CN105466752A - Pretreatment method for determining of heavy metal in soil - Google Patents
Pretreatment method for determining of heavy metal in soil Download PDFInfo
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- CN105466752A CN105466752A CN201610012882.2A CN201610012882A CN105466752A CN 105466752 A CN105466752 A CN 105466752A CN 201610012882 A CN201610012882 A CN 201610012882A CN 105466752 A CN105466752 A CN 105466752A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition
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- Sampling And Sample Adjustment (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a pretreatment method for determining of heavy metal in soil. The pretreatment method includes the following steps that S1, 0.2-0.5 g of a sample is accurately weighed inside a digestion tank, and 8 ml of aqua regia is added for digestion; S2, according to the digestion process, temperature reaches 100 DEG C through 4 minutes of climbing at 1200 W to be kept for 3 minutes; temperature reaches 150 DEG C through 5 minutes of climbing at 1200 W to be kept for 5 minutes; temperature reaches 180 DEG C through 5 minutes of climbing at 1200 W to be kept for 25 minutes; S3, the digested sample obtained through S2 is transferred into a teflon crucible of 50 ml, 5 ml of nitric acid, 5 ml of hydrofluoric acid and 3ml of perchloric acid are added, a cover covers the teflon crucible, then the teflon crucible is placed on an electric hot plate to be heated for about 1 h at medium temperature, and finally the cover is opened; the temperature of the electric hot plate is controlled to be 150 DEG C-200 DEG C, heating is performed continuously to remove silicon, and when thick perchloric acid smoke or about 1 ml of solution remains through heating, the crucible is taken down to be slightly cooled; S4, after S3 is completed, 1 ml of hydrochloric acid is added, soluble residues are dissolved through warming, the total quantity of solution is transferred into a volumetric flask of 50 ml, the volume is metered to a marked line with water after cooling, and even shaking is performed. The pretreatment method has the advantages that the soil sample can be digested completely, and digestion speed can be increased.
Description
Technical field
The present invention relates to environmental monitoring technology field, particularly relate to heavy metal in soil and measure pre-treating method.
Background technology
Aas determination is analyzed in the process of heavy metal content in soil, and sample pre-treatments is crucial.The pre-treating method of pedotheque is a lot, has Wet, micro-wave digestion etc.These methods respectively have relative merits.Wet is wasted time and energy, and same sample needs repeatedly to clear up, and microwave digestion time is fast, automatically controls, but often clears up complete not.
Therefore prior art haves much room for improvement and develops.
Summary of the invention
The technical problem to be solved in the present invention to be to provide after a kind of first micro-wave digestion Wet again, and can either clear up pedotheque completely, the heavy metal in soil that also can improve oxidation rate measures pre-treating method.
Technical solution of the present invention is: heavy metal in soil measures pre-treating method, comprises the following steps,
S1: accurately take 0.2 ~ 0.5g sample in counteracting tank, adds 8ml chloroazotic acid and clears up;
S2: clearing up program is that 1200W climbs 4 minutes to 100 DEG C time successively, keeps 3 minutes; 1200W climbs 5 minutes to 150 DEG C time, keeps 5 minutes; 1200W climbs 5 minutes to 180 DEG C time, keeps 25 minutes;
S3: the sample of clearing up obtained after S2 is transferred in 50ml teflon crucible, add 5ml nitric acid, 5ml hydrofluorite, 3ml perchloric acid add a cover after in the upper temperature heating of electric hot plate about 1h, then uncap; Electric plate temperature controls at 150-200 DEG C, continues heating silica removal, when being heated to emit the white cigarette of dense perchloric acid or solution residue about 1ml, takes off crucible slightly cold;
S4: add 1ml hydrochloric acid solution after S3, warm dissolving soluble residues, full dose is transferred in 50ml volumetric flask, is settled to graticule, shakes up after cooling with water.
Sample mass in S1 is accurate to 0.0002g.
In S3, heat silica removal process often should shake crucible.
Beneficial effect of the present invention:
Heavy metal in soil provided by the invention measures pre-treating method, to adopt after first micro-wave digestion Wet again, can either clear up pedotheque completely, also can improve oxidation rate.
