CN114778265A - Heating-free digestion method and device for chemical analysis sample - Google Patents
Heating-free digestion method and device for chemical analysis sample Download PDFInfo
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- 238000007599 discharging Methods 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 8
- 229910000616 Ferromanganese Inorganic materials 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- DALUDRGQOYMVLD-UHFFFAOYSA-N iron manganese Chemical compound [Mn].[Fe] DALUDRGQOYMVLD-UHFFFAOYSA-N 0.000 claims description 6
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 3
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Pathology (AREA)
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Abstract
The invention provides a heating-free digestion method and a heating-free digestion device for a chemical analysis sample, wherein the heating-free digestion method for the chemical analysis sample comprises the following steps: adding a chemical analysis sample into a container, and adding a composite digestion solution into the container to obtain a sample mixed solution; and digesting the sample mixed solution by ultrasonic waves, and then performing constant volume to obtain a sample digestion solution. According to the invention, the sample mixed liquid is subjected to high-frequency vibration through ultrasonic waves, so that the collision frequency of the chemical analysis sample and the composite digestion solution is improved, the reaction rate between the chemical analysis sample and the composite digestion solution is accelerated, meanwhile, the chemical analysis sample and the composite digestion solution can be fully contacted, and the digestion efficiency is improved; in addition, the sample digestion solution is digested by ultrasonic waves, the sample digestion solution does not need to be heated, but the chemical analysis sample is digested by mechanical energy, the digestion of the chemical analysis sample is realized in a heating-free mode, the problem that the temperature is raised and lowered to cause too long time is solved, the digestion time is short, and the operation is simple.
Description
Technical Field
The invention relates to the technical field of material analysis, in particular to a heating-free digestion method and a heating-free digestion device for a chemical analysis sample.
Background
In the chemical analysis process of the sample, the important ring in the chemical wet analysis is generated when the sample is digested. In the prior art, a sample needs to be subjected to multi-step chemical reaction, so that various components to be analyzed in the sample are uniformly dissolved and dispersed in an acidic solution and then used for subsequent analysis and measurement. Wherein, some samples can be directly digested by chemical hot acid under the heating condition of diluted acid with a certain concentration range, and the main technical process comprises the following steps: placing a sample in a digestion container, adding an acidic digestion solution, heating for digestion, adding other reagents to complete digestion, and further performing constant volume cooling after digestion, wherein the specific steps are as follows: natural cooling or running water cooling, adding other reagents, transferring to a constant volume container, transferring the washing liquid in the container to the constant volume container, and performing constant volume by using distilled water.
The common digestion modes comprise an electrothermal digestion method, a microwave digestion method and a graphite digestion method, wherein heating sources are different, but the heating digestion modes are adopted. The heating and cooling are needed, so that the time consumption is long, the operation is complicated, reagent splashing is easy to occur when the acid solution is heated, the component pollution is caused, and even the safety accident is caused.
Disclosure of Invention
The invention solves the problem of how to provide a heating-free digestion method which does not need heating, has short digestion time and is simple to operate.
To solve at least one of the above problems, the present invention provides a heating-free digestion method for a chemical analysis sample, comprising the steps of:
step S1, adding the chemical analysis sample into a container, and adding the composite digestion solution into the container to obtain a sample mixed solution;
and step S2, digesting the sample mixed solution through ultrasonic waves, and then performing constant volume to obtain a sample digestion solution.
Preferably, the chemical analysis sample comprises non-ferrous metals and alloys thereof, ferrous materials, cement, metallurgical slag, metallic manganese, low carbon ferromanganese or nickel.
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 further comprises an organic solvent and/or water.
Preferably, in step S2, the digesting the sample mixture by ultrasonic waves includes: and putting the sample mixed solution into an ultrasonic device, starting the ultrasonic device and stirring, and digesting the sample mixed solution.
Preferably, in step S2, the performing constant volume to obtain a sample digestion solution includes: and quantitatively adding the test solution with proper temperature according to the temperature of the sample mixed solution, so that the temperature and the volume of the obtained sample digestion solution reach preset values.
