CN104374629A - Ultrasonic extraction method of heavy metal elements in vegetables - Google Patents
Ultrasonic extraction method of heavy metal elements in vegetables Download PDFInfo
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Abstract
The invention discloses an ultrasonic extraction method of heavy metal elements in vegetables. The ultrasonic extraction method comprises the following steps: firstly, rinsing a sample thoroughly with water, next, washing with distilled water and deionized water, air-drying, weighing, drying in a drying oven, homogenizing the dried sample by use of agate mortar, sieving, and preserving in a dryer at normal temperature in a polyethylene bottle for later use; weighing 0.1g of the treated vegetable sample and putting the sample into a centrifugal tube, adding an acidic extracting agent, putting into ultrasonic bath for ultrasonic extraction, centrifuging and separating out the supernatant; cleaning the residue by use of ultrapure water before ultrasonic extraction and centrifuging, also taking the supernatant for blending with the acid extract, preserving in the polyethylene bottle at 4 DEG C for later use after the volume is constant, and then measuring the content of each element of Cd, Cr, Ni, Pb and Zn by virtue of atomic absorption spectrophotometry. According to the ultrasonic extraction method of heavy metal elements in vegetables, a pretreatment method for ultrasonically extracting heavy metal elements in vegetables is established and has the advantages of simplicity and quickness, high recovery rate, good safety, low pollution, low reagent consumption, low residue and the like.
Description
Technical field
The present invention relates to heavy metal pre-treating method technical field, particularly relate to the ultrasonic extracting method of Cadmium in Vegetables, chromium, nickel, lead, zinc five Heavy Metallic Elements.
Background technology
Assay method such as atomic absorption spectrography (AAS), ICP-AES, the inductively coupled plasma mass spectrometry etc. of heavy metal element require solid sample to clear up usually, and the normal digestion procedure adopted has dry ashing method, Wet digestion, Microwave Digestion etc.But dry ashing method is consuming time longer, usually needs 6 ~ 14h, and also relatively stricter to the requirement of ashing temperature, ashing temperature is too low, and organism can not be completely broken down, and ashing temperature is too high, then easily cause the loss of element to be measured; Wet digestion carries out usually on hot plate, batch samples can be cleared up simultaneously, but in digestion process, in order to complete decomposing organic matter, the red fuming nitric acid (RFNA) that many uses are a large amount of and perchloric acid, reaction is relatively more violent, and security is poor, and clears up the unlimited system of many employings, lose larger, blank value is higher, and precision is poor, and can produce NO in digestion process
2deng toxic gas, environmental pollution is serious; Microwave Digestion to utilize in test solution charged particle at the elect magnetic field travel motion back and forth of alternation, specimen temperature is raised, sample and solvent react under high heat effect, generation gas forms high pressure thus reaches in airtight cup to be cleared up completely, Microwave Digestion speed, is generally no more than 30min; Arrange clear up program under, service condition is consistent, therefore be disturbed less in digestion process, blank value is little, in high-pressure sealed environment, loss is few, be specially adapted to volatile sample or element, have in addition solvent load few, pollute little and precision advantages of higher, but shortcoming be Microwave Digestion require High Temperature High Pressure, reaction is violent, and security is not high.Therefore the present invention proposes one and can solve length consuming time in above-mentioned general digestion method, require concentrated acid, high temperature, high pressure, the shortcomings such as reaction is violent, pollution is large, poor stability, establish a kind of pre-treating method of ultrasonic extraction Heavy Metals In Vegetables element, reach easy fast, the recovery compared with high, security better, pollute little, reagent consumption less, the pre-treatment object such as residue is few.
The mechanical effect that ultrasonic wave extraction utilizes ultrasound wave to have, cavitation effect and thermal effect, by the strong cavitation, mechanical agitation, the emulsification that produce, spread, smash, the multistage effect such as chemical effect, increase molecular motion of material frequency and speed, strengthen solvent penetration power, accelerate target component enter solvent, therefore ultrasonic as a kind of auxiliary energy can shorten the running time and improve extraction ratio.Ultrasound wave is extracted in the aspects such as the extraction of Chinese crude drug and animals and plants effective constituent and has a wide range of applications, but application in food in landfill is less.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the invention provides a kind of ultrasonic extracting method of Heavy Metals In Vegetables element.
