CN101634617A - Digestion method of soil metal elements - Google Patents
Digestion method of soil metal elements Download PDFInfo
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- CN101634617A CN101634617A CN200910041950A CN200910041950A CN101634617A CN 101634617 A CN101634617 A CN 101634617A CN 200910041950 A CN200910041950 A CN 200910041950A CN 200910041950 A CN200910041950 A CN 200910041950A CN 101634617 A CN101634617 A CN 101634617A
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Abstract
The invention discloses a digestion method of soil metal elements. The method comprises the following steps: (1) weighing a soil sample; (2) preparing a mixed acid A which has a volume ratio of nitric acid to hydrofluoric acid to perchloric acid of 6-10:4-5:2; (3) preparing a mixed acid B which has a volume ratio of the hydrofluoric acid to perchloric acid of 8-10:1; (4) adding the mixed acid A to a digestion cup to decompose soil; (5) adding the mixed acid B to escape silicon; (6) removing acid: washing off acid globules suspending on the cup wall with 0.2-5% diluted hydrochloric acid or diluted nitric acid, controlling temperature of an electric heating plate at 110-130 DEG C and distilling to dryness; and (7) make constant volume: adding the diluted nitric acid to dissolve residue in the digestion cup, and adding the diluted nitric acid of the same concentration to the fixed volume for measurement. The method has high efficiency and improved safety. The method is applicable to measurement of metal elements such as Cu, Zn, Fe, Mn, Ca, Mg, Ni, Pb, Cd and the like in soil and produces accurate and reliable determination results.
Description
Technical field
The present invention relates to the mensuration of metal in the soil, especially the digestion procedure of soil metal elements.
Background technology
In the environmental monitoring process, often need the metal in the soil is measured, method in common is to adopt atomic absorption spectrophotometry at present, needs pedotheque is cleared up before measuring.
Cu in soil, Zn, Fe, Mn, Ca, Mg, Ni, Pb, in the mensuration process of metals such as Cd, existing digestion procedure is: take by weighing 0.2～0.5g (being accurate to 0.0002g) sample in 50ml teflon crucible, with adding 10ml hydrochloric acid (top grade is pure) after the water-wet, low-temperature heat on the electric hot plate in fuming cupboard, sample is tentatively decomposed, to be evaporated during to the surplus approximately 3ml left and right sides, take off coldly slightly, add 5ml nitric acid (top grade is pure) then, 5ml hydrofluorite (top grade is pure), 3ml perchloric acid (top grade is pure), add a cover the back on electric hot plate in about temperature heating 1h, uncap then, continue to heat silica removal, in order to reach the good silicon effect that flies, should often shake crucible.When being heated to when emitting the white cigarette of dense perchloric acid, add a cover, the organic carbonide of black is decomposed.After treating the black organism disappearance on the sidewall of crucible, uncap, drive white cigarette and steam to content extremely thick.Look the situation of clearing up, can add 3ml nitric acid (top grade is pure) again, 3ml hydrofluorite (top grade is pure), 1ml perchloric acid (top grade is pure) repeats above digestion process.When white cigarette emits to the greatest extent and content when being thick once more, take off cold slightly, water flushing inwall and crucible cover, and add the warm dissolved residue of 1ml dilute nitric acid solution.Full dose is transferred in the 50ml volumetric flask then, is settled to graticule after the cooling, is equipped with to survey.
In the existing digestion procedure, the time generally needs 8～10 hours.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, the digestion procedure of the fast soil metal elements of a kind of digestion time is provided.
Technical scheme of the present invention is as follows:
A kind of digestion procedure of soil metal elements may further comprise the steps:
(1) takes by weighing 0.2000～0.5000g pedotheque in clearing up cup;
(2) preparation acid mixture A: its volume ratio is nitric acid: hydrofluorite: perchloric acid=6～10: 4～5: 2; Used nitric acid, hydrofluorite, perchloric acid acid are guaranteed reagent;
(3) preparation acid mixture B: its volume ratio is hydrofluorite: perchloric acid=8～10: 1; Used hydrofluorite, perchloric acid acid are guaranteed reagent;
(4) soil decomposes: add 10～20ml acid mixture A in clearing up cup, add a cover closely, low temperature disappears for 130～150 ℃ and boils 0.5～1h on the electric hot plate in fuming cupboard, and pedotheque is tentatively decomposed; Middle then high temperature disappears for 150～200 ℃ and boils 1～3h and become clear liquid to soil digestion, and wall of cup loses till the grey black organism adheres to;
(5) fly silicon: take off lid, add 5～15ml acid mixture B, to emitting white cigarette, take out when remaining 1～2ml when solution steams at 140～180 ℃ of complete uncovered silicon that fly;
(6) catch up with acid: with volumetric concentration is 0.2～5% watery hydrochloric acid or rare nitric acid, and the flushing wall of cup hangs sour pearl, and the control electric plate temperature is at 110～130 ℃, evaporate to dryness;
(7) constant volume: add 1～5ml volumetric concentration and be rare nitric acid of 0.1～2% and will clear up a glass interior residuals dissolving,, be equipped with survey with rare nitric acid constant volume of same concentration.