According to the invention, the chemical analysis sample and the composite digestion solution are mixed to obtain a sample mixed solution, and then the sample mixed solution is subjected to high-frequency vibration through ultrasonic waves, so that the collision frequency of the chemical analysis sample and the composite digestion solution is improved, the reaction rate between the chemical analysis sample and the composite digestion solution is accelerated, and meanwhile, the chemical analysis sample can be rapidly diffused into the composite digestion solution due to the high-frequency vibration of the sample mixed solution, so that the chemical analysis sample is fully contacted with the composite digestion solution, and the digestion efficiency is improved; in addition, the sample digestion solution is digested by ultrasonic waves, and the chemical analysis sample is digested by mechanical energy without being heated; the digestion of the chemical analysis sample is realized in a heating-free mode, the problem of long consumed time caused by temperature rise and temperature reduction is avoided, the digestion time is short, and the operation is simple.
The invention also aims to provide a chemical analysis sample heating-free digestion device, which comprises a quantitative liquid adding module and a digestion module; the quantitative liquid adding module is used for quantitatively adding a test solution; the digestion module is used for digesting the sample mixed liquid through ultrasonic waves.
Preferably, the quantitative liquid adding module comprises a constant-temperature liquid storage tank, a liquid transferring pump and a pump pipe.
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.
Preferably, the digestion module comprises an ultrasonic generator and an energy converter.
Preferably, the chemical analysis sample heating-free digestion device further comprises at least one of a sample stage, a cleaning and waste liquid discharge module and an exhaust gas discharge module; the sample table is used for storing a sample to be digested; the cleaning and waste liquid discharging module is used for cleaning the digestion container and storing waste liquid; the waste gas discharging module is used for discharging waste gas generated in the digestion process.
Compared with the prior art, the chemical analysis sample heating-free digestion device provided by the invention has the same beneficial effects as the chemical analysis sample heating-free digestion method, and is not repeated herein.
Drawings
FIG. 1 is a flow chart of a process for the heating-free digestion of a chemical analysis sample in an embodiment of the present invention;
FIG. 2 is a schematic front view of a chemical analysis sample heating-free digestion apparatus in an embodiment of the present invention;
FIG. 3 is a schematic side view of a heating-free digestion apparatus for chemical analysis samples in the embodiment of the invention.
Description of the reference numerals:
1. a container storage area; 2. a first fluid transfer pump; 3. a first ultrasonic generator; 4. a first energy converter; 5. a first magnetic stirrer; 6. a first pump tube; 7. a second liquid transfer pump; 8. a second pump tube; 9. a third liquid transfer pump; 10. a second ultrasonic generator; 11. a second magnetic stirrer; 12. a second energy converter; 13. a control panel; 14. a normal temperature liquid storage tank; 15. a waste liquid storage tank; 16. a constant temperature liquid storage tank; 17. a constant temperature reservoir controller; 18. and (4) separating and taking a dilution liquid adding pipe.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, embodiments of the present invention are described in detail below.
It should be noted that the features of the embodiments of the present invention may be combined with each other without conflict. The terms "comprising", "including", "containing" and "having" are intended to be non-limiting, i.e., that other steps and other ingredients can be added which do not affect the result. The above terms encompass the terms "consisting of … …" and "consisting essentially of … …". Materials, equipment and reagents were all commercially available unless otherwise specified. Also, it is noted that the terms "first," "second," and the like in the description and claims of the present invention and in the above-described drawings are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein.
The embodiment of the invention provides a heating-free digestion method for a chemical analysis sample, which comprises the following steps as shown in figure 1:
step S1, adding the chemical analysis sample into a container, and adding the composite digestion solution into the container to obtain a sample mixed solution;
and step S2, digesting the sample mixed solution through ultrasonic waves, and then performing constant volume to obtain a sample digestion solution.
In step S1, the chemical analysis sample and the composite digestion solution are mixed in a container to obtain a sample mixture.
Wherein, the chemical analysis sample comprises nonferrous metals and alloys thereof, steel materials, cement, metallurgical slag, metal manganese, low-carbon ferromanganese or nickel. 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 also comprises an organic solvent and/or water; the organic solvent comprises at least one of liquid aromatic hydrocarbons and derivatives thereof, petroleum ether, liquid petroleum products, alcohol and derivatives thereof, and liquid hydrocarbons and derivatives thereof; in the composite digestion solution, hydrochloric acid, nitric acid, sulfuric acid, perchloric acid, hydrobromic acid, hydroiodic acid, citric acid, tartaric acid, hydrofluoric acid and an organic solvent respectively occupy 0.01-90% of mass concentration ratio, or respectively occupy 0.1-90% of volume concentration ratio, or respectively occupy 0.01-15mmol of molar concentration ratio.