The technical solution adopted in the present invention is:
A kind of ultrasonic extracting method of Heavy Metals In Vegetables element.It is characterized in that:
(1) preparation of sample: get vegetable sample, get edible portion, first clean with running water, then use distilled water, washed with de-ionized water, air-dry, weigh, put baking oven 60 DEG C of dry 72h, dry sample agate mortar is homogeneous, sieves, saves backup under room temperature;
(2) content of Cd, Cr, Ni, Pb, Zn in sample is tested out,
(3) ultrasonic extraction: take sample in centrifuge tube, solubilizer 65%HNO
3-30%H
2o
2(2:1, V/V), put into ultrasonic 20min at ultra sonic bath 70 DEG C, the addition of solvent needs solvent 5 ~ 10mL according to the every 0.02 μ g of Cd, and the every 0.3 μ g of Cr needs the every 0.2 μ g of solvent 5 ~ 10mL, Ni to need the every 2 μ g of solvent 5 ~ 10mL, Pb to need the every 5 μ g of solvent 5 ~ 10mL and Zn to need solvent 5 ~ 10mL; With 4500r min
-1centrifugal 5min, gets upper strata acid leaching liquor; Ultrasonic 2min again after residue cleaning, with 4500r min
-1centrifugal 5min, gets supernatant liquor and merges with acid leaching liquor.
More specifically:
(1) preparation of sample: get vegetable sample, get edible portion (stalk, core etc.), first clean with running water, use distilled water, washed with de-ionized water again, air-dry, weigh, put baking oven 60 DEG C of dry 72h, dry sample agate mortar is homogeneous, sieves, saves backup in polyethylene bottle under room temperature in exsiccator;
(2) selection of ultrasonic time: take sample in centrifuge tube, solubilizer 65%HNO
3-30%H
2o
2(2:1, V/V), puts into ultra sonic bath, ultrasonic 5 under room temperature, 10,15,20,25,30min, with 4500r min
-1centrifugal 5min, gets upper strata acid leaching liquor; Residue 2mL ultrapure water cleaning, more ultrasonic 2min, with 4500r min
-1centrifugal 5min, gets supernatant liquor and merges with acid leaching liquor, being finally settled to 10mL, and in polyethylene bottle, 4 DEG C save backup, and do blank test simultaneously; Measure the content of Cd, Cr, Ni, Pb, Zn in the ultrasonic extract of said extracted with atomic absorption spectrophotometer (AAS), instrument condition of work is in table 1 and table 2.The impact of ultrasonic time heavy metal concentration as shown in Figure 1; Detect metallic element extracted amount increase along with the increase of ultrasonic time, when ultrasonic time reaches 20min, Cd, Cr, Pb and Zn all reach maximum extracted amount, then increase ultrasonic time to metallic element extraction ratio without impact;
(3) selection of ultrasonic temperature: take sample in centrifuge tube, solubilizer 65%HNO
3-30%H
2o
2(2:1, V/V), puts into ultra sonic bath, respectively ultrasonic 20min at 30,40,50,60,70,80 DEG C, with 4500r min
-1centrifugal 5min, gets upper strata acid leaching liquor; Residue 2mL ultrapure water cleaning, more ultrasonic 2min, with 4500r min
-1centrifugal 5min, gets supernatant liquor and merges with acid leaching liquor, being finally settled to 10mL, and in polyethylene bottle, 4 DEG C save backup, and do blank test simultaneously; Measure the content of Cd, Cr, Ni, Pb, Zn in the ultrasonic extract of said extracted with atomic absorption spectrophotometer (AAS), instrument condition of work is in table 1 and table 2.The impact of ultrasonic temperature heavy metal concentration as shown in Figure 2; Fluid temperature is higher, more favourable to the generation of cavitation, but when temperature is too high, in microbubble, surface tension reduces, and vapour pressure increases, and then enhances buffer action and cavitation is weakened when causing bubble to close.When ultrasonic temperature is all reached maximum extracted amount by detecting metallic element when 70 DEG C;
(4) selection of solvent: take sample in centrifuge tube, adds different solvents 36%HCl, 36%HCl-65%HNO respectively
3(3:1, V/V) and 65%HNO
3-30%H
2o
2(2:1, V/V), puts into ultra sonic bath, respectively ultrasonic 20min at 70 DEG C, with 4500r min
-1centrifugal 5min, gets upper strata acid leaching liquor; Residue 2mL ultrapure water cleaning, more ultrasonic 2min, with 4500r min
