultrasonic device, turning on the ultrasonic device and stirring to digest the sample mixture.

[0011] Preferably, in step S2, the step of adjusting the volume to obtain the sample digestion solution comprises: according to the temperature of the sample mixture, quantitatively adding a test solution of a suitable temperature so that the temperature and volume of the obtained sample digestion solution reach preset values.

[0012] The present invention obtains a sample mixed solution by mixing a chemical analysis sample and a composite digestion solution, and then causes the sample mixed solution to vibrate at a high frequency by using ultrasound, thereby increasing the collision frequency of the chemical analysis sample and the composite digestion solution and accelerating the reaction rate therebetween. At the same time, due to the high-frequency vibration of the sample mixed solution, the chemical analysis sample can be quickly diffused into the composite digestion solution, so that the chemical analysis sample and the composite digestion solution are fully in contact, thereby improving the digestion efficiency. In addition, the sample digestion solution is digested by ultrasound without heating, but mechanical energy is used to digest the chemical analysis sample. The digestion of the chemical analysis sample is achieved in a heating-free manner, thereby avoiding the problem of excessively long time consumption caused by heating and cooling, and the digestion time is short and the operation is simple.

[0013] Another object of the present invention is to provide a chemical analysis sample digestion device without heating, comprising a quantitative liquid addition module and a digestion module; wherein the quantitative liquid addition module is used to quantitatively add a test solution; and the digestion module is used to digest the sample mixture by ultrasonic wave.

[0014] Preferably, the quantitative liquid adding module comprises a constant temperature liquid storage tank, a pipette pump and a pump tube.

[0015] Preferably, the constant temperature liquid storage tank includes at least one of a low temperature liquid storage tank, a medium temperature liquid storage tank and a high temperature liquid storage tank.

[0016] Preferably, the digestion module comprises an ultrasonic generator and an energy converter.

[0017] Preferably, the chemical analysis sample heating-free digestion device also includes at least one of a sample table, a cleaning and waste liquid discharge module, and a waste gas discharge module; wherein the sample table is used to store samples to be digested; the cleaning and waste liquid discharge module is used to clean the digestion container and store waste liquid; and the waste gas discharge module is used to discharge waste gas generated during the digestion process.

[0018] Compared with the prior art, the device for digesting chemical analysis samples without heating provided by the present invention has the same beneficial effects as the method for digesting chemical analysis samples without heating, which will not be described in detail here. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1Flow chart of a method for digesting a chemical analysis sample without heating in an embodiment of the present invention;

[0020] Figure 2 It is a front view structural schematic diagram of a device for digesting chemical analysis samples without heating in an embodiment of the present invention;

[0021] Figure 3 It is a side structural schematic diagram of a device for digesting chemical analysis samples without heating in an embodiment of the present invention.

[0022] Description of reference numerals:

[0023] 1. Container storage area; 2. First pipetting pump; 3. First ultrasonic generator; 4. First energy converter; 5. First magnetic stirrer; 6. First pump tube; 7. Second pipetting pump; 8. Second pump tube; 9. Third pipetting pump; 10. Second ultrasonic generator; 11. Second magnetic stirrer; 12. Second energy converter; 13. Control panel; 14. Normal temperature liquid storage tank; 15. Waste liquid storage tank; 16. Constant temperature liquid storage tank; 17. Constant temperature liquid storage tank controller; 18. Dispensing, dilution and liquid addition tube. DETAILED DESCRIPTION

[0024] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, specific embodiments of the present invention are described in detail below.

[0025] It should be noted that, in the absence of conflict, the features in the embodiments of the present invention can be combined with each other. The meanings of the terms "comprise", "include", "contain", and "have" are non-restrictive, that is, other steps and other components that do not affect the results can be added. The above terms cover the terms "consisting of..." and "consisting essentially of...". Unless otherwise specified, materials, equipment, and reagents are all commercially available. At the same time, it should be noted that the terms "first", "second", etc. in the specification and claims of the present invention and the above-mentioned drawings are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequence. It should be understood that the data used in this way can be interchangeable where appropriate, so that the embodiments of the present invention described here can be implemented in an order other than those illustrated or described here.

