CN108279153B - Method for digesting metal elements in soil - Google Patents
Method for digesting metal elements in soil Download PDFInfo
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- CN108279153B CN108279153B CN201810012388.5A CN201810012388A CN108279153B CN 108279153 B CN108279153 B CN 108279153B CN 201810012388 A CN201810012388 A CN 201810012388A CN 108279153 B CN108279153 B CN 108279153B
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Abstract
The invention discloses a method for digesting metal elements in soil, which comprises the steps of sample preparation, quantitative addition of sulfuric acid, quantitative addition of hydrofluoric acid and soil digestion, wherein the sulfuric acid and the hydrofluoric acid required for digestion are respectively quantitatively judged, so that the accuracy of the addition of the sulfuric acid and the hydrofluoric acid in the digestion process can be improved, the phenomenon that operators adsorb a large amount of smoke due to multiple additions caused by insufficient additions each time due to uncertain addition can be reduced, the addition of the sulfuric acid and the hydrofluoric acid is accurate, the addition of the acid can be completed at least once, and the digestion speed is high.
Description
Technical Field
The invention relates to the technical field of soil detection, in particular to a method for digesting metal elements in soil.
Background
The soil is complex in composition and structure, the soil must be digested when the content of heavy metals in the soil is tested, and the conventional digestion methods comprise wet digestion, high-pressure digestion, microwave digestion, dry ashing and the like. Each of these methods has advantages and disadvantages.
The digestion by a wet method in the national standard is as follows: wetting with water, adding 10ml hydrochloric acid, heating at low temperature on an electric heating plate in a fume hood to decompose the sample, taking down the sample to be slightly cold when the residual 3ml is evaporated, adding 5ml nitric acid, 5ml hydrofluoric acid and 3ml perchloric acid, covering, heating at medium temperature on the electric heating plate for about 1h, opening the cover, and continuously heating to remove silicon. Washing the inner wall with water, adding 1ml of nitric acid solution to dissolve residues additionally, transferring the solution into a 25ml volumetric flask, cooling, metering volume, shaking up for preparation, and generally completing the digestion process for 8-10 hours.
Nitric acid, hydrochloric acid, hydrofluoric acid and perchloric acid are decomposed to generate a large amount of acid mist in the whole experiment process, if the operation is carried out for a long time under the condition of poor ventilation conditions, the health of operators can be affected, and the inhaled acid mist can harm respiratory tracts and the health of the operators.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for digesting metal elements in soil, which can shorten the reaction time and reduce the suction of acid mist by workers so as to reduce the influence on the bodies of the workers.
The technical purpose of the invention is realized by the following technical scheme: a method for digesting metal elements in soil comprises the following detection steps:
step 1: sample preparation: collecting soil to be detected by using a soil collector, and analyzing whether the soil type belongs to sandy soil, clayey soil or loam;
step 2: placing 0.2-0.5 g of soil into a first digestion tank, adding sulfuric acid to preliminarily digest organic matters in the soil, and judging the addition amount of the sulfuric acid;
and step 3: placing 0.2-0.5 g of soil in a second digestion tank, adding hydrofluoric acid to preliminarily digest silicate in the soil, and judging the addition amount of the hydrofluoric acid;
and 4, step 4: decomposing soil, putting another 0.2-0.5 g of soil into a third digestion tank, adding the same amount of sulfuric acid in the step 2 for digestion, standing for 25min, transferring to a polytetrafluoroethylene crucible, covering and sealing, digesting for 15min in a ventilated kitchen at 150-200 ℃, cooling slightly, adding perchloric acid, fully decomposing organic matters at 200-250 ℃, and taking down for cooling slightly;
and 5: opening the cover, adding the amount of hydrofluoric acid in the step (3), heating, fully opening the cover in a ventilation kitchen at 140-180 ℃ until white smoke is emitted, and taking down the solution when the solution is steamed to the residual 1-2 ml;
step 6: adding a sulfuric acid solution into a polytetrafluoroethylene crucible, and dissolving residues at 150-200 ℃;
and 7: and (3) fixing the volume, adding the digested sample in a polytetrafluoroethylene crucible into a 100ml separating funnel, adding water to about 50ml, adding an ascorbic acid solution and a potassium iodide solution, shaking up, adding 5ml of methyl isobutyl ketone, shaking, standing for layering, and taking an organic phase for detection.