-1centrifugal 5min, gets supernatant liquor and merges with acid leaching liquor, being finally settled to 10mL, and in polyethylene bottle, 4 DEG C save backup, and do blank test simultaneously; Measure the content of Cd, Cr, Ni, Pb, Zn in the ultrasonic extract of said extracted with atomic absorption spectrophotometer (AAS), instrument condition of work is in table 1 and table 2.The impact of solvent kind heavy metal concentration as shown in Figure 3; Different solvents is different on extract impact of different nature, and sample is after HCl process, and metallic element extracted amount is lower, and the organism in interpret sample can not, by HCl complete oxidation, need oxygenant as H usually
2o
2and HNO
3deng.65%HNO
3-30%H
2o
2(2:1, V/V) all detection elements can be extracted and extracted amount is the highest;
(5) selection of solvent volume: take sample in centrifuge tube, add 1 respectively, 3,5,7, the solvent 65%HNO of 9mL
3-30%H
2o
2(2:1, V/V), puts into ultra sonic bath, respectively ultrasonic 20min at 70 DEG C, with 4500r min
-1centrifugal 5min, gets upper strata acid leaching liquor; Residue 2mL ultrapure water cleaning, more ultrasonic 2min, with 4500r min
-1centrifugal 5min, gets supernatant liquor and merges with acid leaching liquor, being finally settled to 10mL, and in polyethylene bottle, 4 DEG C save backup, and do blank test simultaneously; Measure the content of Cd, Cr, Ni, Pb, Zn in the ultrasonic extract of said extracted with atomic absorption spectrophotometer (AAS), instrument condition of work is in table 1 and table 2.The impact of solvent volume heavy metal concentration as shown in Figure 4; Solvent load is excessive, and can increase cost, even cause waste, solvent load is very few, and element extraction is incomplete, affects extraction ratio; Therefore need to select suitable solvent and consumption, to raise the efficiency, to reduce costs.When reaching maximum extracted amount, each element at least needs solvent load to be 5 ~ 10mL;
(6) selection of amount of samples: take respectively sample 0.05,0.10,0.15,0.20,0.25,0.30g in centrifuge tube, add 5mL 65%HNO
3-30%H
2o
2(2:1, V/V), puts into ultra sonic bath, respectively ultrasonic 20min at 70 DEG C, with 4500r min
-1centrifugal 5min, gets upper strata acid leaching liquor; Residue 2mL ultrapure water cleaning, more ultrasonic 2min, with 4500r min
-1centrifugal 5min, gets supernatant liquor and merges with acid leaching liquor, being finally settled to 10mL, and in polyethylene bottle, 4 DEG C save backup, and do blank test simultaneously; Measure the content of Cd, Cr, Ni, Pb, Zn in the ultrasonic extract of said extracted with atomic absorption spectrophotometer (AAS), instrument condition of work is in table 1 and table 2.The impact of sample size heavy metal concentration as shown in Figure 5; For the solvent of certain volume, can be limited by the amount of element of ultrasonic extraction, when sample size Cr is greater than 0.2g in this experiment, when Cd, Pb, Ni and Zn are greater than 0.15g, the extracted amount of each element obviously reduces;
(7) selection of particle diameter: by homogeneous for the sample agate mortar of drying, cross 200 orders (74 μm), 100 orders (150 μm) and 50 orders (280 μm) sieve, take above-mentioned different-grain diameter sample 0.1g respectively in centrifuge tube, add 5mL65%HNO
3-30%H
2o
2(2:1, V/V), puts into ultra sonic bath, respectively ultrasonic 20min at 70 DEG C, with 4500r min
-1centrifugal 5min, gets upper strata acid leaching liquor; Residue 2mL ultrapure water cleaning, more ultrasonic 2min, with 4500r min
-1centrifugal 5min, gets supernatant liquor and merges with acid leaching liquor, being finally settled to 10mL, and in polyethylene bottle, 4 DEG C save backup, and do blank test simultaneously; Measure the content of Cd, Cr, Ni, Pb, Zn in the ultrasonic extract of said extracted with atomic absorption spectrophotometer (AAS), instrument condition of work is in table 1 and table 2.The impact of particle diameter heavy metal concentration as shown in Figure 6; Particle diameter is one of key factor affecting ultrasonic extraction efficiency, increase the contact area between element and solvent, object transfers to liquid phase mass transfer rate from solid phase can be improved, be conducive to the ultrasonic extraction of heavy metal element, in this experiment, institute's detection elements is as particle diameter > 74 μm, and the extracted amount of 4 kinds of metallic elements all reduces.