[0026] The embodiment of the present invention provides a method for digestion of chemical analysis samples without heating, such as Figure 1 As shown, the following steps are included:

[0027] Step S1, adding a chemical analysis sample into a container, and adding a composite digestion solution into the container to obtain a sample mixture;

[0028] Step S2, digesting the sample mixture by ultrasonic wave, and then fixing the volume to obtain a sample digestion solution.

[0029] In step S1, the chemical analysis sample and the composite digestion solution are mixed in a container to obtain a sample mixture.

[0030] Wherein, the chemical analysis sample includes nonferrous metals and their alloys, steel materials, cement, metallurgical slag, metallic manganese, low-carbon ferromanganese or nickel. The composite digestion solution includes at least one of hydrochloric acid, nitric acid, sulfuric acid, perchloric acid, hydrobromic acid, hydroiodic acid, citric acid, tartaric acid and hydrofluoric acid, and the composite digestion solution also includes an organic solvent and / or water; the organic solvent includes at least one of liquid aromatic hydrocarbons and their derivatives, petroleum ether, liquid petroleum products, alcohols and their derivatives, and liquid hydrocarbons and their liquid hydrocarbon derivatives; in the composite digestion solution, hydrochloric acid, nitric acid, sulfuric acid, perchloric acid, hydrobromic acid, hydroiodic acid, citric acid, tartaric acid, hydrofluoric acid and organic solvent respectively occupy a mass concentration ratio of 0.01-90%, or respectively occupy a volume concentration ratio of 0.1-90%, or respectively occupy a molar concentration ratio of 0.01-15mmol.

[0031] In step S2, the sample mixture is placed in an ultrasonic device, the ultrasonic device is turned on and stirred to digest the sample mixture, and then a test solution of a suitable temperature is quantitatively added to obtain a sample digestion solution whose temperature and volume both reach preset values.

[0032] Specifically, after the ultrasonic device is turned on, the chemical analysis sample and the composite digestion solution in the sample mixture undergo high-frequency vibration, so that the two are fully in contact and the reaction rate is accelerated, replacing the heating method to achieve the purpose of accelerating the reaction, and then a test solution of suitable temperature is added quantitatively to fix the volume, so that the temperature and volume of the obtained sample digestion solution reach the preset values, and there is no need to repeatedly fix the volume and cool down, saving digestion time.

[0033] It should be understood that, depending on the different subsequent detection methods, different test solutions can be added to make up the volume, and the test solutions include water and internal standard solutions.

[0034] Exemplarily, a chemical analysis sample and 40 mL of a composite digestion solution at a temperature of 50°C are mixed in a container to obtain a sample mixture, and the sample mixture is digested by ultrasound, and then 10 mL of an internal standard solution at a temperature of 20°C and 50 mL of distilled water at a temperature of 2°C are added to obtain a sample digestion solution with a total volume of 100 mL and a temperature of 23.5°C. The temperature and volume are both preset values, avoiding repeated volume adjustment and cooling processes and saving time.

[0035] The chemical analysis sample and the composite digestion solution are mixed to obtain a sample mixed solution, and then the sample mixed solution is vibrated at high frequency by ultrasonic waves, so that the collision frequency of the chemical analysis sample and the composite digestion solution is increased, and the reaction rate between the two is accelerated. At the same time, due to the high-frequency vibration of the sample mixed solution, the chemical analysis sample can be quickly diffused into the composite digestion solution, so that the chemical analysis sample and the composite digestion solution are fully in contact, and the digestion efficiency is improved, and the digestion can be completed in 1-3 minutes. In addition, the sample digestion solution is digested by ultrasonic waves without heating it, but mechanical energy is used to digest the chemical analysis sample, and the digestion of the chemical analysis sample is achieved in a heating-free manner, avoiding the problem of excessively long time caused by heating and cooling, and the digestion time is short and the operation is simple.

[0036] Another embodiment of the present invention provides a chemical analysis sample heating-free digestion device, comprising a quantitative liquid adding module and a digestion module; wherein the quantitative liquid adding module is used to quantitatively add a test solution; and the digestion module is used to digest the sample mixture by ultrasonic wave.