By adopting the technical scheme, after the soil is collected in the step 1, the analysis of the type of the soil is helpful for knowing the approximate range of the content of organic matters and silicates in the soil; then adding sulfuric acid into the digestion tank I in the step 2 to preliminarily determine the approximate content and usage of the sulfuric acid required in the digestion process; the operation in the step 3 can preliminarily judge the amount of hydrofluoric acid needed by the preliminary digestion process in the digestion tank II, the amount of acid mist generated in the process without heating is less, then a standard soil sample is selected in the step 3 for digestion, sulfuric acid with the same amount as that in the step 2 is added, the organic matter is carbonized under the condition of high oxidability of the sulfuric acid, then the organic matter is added into a polytetrafluoroethylene crucible, the carbonized organic matter is digested by the heating operation, and a small amount of perchloric acid is added after the digestion is carried out for 15min so that the digestion is more thorough; then, the amount of hydrofluoric acid added in the step 5 can enable silicate in the soil to be digested; the sulfuric acid solution added in the step 6 can further wash down the organic matters on the edge of the polytetrafluoroethylene crucible for further dissolution, so that the accuracy of the test structure is improved. The amount of sulphuric acid or hydrofluoric acid keeps in the state of a more accurate addition in whole process of digesting, it is longer that it needs to add the digestion time that acid oxidizing agent caused many times when having reduced the in-service use and having surveyd according to the standard, digestion time is long then can inhale a larger amount of acid mist, acid mist can influence operator health, and the addition of sulphuric acid and hydrofluoric acid of ration at first in the method of this application, follow-up in order to increase the completeness of digesting adding perchloric acid, it is shorter to digest the duration, then just can reduce the amount of the acid mist that the staff inhaled.
The invention is further configured to: no black organic matter is produced during digestion in step 2 as an end point for adding sulfuric acid.
Through the technical scheme, the addition amount of the sulfuric acid can be determined according to the amount of the carbonized black organic matters in the soil, when the black organic matters are not generated any more or the generation speed is low, the addition of the sulfuric acid is stopped at the moment, and the recorded amount of the added sulfuric acid is taken as the addition amount of the sulfuric acid, so that a large amount of acid mist is not easily generated in the process, and the process is environment-friendly.
The invention is further configured to: and 3, generating white smoke during digestion in the step 3 as an end point of adding hydrofluoric acid.
According to the technical scheme, when the adding amount of the hydrofluoric acid is judged, the generation of white smoke can be observed, and the approximate adding amount can be judged through the step.
The invention is further configured to: and 5, after hydrofluoric acid is added, shaking the polytetrafluoroethylene crucible.
Through above-mentioned technical scheme, the process of rocking can make the reaction more abundant on the one hand.
The invention is further configured to: an acid mist absorber is arranged in the ventilation kitchen.
Through the technical scheme, a large amount of acid mist can be generated in the actual digestion process, the arranged acid mist absorber can absorb a part of acid mist, the content of the acid mist in the ventilation kitchen is reduced, and the absorption amount of the acid mist of operators is reduced.
The invention is further configured to: the acid mist absorber comprises an absorption cavity, the absorption cavity comprises a net-shaped shell and a filter cloth layer arranged in the net-shaped shell, and an acid mist acid-absorbing agent is arranged in the filter cloth layer.
Through above-mentioned technical scheme, acid mist absorbent can absorb partly acid mist, reduces the existence volume of acid mist in the cavity, and the filter cloth layer can adsorb partly solid particle impurity, and the cooperation is used and can be absorbed partial acid mist.
The invention is further configured to: the acid mist acid absorbent is SDG acid gas adsorbent.
Through the technical scheme, the SDG acid gas adsorbent is a solid granular inorganic substance with a large specific surface area, and when acid gas in purified gas diffuses and moves to reach an adsorption force field on the surface of the SDG acid gas adsorbent, the acid gas is fixed on the surface of the SDG acid gas adsorbent and then chemically reacts with active ingredients in the SDG acid gas adsorbent to generate a new neutral salt substance which is stored in the structure of the SDG adsorbent.
