CN105203386A - Method for digesting metallic elements in peat soil - Google Patents
Method for digesting metallic elements in peat soil Download PDFInfo
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- CN105203386A CN105203386A CN201510756557.2A CN201510756557A CN105203386A CN 105203386 A CN105203386 A CN 105203386A CN 201510756557 A CN201510756557 A CN 201510756557A CN 105203386 A CN105203386 A CN 105203386A
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- peat soil
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Abstract
The invention relates to a method for digesting metallic elements in peat soil and particularly relates to a method applicable to the digestion of the metallic elements in the peat soil rich in organic matters. According to the method, the problem of poor digestion effect of the metallic elements in the peat soil is solved. The method particularly comprises the following steps: (1) pretreatment of the peat soil; (2) ashing treatment of the peat soil; and (3) digestion of the peat soil: digesting the peat soil by virtue of concentrated HNO3, HClO4 and HF. By virtue of the method provided by the invention, the digestion effect of a sample is improved when the experiment cost is saved and the loss of the sample is reduced. The method for digesting the metallic elements is applied to the digestion of the metallic elements in the peat soil rich in organic matters.
Description
Technical field
The present invention relates to the digestion procedure of metallic element.
Background technology
At present, the digestion procedure of metal element content in plant is measured mainly with HNO
3-HCLO
4clear up (People's Republic of China's forestry industry standard, LY/T1270-1999), measure the digestion procedure of metal elements in soil content mainly with HNO
3-HCL-H
2sO4 or HNO
3-HCL-HCLO
4clear up preparation liquid to be measured (People's Republic of China's forestry industry standard, LY/T1256-1999).And for the peat soil in Marsh Wetland, still there is no the metallic element digestion procedure of standard.Be rich in organic principle in peat soil, mainly the organic matter such as cellulose, hemicellulose, lignin, humic acid, bituminous material, its content 30% even up to more than 95%; Inorganic constituents is clay, quartz and other dirts mainly.Therefore, simple with metal element content assay method in plant or clear up peat samples by metal elements in soil content assaying method, to there is in digestion process easily loss and metallic element clears up incomplete phenomenon, satisfied mensuration effect can not be reached.
Summary of the invention
The object of the invention is to clear up the bad problem of effect to solve metallic element in peat soil, a kind of digestion procedure being more suitable for being rich in metallic element in organic peat soil is provided.
Measuring the digestion procedure of metallic element in peat soil in the present invention is carry out according to the following steps:
One, the pre-treatment of peat soil: peat soil is put into baking oven, dries 5h ~ 7h at 100 DEG C ~ 110 DEG C, naturally cools, grind with porcelain mortar after taking out, and crossing aperture is the nylon mesh of 0.120 ~ 0.250mm, obtains peat soil sample;
Two, the ashing process of peat soil: take peat soil sample 0.2g ~ 0.3g (being accurate to 0.0001g) of handling well in porcelain crucible, high temperature ashing 20min ~ 40min in 480 DEG C ~ 500 DEG C muffle furnaces;
Three, the clearing up of peat soil: the sample deionized water after ashing is repeatedly rinsed in teflon crucible on a small quantity from porcelain crucible, then adds the dense HNO that 3mL ~ 8mL massfraction is 60% ~ 65% successively
3, 1mL ~ 3mLHClO
4with 3mL ~ 8mLHF, on 340 DEG C in ventilating kitchen ~ 360 DEG C electric hot plates, heating and decompose is to emitting white cigarette, and sample (as color is comparatively dark, can add a small amount of dense HNO again in white or pale precipitation
3, HCIO
4continue to clear up to meeting the requirements.Digestion can't make content evaporate to dryness zoom or rubescent look shape to during near doing, and can make the metallic element dehydrations such as copper like this, not easy-to-use diluted acid dissolves), namely complete clearing up of peat soil.
The ICPS-7500 type inductively coupled plasma atomic emission (ICP-AES) that the present invention utilizes Japanese Shimadzu Corporation to produce measures the content of metallic element in peat samples.Computing formula:
Wherein: W is metal element content, unit mg/kg;
C
1for Gold Samples belongs to element determination value, unit mg/L;
C
0for Determination of Metals value in blank, unit mg/L;
V is sample constant volume, units/ml;
M is sample quality, unit g.