Embodiment
Embodiment:
Accurately take 0.2 ~ 0.5g sample in counteracting tank, sample mass is accurate to 0.0002g, adds 8ml chloroazotic acid and clears up.Clearing up program is that 1200W climbs 4 minutes to 100 DEG C time, keeps 3 minutes; 1200W climbs 5 minutes to 150 DEG C time, keeps 5 minutes; 1200W climbs 5 minutes to 180 DEG C time, keeps 25 minutes, for subsequent use.
Above-mentioned sample of clearing up is transferred in 50ml teflon crucible; According to the regulation in HJ491-2009 " the mensuration atomic absorption spectrophotometry of total Chromium in Soil " standard, add 5ml nitric acid, 5ml hydrofluorite, 3ml perchloric acid, in the upper temperature heating of electric hot plate about 1h after adding a cover, then uncap, electric plate temperature controls at 150-200 DEG C, and temperature is too high may cause some metal loss, continues heating silica removal, flying silicon effect to reach good, often should shake crucible.When being heated to emit the white cigarette of dense perchloric acid or solution residue about 1ml, take off crucible slightly cold, add 1ml hydrochloric acid solution, warm dissolving soluble residues, full dose is transferred in 50ml volumetric flask, be settled to graticule with water after cooling, shake up, atomic absorption spectrophotometry then can be adopted to carry out sample analysis.
In the process of heavy metal content in soil, sample pre-treatments is crucial.The pre-treating method of pedotheque is a lot, has Wet, micro-wave digestion etc.Wet is wasted time and energy, and same sample needs repeatedly to clear up, and microwave digestion time is fast, automatically controls, but often clears up complete not.And the present invention adopts first Wet again after micro-wave digestion, has both cleared up pedotheque completely, and has also improved oxidation rate.Almost all pedotheques are obtained and good clear up effect.
Above-listed detailed description is illustrating for possible embodiments of the present invention, and this embodiment is also not used to limit the scope of the claims of the present invention, and the equivalence that all the present invention of disengaging do is implemented or changed, and all should be contained in the scope of the claims of this case.
Claims (3)
1. heavy metal in soil measures pre-treating method, it is characterized in that: comprise the following steps,
S1: accurately take 0.2 ~ 0.5g sample in counteracting tank, adds 8ml chloroazotic acid and clears up;
S2: clearing up program is that 1200W climbs 4 minutes to 100 DEG C time successively, keeps 3 minutes; 1200W climbs 5 minutes to 150 DEG C time, keeps 5 minutes; 1200W climbs 5 minutes to 180 DEG C time, keeps 25 minutes;
S3: the sample of clearing up obtained after S2 is transferred in 50ml teflon crucible, add 5ml nitric acid, 5ml hydrofluorite, 3ml perchloric acid add a cover after in the upper temperature heating of electric hot plate about 1h, then uncap; Electric plate temperature controls at 150-200 DEG C, continues heating silica removal, when being heated to emit the white cigarette of dense perchloric acid or solution residue about 1ml, takes off crucible slightly cold;
S4: add 1ml hydrochloric acid solution after S3, warm dissolving soluble residues, full dose is transferred in 50ml volumetric flask, is settled to graticule, shakes up after cooling with water.
2. heavy metal in soil according to claim 1 measures pre-treating method, it is characterized in that: the sample mass in S1 is accurate to 0.0002g.
3. heavy metal in soil according to claim 1 and 2 measures pre-treating method, it is characterized in that: in S3, heat silica removal process often should shake crucible.