The invention is further configured to: the bottom of the absorption cavity is provided with an alkaline solution cavity for containing alkaline solution.
Through the technical scheme, the alkali liquor contained in the alkali liquor cavity can neutralize part of acid mist which is not adsorbed by the acid mist acid absorbing agent, so that the acid mist content in the ventilation kitchen is less, and the operation is safer.
The invention is further configured to: an opening is arranged on the side wall of the alkali liquor cavity close to the upper part.
Through above-mentioned technical scheme, the open-ended setting makes things convenient for the passing through of acid mist, increases the volume of acid mist of neutralization.
In summary, compared with the prior art, the beneficial effects of the invention are as follows:
1. quantitative judgment is respectively made on the sulfuric acid and the hydrofluoric acid required by digestion in the step 2 and the step 3, so that the accuracy of the addition of the sulfuric acid and the hydrofluoric acid in the digestion process can be improved, the phenomenon that an operator adsorbs a large amount of smoke due to multiple addition caused by insufficient addition of each time due to uncertain addition can be reduced, the addition of the acid can be completed at least once due to the accurate addition of the sulfuric acid and the hydrofluoric acid, and the digestion speed is high;
2. the acid mist absorber can absorb part of acid mist, so that the concentration of the acid mist in the ventilation kitchen is reduced, and the suction amount of operators is reduced.
Drawings
Fig. 1 is a structural view of an acid mist absorber of an embodiment.
Reference numerals: 1. an acid mist absorber; 2. an absorption chamber; 3. a mesh-shaped housing; 4. a filter cloth layer; 5. an acid mist acid scavenger; 6. an alkaline liquid cavity; 61. and (4) opening.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
A method for digesting metal elements in soil comprises the following detection steps:
step 1: sample preparation: collecting soil to be detected by using a soil collector, and analyzing whether the soil type belongs to sandy soil, clayey soil or loam;
step 2: placing 0.2g of soil into a digestion tank I, adding sulfuric acid to preliminarily digest organic matters in the soil, judging the addition amount of the sulfuric acid, and taking black organic matters no longer generated during digestion as an end point of adding the sulfuric acid;
and step 3: putting 0.2g of soil into a second digestion tank, adding hydrofluoric acid to preliminarily digest silicate in the soil, judging the addition amount of the hydrofluoric acid, and taking white smoke generated during digestion as an end point for adding the hydrofluoric acid;
and 4, step 4: decomposing soil, putting another 0.2g of soil into a third digestion tank, adding the same amount of sulfuric acid in the step (2) for digestion, standing for 25min, transferring to a polytetrafluoroethylene crucible, covering and sealing, digesting for 15min at 150 ℃ in a ventilated kitchen, cooling slightly, adding perchloric acid, fully decomposing organic matters at 200 ℃, and taking down slightly to cool;
and 5: opening the cover, adding the amount of hydrofluoric acid in the step 3, heating, fully opening the cover in a ventilation kitchen at 140 ℃ until white smoke is emitted, taking down the silicon when the solution is steamed to the residual 1-2 ml, wherein the polytetrafluoroethylene crucible is required to be shaken after the hydrofluoric acid is added;
step 6: adding a sulfuric acid solution into a polytetrafluoroethylene crucible, and dissolving residues at 150 ℃;
and 7: and (3) fixing the volume, adding the digested sample in a polytetrafluoroethylene crucible into a 100ml separating funnel, adding water to about 50ml, adding an ascorbic acid solution and a potassium iodide solution, shaking up, adding 5ml of methyl isobutyl ketone, shaking, standing for layering, and taking an organic phase for detection.
By using the digestion method, the amount of the sulfuric acid and the hydrofluoric acid which are added can be more accurately and quantitatively, and the phenomenon that operators need to suck a large amount of acid mist due to the fact that the digestion time is prolonged by continuously heating caused by adding the acid oxidizing agent for many times is reduced.
