CN107702961A - A kind of method of heavy metal-polluted soil resolution improvement pre-treatment - Google Patents
A kind of method of heavy metal-polluted soil resolution improvement pre-treatment Download PDFInfo
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- CN107702961A CN107702961A CN201711156161.XA CN201711156161A CN107702961A CN 107702961 A CN107702961 A CN 107702961A CN 201711156161 A CN201711156161 A CN 201711156161A CN 107702961 A CN107702961 A CN 107702961A
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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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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Abstract
The invention discloses a kind of method that heavy metal-polluted soil clears up improvement pre-treatment, belong to heavy metal detection method field.Aim to provide one kind and greatly shorten the time, on the premise of reducing manpower and materials, have no effect on the method that the heavy metal-polluted soil resolution of laboratory test results improves pre-treatment.Methods described, comprise the following steps：Choose and weigh laboratory sample；Clear up, detected with flame graphite furnace integral type atomic absorption spectrophotometer, data calculate.
Description
Technical field
The invention belongs to heavy metal detection method field, especially a kind of side of heavy metal-polluted soil resolution improvement pre-treatment
Method.
Background technology
The detection method of national standard heavy metal content is as follows：
Copper zinc：The accurate sample for weighing 0.2g or so adds 10mL hydrochloric acid in fume hood in polytetrafluoroethylene (PTFE) crucible
Electric hot plate on, make sample preliminary exposition, temperature setting is 80 DEG C and is heated to 3mL or so, removes slightly cold, then adds 5mL nitric acid,
5mL hydrofluoric acid, 3mL perchloric acid, 150 DEG C of capping medium temperature are cleared up one hour, uncap except silicon, be heated to emitting dense perchloric acid white cigarette
When, capping, black organic carbon compound is fully decomposed, after the black organic matter on crucible disappears, uncap and drive white cigarette and steam
It is thick to content.Remove slightly cold, add 1+1 nitric acid 1mL, transfer the solution into 50mL volumetric flasks, add 5mL mass fractions 5%
Nitric acid bright-coloured, with deionized water constant volume.
Lead cadmium：The accurate sample for weighing 0.2g or so adds 5mL hydrochloric acid in fume hood in polytetrafluoroethylene (PTFE) crucible
On electric hot plate, make sample preliminary exposition, temperature setting is 80 DEG C and is heated to 3mL or so, removes slightly cold, then adds 5mL nitric acid, 4mL
Hydrofluoric acid, 2mL perchloric acid, 150 DEG C of capping medium temperature are cleared up one hour, uncap except silicon, when being heated to emitting dense perchloric acid white cigarette, add
Lid, makes black organic carbon compound fully decompose, and after the black organic matter on crucible disappears, uncaps and drives white cigarette and steam to content
Thing is thick.Remove slightly cold, add 1+1 nitric acid 1mL, transfer the solution into 25mL volumetric flasks, add the phosphoric acid of 3mL weight fractions 5%
The ammonium of hydrogen two, with deionized water constant volume.
Nickel：The accurate sample for weighing 0.2g or so adds 10mL hydrochloric acid in fume hood in polytetrafluoroethylene (PTFE) crucible
On electric hot plate, make sample preliminary exposition, temperature setting is 80 DEG C and is heated to 3mL or so, removes slightly cold, then adds 5mL nitric acid, 5mL
Hydrofluoric acid, 3mL perchloric acid, 150 DEG C of capping medium temperature are cleared up one hour, uncap except silicon, when being heated to emitting dense perchloric acid white cigarette, add
Lid, makes black organic carbon compound fully decompose, and after the black organic matter on crucible disappears, uncaps and drives white cigarette and steam to content
Thing is thick.Remove slightly cold, add 1+1 nitric acid 1mL, transfer the solution into 50mL volumetric flasks, with deionized water constant volume.
Chromium：The accurate sample for weighing 0.2g or so adds 10mL hydrochloric acid in fume hood in polytetrafluoroethylene (PTFE) crucible
On electric hot plate, make sample preliminary exposition, temperature setting is 80 DEG C and is heated to 3mL or so, removes slightly cold, then adds 5mL nitric acid, 5mL
Hydrofluoric acid, 3mL perchloric acid, 150 DEG C of capping medium temperature are cleared up one hour, uncap except silicon, when being heated to emitting dense perchloric acid white cigarette, add
Lid, makes black organic carbon compound fully decompose, and after the black organic matter on crucible disappears, uncaps and drives white cigarette and steam to content
Thing is thick.Remove slightly cold, add 1+1 nitric acid 1mL, transfer the solution into 50mL volumetric flasks, add 3mL10% ammonium chloride, spend
Ionized water constant volume.