Compared with prior art, the present invention has the following advantages:
(1) the present invention has cancelled the moistening sample step of distilled water, and the moistening sample step of distilled water is little to the practical function of Specimen eliminating, cancels it and has simplified step.
(2) cancelled with hydrochloric acid low temperature and cleared up sample.It is generally acknowledged that after decomposing with hydrochloric acid is preliminary, can improve the speed of clearing up, and facts have proved, it is little to the total speed of clearing up influence that hydrochloric acid low temperature is cleared up sample, the speed of clearing up depends primarily on the temperature of digestion process.
(3) the inventive method has reduced the usage ratio of perchloric acid.Perchloric acid explodes easily, reduces consumption and has just improved security.Also can shorten simultaneously follow-up catching up with the acid time.
(4) catch up with sour step thoroughly to drive residual acid in the inventive method, guarantee that final constant volume liquid acidity reaches unanimity.And the end of catching up with acid in the existing method is to be benchmark with " white cigarette emit to the greatest extent and content when being thick ".This step operation has very big subjective random.In fact, disappear that it is dry to boil solution, white cigarette is yet emitting.If judge, also need very rich experience to hold well to be thick.During practical operation, how much being difficult to of residual acid holds consistent, causes last constant volume liquid (liquid to be measured) acidity inconsistent, influences result's accuracy and reappearance.In addition: if in the residual acid HF is arranged, also can etching glass, it is smudgy to cause the volumetric flask inboard to be corroded into.If residual HClO
4Too much, just might the molten filter paper of wearing during filtration.Among the present invention, the watery hydrochloric acid with 0.2～5% or rare nitric acid, the flushing wall of cup hangs sour pearl, controls electric plate temperature at 110～130 ℃, evaporate to dryness, the about 1～1.5h of this process; Under this temperature, element to be measured can not lose, and does not worry that cup is roasting to distortion, the precision and the accuracy that have improved experimental result yet.
(5) this digestion procedure 3～6.5h that takes time altogether, and existing digestion procedure often needs 8～10h, the present invention can significantly improve efficient.
(6) the inventive method is applicable to Determination of Metal Elements such as Cu in the soil, Zn, Fe, Mn, Ca, Mg, Ni, Pb, Cd, measures the national standard pedotheque with the inventive method, and result's accordance is fine.
Embodiment
The present invention is further detailed explanation below in conjunction with embodiment.The concentration of following diluted acid is volumetric concentration.
Embodiment 1
(1) takes by weighing 0.2000g soil standard model in clearing up cup;
(2) preparation acid mixture A: its volume ratio is nitric acid: hydrofluorite: perchloric acid=6: 4: 2; Used nitric acid, hydrofluorite, perchloric acid acid are guaranteed reagent;
(3) preparation acid mixture B: its volume ratio is hydrofluorite: perchloric acid=9: 1; Used hydrofluorite, perchloric acid acid are guaranteed reagent;
(4) soil decomposes: add 10ml acid mixture A in clearing up cup, add a cover closely, low temperature disappears for 130～150 ℃ and boils 0.5h on the electric hot plate in fuming cupboard, and pedotheque is tentatively decomposed; Middle then high temperature disappears for 150～200 ℃ to boil to soil digestion and becomes clear liquid, and wall of cup loses till the grey black organism adheres to, the about 1.5h of this process;
(5) fly silicon: take off lid, add 5ml acid mixture B, to emitting white cigarette, take out when remaining 1ml when solution steams at 140～180 ℃ of complete uncovered silicon that fly;
(6) catch up with acid: the watery hydrochloric acid with 0.2%, the flushing wall of cup hangs sour pearl, controls electric plate temperature at 110～130 ℃, evaporate to dryness;
(7) constant volume: the rare nitric acid that adds 1ml 0.1% will be cleared up a glass interior residuals dissolving, with rare nitric acid constant volume of same concentration, be equipped with and will survey.