[0037] The quantitative liquid adding module includes a constant temperature liquid storage tank, a transfer pump and a pump tube. The constant temperature liquid storage tank is used to store the test solution that needs to be added during the digestion process, the transfer pump is used to control the amount of test solution added, and the pump tube is used to add the test solution into the container; the constant temperature liquid storage tank includes at least one of a low temperature liquid storage tank, a medium temperature liquid storage tank and a high temperature liquid storage tank. The low temperature liquid storage tank is used to store the test solution with a temperature of -10-20°C, the medium temperature liquid storage tank is used to store the test solution with a temperature of 20-25°C, and the high temperature liquid storage tank is used to store the test solution with a temperature of 20-99°C. By quantitatively adding the test solution of appropriate temperature through the quantitative liquid adding module, the temperature and volume of the obtained sample digestion solution can reach the preset values.

[0038] The digestion module includes an ultrasonic generator and an energy converter, wherein the ultrasonic generator is a device that converts mains electricity into a high-frequency alternating current signal that matches the energy converter; and the energy converter is a device that receives the high-frequency alternating current signal generated by the ultrasonic generator and converts it into mechanical power (i.e., ultrasonic waves). The ultrasonic generator and the energy converter can cause the sample digestion solution to vibrate at a high frequency, thereby improving the digestion efficiency.

[0039] In addition, the digestion module also includes a stirring device. By the ultrasonic generator, energy converter and stirring device working simultaneously, the digestion efficiency can be further improved and the digestion time can be saved.

[0040] In addition, the chemical analysis sample heating-free digestion device also includes at least one of a sample table, a cleaning and waste liquid discharge module, and a waste gas discharge module; wherein the sample table is used to store samples to be digested; the cleaning and waste liquid discharge module is used to clean the digestion container and store waste liquid; and the waste gas discharge module is used to discharge waste gas generated during the digestion process.

[0041] For example, Figure 2 and Figure 3 As shown, the chemical analysis sample heating-free digestion device includes a container storage area 1, a first pipetting pump 2, a first ultrasonic generator 3, a first energy converter 4, a first magnetic stirrer 5, a first pump tube 6, a second pipetting pump 7, a second pump tube 8, a third pipetting pump 9, a second ultrasonic generator 10, a second magnetic stirrer 11, a second energy converter 12, a control panel 13, a room temperature liquid storage tank 14, a waste liquid storage tank 15, a constant temperature liquid storage tank 16, a constant temperature liquid storage tank controller 17 and a separation and dilution adding tube 18.

[0042] The container storage area 1 is used to store digestion containers, and the test solution can be added to the digestion container through the first pipetting pump 2; the first ultrasonic generator 3 and the second ultrasonic transmitter 10 are used to convert the mains electricity into a high-frequency AC signal that matches the energy converter, and the first energy converter 4 and the second energy converter 12 receive the high-frequency AC signal generated by the first ultrasonic generator 3 and the second ultrasonic generator 10, and convert it into mechanical power (i.e., ultrasonic wave); the first magnetic stirrer 5 and the second magnetic stirrer 11 are used to stir the sample mixture; the second pipetting pump 7 and the third pipetting pump 9 are used to quantitatively add the test solution, and the second pipetting pump 7 and the third pipetting pump 9 are connected to the constant temperature liquid storage tank 16, and the test solution stored in the constant temperature liquid storage tank 16 is quantitatively added to the digestion container through the first pump tube 6 and the second pump tube 8; the normal temperature liquid storage tank 14 is used to store the sample digestion solution, and the waste liquid storage tank 15 is used to store the waste liquid generated during the digestion process; the control panel 13 is used to control the chemical analysis sample heating-free digestion device, such as controlling the opening and closing of the ultrasonic generator and controlling the addition amount of the pipetting pump; the constant temperature liquid storage tank controller 17 is used to control the temperature of the constant temperature liquid storage tank; the dilution and liquid adding tube 18 is used to take out the sample digestion solution from the normal temperature liquid storage tank 16 and then dilute it.

[0043] It should be understood that the constant temperature liquid storage tank 16 may include multiple ones, and different temperatures can be set. When there are multiple constant temperature liquid storage tanks 16, the second pipette pump 7, the third pipette pump 9, the pump tube 6 and the pump tube 8 are also correspondingly set to multiple ones. Among them, when there are multiple first pump tubes 6 and second pump tubes 7, a collection tube method can be adopted.

