CN107202832A - Heavy metal detection method in the soil water termination contaminated stream of Near Antimony Mine Area - Google Patents
Heavy metal detection method in the soil water termination contaminated stream of Near Antimony Mine Area Download PDFInfo
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- CN107202832A CN107202832A CN201710409102.2A CN201710409102A CN107202832A CN 107202832 A CN107202832 A CN 107202832A CN 201710409102 A CN201710409102 A CN 201710409102A CN 107202832 A CN107202832 A CN 107202832A
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Abstract
The invention belongs to heavy metal analysis technical field, and in particular to heavy metal detection method in a kind of native water termination contaminated stream in Near Antimony Mine Area.By based on the sample of the native water termination sampled point collection in Near Antimony Mine Area, using anode voltammetry, using three-electrode system, using carboxylated graphene modified glass-carbon electrode as working electrode, being tested and data processing.The inventive method measure cycle is only 10min, and precision substantially increases minute up to 0.24%, and precision is high, the degree of accuracy is good, convenient, fast and efficient, test limit is relatively low, and measurement sensitivity is higher, is adapted to this complicated Pollution System of the native water termination in Near Antimony Mine Area.
Description
Technical field
The invention belongs to heavy metal analysis technical field, and in particular to heavy metal in a kind of native water termination contaminated stream in Near Antimony Mine Area
Detection method.
Background technology
With the progress of human civilization, industrial development process is more and more faster, demand and exploitation of the mankind to mineral resources
It is growing, it is at the same time, unavoidable along with the deterioration of ecological environment and to nature in the development process to mineral resources
Destruction, resulting heavy metal pollution can not look down upon.The buried metal in underground of exploitation of mineral resources movable handle script of the mankind
Ore in air and earth's surface, by the hydrologic cycles such as rainfall, runoff, sedimentation cause heavy metal element be diffused into river,
In soil, air, ecological environment is polluted, while also the living environment to the mankind constitutes a threat to.
Wherein, antimony ore paneling and selecting is produced during smelting solid waste (ore, ettle, CHARACTERISTICS OF TAILINGS SAND, waste residue etc.) and raw
Production sewage etc. enters mining soil by different approaches and causes heavy metal pollution of soil.Cut by rainfall or snowmelt runoff
Cut, hit, washing away, leaching, the collective effect such as immersion, the various heavy metal contaminants in soil are between soil-footpath stream interface
A variety of physical-chemical reactions such as generation diffusion, disperse, desorption, dissociation, ultimately form mining area soil-water termination heavy metal pollution stream,
Its pollutant contains nutrients such as each heavy metal species, persistent organism and nitrogen, phosphorus etc., is also one kind of non-point pollution
Special representing form.It is special that different heavy metal elements shows different spatial distributions in soil-water termination heavy metal pollution stream
Levy.Because non-ferrous metal mining area soil-water termination heavy metal pollution stream and ecological environment or even human health are closely bound up, always all
It is the research field received much concern in environmental science.This requires fast and accurately to detect Polluted Soil-water termination heavy metal
In contaminated stream, the pollution level of heavy metal.
The content of the invention
The technical problems to be solved by the invention are to provide heavy metal analysis side in a kind of native water termination contaminated stream in Near Antimony Mine Area
Method, the detection method comprises the following steps：
(1) sample and pre-process：Mining area sample area area about 2.5~3.0km2, sampled point is evenly distributed in region,
Sampling density is 0.03~0.04/km2Point, arranges sampled point 125~140 altogether；Ooze strong in the case where natural precipitation intensity is more than
When degree produces runoff, each sampled point gathers earth's surface runoff water 0.8~2.5L of sample, and the liquid collected is kept in dark place and taken back；
Institute's water sampling is shaken up before sample preparation, natural subsidence at least 40min, the non-settlement section in siphon upper strata, then with 0.2 μm of membrane filtration,
Add HNO3PH is acidified between 1.5~3.5, gained water sample is stored refrigerated to post label；
(2) it is then placed in Hyperfrequency waves eliminating stove as the dissolved oxygen being passed through in water sample in inert gas removing water sample before test sample
Carry out micro-wave digestion；
(3) test sample：With anodic stripping voltammetry, working electrode, Pt/ are used as using carboxylated graphene modified glass-carbon electrode
Ti electrodes are used as reference electrode as auxiliary electrode, saturation Ag/AgCl electrodes；Specifically test condition is：The work of enrichment process
Potential is -1.2-1.1V, quiescent time 40s, 300~500s of enrichment time, sweep speed 10mV/s, and water is made under agitation
Heavy metal ion enrichment in sample is on working electrode；Process in leaching working electrode potential is by -0.8-0.3V forward scans, scanning
Speed 10mV/s, makes to be enriched to the heavy metal particle dissolution on working electrode；Register instrument data after completing are determined, then are carried out
The analysis of data；Obtain the content of beary metal in sample；
(4) data processing：Data processing is carried out to the content of beary metal in above-mentioned sample, measurement result is chosen more steady
Group data of the fixed, numeric ratio compared with concentration；Finally calculated, mainly precision, the degree of accuracy and recovery of standard addition calculated,
Contrast the data obtained and result of calculation.