In step S2, the sample mixed solution is placed in an ultrasonic device, the ultrasonic device is started and stirred, the sample mixed solution is digested, and then a test solution with a suitable temperature is quantitatively added to obtain a sample digestion solution with a temperature and a volume both reaching preset values.
Specifically, after the ultrasonic device is started, the chemical analysis sample and the composite digestion solution in the sample mixed solution are subjected to high-frequency vibration, the chemical analysis sample and the composite digestion solution are fully contacted and the reaction rate is accelerated, the purpose of accelerating the reaction is realized by replacing a heating mode, then the test solution with proper temperature is added quantitatively to perform constant volume, the temperature and the volume of the obtained sample digestion solution reach preset values, the constant volume and the cooling are not required to be repeatedly performed, and the digestion time is saved.
It should be understood that different test solutions can be added for constant volume according to the subsequent detection mode, and the test solutions comprise water and internal standard solution.
Illustratively, a chemical analysis sample and 40mL of composite digestion solution with the temperature of 50 ℃ are mixed in a container to obtain a sample mixed solution, the sample mixed solution is digested by ultrasonic waves, then 10mL of internal standard solution with the temperature of 20 ℃ and 50mL of distilled water with the temperature of 2 ℃ are added to obtain the sample digestion solution with the total volume of 100mL and the temperature of 23.5 ℃, the temperature and the volume are preset values, the repeated volume fixing and cooling processes are avoided, and the time is saved.
The chemical analysis sample and the composite digestion solution are mixed to obtain a sample mixed solution, and then the sample mixed solution is subjected to high-frequency vibration through ultrasonic waves, so that the collision frequency of the chemical analysis sample and the composite digestion solution is improved, the reaction rate between the chemical analysis sample and the composite digestion solution is accelerated, meanwhile, the chemical analysis sample can be rapidly diffused into the composite digestion solution due to the high-frequency vibration of the sample mixed solution, the chemical analysis sample is fully contacted with the composite digestion solution, the digestion efficiency is improved, and digestion can be completed within 1-3 min; in addition, the sample digestion solution is digested by ultrasonic waves, the sample digestion solution does not need to be heated, but the chemical analysis sample is digested by mechanical energy, the digestion of the chemical analysis sample is realized in a heating-free mode, the problem that the time consumption is too long due to temperature rise and temperature reduction is avoided, the digestion time is short, and the operation is simple.
The invention provides a chemical analysis sample heating-free digestion device, which comprises a quantitative liquid adding module and a digestion module, wherein the quantitative liquid adding module comprises a liquid inlet, a liquid outlet and a liquid outlet; the quantitative liquid adding module is used for quantitatively adding a test solution; the digestion module is used for digesting the sample mixed liquid through ultrasonic waves.
The quantitative liquid adding module comprises a constant-temperature liquid storage tank, a liquid transfer pump and a pump pipe, wherein the constant-temperature liquid storage tank is used for storing a test solution to be added in the digestion process, the liquid transfer pump is used for controlling the adding amount of the test solution, and the pump pipe is used for adding the test solution into a container; the constant-temperature liquid storage tank comprises 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 for storing the test solution with the temperature of-10-20 ℃, the medium-temperature liquid storage tank is used for storing the test solution with the temperature of 20-25 ℃, the high-temperature liquid storage tank is used for storing the test solution with the temperature of 20-99 ℃, and the quantitative liquid adding module is used for quantitatively adding the test solution with the proper temperature, so that the temperature and the volume of the obtained sample digestion solution can both reach preset values.
The digestion module comprises an ultrasonic generator and an energy converter, wherein the ultrasonic generator is a device for converting commercial power into a high-frequency alternating current signal matched with the energy converter; the energy converter is a device for receiving the high-frequency alternating current signal generated by the ultrasonic generator and converting the high-frequency alternating current signal into mechanical power (namely ultrasonic waves), and the sample digestion solution can be subjected to high-frequency vibration through the ultrasonic generator and the energy converter, so that the digestion efficiency is improved.
In addition, the digestion module also comprises a stirring device, and the ultrasonic generator, the energy converter and the stirring device work simultaneously, so that the digestion efficiency can be further improved, and the digestion time can be saved.
In addition, the heating-free digestion device for the chemical analysis sample further comprises at least one of a sample stage, a cleaning and waste liquid discharge module and an exhaust gas discharge module; the sample table is used for storing a sample to be digested; the cleaning and waste liquid discharging module is used for cleaning the digestion container and storing waste liquid; the waste gas discharging module is used for discharging waste gas generated in the digestion process.