It is longer the time required to this method, consume substantial amounts of manpower and materials.
The content of the invention
For above-mentioned deficiency, the present invention is intended to provide one kind greatly shortens the time, on the premise of reducing manpower and materials, not
Influence the method for the heavy metal-polluted soil resolution improvement pre-treatment of laboratory test results.
In order to realize above-mentioned technique effect, technical scheme provided by the invention is such：A kind of heavy metal-polluted soil resolution
The method for improveing pre-treatment, comprises the following steps：；
Step 1：Choose and weigh laboratory sample；
Step 2：The accurate sample for weighing 0.2g adds electricity of the 10mL hydrochloric acid in fume hood in polytetrafluoroethylene (PTFE) crucible
On hot plate, make sample preliminary exposition, temperature setting is 80 DEG C and is heated to 3mL or so, removes slightly cold, then adds 5mL nitric acid, 5mL hydrogen
Fluoric acid, 3mL perchloric acid, 150 DEG C of capping medium temperature are cleared up one hour, uncap except silicon, when being heated to emitting dense perchloric acid white cigarette, add
Lid, makes black organic carbon compound fully decompose, and after the black organic matter on crucible disappears, uncaps and drives white cigarette and steam to content
Thing is thick；Resolution to black organic matter disappears, and removes slightly cold, adds 1+1 nitric acid 1mL, warm dissolving soluble residues, directly determines
Hold to 25mL volumetric flasks；
Step 3：Detected with flame graphite furnace integral type atomic absorption spectrophotometer；
Step 4：Data calculate.
Wherein, described step 2 is further comprising the steps of after 25mL volumetric flasks are settled to：
Step s1：The nitric acid bright-coloured that 5mL samples add 1mL mass fractions 5% is accurately pipetted with pipette, with deionized water constant volume
Into the soft test tube of 10mL plastics；
Step s2：The diammonium hydrogen phosphate that 5mL samples add 1mL weight fractions 5% is accurately pipetted with pipette, uses deionized water
It is settled in the soft test tube of 10mL plastics；
Step s3：The ammonium chloride that 5mL samples add 1mL10% is accurately pipetted with pipette, 10mL is settled to deionized water
In the soft test tube of plastics；
Step s4：Directly use stoste.
The method of the invention and national standard method detection gained sample data deviation are less than≤10%, standard sample all in matter
In the range of control；Tested suitable for detection, greatly shorten the time, on the premise of reducing manpower and materials, have no effect on the detection of experiment
As a result.
Brief description of the drawings
Fig. 1 is the Fitting curve equation figure of lead；
Fig. 2 is the Fitting curve equation figure of cadmium；
Fig. 3 is the Fitting curve equation figure of copper；
Fig. 4 is the Fitting curve equation figure of zinc；
Fig. 5 is the Fitting curve equation figure of nickel；
Fig. 6 is the Fitting curve equation figure of chromium.
Embodiment
With reference to embodiment, the claim of the present invention is described in further detail, but not formed pair
Any restrictions of the present invention, any limited number of time modification made in the claims in the present invention protection domain, still the present invention's
In claims.
Embodiment 1
National standard method：
Copper zinc：The accurate sample for weighing 0.2g or so adds 10mL hydrochloric acid in fume hood in polytetrafluoroethylene (PTFE) crucible
Electric hot plate on, make sample preliminary exposition, temperature setting is 80 DEG C and is heated to 3mL or so, removes slightly cold, then adds 5mL nitric acid,
5mL hydrofluoric acid, 3mL perchloric acid, 150 DEG C of capping medium temperature are cleared up one hour, uncap except silicon, be heated to emitting dense perchloric acid white cigarette
When, capping, black organic carbon compound is fully decomposed, after the black organic matter on crucible disappears, uncap and drive white cigarette and steam
It is thick to content.Remove slightly cold, add 1+1 nitric acid 1mL, transfer the solution into 50mL volumetric flasks, add 5mL mass fractions 5%
Nitric acid bright-coloured, with deionized water constant volume.
