CN110618020A - Method for rapidly digesting heavy metal soil sample - Google Patents
Method for rapidly digesting heavy metal soil sample Download PDFInfo
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- CN110618020A CN110618020A CN201910866428.7A CN201910866428A CN110618020A CN 110618020 A CN110618020 A CN 110618020A CN 201910866428 A CN201910866428 A CN 201910866428A CN 110618020 A CN110618020 A CN 110618020A
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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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Abstract
The invention discloses a method for rapidly digesting a heavy metal soil sample, which is prepared by uniformly mixing different acid anhydride proportions; the acid anhydride comprises the following components in parts by weight: 3 parts of hydrochloric acid, 1 part of nitric acid, 1-2 parts of hydrofluoric acid and 1-2 parts of perchloric acid. When in use, the 4 acids are mixed and stirred uniformly according to different volume ratio, and then the prepared anhydride is added in the digestion process. The medicament used by the invention is mainly analytically pure, has lower realization price, solves the problem of high acid, and is beneficial to improving digestion time and digestion efficiency in the digestion process.
Description
Technical Field
The invention relates to the technical field of sample pretreatment, in particular to a method for quickly digesting a heavy metal soil sample.
Background
The determination of the heavy metal in the soil is mainly divided into pretreatment digestion and quantitative determination, the pretreatment of the sample is a key, and different digestion modes have influence on the accuracy of the determination result. At present, the pretreatment digestion adopted by the national standard method is an electric heating plate digestion method, but the method has the disadvantages of long digestion time, high acid consumption, high blank value, volatilization of a large amount of acid in the digestion process and serious environmental pollution.
The fully automatic graphite digestion method which has appeared in recent years has gradually replaced the electric heating plate digestion method. The full-automatic graphite digestion method and the electric heating plate digestion method can accurately measure the content of heavy metals in the soil standard sample, and the two methods can be equivalently used. Meanwhile, the full-automatic graphite digestion method can process samples in large batch, greatly improves the working efficiency, reduces the human error in operation, is more favorable for ensuring the accuracy and reproducibility of the measurement result, and effectively reduces the problems generated in the process of the electric heating plate digestion method.
And (3) an electric heating plate heating digestion method: the equipment is simple, the cost is low, the consumed time is long, the operation is complicated, a large amount of generated acid mist brings harm to operators, if the manual operation is improper, the component loss is easy to cause, and particularly the Cr element is not easy to control.
A microwave digestion method comprises the following steps: the method has the advantages of high sample determination accuracy, good precision, low acid consumption, convenient operation and greatly shortened digestion time, and has the defects of still placing on an electric heating plate for heating and dispelling acid, less digestion tanks and being not suitable for analyzing mass samples.
Fully-automatic graphite digestion: the steps of adding acid, heating temperature control, cooling constant volume and the like can be completed automatically, manpower is greatly saved, the generated acid mist cannot harm operators, and the method is particularly suitable for analysis of large quantities of samples. The full-automatic graphite digestion is realized by controlling all steps by a program, so that the influence caused by improper manual operation is avoided, and the precision and the accuracy are better.
Therefore, it is necessary to find a method for rapidly digesting the heavy metal soil sample, which can solve the above problems.
Disclosure of Invention
The invention aims to: by changing the dosage and the using method of acid (hydrochloric acid, hydrofluoric acid, nitric acid and perchloric acid) in a digestion system and the soaking time of four kinds of acid before the soil standard sample is heated and digested, the precision and the accuracy of the standard soil sample containing 5 heavy metals such as copper, zinc, lead, cadmium, arsenic and the like in the digestion solution and the dosage and the time of the acid in the digestion process are analyzed and compared.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
a method for rapidly digesting a heavy metal soil sample adopts an acid anhydride, wherein the acid anhydride comprises the following raw materials in parts by weight: 3 parts of hydrochloric acid, 1 part of nitric acid, 1-2 parts of hydrofluoric acid and 1-2 parts of perchloric acid.
Furthermore, the heavy metal soil sample is a standard soil sample containing 5 kinds of heavy metal content including arsenic, cadmium, zinc, lead and copper.