[0044] When the chemical analysis sample heating-free digestion device is used for digestion, the sample is placed in the digestion container in the container storage area 1, and then the composite digestion solution is quantitatively added through the first pipetting pump 2 to obtain a sample mixed solution; the digestion container containing the chemical analysis sample and the composite digestion solution is transferred to the digestion module (i.e., the digestion tank corresponding to the first energy converter 4 and the second energy converter 12), the first ultrasonic generator 3 and the second ultrasonic generator 10 are turned on, and the first energy converter 4 and the second energy converter 12 are converted into ultrasonic waves to make the chemical analysis sample and the composite digestion solution vibrate at a high frequency, and the first magnetic stirrer 5 and the second magnetic stirrer are turned on at the same time. Stirrer 11, 1-3min to complete sample digestion; the test solution (such as internal standard solution or water) is quantitatively pumped out from the constant temperature liquid storage tank 16 by the second pipette pump 7 and the third pipette pump 9, and is added into the digestion container through the first pump tube 6 and the second pump tube 8 respectively, and mixed evenly to obtain the sample digestion solution, and the temperature of the test solution in the constant temperature liquid storage tank 16 can be controlled to make the obtained sample digestion solution reach a preset value; the sample digestion solution can be stored in the room temperature liquid storage tank 14, and if the sample digestion solution needs to be diluted, it can be diluted after being quantitatively taken out through the dilution liquid taking tube 18; during the process, the device can be controlled by the control panel 13 and the constant temperature liquid storage tank controller 17.

[0045] The present invention will be further described below in conjunction with specific examples. It should be understood that these examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention. The experimental methods in the following examples without specifying specific conditions are usually based on the conditions recommended by the manufacturer.

[0046] Example

[0047] The structure of the chemical analysis sample non-heating digestion device is as follows Figure 2 and Figure 3 As shown, the constant temperature liquid storage tank 16 includes one low-temperature liquid storage tank, one medium-temperature liquid storage tank and two high-temperature liquid storage tanks, wherein the low-temperature liquid storage tank stores distilled water at a temperature of 4°C, the medium-temperature liquid storage tank stores yttrium standard solution (0.1% yttrium nitrate solution) at a temperature of 20°C, and the two high-temperature liquid storage tanks respectively store 1+2 nitric acid (1 volume of nitric acid and 2 volumes of pure water are soluble) and 1+1 hydrochloric acid (1 volume of hydrochloric acid and 1 volume of pure water are soluble) at a temperature of 50°C; the pipetting parameters of each test solution are set, wherein 1+2 nitric acid is 20mL, 1+1 hydrochloric acid is 20mL, yttrium standard solution is 10mL, and distilled water is 50mL; the digestion sample is GSB03-1316-201 low-carbon ferromanganese, which is ground to 80 mesh before digestion.

[0048] The following steps are involved:

[0049] 1.1. Weigh 0.2g of low carbon ferromanganese sample, accurate to 0.1mg, and put it into a 250mL beaker;

[0050] 1.2. Add 20 mL of 1+2 nitric acid at 50°C to the beaker, start the magnetic stirrer and ultrasonic generator, keep for 1 min, then add 20 mL of 1+1 hydrochloric acid at 50°C and 10 mL of yttrium standard solution at 20°C, keep for 1 min;

[0051] 1.3. Add 50 mL of distilled water at 4°C to the solution in step 1.2, turn off the magnetic stirrer and ultrasonic generator to obtain the sample digestion solution, and complete the sample digestion process.

[0052] Thus, a sample digestion solution with a total volume of 100 mL and a temperature of room temperature (about 25° C.) is obtained, and multiple volume adjustment and cooling are not required.

[0053] Experimental example

[0054] The sample digestion solution obtained in the example was subjected to spectral analysis by ICP-AES, and the analysis items were silicon and phosphorus.