The present invention is relative to its advantage of prior art:
1. utilize the peat soil of the digestion procedure of metallic element in peat soil of the present invention to the organic matter containing different amount to process respectively, wherein organic content is respectively 20.20%, 31.22%, 40.45%, 50.18%, 61.22%, 72.34%, 80.82% and 92.45%, and the content of the copper utilizing the digestion procedure of metallic element in peat soil of the present invention to record is respectively 8.02mg/kg, 5.79mg/kg, 26.95mg/kg, 14.36mg/kg, 16.23mg/kg, 22.91mg/kg, 12.80mg/kg and 5.15mg/kg.Copper content in the peat soil comparatively adopting plant digestion procedure and employing Methods of Soil Digestion to measure, improves 4.4 ~ 16.1% and 8.9 ~ 18.5% respectively.Therefore, digestion procedure provided by the present invention is more suitable for and is rich in clearing up of metallic element in organic peat soil, namely improves and clears up effect, solve again clay fraction in peat soil and clear up incomplete problem, the content of metallic element in peat samples can better be obtained, measure respond well.
2. the digestion procedure of metallic element in a kind of peat soil provided by the invention, is applicable to the mensuration being rich in metal element content in organic peat soil.First, be rich in organic peat samples through ashing, eliminate too much carbon content, gas can not be discharged fast because carbon content is too high when clearing up and make sample splash, avoid the loss of metallic element.Finally, add HF and be conducive to destroying element structure in the mineralogical composition lattices such as clay in peat samples, to reach clearing up completely of metallic element in peat samples.Therefore, saving experimental cost, reducing on the basis of sample loss, sample is fully cleared up, and what improve sample clears up effect, ensure that the accuracy of data; ICP-AES multielement simultaneous determination, eliminate the disturbing effect between metallic element, remove the use of anti-interference agent during different metal element determination, avoid repeatedly using chemical reagent clear up sample and cause the harmful effect to environment, be conducive to reducing and pollution abatement from source, meet Green Chemistry.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the combination in any between each embodiment.
Embodiment one: the method that in the peat soil of present embodiment, metallic element is cleared up, is characterized in that: the method that in described peat soil, metallic element is cleared up is carried out according to the following steps:
One, the pre-treatment of peat soil: peat soil is put into baking oven, dries 5h ~ 7h at 100 DEG C ~ 110 DEG C, naturally cools, grind with porcelain mortar after taking out, and crossing aperture is the nylon mesh of 0.120 ~ 0.250mm, obtains peat soil sample;
Two, the ashing process of peat soil: take peat soil sample 0.2g ~ 0.3g (being accurate to 0.0001g) of handling well in porcelain crucible, high temperature ashing 20min ~ 40min in 480 DEG C ~ 500 DEG C muffle furnaces, obtains the sample after ashing;
Three, the clearing up of peat soil: the sample deionized water after ashing is rinsed from porcelain crucible in teflon crucible, rinse 5 times ~ 8 times, then add the dense HNO that 3mL ~ 8mL massfraction is 60% ~ 65% successively
3, 1mL ~ 3mLHCLO
4with 3mL ~ 8mLHF, on 340 DEG C in ventilating kitchen ~ 360 DEG C electric hot plates, heating and decompose is to emitting white cigarette, and sample (as color is comparatively dark, can add a small amount of dense HNO again in white or pale precipitation
3, HCIO
4continue to clear up to meeting the requirements.Digestion can't make content evaporate to dryness zoom or rubescent look shape to during near doing, and can make the metallic element dehydrations such as copper like this, not easy-to-use diluted acid dissolves), namely complete clearing up of peat soil.
Embodiment two: present embodiment and embodiment one unlike, the aperture of nylon mesh described in step one is 0.149mm.Other steps are identical with embodiment one with parameter.
Embodiment three: present embodiment and embodiment one unlike, take the peat soil sample 0.25g handled well in step 2.Other steps are identical with embodiment one with parameter.
Embodiment four: present embodiment and embodiment one unlike, step 2 is high temperature ashing 30min in 500 DEG C of muffle furnaces, obtains the sample after ashing.Other steps are identical with embodiment one with parameter.