With atomic absorption spectrophotometry metals such as the Cu in the pedotheque, Zn, Fe, Mn, Ca, Mg, Ni, Pb, Cd are measured, measured value all meets the national standard reference value.Determination data is as shown in table 1.
Embodiment 2
(1) takes by weighing the 0.5000g pedotheque in clearing up cup;
(2) preparation acid mixture A: its volume ratio is nitric acid: hydrofluorite: perchloric acid=8: 4: 2; Used nitric acid, hydrofluorite, perchloric acid acid are guaranteed reagent;
(3) preparation acid mixture B: its volume ratio is hydrofluorite: perchloric acid=9: 1; Used hydrofluorite, perchloric acid acid are guaranteed reagent;
(4) soil decomposes: add 20ml acid mixture A in clearing up cup, add a cover closely, low temperature disappears for 130～150 ℃ and boils 1h on the electric hot plate in fuming cupboard, and pedotheque is tentatively decomposed; Middle then high temperature disappears for 150～200 ℃ to boil to soil digestion and becomes clear liquid, and wall of cup loses till the grey black organism adheres to, the about 2h of this process;
(5) fly silicon: take off lid, add 15ml acid mixture B, to emitting white cigarette, take out when remaining 2ml when solution steams at 140～180 ℃ of complete uncovered silicon that fly;
(6) catch up with acid: the rare nitric acid with 5%, the flushing wall of cup hangs sour pearl, controls electric plate temperature at 110～130 ℃, evaporate to dryness;
(7) constant volume: the rare nitric acid that adds 5ml 2% will be cleared up a glass interior residuals dissolving, with rare nitric acid constant volume of same concentration, be equipped with and will survey.
With atomic absorption spectrophotometry metals such as the Cu in the pedotheque, Zn, Fe, Mn, Ca, Mg, Ni, Pb, Cd are measured, measured value all meets the national standard reference value.Determination data is as shown in table 1.
Embodiment 3
(1) takes by weighing the 0.3000g pedotheque in clearing up cup;
(2) preparation acid mixture A: its volume ratio is nitric acid: hydrofluorite: perchloric acid=10: 5: 2; Used nitric acid, hydrofluorite, perchloric acid acid are guaranteed reagent;
(3) preparation acid mixture B: its volume ratio is hydrofluorite: perchloric acid=9: 1; Used hydrofluorite, perchloric acid acid are guaranteed reagent;
(4) soil decomposes: add 15ml acid mixture A in clearing up cup, add a cover closely, low temperature disappears for 130～150 ℃ and boils 0.75h on the electric hot plate in fuming cupboard, and pedotheque is tentatively decomposed; Middle then high temperature disappears for 150～200 ℃ to boil to soil digestion and becomes clear liquid, and wall of cup loses till the grey black organism adheres to, the about 3h of this process;
(5) fly silicon: take off lid, add 15ml acid mixture B, to emitting white cigarette, take out when remaining 1.5ml when solution steams at 140～180 ℃ of complete uncovered silicon that fly;
(6) catch up with acid: the rare nitric acid with 1%, the flushing wall of cup hangs sour pearl, controls electric plate temperature at 110～130 ℃, evaporate to dryness;
(7) constant volume: the rare nitric acid that adds 5ml 1% will be cleared up a glass interior residuals dissolving, with rare nitric acid constant volume of same concentration, be equipped with and will survey.
With atomic absorption spectrophotometry metals such as the Cu in the pedotheque, Zn, Fe, Mn, Ca, Mg, Ni, Pb, Cd are measured, measured value all meets the national standard reference value.Determination data is as shown in table 1.
Embodiment 4
(1) takes by weighing the 0.2000g pedotheque in clearing up cup;
(2) preparation acid mixture A: its volume ratio is nitric acid: hydrofluorite: perchloric acid=8: 4: 2; Used nitric acid, hydrofluorite, perchloric acid acid are guaranteed reagent;
(3) preparation acid mixture B: its volume ratio is hydrofluorite: perchloric acid=8: 1; Used hydrofluorite, perchloric acid acid are guaranteed reagent;
(4) soil decomposes: add 15ml acid mixture A in clearing up cup, add a cover closely, low temperature disappears for 130～150 ℃ and boils 0.75h on the electric hot plate in fuming cupboard, and pedotheque is tentatively decomposed; Middle then high temperature disappears for 150～200 ℃ to boil to soil digestion and becomes clear liquid, and wall of cup loses till the grey black organism adheres to, the about 2.5h of this process;
(5) fly silicon: take off lid, add 15ml acid mixture B, to emitting white cigarette, take out when remaining 1.8ml when solution steams at 140～180 ℃ of complete uncovered silicon that fly;
(6) catch up with acid: the rare nitric acid with 1%, the flushing wall of cup hangs sour pearl, controls electric plate temperature at 110～130 ℃, evaporate to dryness;
(7) constant volume: the rare nitric acid that adds 5ml 1% will be cleared up a glass interior residuals dissolving, with rare nitric acid constant volume of same concentration, be equipped with and will survey.