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| CN201610012882.2A CN105466752A (en) | 2016-01-09 | 2016-01-09 | Pretreatment method for determining of heavy metal in soil |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106124605A (en) * | 2016-07-13 | 2016-11-16 | 上海实朴检测技术服务有限公司 | Measure the method for leachable metal in soil |
| CN106370510A (en) * | 2016-10-21 | 2017-02-01 | 天津大学 | Method for microwave digestion of glass body |
| CN106644984A (en) * | 2016-12-29 | 2017-05-10 | 贵州省土壤肥料研究所 | Method and correction factor for determining content of chromium in limestone soil of Guizhou province |
| CN106706606A (en) * | 2016-12-29 | 2017-05-24 | 贵州省土壤肥料研究所 | Method for determining lead content of limestone soil in Guizhou province and correction factor thereof |
| CN106769924A (en) * | 2016-11-30 | 2017-05-31 | 马健 | A kind of method for detecting heavy metal content in soil |
| CN107702961A (en) * | 2017-11-20 | 2018-02-16 | 郑州德析检测技术有限公司 | A kind of method of heavy metal-polluted soil resolution improvement pre-treatment |
| CN107796797A (en) * | 2017-10-17 | 2018-03-13 | 浙江中煤检测有限公司 | The assay method of arsenic, antimony, bismuth, mercury, selenium in a kind of soil |
| CN108120823A (en) * | 2018-01-10 | 2018-06-05 | 伊犁师范学院 | A kind of heavy metal content in soil feature and its potential risk evaluation method and system |
| CN108693016A (en) * | 2018-04-24 | 2018-10-23 | 广东省农业科学院农产品公共监测中心 | A kind of pre-treating method for the detection of batch heavy metal in soil |
| CN109358014A (en) * | 2018-12-13 | 2019-02-19 | 安徽省公众检验研究院有限公司 | A method of detection heavy metal in soil |
| CN109425602A (en) * | 2017-08-24 | 2019-03-05 | 上海利元环保检测技术有限公司 | Soil Copper, zinc, lead, cadmium, nickel, beryllium rapid-digestion method |
| CN111398399A (en) * | 2020-03-31 | 2020-07-10 | 广西壮族自治区地质矿产测试研究中心 | Method for determining silver by inductively coupled plasma mass spectrometry |
| CN112114113A (en) * | 2020-08-26 | 2020-12-22 | 西藏自治区农牧科学院农业质量标准与检测研究所 | Agricultural product heavy metal risk assessment method based on soil-crop system |
| CN112394158A (en) * | 2020-09-27 | 2021-02-23 | 中地宝联(北京)国土资源勘查技术开发集团有限公司 | Evaluation method for human health risks based on soil heavy metal forms |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106124605A (en) * | 2016-07-13 | 2016-11-16 | 上海实朴检测技术服务有限公司 | Measure the method for leachable metal in soil |
| CN106370510A (en) * | 2016-10-21 | 2017-02-01 | 天津大学 | Method for microwave digestion of glass body |
| CN106769924A (en) * | 2016-11-30 | 2017-05-31 | 马健 | A kind of method for detecting heavy metal content in soil |
| CN106644984A (en) * | 2016-12-29 | 2017-05-10 | 贵州省土壤肥料研究所 | Method and correction factor for determining content of chromium in limestone soil of Guizhou province |
| CN106706606A (en) * | 2016-12-29 | 2017-05-24 | 贵州省土壤肥料研究所 | Method for determining lead content of limestone soil in Guizhou province and correction factor thereof |
| CN109425602A (en) * | 2017-08-24 | 2019-03-05 | 上海利元环保检测技术有限公司 | Soil Copper, zinc, lead, cadmium, nickel, beryllium rapid-digestion method |
| CN107796797A (en) * | 2017-10-17 | 2018-03-13 | 浙江中煤检测有限公司 | The assay method of arsenic, antimony, bismuth, mercury, selenium in a kind of soil |
| CN107796797B (en) * | 2017-10-17 | 2020-08-07 | 中煤浙江检测技术有限公司 | Method for measuring arsenic, antimony, bismuth, mercury and selenium in soil |
| CN107702961A (en) * | 2017-11-20 | 2018-02-16 | 郑州德析检测技术有限公司 | A kind of method of heavy metal-polluted soil resolution improvement pre-treatment |
| CN108120823A (en) * | 2018-01-10 | 2018-06-05 | 伊犁师范学院 | A kind of heavy metal content in soil feature and its potential risk evaluation method and system |
| CN108693016A (en) * | 2018-04-24 | 2018-10-23 | 广东省农业科学院农产品公共监测中心 | A kind of pre-treating method for the detection of batch heavy metal in soil |
| CN109358014A (en) * | 2018-12-13 | 2019-02-19 | 安徽省公众检验研究院有限公司 | A method of detection heavy metal in soil |
| CN111398399A (en) * | 2020-03-31 | 2020-07-10 | 广西壮族自治区地质矿产测试研究中心 | Method for determining silver by inductively coupled plasma mass spectrometry |
| CN112114113A (en) * | 2020-08-26 | 2020-12-22 | 西藏自治区农牧科学院农业质量标准与检测研究所 | Agricultural product heavy metal risk assessment method based on soil-crop system |
| CN112394158A (en) * | 2020-09-27 | 2021-02-23 | 中地宝联(北京)国土资源勘查技术开发集团有限公司 | Evaluation method for human health risks based on soil heavy metal forms |
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Application publication date: 20160406 |