Illustratively, as shown in fig. 2 and 3, the chemical analysis sample non-heating digestion apparatus 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 dispensing dilution liquid feeding tube 18.
The container storage area 1 is used for storing digestion containers, and a test solution can be added into the digestion containers through a first liquid transfer pump 2; the first ultrasonic generator 3 and the second ultrasonic transmitter 10 are used for converting the commercial power into a high-frequency alternating current signal matched with the energy converter, and the first energy converter 4 and the second energy converter 12 receive the high-frequency alternating current signal generated by the first ultrasonic generator 3 and the second ultrasonic transmitter 10 and convert the high-frequency alternating current signal into mechanical power (namely ultrasonic waves); the first magnetic stirrer 5 and the second magnetic stirrer 11 are used for stirring the sample mixed liquid; the second liquid transferring pump 7 and the third liquid transferring pump 9 are used for quantitatively adding test liquid, the second liquid transferring pump 7 and the third liquid transferring pump 9 are connected with the constant-temperature liquid storage tank 16, and the test liquid stored in the constant-temperature liquid storage tank 16 is quantitatively added into the digestion container through the first pump pipe 6 and the second pump pipe 8; the normal-temperature liquid storage tank 14 is used for storing sample digestion liquid, and the waste liquid storage tank 15 is used for storing waste liquid generated in the digestion process; the control panel 13 is used for controlling the chemical analysis sample heating-free digestion device, such as controlling the on and off of the ultrasonic generator and controlling the adding amount of the liquid-moving pump; the constant-temperature liquid storage tank controller 17 is used for controlling the temperature of the constant-temperature liquid storage tank; the separate dilution liquid adding pipe 18 is used for taking out the sample digestion liquid from the normal-temperature liquid storage tank 16 and then diluting.
It should be understood that the constant temperature tank 16 may include a plurality of tanks and different temperatures can be set, and when the constant temperature tank 16 is a plurality of tanks, the second liquid-displacement pump 7, the third liquid-displacement pump 9, the pump tube 6, and the pump tube 8 are correspondingly provided in a plurality, wherein when the first pump tube 6 and the second pump tube 7 are a plurality, a manifold form may be adopted.
When the chemical analysis sample heating-free digestion device is used for digestion, a sample is placed into a digestion container in a container storage area 1, and then a composite digestion solution is quantitatively added through a first liquid transfer pump 2 to obtain a sample mixed solution; transferring a digestion container containing a chemical analysis sample and a composite digestion solution into a digestion module (namely, digestion tanks corresponding to a first energy converter 4 and a second energy converter 12), starting a first ultrasonic generator 3 and a second ultrasonic generator 10, converting the first energy converter 4 and the second energy converter 12 into ultrasonic waves, vibrating the chemical analysis sample and the composite digestion solution at high frequency, starting a first magnetic stirrer 5 and a second magnetic stirrer 11 at the same time, and completing sample digestion within 1-3 min; quantitatively pumping out a test solution (such as an internal standard solution or water) from the constant-temperature liquid storage tank 16 through a second liquid transfer pump 7 and a third liquid transfer pump 9, adding the test solution and the internal standard solution into a digestion container through a first pump pipe 6 and a second pump pipe 8 respectively, uniformly mixing to obtain a sample digestion solution, and controlling the temperature of the test solution in the constant-temperature liquid storage tank 16 to enable the obtained sample digestion solution to reach a preset value; the sample digestion solution can be stored in the normal-temperature liquid storage tank 14, and if the sample digestion solution needs to be diluted, the sample digestion solution can be quantitatively taken out through the branch dilution liquid taking pipe 18 and then diluted; the process can be controlled by the control panel 13 and the thermostatic reservoir controller 17.
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The following examples are examples of experimental procedures not specified under specific conditions, generally according to the conditions recommended by the manufacturer.