Compared with the pre-treating methods such as existing Wet digestion, dry ashing method and Microwave Digestion, the advantage that the present invention has is:
The strong cavitation that ultrasonic wave extraction utilizes Ultrasonic Radiation pressure to produce, mechanical agitation, emulsification, spread, the multistage effect such as to smash, increase molecular motion of material frequency and speed, strengthen solvent penetration power, accelerate target component and enter solvent, therefore ultrasonic as a kind of auxiliary energy can shorten the running time and improve extraction ratio, be a kind of pre-treating method be worthy to be popularized.
(1) the ultrasonic extraction pre-treatment time is faster, shortens charing in dry ashing method, heating, drying, cools the time with steps such as being separated;
(2) ultrasonic extraction reagent dosage is few, residue is few, it is little to pollute, and reduces the consumption of concentrated acid in Wet digestion and the discharge of poisonous and harmful and corrosive gas;
(3) the more gentle safety of ultrasonic extraction reaction, avoids the process of Microwave Digestion High Temperature High Pressure.
Accompanying drawing explanation
Fig. 1 is the impact of ultrasonic time on Heavy Metals In Vegetables element extraction rate.On curve, often represents the mean value of 6 parallel determinations, and in order to react the Changing Pattern of often kind of element on a figure clearly, the measurement result of Zn and Pb reduces 1/10 process (as figure indicates).
Fig. 2 is the impact of ultrasonic water bath temperature on Heavy Metals In Vegetables element extraction rate.
Fig. 3 is the impact of solvent on Heavy Metals In Vegetables element extraction rate.
Fig. 4 is the impact of solvent load on Heavy Metals In Vegetables element extraction rate.
Fig. 5 is the impact of sample size on Heavy Metals In Vegetables element extraction rate.
Fig. 6 is the impact of particle diameter on Heavy Metals In Vegetables element extraction rate.
Embodiment
Below in conjunction with accompanying drawing the present invention is further described our bright method.
36% hydrochloric acid, 65% nitric acid, 70% perchloric acid that the present invention adopts, that 30% hydrogen peroxide is top grade is pure.
The cadmium that the present invention adopts, chromium, nickel, lead, Zinc standard solution (1000 μ g/mL) are bought from China National Measuring Science Research Inst..
Accepted standard product of the present invention are GBW10015 spinach.
The glass that the present invention adopts and tygon instrument all use salpeter solution (1+9) to soak 24h, and secondary deionized water is rinsed, and dries rear for subsequent use.
The extraction of heavy metal element of the invention process adopts KQ100DB type ultrasonic cleaner (temperature 30 ~ 80 DEG C, frequency 40kHz, electric power 100W, volume 4L) (Kunshan Ultrasonic Instruments Co., Ltd.).
The detection of heavy metal element of the invention process adopts AA320N atomic absorption spectrophotometer (AAS) and GA 3202 graphite furnace system (Shanghai Precision Scientific Apparatus Co., Ltd).
Embodiment 1:
(1) GBW10015 spinach is got, first clean with running water, use distilled water, washed with de-ionized water again, air-dry, weigh, put baking oven 60 DEG C of dry 72h, dry sample agate mortar is homogeneous, cross 200 orders (74 μm) sieve, save backup in exsiccator under room temperature in polyethylene bottle.
(2) Wet digestion: take sample 1.0g in high pin beaker, put several beaded glasses, add 10mL65%HNO
3-70%HClO
4(9:1, V/V) adds a cover soaked overnight, heating and decompose on electric hot plate, if change brownish black, then add acid mixture, until Mao Baiyan, until digestive juice is water white transparency or yellowish, by near for excessive acid evaporation dry, cooling, washes in 25mL volumetric flask with dropper by digestive juice, high pin beaker is repeatedly washed with a small amount of water, washing lotion to be incorporated in volumetric flask and to be settled to scale, mixes for subsequent use, does blank test simultaneously.