With atomic absorption spectrophotometry metals such as the Cu in the pedotheque, Zn, Fe, Mn, Ca, Mg, Ni, Pb, Cd are measured, measured value all meets the national standard reference value.Determination data is as shown in table 1.
Embodiment 5
(1) takes by weighing the 0.5000g pedotheque in clearing up cup;
(2) preparation acid mixture A: its volume ratio is nitric acid: hydrofluorite: perchloric acid=8: 4: 2; Used nitric acid, hydrofluorite, perchloric acid acid are guaranteed reagent;
(3) preparation acid mixture B: its volume ratio is hydrofluorite: perchloric acid=10: 1; Used hydrofluorite, perchloric acid acid are guaranteed reagent;
(4) soil decomposes: add 10ml acid mixture A in clearing up cup, add a cover closely, low temperature disappears for 130～150 ℃ and boils 0.75h on the electric hot plate in fuming cupboard, and pedotheque is tentatively decomposed; Middle then high temperature disappears for 150～200 ℃ to boil to soil digestion and becomes clear liquid, and wall of cup loses till the grey black organism adheres to, the about 2h of this process;
(5) fly silicon: take off lid, add 10ml acid mixture B, to emitting white cigarette, take out when remaining 1.3ml when solution steams at 140～180 ℃ of complete uncovered silicon that fly;
(6) catch up with acid: the rare nitric acid with 1%, the flushing wall of cup hangs sour pearl, controls electric plate temperature at 110～130 ℃, evaporate to dryness;
(7) constant volume: the rare nitric acid that adds 5ml 1% will be cleared up a glass interior residuals dissolving, with rare nitric acid constant volume of same concentration, be equipped with and will survey.
With atomic absorption spectrophotometry metals such as the Cu in the pedotheque, Zn, Fe, Mn, Ca, Mg, Ni, Pb, Cd are measured, measured value all meets the national standard reference value.Determination data is as shown in table 1.
Each embodiment determination data of table 1
| ??Pb ??(mg/kg) | ??Ni ??(mg/kg) | ??Cd ??(mg/kg) | ??Cu ??(mg/kg) | ??Zn ??(mg/kg) | ??Fe 2O 3??(％) | ??Mn ??(mg/kg) | ??Ca?O ??(％) | ??Mg?O ??(％) | |
| Standard value | ??314± ??20 | ??53±5 | ??0.13 ??±0.04 | ??390±22 | ??97±9 | ??8.09± ??0.19 | ??0.145 ??±0.03 | ??0.22± ??0.04 | ??0.34 ??± ??0.07 |
| Embodiment 1 | ??314 | ??49 | ??0.10 | ??391 | ??92 | ??8.00 | ??0.145 | ??0.21 | ??0.32 |
| Embodiment 2 | ??298 | ??56 | ??0.13 | ??388 | ??97 | ??8.02 | ??0.125 | ??0.20 | ??0.34 |
| Embodiment 3 | ??301 | ??50 | ??0.16 | ??394 | ??100 | ??8.19 | ??0.134 | ??0.24 | ??0.29 |
| Embodiment 4 | ??312 | ??49 | ??0.15 | ??389 | ??98 | ??8.09 | ??0.154 | ??0.19 | ??0.40 |
| Embodiment 5 | ??320 | ??53 | ??0.11 | ??395 | ??103 | ??7.99 | ??0.144 | ??0.25 | ??0.39 |
Claims (1)
1, a kind of digestion procedure of soil metal elements may further comprise the steps:
(1) takes by weighing 0.2000～0.5000g pedotheque in clearing up cup;
(2) preparation acid mixture A: its volume ratio is nitric acid: hydrofluorite: perchloric acid=6～10: 4～5: 2; Used nitric acid, hydrofluorite, perchloric acid acid are guaranteed reagent;
(3) preparation acid mixture B: its volume ratio is hydrofluorite: perchloric acid=8～10: 1; Used hydrofluorite, perchloric acid acid are guaranteed reagent;
(4) soil decomposes: add 10～20ml acid mixture A in clearing up cup, add a cover closely, low temperature disappears for 130～150 ℃ and boils 0.5～1h on the electric hot plate in fuming cupboard, and pedotheque is tentatively decomposed; Middle then high temperature disappears for 150～200 ℃ and boils 1～3h and become clear liquid to soil digestion, and wall of cup loses till the grey black organism adheres to;
(5) fly silicon: take off lid, add 5～15ml acid mixture B, to emitting white cigarette, take out when remaining 1～2ml when solution steams at 140～180 ℃ of complete uncovered silicon that fly;
(6) catch up with acid: with volumetric concentration is 0.2～5% watery hydrochloric acid or rare nitric acid, and the flushing wall of cup hangs sour pearl, and the control electric plate temperature is at 110～130 ℃, evaporate to dryness;
(7) constant volume: add 1～5ml volumetric concentration and be rare nitric acid of 0.1～2% and will clear up a glass interior residuals dissolving,, be equipped with survey with rare nitric acid constant volume of same concentration.