Embodiment five: present embodiment and embodiment one unlike, step 3 adds the dense HNO that massfraction is 60% ~ 65%
35mL.Other steps are identical with embodiment one with parameter.
Embodiment six: present embodiment and embodiment one unlike, step 3 adds HCLO
4volume be 2mL.Other steps are identical with embodiment one with parameter.
Embodiment seven: present embodiment and embodiment one unlike, the volume that step 3 adds HF is 5mL.Other steps are identical with embodiment one with parameter.
Embodiment 1
Get the peat soil that 8 kinds of contents of organic matter are different, respectively following operation carried out to it:
One, pre-treatment: get a certain amount of air-dry peat samples and put into baking oven, dry 6h at 105 DEG C, takes out cooling, grinds with porcelain mortar, crosses 0.149mm nylon mesh, stand-by;
Two, ashing: take the peat samples 0.25g (being accurate to 0.0001g) that handles well in 50ml porcelain crucible, in 500 DEG C of muffle furnaces high temperature ashing 30 minutes, obtains the sample after ashing;
Three, clear up: a small amount of deionized water of the sample after ashing is repeatedly rinsed in 50ml teflon crucible, add the dense HNO that massfraction is 65% successively
35ml, 2mlHCLO
4and 5mlHF, in ventilating kitchen, on 350 DEG C of electric hot plates, heating and decompose is to emitting white cigarette, and sample, in white or pale precipitation, takes off and is down to normal temperature, add the rare HNO of 2ml10%
3solubilize, with deionized water constant volume in 25ml volumetric flask, makes liquid to be measured with Filter paper filtering in plastic bottle, to be measured; Do blank assay simultaneously.
Four, measure: the ICPS-7500 type inductively coupled plasma atomic emission (ICP-AES) produced with Japanese Shimadzu Corporation measures the content of copper in peat samples.
(5) measurement result is in table 1.
(6) simultaneously, measure the content of metallic element copper in soil constituent analytical standard material (GBW07401) by step 2, three, four, measurement result is in table 2.
Table 1
Table 2
Table 1 shows in the peat soil of different organic matter contents, the content of its copper utilizing the digestion procedure of the present embodiment to obtain.The value that table 2 shows to utilize the digestion procedure of the present embodiment to record, in the scope of standard value, meets standard, illustrates that digestion procedure measurement result of the present invention is credible.
Comparative example 1 adopts plant digestion procedure: the HNO in forest plants and forest litter total silicon, iron, aluminium, calcium, magnesium, potassium, sodium, phosphorus, sulphur, manganese, copper and Direct spectrophotometry (LY/T1270-1999) method
3-HCIO
4resolution method, 8 kinds of different peat soils in Example 1, carry out following operation to it respectively:
One, sample: take 8, the sample that 0.25g is corresponding respectively with embodiment 1 respectively, put into 150ml triangular flask respectively;
Two, clear up: add the dense HNO of 5mL respectively
3and 1mLHCIO
4, triangle bottleneck puts a little funnel, and in the sand-bath having ventilating kitchen, heating and decompose is not being emerged to Brown gas.Take off and be down to normal temperature, add the rare HNO of 2ml10%
3solubilize, with deionized water constant volume in 25ml volumetric flask, makes liquid to be measured with Filter paper filtering to be measured in plastic bottle;
Three, measure: measure with ICPS-7500 type inductively coupled plasma atomic emission (ICP-AES), obtain the content of metallic element copper in peat samples.
Four, measurement result is in table 3.
Table 3
Comparative example 2 adopts Methods of Soil Digestion: the HNO in mensuration (LY/T1256-1999) method of forest soil strong acid digestion element
3-HCI-HCIO
4resolution method, 8 kinds of different peat soils in Example 1, carry out following operation to it respectively:
One, sample: take 8, the sample that 0.25g is corresponding respectively with embodiment 1 respectively, put into 150ml triangular flask respectively;
Two, clear up: add the dense HCI of 7.5mL respectively, adding the dense HNO of 2.5ml
3and 5mLHCIO
4, triangle bottleneck puts a little funnel, and in the sand-bath having ventilating kitchen, heating and decompose is to emitting white cigarette.Take off and be down to normal temperature, add the rare HNO3 solubilize of 2ml10%, with deionized water constant volume in 25ml volumetric flask, in plastic bottle, make liquid to be measured with Filter paper filtering, to be measured
Three, measure: measure with ICPS-7500 type inductively coupled plasma atomic emission (ICP-AES), obtain the content of copper in peat samples.