As shown in fig. 1, in order to further reduce the amount of acid mist absorbed, an acid mist absorber 1 is disposed in the fume hood, the acid mist absorber 1 includes an absorption chamber 2, the absorption chamber 2 includes a mesh-shaped housing 3 and a filter cloth layer 4 disposed in the mesh-shaped housing 3, and an acid mist absorbent 5 is disposed in the filter cloth layer 4. The acid mist acid scavenger 5 is selected from SDG acid gas adsorbent. Meanwhile, the bottom of the absorption cavity 2 is provided with an alkali liquor cavity 6 for containing alkali liquor, the alkali liquor is sodium carbonate aqueous solution, and the side wall of the alkali liquor cavity 6 close to the upper part is provided with a plurality of openings 61.
The acid mist concentration in the fume hood can be reduced under the combined action of the acid mist acid absorbing agent 5 and the alkali liquor cavity 6 in the acid mist absorber 1, the operation safety is enhanced, the acid mist discharged to the atmosphere is reduced, and the influence on the environment is reduced.
Example 2
A method for digesting metal elements in soil comprises the following detection steps:
step 1: sample preparation: collecting soil to be detected by using a soil collector, and analyzing whether the soil type belongs to sandy soil, clayey soil or loam;
step 2: placing 0.3g of soil into a digestion tank I, adding sulfuric acid to preliminarily digest organic matters in the soil, judging the addition amount of the sulfuric acid, and taking black organic matters no longer generated during digestion as an end point of adding the sulfuric acid;
and step 3: putting 0.3g of soil into a second digestion tank, adding hydrofluoric acid to preliminarily digest silicate in the soil, judging the addition amount of the hydrofluoric acid, and taking white smoke generated during digestion as an end point for adding the hydrofluoric acid;
and 4, step 4: decomposing soil, putting another 0.3g of soil into a third digestion tank, adding the same amount of sulfuric acid in the step (2) for digestion, standing for 25min, transferring to a polytetrafluoroethylene crucible, covering and sealing, digesting for 15min at 160 ℃ in a ventilated kitchen, cooling slightly, adding perchloric acid, fully decomposing organic matters at 210 ℃, and taking down slightly to cool;
and 5: opening the cover, adding the amount of hydrofluoric acid in the step 3, heating, fully opening the cover in a ventilation kitchen at 150 ℃ until white smoke is emitted, taking down the silicon when the solution is steamed to the residual 1-2 ml, wherein the polytetrafluoroethylene crucible is required to be shaken after the hydrofluoric acid is added;
step 6: adding a sulfuric acid solution into a polytetrafluoroethylene crucible, and dissolving residues at 160 ℃;
and 7: and (3) fixing the volume, adding the digested sample in a polytetrafluoroethylene crucible into a 100ml separating funnel, adding water to about 50ml, adding an ascorbic acid solution and a potassium iodide solution, shaking up, adding 5ml of methyl isobutyl ketone, shaking, standing for layering, and taking an organic phase for detection.
Example 3
A method for digesting metal elements in soil comprises the following detection steps:
step 1: sample preparation: collecting soil to be detected by using a soil collector, and analyzing whether the soil type belongs to sandy soil, clayey soil or loam;
step 2: placing 0.4g of soil into a digestion tank I, adding sulfuric acid to preliminarily digest organic matters in the soil, judging the addition amount of the sulfuric acid, and taking black organic matters no longer generated during digestion as an end point of adding the sulfuric acid;
and step 3: putting 0.4g of soil into a second digestion tank, adding hydrofluoric acid to preliminarily digest silicate in the soil, judging the addition amount of the hydrofluoric acid, and taking white smoke generated during digestion as an end point for adding the hydrofluoric acid;
and 4, step 4: decomposing soil, putting another 0.4g of soil into a third digestion tank, adding the same amount of sulfuric acid in the step (2) for digestion, standing for 25min, transferring to a polytetrafluoroethylene crucible, covering and sealing, digesting for 15min at 170 ℃ in a ventilated kitchen, cooling slightly, adding perchloric acid, fully decomposing organic matters at 220 ℃, and taking down slightly to cool;
and 5: opening the cover, adding the amount of hydrofluoric acid in the step 3, heating, fully opening the cover in a ventilation kitchen at 160 ℃ until white smoke is emitted, taking down the silicon when the solution is steamed to the residual 1-2 ml, wherein the polytetrafluoroethylene crucible is required to be shaken after the hydrofluoric acid is added;
step 6: adding a sulfuric acid solution into a polytetrafluoroethylene crucible, and dissolving residues at 170 ℃;
and 7: and (3) fixing the volume, adding the digested sample in a polytetrafluoroethylene crucible into a 100ml separating funnel, adding water to about 50ml, adding an ascorbic acid solution and a potassium iodide solution, shaking up, adding 5ml of methyl isobutyl ketone, shaking, standing for layering, and taking an organic phase for detection.