(3) ultrasonic extraction: take sample 0.1g in centrifuge tube, add 5mL 65%HNO
3-30%H
2o
2(2:1, V/V), puts into ultra sonic bath, and 70 DEG C of ultrasonic 20min, with 4500r min
-1centrifugal 5min, gets upper strata acid leaching liquor; Residue 2mL ultrapure water cleaning, more ultrasonic 2min, with 4500r min
-1centrifugal 5min, gets supernatant liquor and merges with acid leaching liquor, being finally settled to 10mL, and in polyethylene bottle, 4 DEG C save backup, and do blank test simultaneously.
(4) measure the content of Cd, Cr, Ni, Pb, Zn in Wet liquid and ultrasonic extract with atomic absorption spectrophotometer (AAS), condition of work is in table 1 and table 2, and experimental result is in table 3.Ultrasonic extraction reagent dosage is few, residue is few, it is little to pollute, and reduces the consumption of concentrated acid in Wet digestion and the discharge of poisonous and harmful and corrosive gas.
Embodiment 2:
(1) spinach is got, first clean with running water, then use distilled water, washed with de-ionized water, air-dry, weigh, put baking oven 70 DEG C of dry 48h, dry sample agate mortar is homogeneous, crosses 150 orders (104 μm) sieve, saves backup in polyethylene bottle under room temperature in exsiccator.
(2) dry ashing: take sample 1.0g in porcelain crucible, add 1mL phosphoric acid (1+10), soak more than 1h, crucible is placed on heating plate, little live charcoalization moves in muffle furnace after smokeless, 500 ± 25 DEG C of ashing are about 8h, be greyish white shape to sample, taking-up lets cool, add a small amount of hydrochloric acid (1+11) again, little fire heating, do not make to dry up, add a little acid mixture if desired, so repeatedly process, until without carbon granule in residue, 10mL hydrochloric acid (1+11) is added after slightly cold, dissolved residue also moves in 10mL volumetric flask, use hydrochloric acid (1+11) cyclic washing crucible again, washing lotion is incorporated in volumetric flask, and be diluted to scale, mix for subsequent use, do blank test simultaneously.
(3) ultrasonic extraction: take sample 0.15g in beaker, add 7mL 65%HNO
3-30%H
2o
2(2:1, V/V), puts into ultra sonic bath, and 70 DEG C of ultrasonic 25min, with 3000r min
-1centrifugal 10min, gets upper strata acid leaching liquor; Residue 2mL ultrapure water cleaning, more ultrasonic 2min, with 3000r min
-1centrifugal 10min, gets supernatant liquor and merges with acid leaching liquor, being finally settled to 10mL, and in polyethylene bottle, 4 DEG C save backup, and do blank test simultaneously.
(4) measure the content of Cd, Cr, Ni, Pb, Zn in dry method digestion solution and ultrasonic extract with atomic absorption spectrophotometer (AAS), condition of work is in table 1 and table 2, and experimental result is in table 4.The ultrasonic extraction pre-treatment time is faster, shortens charing in dry ashing method, heating, drying, cools the time with steps such as being separated.
Embodiment 3:
(1) celery, Chinese cabbage, leek and garlic bolt sample is got, first clean with running water, use distilled water, washed with de-ionized water again, air-dry, weigh, put baking oven 65 DEG C of dry 60h, dry sample agate mortar is homogeneous, cross 170 orders (88 μm) sieve, save backup in exsiccator under room temperature in polyethylene bottle.
(2) Microwave Digestion: take sample 0.5g in teflon counteracting tank, adds 5mL65% nitric acid and 1mL 30% hydrogen peroxide, is placed in microwave eliminating device, clears up according to program: 0.2MPa, 2min; 0.5MPa, 2min; 1.0MPa, 2min; 1.5MPa, 5min; 2.0MPa, 5min; Cooling 10min.Be cooled to room temperature after having cleared up, electric hot plate be heated near dry, after cooling by solution constant volume in 50 ~ 100mL volumetric flask.Do blank test simultaneously.
(3) ultrasonic extraction: take sample 0.1g in beaker, add 20mL 65%HNO
3-30%H
2o
2(2:1, V/V), puts into ultra sonic bath, and 70 DEG C of ultrasonic 30min, with 4000r min
-1centrifugal 8min, gets upper strata acid leaching liquor; Residue 2mL ultrapure water cleaning, more ultrasonic 2min, with 4000r min
-1centrifugal 8min, gets supernatant liquor and merges with acid leaching liquor, being finally settled to 10mL, and in polyethylene bottle, 4 DEG C save backup, and do blank test simultaneously.