Further, in the native water termination contaminated stream in above-mentioned Near Antimony Mine Area in heavy metal detection method, HNO in the step (1)3
Concentration be 8~13wt%.
Further, it is lazy in the step (2) in the native water termination contaminated stream in above-mentioned Near Antimony Mine Area in heavy metal detection method
Property gas be nitrogen, nitrogen is passed through the time for 10~15min.
Further, in the native water termination contaminated stream in above-mentioned Near Antimony Mine Area in heavy metal detection method, the carboxylic in the step (3)
Base graphite alkene modified glassy carbon electrode is prepared by following methods：By the nano-graphene piece of carboxymethyl functionalization according to solid-liquid
Than 1:1 ratio is added in redistilled water, 30~40min of ultrasonic disperse, obtains carboxy methylation graphene suspension；Glass carbon
Electrode is polished to be cleaned by ultrasonic 4min in absolute ethyl alcohol and redistilled water successively in after minute surface, is dried under infrared lamp；
Take 8~10uL carboxy methylations graphene suspension to be added dropwise with microsyringe to dry under glassy carbon electrode surface, infrared lamp.
Further, in the native water termination contaminated stream in above-mentioned Near Antimony Mine Area in heavy metal detection method, the stirring is stirred for magnetic force
Mix, rotating speed is 200~300rpm.
Compared in prior art, the beneficial effects of the invention are as follows：In the native water termination contaminated stream in Near Antimony Mine Area that the present invention is provided
Heavy metal element detection method, by based on the sample of the native water termination sampled point collection in Near Antimony Mine Area, using anode voltammetry,
Using three-electrode system, using carboxylated graphene modified glass-carbon electrode as working electrode, tested, this method is greatly improved
Minute, and precision is high, the degree of accuracy is good, and convenient, fast and efficient, test limit is relatively low, measurement sensitivity is higher, fits
Close this complicated Pollution System of Near Antimony Mine Area soil-water termination.In addition, the present invention can rapidly detect the degree of pollution, it is
Follow-up improvement, which is safeguarded, provides help, with great application value and social benefit.
Embodiment
The invention provides heavy metal detection method in a kind of native water termination contaminated stream in Near Antimony Mine Area, the detection method include with
Lower step：
(1) sample and pre-process：Mining area sample area area about 2.5~3.0km2, sampled point is evenly distributed in region,
Sampling density is 0.03~0.04/km2Point, arranges sampled point 125~140 altogether；Ooze strong in the case where natural precipitation intensity is more than
When degree produces runoff, each sampled point gathers earth's surface runoff water 0.8~2.5L of sample, and the liquid collected is kept in dark place and taken back；
Institute's water sampling is shaken up before sample preparation, natural subsidence at least 40min, the non-settlement section in siphon upper strata, then with 0.2 μm of membrane filtration,
Add the HNO that concentration is 8~13wt%3PH is acidified between 1.5~3.5, gained water sample is stored refrigerated to post label；
(2) it is then placed in Hyperfrequency waves eliminating stove as the dissolved oxygen being passed through in water sample in inert gas removing water sample before test sample
Carry out micro-wave digestion；
(3) test sample：With anodic stripping voltammetry, working electrode, Pt/ are used as using carboxylated graphene modified glass-carbon electrode
Ti electrodes are used as reference electrode as auxiliary electrode, saturation Ag/AgCl electrodes；Specifically test condition is：The work of enrichment process
Potential is -1.2-1.1V, quiescent time 40s, 300~500s of enrichment time, sweep speed 10mV/s, and water is made under agitation
Heavy metal ion enrichment in sample is on working electrode；Process in leaching working electrode potential is by -0.8-0.3V forward scans, scanning
Speed 10mV/s, makes to be enriched to the heavy metal particle dissolution on working electrode；Register instrument data after completing are determined, then are carried out
The analysis of data；Obtain the content of beary metal in sample；
(4) data processing：Data processing is carried out to the content of beary metal in above-mentioned sample, measurement result is chosen more steady
Group data of the fixed, numeric ratio compared with concentration；Finally calculated, mainly precision, the degree of accuracy and recovery of standard addition calculated,
Contrast the data obtained and result of calculation.