Example 4
A method for digesting metal elements in soil comprises the following detection steps:
step 1: sample preparation: collecting soil to be detected by using a soil collector, and analyzing whether the soil type belongs to sandy soil, clayey soil or loam;
step 2: placing 0.5g of soil into a digestion tank I, adding sulfuric acid to preliminarily digest organic matters in the soil, judging the addition amount of the sulfuric acid, and taking black organic matters no longer generated during digestion as an end point of adding the sulfuric acid;
and step 3: putting 0.5g of soil into a second digestion tank, adding hydrofluoric acid to preliminarily digest silicate in the soil, judging the addition amount of the hydrofluoric acid, and taking white smoke generated during digestion as an end point for adding the hydrofluoric acid;
and 4, step 4: decomposing soil, putting another 0.5g of soil into a third digestion tank, adding the same amount of sulfuric acid in the step (2) for digestion, standing for 25min, transferring to a polytetrafluoroethylene crucible, covering and sealing, digesting for 15min at 180 ℃ in a ventilated kitchen, cooling slightly, adding perchloric acid, fully decomposing organic matters at 230 ℃, and taking down slightly to cool;
and 5: opening the cover, adding the amount of hydrofluoric acid in the step 3, heating, fully opening the cover in a ventilation kitchen at 160 ℃ until white smoke is emitted, taking down the silicon when the solution is steamed to the residual 1-2 ml, wherein the polytetrafluoroethylene crucible is required to be shaken after the hydrofluoric acid is added;
step 6: adding a sulfuric acid solution into a polytetrafluoroethylene crucible, and dissolving residues at 180 ℃;
and 7: and (3) fixing the volume, adding the digested sample in a polytetrafluoroethylene crucible into a 100ml separating funnel, adding water to about 50ml, adding an ascorbic acid solution and a potassium iodide solution, shaking up, adding 5ml of methyl isobutyl ketone, shaking, standing for layering, and taking an organic phase for detection.
Example 5
A method for digesting metal elements in soil comprises the following detection steps:
step 1: sample preparation: collecting soil to be detected by using a soil collector, and analyzing whether the soil type belongs to sandy soil, clayey soil or loam;
step 2: placing 0.5g of soil into a digestion tank I, adding sulfuric acid to preliminarily digest organic matters in the soil, judging the addition amount of the sulfuric acid, and taking black organic matters no longer generated during digestion as an end point of adding the sulfuric acid;
and step 3: putting 0.5g of soil into a second digestion tank, adding hydrofluoric acid to preliminarily digest silicate in the soil, judging the addition amount of the hydrofluoric acid, and taking white smoke generated during digestion as an end point for adding the hydrofluoric acid;
and 4, step 4: decomposing soil, putting another 0.5g of soil into a third digestion tank, adding the same amount of sulfuric acid in the step (2) for digestion, standing for 25min, transferring to a polytetrafluoroethylene crucible, covering and sealing, digesting for 15min at 200 ℃ in a ventilated kitchen, cooling slightly, adding perchloric acid, fully decomposing organic matters at 250 ℃, and taking down slightly to cool;
and 5: opening the cover, adding the amount of hydrofluoric acid in the step 3, heating, fully opening the cover in a ventilation kitchen at 180 ℃ until white smoke is emitted, taking down the silicon when the solution is steamed to the residual 1-2 ml, wherein the polytetrafluoroethylene crucible is required to be shaken after the hydrofluoric acid is added;
step 6: adding a sulfuric acid solution into a polytetrafluoroethylene crucible, and dissolving residues at 200 ℃;
and 7: and (3) fixing the volume, adding the digested sample in a polytetrafluoroethylene crucible into a 100ml separating funnel, adding water to about 50ml, adding an ascorbic acid solution and a potassium iodide solution, shaking up, adding 5ml of methyl isobutyl ketone, shaking, standing for layering, and taking an organic phase for detection.