Examples
The structure of the chemical analysis sample heating-free digestion device is shown in fig. 2 and fig. 3, the constant-temperature liquid storage tank 16 comprises 1 low-temperature liquid storage tank, 1 medium-temperature liquid storage tank and 2 high-temperature liquid storage tanks, wherein the low-temperature liquid storage tank stores distilled water at the temperature of 4 ℃, the medium-temperature liquid storage tank stores yttrium standard solution (0.1% yttrium nitrate solution) at the temperature of 20 ℃, and the two high-temperature liquid storage tanks respectively store 1+2 nitric acid (1 volume of nitric acid is compatible with 2 volumes of pure water) and 1+1 hydrochloric acid (1 volume of hydrochloric acid is compatible with 1 volume of pure water) at the temperature of 50 ℃; setting the liquid transfer parameters of each test solution, wherein the volume of 1+2 nitric acid is 20mL, the volume of 1+1 hydrochloric acid is 20mL, the volume of yttrium standard solution is 10mL, and the volume of distilled water is 50 mL; the digestion sample is GSB 03-1316-.
The method comprises the following steps:
1.1, weighing 0.2g of a low-carbon ferromanganese sample, accurately measuring to 0.1mg, and putting the sample into a beaker with the capacity of 250 mL;
1.2, adding 20mL of 1+2 nitric acid with the temperature of 50 ℃ into a beaker, starting a magnetic stirrer and an ultrasonic generator, keeping for 1min, adding 20mL of 1+1 hydrochloric acid with the temperature of 50 ℃ and 10mL of yttrium standard solution with the temperature of 20 ℃ and keeping for 1 min;
1.3, continuously adding 50mL of distilled water with the temperature of 4 ℃ into the solution obtained in the step 1.2, closing the magnetic stirrer and the ultrasonic generator to obtain a sample digestion solution, and finishing the sample digestion process.
Thus, the sample digestion solution with the total volume of 100mL and the temperature of room temperature (about 25 ℃) is obtained, and multiple times of volume fixing and cooling are not needed.
Examples of the experiments
The sample digestion solution obtained in the examples was subjected to spectral analysis by ICP-AES, and analysis items were silicon and phosphorus.
The analysis method comprises the following steps: compounding standard solutions of each mass concentration point of an ICP working curve by using a standard sample or a reference reagent, selecting a proper analysis line, testing the standard solutions, and establishing a silicon and phosphorus working curve; the digestion solution obtained in the example is analyzed by ICP-AES spectrum, and the mass fractions of silicon and phosphorus are obtained by a working curve. The results obtained were compared with standard sample values and are shown in table 1:
TABLE 1 comparison of the results of the low carbon ferromanganese analysis with the values of the standard samples (w%)
As can be seen from Table 1, the error between the analysis result of the low-carbon ferromanganese detected by the embodiment of the invention and the standard sample value is low, which indicates that the digestion effect can be ensured by the chemical analysis sample heating-free digestion method and device provided by the embodiment of the invention.
In conclusion, the heating-free digestion method and digestion device for the chemical analysis sample, provided by the embodiment of the invention, can be used for rapidly completing sample digestion, and are good in digestion effect and simple to operate.
Although the present disclosure has been described above, the scope of the present disclosure is not limited thereto. Various changes and modifications may be made by those skilled in the art without departing from the spirit and scope of the disclosure, and these changes and modifications are intended to fall within the scope of the invention.
Claims (10)
1. A heating-free digestion method for a chemical analysis sample, which is characterized by comprising the following steps:
step S1, adding the chemical analysis sample into a container, and adding the composite digestion solution into the container to obtain a sample mixed solution;
and step S2, digesting the sample mixed solution through ultrasonic waves, and then performing constant volume to obtain a sample digestion solution.
2. The heating-free digestion process for chemical analysis samples according to claim 1, wherein said chemical analysis samples comprise non-ferrous metals and their alloys, ferrous materials, cement, metallurgical slag, metallic manganese, low-carbon ferromanganese or nickel.
3. The heating-free digestion method for the chemical analysis sample according to claim 1, wherein 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 further comprises an organic solvent and/or water.
4. The method for digestion-free of chemical analysis sample according to claim 1, wherein the step S2 of digesting the sample mixture by ultrasonic waves comprises:
and putting the sample mixed solution into an ultrasonic device, starting the ultrasonic device and stirring, and digesting the sample mixed solution.
5. The heating-free digestion method for chemical analysis samples as claimed in claim 1, wherein in step S2, the performing constant volume to obtain a sample digestion solution comprises:
and quantitatively adding the test solution with proper temperature according to the temperature of the sample mixed solution, so that the temperature and the volume of the obtained sample digestion solution reach preset values.