Further, it is lazy in the step (2) in the native water termination contaminated stream in above-mentioned Near Antimony Mine Area in heavy metal detection method
Property gas be nitrogen, nitrogen is passed through the time for 10~15min.
Further, in the native water termination contaminated stream in above-mentioned Near Antimony Mine Area in heavy metal detection method, the carboxylic in the step (3)
Base graphite alkene modified glassy carbon electrode is prepared by following methods：By the nano-graphene piece of carboxymethyl functionalization according to solid-liquid
Than 1:1 ratio is added in redistilled water, 30~40min of ultrasonic disperse, obtains carboxy methylation graphene suspension；Glass carbon
Electrode is polished to be cleaned by ultrasonic 4min in absolute ethyl alcohol and redistilled water successively in after minute surface, is dried under infrared lamp；
Take 8~10uL carboxy methylations graphene suspension to be added dropwise with microsyringe to dry under glassy carbon electrode surface, infrared lamp.
Further, in the native water termination contaminated stream in above-mentioned Near Antimony Mine Area in heavy metal detection method, the stirring is stirred for magnetic force
Mix, rotating speed is 200~300rpm.
The present invention is made further explanation and description below in conjunction with specific embodiment, but and is not so limited the present invention
Protection domain.
Embodiment
Heavy metal detection method comprises the following steps in the soil water termination contaminated stream of Near Antimony Mine Area：
(1) research area is located at the precious Daxing Near Antimony Mine Area of Hunan Lengshuijiang City tinnery, and it is located at Lengshuijiang City mine township, tin
Ji Zhonglian townshiies of mine office boundary position, south is east longitude 111 ° 25 ' 47 away from the km of Lengshuijiang City 13, geographical coordinate "~
111 ° 31 ' 22 ", 27 ° 49 ' 28 of north latitude "~27 ° 43 ' 05 ".Sample area area about 2.6km2, sampled point more uniform distribution grinding
Study carefully in area, sampling density is 0.03/km2Point, arranges sampled point 130 altogether；Produced in natural precipitation intensity more than infltration intensity
During raw runoff, each sampled point gathers earth's surface runoff water sample 2.0L, is put into polyethylene bottle and is taken back after being packed with black plastic bag
Laboratory.Institute's water sampling is shaken up in laboratory, natural subsidence 40min, the non-settlement section in siphon upper strata, then filtered with 0.2 μm
Membrane filtration, adds the HNO that concentration is 10wt%3PH 2.0 is acidified to, gained water sample is stored refrigerated to post label, carries out sampling note
Record；
(2) it is then placed in Hyperfrequency waves eliminating stove as the dissolved oxygen being passed through in water sample in inert gas removing water sample before test sample
Carry out micro-wave digestion；
(3) test sample：With anodic stripping voltammetry, working electrode, Pt/ are used as using carboxylated graphene modified glass-carbon electrode
Ti electrodes are used as reference electrode as auxiliary electrode, saturation Ag/AgCl electrodes；Specifically test condition is：The work of enrichment process
Potential is -1.2-1.1V, quiescent time 40s, enrichment time 500s, sweep speed the 10mV/s, (rotating speed under the conditions of magnetic agitation
200rpm) make heavy metal ion enrichment in water sample to working electrode；Process in leaching working electrode potential by -0.8-0.3V just
To scanning, sweep speed 10mV/s makes to be enriched to the heavy metal particle dissolution on working electrode；Determine register instrument after completing
Data, then carry out the analysis of data；Obtain the content of beary metal in sample；
Wherein, carboxylated graphene modified glass-carbon electrode is prepared by following methods：By the nanometer of carboxymethyl functionalization
Graphene film is according to solid-to-liquid ratio 1:1 ratio is added in redistilled water, ultrasonic disperse 40min, obtains 1mg/mL carboxylic first
Base graphite alkene suspension；Glass-carbon electrode is polished in after minute surface, is cleaned by ultrasonic successively in absolute ethyl alcohol and redistilled water
4min, is dried under infrared lamp；9uL carboxy methylations graphene suspension is taken to be added dropwise in glass-carbon electrode table with microsyringe
Dried under face, infrared lamp；
(4) data processing：Data processing is carried out to the content of beary metal in above-mentioned sample, measurement result is chosen more steady
Group data of the fixed, numeric ratio compared with concentration；Finally calculated, mainly precision, the degree of accuracy and recovery of standard addition calculated,
Contrast the data obtained and result of calculation；
The test result of heavy metal is shown in Table 1 in the soil water termination contaminated stream of Near Antimony Mine Area：
Table 1.