(4) measure the content of Cd, Cr, Ni, Pb, Zn in ultrasonic extract and micro-wave digestion liquid with atomic absorption spectrophotometer (AAS), condition of work is in table 1 and table 2.Experimental result is in table 5.The more gentle safety of ultrasonic extraction reaction, avoids the process of Microwave Digestion High Temperature High Pressure.
Table 1 sampling Graphite Furnace Atomic Absorption spectrophotometer condition of work.
Table 2 flame atomic absorption spectrophotometer condition of work.
Table 3 wet method and ultrasonic extraction experimental result.
Table 4 dry method and ultrasonic extraction result.
Table 5 Microwave Digestion and ultrasonic extraction experimental result.
Table 1
Table 2
Table 3
Table 4
Table 5
Claims (1)
1. the ultrasonic extracting method of a Heavy Metals In Vegetables element.It is characterized in that:
(1) preparation of sample: get vegetable sample, get edible portion, first clean with running water, then use distilled water, washed with de-ionized water, air-dry, weigh, put baking oven 60 DEG C of dry 72h, dry sample agate mortar is homogeneous, sieves, saves backup under room temperature;
(2) content of Cd, Cr, Ni, Pb, Zn in sample is tested out,
(3) ultrasonic extraction: take sample in centrifuge tube, solubilizer 65%HNO
3-30%H
2o
2(2:1, V/V), put into ultrasonic 20min at ultra sonic bath 70 DEG C, the addition of solvent needs solvent 5 ~ 10mL according to the every 0.02 μ g of Cd, and the every 0.3 μ g of Cr needs the every 0.2 μ g of solvent 5 ~ 10mL, Ni to need the every 2 μ g of solvent 5 ~ 10mL, Pb to need the every 5 μ g of solvent 5 ~ 10mL and Zn to need solvent 5 ~ 10mL; With 4500r min
-1centrifugal 5min, gets upper strata acid leaching liquor; Ultrasonic 2min again after residue cleaning, with 4500r min
-1centrifugal 5min, gets supernatant liquor and merges with acid leaching liquor.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104749240A (en) * | 2015-03-31 | 2015-07-01 | 广州禾信分析仪器有限公司 | Method for detecting heavy metals in vegetables |
| CN107655736A (en) * | 2017-09-26 | 2018-02-02 | 苏州莱铯科技有限公司 | The pre-treating method of inorganic elements laser analysis in a kind of plant sample |
| CN110320298A (en) * | 2019-07-15 | 2019-10-11 | 江苏天宇检测技术有限公司 | The detection method of heavy metal element in a kind of solid waste |
| CN111442960A (en) * | 2020-04-20 | 2020-07-24 | 北京仪达仪器有限责任公司 | Kit and method for rapidly extracting heavy metals in soil |
| CN114778265A (en) * | 2022-04-28 | 2022-07-22 | 中国第一重型机械股份公司 | Heating-free digestion method and device for chemical analysis sample |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104749240A (en) * | 2015-03-31 | 2015-07-01 | 广州禾信分析仪器有限公司 | Method for detecting heavy metals in vegetables |
| CN107655736A (en) * | 2017-09-26 | 2018-02-02 | 苏州莱铯科技有限公司 | The pre-treating method of inorganic elements laser analysis in a kind of plant sample |
| CN107655736B (en) * | 2017-09-26 | 2020-06-23 | 苏州莱铯科技有限公司 | Pretreatment method for laser analysis of inorganic elements in plant sample |
| CN110320298A (en) * | 2019-07-15 | 2019-10-11 | 江苏天宇检测技术有限公司 | The detection method of heavy metal element in a kind of solid waste |
| CN111442960A (en) * | 2020-04-20 | 2020-07-24 | 北京仪达仪器有限责任公司 | Kit and method for rapidly extracting heavy metals in soil |
| CN111442960B (en) * | 2020-04-20 | 2023-12-29 | 北京仪达仪器有限责任公司 | Kit and method for rapidly extracting heavy metals in soil |
| CN114778265A (en) * | 2022-04-28 | 2022-07-22 | 中国第一重型机械股份公司 | Heating-free digestion method and device for chemical analysis sample |
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