Four, measurement result is in table 4.
Table 4
Conclusion: the measurement result contrast according to table 1, table 3 and table 4 can be found out, the digestion procedure of copper assay in a kind of peat soil provided by the invention, its measurement result value, higher than copper content in the peat soil adopting plant digestion procedure and adopt Methods of Soil Digestion to measure, improves 4.4 ~ 16.1% and 8.9 ~ 18.5% respectively.Therefore, digestion procedure provided by the present invention is more suitable for and is rich in clearing up of metallic element in organic peat soil, namely improves and clears up effect, solve again clay fraction in peat soil and clear up incomplete problem, the content of metallic element in peat samples can better be obtained, measure respond well.
Claims (7)
1. the digestion procedure of metallic element in peat soil, is characterized in that: in described peat soil, the digestion procedure of metallic element carries out according to the following steps:
One, the pre-treatment of peat soil: peat soil is put into baking oven, dries 5h ~ 7h at 100 DEG C ~ 110 DEG C, naturally cools, grind with porcelain mortar after taking out, and crossing aperture is the nylon mesh of 0.120 ~ 0.250mm, obtains peat soil sample;
Two, the ashing process of peat soil: take the peat soil sample 0.2g ~ 0.3g handled well and be placed in porcelain crucible, high temperature ashing 20min ~ 40min in 480 DEG C ~ 500 DEG C muffle furnaces, obtains the sample after ashing;
Three, the clearing up of peat soil: the sample deionized water after ashing is rinsed from porcelain crucible in teflon crucible, rinse 5 times ~ 8 times, then add the dense HNO that 3mL ~ 8mL massfraction is 60% ~ 65% successively in teflon crucible
3, 1mL ~ 3mLHCLO
4with 3mL ~ 8mLHF, on 340 DEG C in ventilating kitchen ~ 360 DEG C electric hot plates, heating and decompose is to emitting white cigarette, and sample, in white or pale precipitation, namely completes clearing up of metallic element in peat soil.
2. the digestion procedure of metallic element in a kind of peat soil according to claim 1, is characterized in that: the aperture of nylon mesh described in step one is 0.149mm.
3. the digestion procedure of metallic element in a kind of peat soil according to claim 1, is characterized in that: take the peat soil sample 0.25g handled well in step 2.
4. the digestion procedure of metallic element in a kind of peat soil according to claim 1, is characterized in that: step 2 is high temperature ashing 30min in 500 DEG C of muffle furnaces, obtains the sample after ashing.
5. the digestion procedure of metallic element in a kind of peat soil according to claim 1, is characterized in that: step 3 adds the dense HNO that massfraction is 60% ~ 65%
35mL.
6. the digestion procedure of metallic element in a kind of peat soil according to claim 1, is characterized in that: step 3 adds HCLO
4volume be 2mL.
7. the digestion procedure of metallic element in a kind of peat soil according to claim 1, is characterized in that: the volume that step 3 adds HF is 5mL.
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|---|---|---|---|
| CN201510756557.2A CN105203386A (en) | 2015-11-09 | 2015-11-09 | Method for digesting metallic elements in peat soil |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102866046A (en) * | 2012-09-18 | 2013-01-09 | 北京市农林科学院 | Method for determining contents of heavy metals in sample |
-
2015
- 2015-11-09 CN CN201510756557.2A patent/CN105203386A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102866046A (en) * | 2012-09-18 | 2013-01-09 | 北京市农林科学院 | Method for determining contents of heavy metals in sample |
Non-Patent Citations (3)
| Title |
|---|
| 于天霞等: "用原子吸收法分析污泥、土壤时几种分析方法的比较", 《化学工程师》 * |
| 周敏等: "TOA-MIBK萃取火焰原子吸收法同时测定土壤及蔬菜中铅镉", 《四川环境》 * |
| 贾海东: "干式消解-原子吸收光谱法测定土壤中部分重金属的探讨", 《环境工程》 * |
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Application publication date: 20151230 |