| Heavy metal | Sb | Zn | Cu | Ni | Pb | Cd |
| Average value (mg/L) | 1.1597 | 1.005 | 0.7991 | 0.0074 | 0.0113 | 0.0048 |
Detection method determines the cycle for 10min, and precision is up to 0.24%, and the measure cycle is short, and precision is accurate, fits
Close native water termination pollution complicated and changeable.
Described above is the preferred embodiments of the present invention, it is noted that for those skilled in the art, do not taken off
On the premise of structure of the present invention, various modifications and improvements can be made, these should also be as being considered as protection scope of the present invention,
The practicality of these effects implemented all without the influence present invention and this patent.
Claims (5)
1. heavy metal detection method in the soil water termination contaminated stream of Near Antimony Mine Area, it is characterised in that the detection method comprises the following steps：
(1) sample and pre-process：Mining area sample area area about 2.5~3.0km2, sampled point is evenly distributed in region, is sampled
Density is 0.03~0.04/km2Point, arranges sampled point 125~140 altogether；Produced in natural precipitation intensity more than infltration intensity
During raw runoff, each sampled point gathers earth's surface runoff water 0.8~2.5L of sample, and the liquid collected is kept in dark place and taken back；Sample preparation
It is preceding to shake up institute's water sampling, natural subsidence at least 40min, the non-settlement section in siphon upper strata, then with 0.2 μm of membrane filtration, add
HNO3PH is acidified between 1.5~3.5, gained water sample is stored refrigerated to post label；
(2) it is then placed in Hyperfrequency waves eliminating stove progress as the dissolved oxygen being passed through in water sample in inert gas removing water sample before test sample
Micro-wave digestion；
(3) test sample：With anodic stripping voltammetry, working electrode, Pt/Ti electricity are used as using carboxylated graphene modified glass-carbon electrode
Pole is used as reference electrode as auxiliary electrode, saturation Ag/AgCl electrodes；Specifically test condition is：The work potential of enrichment process
For -1.2-1.1V, quiescent time 40s, 300~500s of enrichment time, sweep speed 10mV/s, make under agitation in water sample
Heavy metal ion enrichment on working electrode；Process in leaching working electrode potential is by -0.8-0.3V forward scans, sweep speed
10mV/s, makes to be enriched to the heavy metal particle dissolution on working electrode；Register instrument data after completing are determined, then carry out data
Analysis；Obtain the content of beary metal in sample；
(4) data processing：Data processing is carried out to the content of beary metal in above-mentioned sample, selection measurement result is more stable, number
Value compares the group data of concentration；Finally calculated, mainly precision, the degree of accuracy and recovery of standard addition are calculated, contrasted
The data obtained and result of calculation.
2. heavy metal detection method in the native water termination contaminated stream in Near Antimony Mine Area according to claim 1, it is characterised in that described
HNO in step (1)3Concentration be 8~13wt%.
3. heavy metal detection method in the native water termination contaminated stream in Near Antimony Mine Area according to claim 1, it is characterised in that described
Inert gas in step (2) is nitrogen, and the time that is passed through of nitrogen is 10~15min.
4. heavy metal detection method in the native water termination contaminated stream in Near Antimony Mine Area according to claim 1, it is characterised in that described
Carboxylated graphene modified glass-carbon electrode in step (3) is prepared by following methods：By the nanometer stone of carboxymethyl functionalization
Black alkene piece is according to solid-to-liquid ratio 1:1 ratio is added in redistilled water, 30~40min of ultrasonic disperse, obtains carboxymethyl fossil
Black alkene suspension；Glass-carbon electrode is polished to be cleaned by ultrasonic 4min in absolute ethyl alcohol and redistilled water successively in after minute surface, then
In drying under infrared lamp；8~10uL carboxy methylations graphene suspension is taken to be added dropwise in glassy carbon electrode surface with microsyringe, it is red
Dried under outer lamp.
5. heavy metal detection method in the native water termination contaminated stream in Near Antimony Mine Area according to claim 1, it is characterised in that described
Stir as magnetic agitation, rotating speed is 200~300rpm.
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