Furthermore, the hydrochloric acid is of national medicine guaranteed reagent, and the concentration is more than or equal to 65%.
Further, the nitric acid is analytically pure, and the concentration of the nitric acid is more than or equal to 65 percent.
Furthermore, the hydrofluoric acid is grade-superior pure GR, and the concentration is more than or equal to 40%.
Furthermore, the perchloric acid is of high-grade purity, and the concentration of the perchloric acid is more than or equal to 70%.
Further, the method comprises the following steps:
(1) firstly, adding 3 parts of hydrochloric acid into heavy metal soil, adding nitric acid, fully stirring, observing the solution until the color of the solution is changed from light yellow to brownish red, pouring the solution into a digestion tank, covering a digestion cover to digest for 30-40min, and simultaneously heating by using an electric heating plate;
(2) taking off the cover, pickling the water drops on the cover into a digestion tank, and continuously digesting for 20-30 min;
(3) stopping heating the electric heating plate, slightly cooling, adding 1-2 parts of hydrofluoric acid, allowing acid anhydride in the solution to boil with explosion, allowing black particles to appear on the wall of the digestion tank, adding glass beads to prevent boiling with explosion, and covering a cover to continue digestion for 20-30 min;
(4) then opening the cover, transferring the cover into a polytetrafluoroethylene beaker, adding perchloric acid, and fully digesting the perchloric acid until the volume of liquid in the beaker is 1-2ml, wherein the digestion time is 30-45 min;
(5) when the liquid in the cup is 1-2ml, adding 10-15ml of ultrapure water until the liquid in the cup is completely digested, and then determining the volume;
(6) and (3) putting the sample with constant volume on a machine to measure heavy metals in copper, zinc, lead, cadmium and arsenic 5 by ICP (inductively coupled plasma).
Further, the heating temperature of the electric heating plate is 210 ℃.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
(1) the anhydride of the invention is different from other methods, and the main raw material adopted by the anhydride is analytically pure acid, so that the cost is reduced and the price is favorable.
(2) The total amount of acid used in the method is about 23-31 ml, the amount of acid is reduced, and the time is 120-175 minutes, so that the time required for digestion is reduced.
(3) The accuracy of the total amount of the heavy metal-containing soil processed by the acid anhydride and the using method can reach more than 95%.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to preferred embodiments. It should be noted, however, that the numerous details set forth in the description are merely for the purpose of providing the reader with a thorough understanding of one or more aspects of the present invention, which may be practiced without these specific details.
Example 1
The acid anhydride of the embodiment is prepared by mixing the following raw materials in parts by weight: 3 parts of hydrochloric acid, 1 part of nitric acid, 1 part of hydrofluoric acid and 1 part of perchloric acid. The hydrochloric acid is Chinese medicine superior pure, and the concentration is more than or equal to 65 percent; the nitric acid is analytically pure, and the concentration is more than or equal to 65 percent; hydrofluoric acid is superior pure GR, and the concentration is more than or equal to 40%; perchloric acid is of high-grade purity, and the concentration is more than or equal to 70%. The heavy metal soil sample is a soil standard substance containing arsenic, cadmium, zinc, lead and copper, and particularly is GBW07407 GSS-7 red soil, and the standard soil sample detection lines of the heavy metal soil sample are respectively arsenic 3.5-6.1 mu g/L, cadmium 0.06-0.1 mu g/L, zinc 131-153 mg/L, lead 11-17 mg/L and copper 91-103 mg/L.