[0055] The analysis method is: use standard samples or reference reagents to prepare standard solutions at each mass concentration point of the ICP working curve, select appropriate analysis lines, test the standard solutions, and establish working curves for silicon and phosphorus; analyze the sample digestion solution obtained in the embodiment by ICP-AES spectroscopy, and obtain the mass fractions of silicon and phosphorus through the working curve. The obtained results are compared with the standard sample values, and the results are shown in Table 1:

[0056] Table 1 Comparison of low carbon ferromanganese analysis results and standard sample values ​​(w%)

[0057]

[0058] It can be seen from Table 1 that the analysis results of low-carbon ferromanganese obtained by the embodiment of the present invention have a lower error than the standard sample value, indicating that the method and device for chemical analysis sample digestion without heating provided by the embodiment of the present invention can ensure the digestion effect.

[0059] In summary, the method and device for digestion of chemical analysis samples without heating provided in the embodiments of the present invention can quickly complete sample digestion, have a good digestion effect, and are easy to operate.

[0060] Although the disclosure is disclosed as above, the protection scope of the disclosure is not limited thereto. Those skilled in the art may make various changes and modifications without departing from the spirit and scope of the disclosure, and these changes and modifications will fall within the protection scope of the present invention.

Claims

1. A method for digestion of chemical analysis samples without heating, characterized in that: The following steps are involved: Step S1, adding a chemical analysis sample into a container, adding a composite digestion solution into the container to obtain a sample mixture; the composite digestion solution includes at least one of hydrochloric acid, nitric acid, sulfuric acid, perchloric acid, hydrobromic acid, hydroiodic acid, citric acid, tartaric acid and hydrofluoric acid, and the composite digestion solution also includes an organic solvent and water, wherein the organic solvent includes at least one of liquid aromatic hydrocarbons and their derivatives, petroleum ether, liquid petroleum products, alcohols and their derivatives, and liquid hydrocarbons and their liquid hydrocarbon derivatives, and in the composite digestion solution, hydrochloric acid, nitric acid, sulfuric acid, perchloric acid, hydrobromic acid, hydroiodic acid, citric acid, tartaric acid, hydrofluoric acid and the organic solvent respectively account for a mass concentration ratio of 0.01-90%; the chemical analysis sample includes metallurgical slag; Step S2, digesting the sample mixture by ultrasonic wave, and then fixing the volume to obtain a sample digestion solution; The step of constant volume to obtain a sample digestion solution comprises: According to the temperature of the sample mixture, a test solution of appropriate temperature is quantitatively added so that the temperature and volume of the obtained sample digestion solution reach preset values, and the test solution includes water and internal standard solution.

2. The method for digestion of chemical analysis samples without heating according to claim 1, characterized in that: The chemical analysis samples also include non-ferrous metals and their alloys, steel materials, cement, metallic manganese, low-carbon ferromanganese or nickel.

3. The method for digestion of chemical analysis samples without heating according to claim 1, characterized in that: In the step S2, the digestion of the sample mixture by ultrasonic wave comprises: The sample mixture is placed in an ultrasonic device, which is turned on and stirred to digest the sample mixture.

4. A chemical analysis sample digestion device without heating, characterized in that: Used for performing the heating-free digestion method for chemical analysis samples as described in any one of claims 1 to 3, comprising a quantitative liquid addition module and a digestion module; Wherein, the quantitative liquid adding module is used to quantitatively add the test solution; The digestion module is used to digest the sample mixture by ultrasonic wave.

5. The chemical analysis sample non-heating digestion device according to claim 4, characterized in that: The quantitative liquid adding module comprises a constant temperature liquid storage tank, a liquid transfer pump and a pump tube.

6. The chemical analysis sample non-heating digestion device according to claim 5, characterized in that: The constant temperature liquid storage tank includes at least one of a low temperature liquid storage tank, a medium temperature liquid storage tank and a high temperature liquid storage tank.

7. The chemical analysis sample non-heating digestion device according to claim 4, characterized in that: The digestion module includes an ultrasonic generator and an energy converter.

8. The chemical analysis sample non-heating digestion device according to claim 4, characterized in that: Also includes at least one of a sample stage, a cleaning and waste liquid discharge module, and a waste gas discharge module; Wherein, the sample table is used to store samples to be digested; The cleaning and waste liquid discharge module is used to clean the digestion container and store waste liquid; The waste gas emission module is used to emit waste gas generated during the digestion process.

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