Lead cadmium：The accurate sample for weighing 0.2g or so adds 5mL hydrochloric acid in fume hood in polytetrafluoroethylene (PTFE) crucible
On electric hot plate, make sample preliminary exposition, temperature setting is 80 DEG C and is heated to 3mL or so, removes slightly cold, then adds 5mL nitric acid, 4mL
Hydrofluoric acid, 2mL perchloric acid, 150 DEG C of capping medium temperature are cleared up one hour, uncap except silicon, when being heated to emitting dense perchloric acid white cigarette, add
Lid, makes black organic carbon compound fully decompose, and after the black organic matter on crucible disappears, uncaps and drives white cigarette and steam to content
Thing is thick.Remove slightly cold, add 1+1 nitric acid 1mL, transfer the solution into 25mL volumetric flasks, add the phosphoric acid of 3mL weight fractions 5%
The ammonium of hydrogen two, with deionized water constant volume.
Nickel：The accurate sample for weighing 0.2g or so adds 10mL hydrochloric acid in fume hood in polytetrafluoroethylene (PTFE) crucible
On electric hot plate, make sample preliminary exposition, temperature setting is 80 DEG C and is heated to 3mL or so, removes slightly cold, then adds 5mL nitric acid, 5mL
Hydrofluoric acid, 3mL perchloric acid, 150 DEG C of capping medium temperature are cleared up one hour, uncap except silicon, when being heated to emitting dense perchloric acid white cigarette, add
Lid, makes black organic carbon compound fully decompose, and after the black organic matter on crucible disappears, uncaps and drives white cigarette and steam to content
Thing is thick.Remove slightly cold, add 1+1 nitric acid 1mL, transfer the solution into 50mL volumetric flasks, with deionized water constant volume.
Chromium：The accurate sample for weighing 0.2g or so adds 10mL hydrochloric acid in fume hood in polytetrafluoroethylene (PTFE) crucible
On electric hot plate, make sample preliminary exposition, temperature setting is 80 DEG C and is heated to 3mL or so, removes slightly cold, then adds 5mL nitric acid, 5mL
Hydrofluoric acid, 3mL perchloric acid, 150 DEG C of capping medium temperature are cleared up one hour, uncap except silicon, when being heated to emitting dense perchloric acid white cigarette, add
Lid, makes black organic carbon compound fully decompose, and after the black organic matter on crucible disappears, uncaps and drives white cigarette and steam to content
Thing is thick.Remove slightly cold, add 1+1 nitric acid 1mL, transfer the solution into 50mL volumetric flasks, add 3mL10% ammonium chloride, spend
Ionized water constant volume.
Embodiment 2
The present invention：
1. the accurate sample for weighing 0.2g or so in polytetrafluoroethylene (PTFE) crucible, adds electricity of the 10mL hydrochloric acid in fume hood
On hot plate, make sample preliminary exposition, temperature setting is 80 DEG C and is heated to 3mL or so, removes slightly cold, then adds 5mL nitric acid, 5mL hydrogen
Fluoric acid, 3mL perchloric acid, 150 DEG C of capping medium temperature are cleared up one hour, uncap except silicon, when being heated to emitting dense perchloric acid white cigarette, add
Lid, makes black organic carbon compound fully decompose, and after the black organic matter on crucible disappears, uncaps and drives white cigarette and steam to content
Thing is thick.Resolution to black organic matter disappears, and removes slightly cold, adds 1+1 nitric acid 1mL, warm dissolving soluble residues, directly determines
Hold to 25mL volumetric flasks..
2. bronze medal zinc：The nitric acid bright-coloured that 5mL samples add 1mL mass fractions 5% is accurately pipetted with pipette, with deionized water constant volume
Into the soft test tube of 10mL plastics,
Lead cadmium：The diammonium hydrogen phosphate that 5mL samples add 1mL weight fractions 5% is accurately pipetted with pipette, is determined with deionized water
Hold into the soft test tube of 10mL plastics,
Chromium：The ammonium chloride that 5mL samples add 1mL10% is accurately pipetted with pipette, 10mL plastics are settled to deionized water
In soft test tube.
Nickel：Directly use stoste.
Experiment detection is carried out with flame graphite furnace integral type atomic absorption spectrophotometer
Refer to accompanying drawing 1-6.