The operation steps of this embodiment are as follows:
(1) firstly, adding 3 parts of GR hydrochloric acid which is a national medicine super grade pure;
(2) secondly, adding 1 part of analytically pure nitric acid, fully stirring and observing the solution until the color of the solution is changed from light yellow to brownish red, pouring the solution into a digestion tank, covering a digestion cover to digest for 30 minutes, and heating the solution by an electric hot plate to 210 ℃;
(3) taking down the cover, putting the water drops on the cover into a digestion tank by acid washing, and continuously digesting for 30 minutes;
(4) taking the digestion tank down from the electric hot plate, adding 1 part of high-grade pure GR hydrofluoric acid after slight cooling, observing that anhydride in the solution is likely to boil off at the time, wherein black particles appear on the wall of the digestion tank, adding 5-10 glass beads to prevent the boiling off, covering a cover to continue digestion for 30 minutes, and heating the electric hot plate to 210 ℃;
(5) then opening a cover to digest, adding 1 part of superior pure perchloric acid into a polytetrafluoroethylene beaker, and fully digesting until the volume of liquid in the beaker is 1-2mL, wherein the required time is 30 minutes;
(6) and when the residual amount of the digestion solution is 1-2mL, adding 10-15mL of ultrapure water, digesting until the liquid in the cup is completely digested, wherein the digestion time is 20 minutes, and fixing the volume after digestion is completed.
(7) And (3) putting the sample after constant volume on a machine for ICP (inductively coupled plasma) to measure 5 heavy metal elements including copper, zinc, lead, cadmium and arsenic.
Examples 2 to 7
The difference from the example 1 is that the weight parts of the raw materials of the acid anhydride are different, the heating digestion time is different, and the operation steps of the other rapid digestion methods are the same as the example 1 as shown in the table 1.
TABLE 1 quantities of the acid anhydrides and digestion times in the examples
The results of rapid digestion methods of heavy metal soil samples in examples 1 to 7 using ICP detection are shown in table 2.
Table 2 results of detection of five heavy metals in examples 1 to 7
Comparative example 1
This example differs from examples 1-7 in that the 2 acids in the anhydride are different and the procedure is the same as the inventive example and is as follows:
(1) firstly, adding 3 parts of GR hydrochloric acid which is a national medicine super grade pure;
(2) secondly, adding 1 part of analytically pure nitric acid, fully stirring and observing the solution until the color of the solution is changed from light yellow to brownish red, pouring the solution into a digestion tank, covering a digestion cover to digest for 30 minutes, and heating the solution by an electric hot plate to 210 ℃;
(3) taking down the cover, putting the water drops on the cover into a digestion tank by acid washing, and continuously digesting for 30 minutes;
(4) taking the digestion tank down from the electric hot plate, adding 1 part of high-grade pure GR concentrated sulfuric acid after slight cooling, observing that anhydride in the solution is likely to boil off, wherein black particles appear on the wall of the digestion tank, adding 5-10 glass beads to prevent the boiling off, covering a cover to continue digestion for 30 minutes, and heating the electric hot plate to 210 ℃;
(5) then opening a cover to clear up, adding 1-2 parts of high-grade pure phosphoric acid into a polytetrafluoroethylene beaker, and fully clearing up until the volume of liquid in the beaker is 1-2mL, wherein the required time is 30 minutes;
(6) and when the residual amount of the digestion solution is 1-2mL, adding 10-15mL of ultrapure water, digesting until the liquid in the cup is digested in 1-2mL for 20 minutes, and fixing the volume after digestion.
Comparative examples 2 to 7
The difference from the comparative example 1 is that the acid anhydride has 4 different acid weight parts and different heating digestion time, the details are shown in Table 3, and the fast digestion method has the same operation steps as the comparative example 1.
TABLE 3 quantities of the individual components of the acid anhydrides and digestion times in the comparative examples
The results of the detection using ICP for each of the comparative examples are shown in table 4 below.
Table 4 test results of each comparative example
In the above data, wherein:
(1) CK in tables 1, 2, 3 and 4 is a sample obtained by adding only acid anhydride and not adding a clay.
(2) As can be seen from the data in tables 1 and 2, the acid anhydride proportion in the invention is combined with the use method thereof to basically achieve the digestion effect; as can be seen from the data in tables 3 and 4, the amount of the soil standard substance was measured by replacing other acid anhydrides but not replacing the amount of the acid used, and only a few of them could reach the standard.
(3) The comparison data of the tables 1, 2 and 3 and 4 show that the method for optimizing the proportioning has shorter digestion time, and compared with other methods, the method for optimizing the proportioning has the obvious advantages of higher accuracy, shorter digestion time and less acid consumption.