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| CN101936884A (en) * | 2010-06-23 | 2011-01-05 | 四川农业大学 | Method for determining total lead and copper content of soil |
| CN102589940A (en) * | 2011-01-14 | 2012-07-18 | 核工业二一六大队 | Dissolving method of fluoritized phenacite and bertrandite |
| CN103063506A (en) * | 2012-12-29 | 2013-04-24 | 上海华碧检测技术有限公司 | Pretreatment method for detecting soil |
| CN103543055A (en) * | 2013-10-25 | 2014-01-29 | 环境保护部华南环境科学研究所 | Pretreatment method for heavy metal element detection in solid sample and application of pretreatment method |
| CN104034720A (en) * | 2014-06-05 | 2014-09-10 | 同济大学 | Detection method for heavy metal in building wastes |
| CN104655479A (en) * | 2015-01-28 | 2015-05-27 | 攀钢集团研究院有限公司 | Method for measuring element content in minerals or soil and sample pretreatment method |
| CN104914061A (en) * | 2015-06-19 | 2015-09-16 | 贵州出入境检验检疫局检验检疫综合技术中心 | Method for determining thallium content of agricultural product by flame atomic absorption spectrometry |
| CN104931330A (en) * | 2015-06-11 | 2015-09-23 | 大连谱尼测试科技有限公司 | Digestion method of detection of heavy metals in soil |
| CN105203386A (en) * | 2015-11-09 | 2015-12-30 | 中国科学院东北地理与农业生态研究所 | Method for digesting metallic elements in peat soil |
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| CN108279153A (en) * | 2018-01-05 | 2018-07-13 | 四川环科检测技术有限公司 | Metal elements in soil digestion procedure |
| CN109632932A (en) * | 2018-12-29 | 2019-04-16 | 上海微谱化工技术服务有限公司 | Elemental analysis method in a kind of lamivudine preparation |
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| CN112147096A (en) * | 2020-09-23 | 2020-12-29 | 浙江求实环境监测有限公司 | Method for detecting effective state lead in soil |
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| CN101936884A (en) * | 2010-06-23 | 2011-01-05 | 四川农业大学 | Method for determining total lead and copper content of soil |
| CN102589940A (en) * | 2011-01-14 | 2012-07-18 | 核工业二一六大队 | Dissolving method of fluoritized phenacite and bertrandite |
| CN103063506A (en) * | 2012-12-29 | 2013-04-24 | 上海华碧检测技术有限公司 | Pretreatment method for detecting soil |
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| CN104034720A (en) * | 2014-06-05 | 2014-09-10 | 同济大学 | Detection method for heavy metal in building wastes |
| CN104034720B (en) * | 2014-06-05 | 2016-08-17 | 同济大学 | Heavy metal detection method in a kind of waste material of buildings |
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| CN104655479B (en) * | 2015-01-28 | 2017-03-15 | 攀钢集团研究院有限公司 | Determine method and its preprocess method of sample of mineral or elements in Soil content |
| CN104931330A (en) * | 2015-06-11 | 2015-09-23 | 大连谱尼测试科技有限公司 | Digestion method of detection of heavy metals in soil |
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| CN112147096A (en) * | 2020-09-23 | 2020-12-29 | 浙江求实环境监测有限公司 | Method for detecting effective state lead in soil |
| 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 |
| CN114324306A (en) * | 2021-12-14 | 2022-04-12 | 武汉钢铁有限公司 | Method for jointly measuring content of phosphorus and arsenic in gas mud and gas ash |
| CN114324306B (en) * | 2021-12-14 | 2024-05-28 | 武汉钢铁有限公司 | Combined measuring method for phosphorus and arsenic content in gas mud and gas ash |
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