6. A heating-free digestion device for chemical analysis samples is characterized by comprising a quantitative liquid adding module and a digestion module;
the quantitative liquid adding module is used for quantitatively adding a test solution;
the digestion module is used for digesting the sample mixed liquid through ultrasonic waves.
7. The chemical analysis sample heating-free digestion apparatus as claimed in claim 6, wherein the dosing module comprises a constant temperature liquid storage tank, a liquid transfer pump and a pump pipe.
8. The chemical analysis sample heating-free digestion apparatus according to claim 7, wherein the constant temperature tank comprises at least one of a low temperature tank, a medium temperature tank, and a high temperature tank.
9. The chemical analysis sample heating-free digestion apparatus as claimed in claim 6, wherein the digestion module comprises an ultrasonic generator and an energy converter.
10. The chemical analysis sample heating-free digestion apparatus according to claim 6, further comprising at least one of a sample stage, a cleaning and waste liquid discharge module and an exhaust gas discharge module;
the sample table is used for storing a sample to be digested;
the cleaning and waste liquid discharging module is used for cleaning the digestion container and storing waste liquid;
the exhaust gas discharge module is used for discharging exhaust gas generated in the digestion process.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05333018A (en) * | 1991-08-29 | 1993-12-17 | Meidensha Corp | Quantitative analysis method of chromium in current limiting element |
| CN104374629A (en) * | 2014-11-17 | 2015-02-25 | 渤海大学 | Ultrasonic extraction method of heavy metal elements in vegetables |
| CN206146708U (en) * | 2016-11-14 | 2017-05-03 | 南京晓庄学院 | A processing apparatus before ultrasonic wave for on --spot short -term test |
| CN108584901A (en) * | 2018-05-30 | 2018-09-28 | 重庆太锦环保科技有限公司 | A method of recycling ceramic grade ferric phosphate from more metal hazardous wastes |
| CN211527983U (en) * | 2019-12-18 | 2020-09-18 | 南京云优生物科技有限公司 | Portable ultrasonic pretreatment device for rapidly detecting heavy metals on site |
| CN112729991A (en) * | 2021-01-19 | 2021-04-30 | 宁夏回族自治区食品检测研究院 | Environment-friendly pretreatment method for determining cadmium in grain processed product based on super microwave |
| CN113702149A (en) * | 2021-08-31 | 2021-11-26 | 上海屹尧仪器科技发展有限公司 | Infrared thermal imaging acid-removing constant volume method |
-
2022
- 2022-04-28 CN CN202210457791.5A patent/CN114778265A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05333018A (en) * | 1991-08-29 | 1993-12-17 | Meidensha Corp | Quantitative analysis method of chromium in current limiting element |
| CN104374629A (en) * | 2014-11-17 | 2015-02-25 | 渤海大学 | Ultrasonic extraction method of heavy metal elements in vegetables |
| CN206146708U (en) * | 2016-11-14 | 2017-05-03 | 南京晓庄学院 | A processing apparatus before ultrasonic wave for on --spot short -term test |
| CN108584901A (en) * | 2018-05-30 | 2018-09-28 | 重庆太锦环保科技有限公司 | A method of recycling ceramic grade ferric phosphate from more metal hazardous wastes |
| CN211527983U (en) * | 2019-12-18 | 2020-09-18 | 南京云优生物科技有限公司 | Portable ultrasonic pretreatment device for rapidly detecting heavy metals on site |
| CN112729991A (en) * | 2021-01-19 | 2021-04-30 | 宁夏回族自治区食品检测研究院 | Environment-friendly pretreatment method for determining cadmium in grain processed product based on super microwave |
| CN113702149A (en) * | 2021-08-31 | 2021-11-26 | 上海屹尧仪器科技发展有限公司 | Infrared thermal imaging acid-removing constant volume method |
Non-Patent Citations (3)
| Title |
|---|
| 杨海燕;朱万学;: "化学需氧量的微波消解检测技术", 石油化工腐蚀与防护, no. 06, 25 December 2014 (2014-12-25) * |
| 滕洪辉;任百祥;田雪;宋健美;黄欢;: "超声波辅助消解凯氏定氮的研究", 中国酿造, no. 24, 30 December 2008 (2008-12-30) * |
| 郭金喜;王霞;孙蕾;: "ICP-MS法和HPLC-HG-AFS法测定婴幼儿配方奶粉中硒质量浓度不确定度的比较", 中国乳品工业, no. 03, 25 March 2018 (2018-03-25) * |
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