The preferable proportion of the acid anhydride provided by the invention can be used for digesting the heavy metal in the soil, so that the digested soil standard sample is in a range, and the detection efficiency and accuracy are improved, and the acid consumption is reduced.
Compared with the acid anhydride shown in the embodiment 1-7, in a comparison test, only a few samples can completely digest the heavy metal of the soil standard sample, the accuracy is low, and the acid consumption and the digestion time are not as optimal as those of the acid anhydride prepared by the method disclosed by the invention.
The acid anhydrides shown in the embodiments 1 to 7 can completely digest the heavy metals of the soil standard sample to be tested in the embodiments 1 to 7, and can meet the index of the on-machine treatment after the digestion. Meanwhile, the main component of the anhydride proportion of the invention is analytically pure acid, which has wide source, low price and easy obtaining, therefore, the prepared anhydride has low cost, no secondary pollution to the environment, good digestion effect and good economic and environmental benefits.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A method for rapidly digesting a heavy metal soil sample is characterized by comprising the following steps: the rapid digestion method adopts an acid anhydride, and the acid anhydride comprises the following raw materials in parts by weight: 3 parts of hydrochloric acid, 1 part of nitric acid, 1-2 parts of hydrofluoric acid and 1-2 parts of perchloric acid.
2. The method for rapidly digesting the heavy metal soil sample according to claim 1 is characterized in that: the heavy metal soil sample is a standard soil sample containing 5 kinds of heavy metal content including arsenic, cadmium, zinc, lead and copper.
3. The method for rapidly digesting the heavy metal soil sample according to claim 1 is characterized in that: the hydrochloric acid is of national medicine top grade purity, and the concentration is more than or equal to 65%.
4. The method for rapidly digesting the heavy metal soil sample according to claim 1 is characterized in that: the nitric acid is analytically pure, and the concentration of the nitric acid is more than or equal to 65 percent.
5. The method for rapidly digesting the heavy metal soil sample according to claim 1 is characterized in that: the hydrofluoric acid is grade-superior pure GR, and the concentration is more than or equal to 40%.
6. The method for rapidly digesting the heavy metal soil sample according to claim 1 is characterized in that: the perchloric acid is of high-grade purity, and the concentration of the perchloric acid is more than or equal to 70%.
7. The method for rapidly digesting the heavy metal soil sample according to claim 1 is characterized in that: the method comprises the following steps:
(1) firstly, adding 3 parts of hydrochloric acid into heavy metal soil, adding nitric acid, fully stirring, observing the solution until the color of the solution is changed from light yellow to brownish red, pouring the solution into a digestion tank, covering a digestion cover to digest for 30-40min, and simultaneously heating by using an electric heating plate;
(2) taking off the cover, pickling the water drops on the cover into a digestion tank, and continuously digesting for 20-30 min;
(3) stopping heating the electric heating plate, slightly cooling, adding 1-2 parts of hydrofluoric acid, allowing acid anhydride in the solution to boil with explosion, allowing black particles to appear on the wall of the digestion tank, adding glass beads to prevent boiling with explosion, and covering a cover to continue digestion for 20-30 min;
(4) then opening the cover, transferring the cover into a polytetrafluoroethylene beaker, adding perchloric acid, and fully digesting the perchloric acid until the volume of liquid in the beaker is 1-2ml, wherein the digestion time is 30-45 min;
(5) when the liquid in the cup is 1-2ml, adding 10-15ml of ultrapure water until the liquid in the cup is completely digested, and then fixing the volume;
(6) and (3) putting the sample with constant volume on a machine to measure heavy metals in copper, zinc, lead, cadmium and arsenic 5 by ICP (inductively coupled plasma).
8. The method for rapidly digesting the heavy metal soil sample according to claim 7 is characterized in that: the heating temperature of the electric heating plate is 210 ℃.
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| CN111650268A (en) * | 2020-07-08 | 2020-09-11 | 刘琳娟 | Adsorption stripping voltammetry for measuring chromium and nickel in seawater |
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| CN112730489A (en) * | 2020-11-09 | 2021-04-30 | 安徽皖仪科技股份有限公司 | Preparation method of standard sample of atmospheric particulates |
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Application publication date: 20191227 |