Wherein, Fig. 1 is represented：Lead-Fitting curve equation：Y=0.0054*x+0.0009R values：0.9998；
Wherein, Fig. 2 is represented：Cadmium-Fitting curve equation：Y=0.0551*x-0.0008R values：0.9999；
Wherein, Fig. 3 is represented：Copper-Fitting curve equation：Y=0.1892*x+0.0005R values：0.9999；
Wherein, Fig. 4 is represented：Zinc-Fitting curve equation：Y=0.7125*x+0.0004R values：0.9998；
Wherein, Fig. 5 is represented：Nickel-Fitting curve equation：Y=0.1349*x-0.0001R values：0.9999；
Wherein, Fig. 6 is represented：Chromium-Fitting curve equation：Y=0.0434*x+0.0006R values：0.9997.
Data calculate
Method one detects data result：
Method two detects data result：
Data comparison
● sample data is analyzed
● standard sample is analyzed
Conclusion
● being found by the data comparison of two methods, sample data deviation is less than≤10%,
● standard sample all in the range of Quality Control,
Pretreatment process merges, and detection experiment is applied in the separated pre-treating method of constant volume step, when greatly shortening
Between, on the premise of reducing manpower and materials, have no effect on the testing result of experiment.
Above-described is only presently preferred embodiments of the present invention, all timess done in the range of the spirit and principles in the present invention
What modifications, equivalent substitutions and improvements etc., should be included within the scope of the present invention.
Claims (2)
- A kind of 1. method of heavy metal-polluted soil resolution improvement pre-treatment, it is characterised in that comprise the following steps：；Step 1：Choose and weigh laboratory sample；Step 2：The accurate sample for weighing 0.2g adds electric hot plate of the 10mL hydrochloric acid in fume hood in polytetrafluoroethylene (PTFE) crucible On, making sample preliminary exposition, temperature setting is 80 DEG C and is heated to 3mL or so, removes slightly cold, then adds 5mL nitric acid, 5mL hydrofluoric acid, 3mL perchloric acid, 150 DEG C of capping medium temperature is cleared up one hour, uncapped except silicon, when being heated to emitting dense perchloric acid white cigarette, capping, makes black Color organic carbon compound is fully decomposed, and after the black organic matter on crucible disappears, is uncapped and is driven white cigarette and steam sticky to content Shape；Resolution to black organic matter disappears, and removes slightly cold, adds 1+1 nitric acid 1mL, warm dissolving soluble residues, is directly settled to 25mL volumetric flasks；Step 3：Detected with flame graphite furnace integral type atomic absorption spectrophotometer；Step 4：Data calculate.
- 2. the method for a kind of heavy metal-polluted soil resolution improvement pre-treatment according to claim 1, it is characterised in that described Step 2 is further comprising the steps of after 25mL volumetric flasks are settled to：Step s1：The nitric acid bright-coloured that 5mL samples add 1mL mass fractions 5% is accurately pipetted with pipette, is settled to deionized water In the soft test tube of 10mL plastics；Step s2：The diammonium hydrogen phosphate that 5mL samples add 1mL weight fractions 5% is accurately pipetted with pipette, with deionized water constant volume Into the soft test tube of 10mL plastics；Step s3：The ammonium chloride that 5mL samples add 1mL10% is accurately pipetted with pipette, 10mL plastics are settled to deionized water In soft test tube；Step s4：Directly use stoste.
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Cited By (5)
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| CN109799198A (en) * | 2018-12-19 | 2019-05-24 | 陕西迈拓克能源科技有限公司 | A kind of heavy metal-polluted soil characterization processes |
| CN110618020A (en) * | 2019-09-12 | 2019-12-27 | 广西博世科环保科技股份有限公司 | Method for rapidly digesting heavy metal soil sample |
| 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 |
| CN113533015A (en) * | 2018-04-24 | 2021-10-22 | 广东省农业科学院农业质量标准与监测技术研究所 | Pretreatment method for detecting heavy metals in batch soil |
| CN114427996A (en) * | 2020-09-25 | 2022-05-03 | 中国石油化工股份有限公司 | Method for dissolving rhodium in rhodium-containing waste liquid and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113533015A (en) * | 2018-04-24 | 2021-10-22 | 广东省农业科学院农业质量标准与监测技术研究所 | Pretreatment method for detecting heavy metals in batch soil |
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| 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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