The experiment time is analyzed, and the digestion time of the embodiments 1-5 is kept within 1-4 h.
The above description is intended to be illustrative of the present invention and not to limit the scope of the invention, which is defined by the claims appended hereto.
Claims (2)
1. A method for digesting metal elements in soil is characterized by comprising the following steps: the method comprises the following detection steps:
step 1: sample preparation: collecting soil to be detected by using a soil collector, and analyzing whether the soil type belongs to sandy soil, clayey soil or loam;
step 2: placing 0.2-0.5 g of soil into a first digestion tank, adding sulfuric acid to preliminarily digest organic matters in the soil, and judging the addition amount of the sulfuric acid;
and step 3: placing 0.2-0.5 g of soil in a second digestion tank, adding hydrofluoric acid to preliminarily digest silicate in the soil, and judging the addition amount of the hydrofluoric acid;
and 4, step 4: decomposing soil, putting another 0.2-0.5 g of soil into a third digestion tank, adding the same amount of sulfuric acid in the step 2 for digestion, standing for 25min, transferring to a polytetrafluoroethylene crucible, covering and sealing, digesting for 15min in a ventilated kitchen at 150-200 ℃, cooling slightly, adding perchloric acid, fully decomposing organic matters at 200-250 ℃, and taking down for cooling slightly;
and 5: opening the cover, adding the amount of hydrofluoric acid in the step (3), heating, fully opening the cover in a ventilation kitchen at 140-180 ℃ until white smoke is emitted, and taking down the solution when the solution is steamed to the residual 1-2 ml;
step 6: adding a sulfuric acid solution into a polytetrafluoroethylene crucible, and dissolving residues at 150-200 ℃;
and 7: adding the digested sample in a polytetrafluoroethylene crucible into a 100ml separating funnel, adding water to 50ml, adding an ascorbic acid solution and a potassium iodide solution, shaking up, adding 5ml of methyl isobutyl ketone, shaking, standing for layering, and taking an organic phase for detection;
an acid mist absorber (1) is arranged in the ventilation kitchen, the acid mist absorber (1) comprises an absorption cavity (2), the absorption cavity (2) comprises a net-shaped shell (3) and a filter cloth layer (4) arranged in the net-shaped shell (3), and an acid mist acid-absorbing agent (5) is arranged in the filter cloth layer (4); the acid mist acid-absorbing agent (5) selects an SDG acid gas adsorbent; the bottom of the absorption cavity (2) is provided with an alkali liquor cavity (6) for containing alkali liquor; a plurality of openings (61) are arranged on the side wall of the alkali liquor cavity (6) close to the upper part; 2, no black organic matter is generated during digestion in the step 2 and is used as a terminal point for adding sulfuric acid; and 3, generating white smoke during digestion in the step 3 as an end point of adding hydrofluoric acid.
2. The method for digesting metal elements in soil as set forth in claim 1, wherein: and 5, after hydrofluoric acid is added, shaking the polytetrafluoroethylene crucible.
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| CN113267388A (en) * | 2020-10-27 | 2021-08-17 | 水口山有色金属有限责任公司 | Rapid digestion device and rapid digestion method for lead concentrate |
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| CN101634617A (en) * | 2009-08-18 | 2010-01-27 | 广东省生态环境与土壤研究所 | Digestion method of soil metal elements |
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| CN2458064Y (en) * | 2000-11-13 | 2001-11-07 | 杨士贤 | Drying box |
| US7521249B2 (en) * | 2003-12-12 | 2009-04-21 | L'oreal | Method and composition for the preparation of a sample for analysis |
| JP5775305B2 (en) * | 2007-11-15 | 2015-09-09 | ザ ユニバーシティー オブ モンタナ | Hydroxy polyamide gel former |
| CN102279123B (en) * | 2011-06-14 | 2013-11-06 | 聚光科技(杭州)股份有限公司 | Pretreatment method and device |
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| CN101634617A (en) * | 2009-08-18 | 2010-01-27 | 广东省生态环境与土壤研究所 | Digestion method of soil metal elements |
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