CN107202832B - 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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- CN107202832B CN107202832B CN201710409102.2A CN201710409102A CN107202832B CN 107202832 B CN107202832 B CN 107202832B CN 201710409102 A CN201710409102 A CN 201710409102A CN 107202832 B CN107202832 B CN 107202832B
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Abstract
The invention belongs to heavy metal analysis technical fields, and in particular to heavy metal detection method in a kind of Near Antimony Mine Area soil water termination contaminated stream.By using anode voltammetry, using three-electrode system, using carboxylated graphene modified glass-carbon electrode as working electrode, carrying out test and data processing based on the sample that Near Antimony Mine Area soil water termination sampled point acquires.The method of the present invention measurement period is only 10min, and precision substantially increases minute up to 0.24%, and precision is high, accuracy is good, convenient, fast and efficient, detection limit is lower, and measurement sensitivity is higher, is suitble to the Pollution System of this complexity of Near Antimony Mine Area soil-water termination.
Description
Technical field
The invention belongs to heavy metal analysis technical fields, and in particular to heavy metal in a kind of Near Antimony Mine Area soil water termination contaminated stream
Detection method.
Background technique
With the progress of human civilization, industrial development process is getting faster, demand of the mankind to mineral resources and exploitation
It is growing, at the same time, inevitably 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 is exposed in atmosphere and earth's surface, by the hydrologic cycles such as rainfall, runoff, sedimentation make heavy metal element be diffused into river,
In soil, atmosphere, ecological environment is polluted, while also being constituted a threat to the living environment of the mankind.
Wherein, antimony ore paneling and the solid waste (ore, ettle, CHARACTERISTICS OF TAILINGS SAND, waste residue etc.) for selecting smelting to generate in the process and life
Sewage etc. is produced to enter mining soil by different approaches and lead to heavy metal pollution of soil.It is cut by rainfall or snowmelt runoff
It cuts, hit, washing away, leaching, the collective effects such as immersion, the various heavy metal contaminants in soil are between soil-diameter stream interface
A variety of physical-chemical reactions such as diffusion, disperse, desorption, dissociation occur, ultimately form mining area soil-water termination heavy metal pollution stream,
Its pollutant contains one kind of nutrients such as each heavy metal species, persistent organism and nitrogen, phosphorus etc. and 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
Sign.Since 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 being concerned 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.
Summary of the invention
Technical problem to be solved by the invention is to provide heavy metal analysis sides in a kind of Near Antimony Mine Area soil water termination contaminated stream
Method, detection method includes the following steps for this:
(1) it samples and pre-processes: mining area sampling 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；It is greater than lower seep by force in natural precipitation intensity
When degree generates runoff, each sampled point acquires earth's surface runoff water 0.8~2.5L of sample, and collected liquid is kept in dark place and is taken back；
Institute's water sampling is shaken up before sample preparation, natural subsidence at least 40min, the non-settlement section in siphon upper layer, then with 0.2 μm of membrane filtration,
HNO is added3PH is acidified between 1.5~3.5, gained water sample is stored refrigerated to post label；
(2) Hyperfrequency waves eliminating stove is then placed in as the dissolved oxygen being passed through in inert gas removing water sample in water sample before test sample
Carry out micro-wave digestion；
(3) test sample: with anodic stripping voltammetry, using carboxylated graphene modified glass-carbon electrode as working electrode, Pt/
Ti electrode is saturated Ag/AgCl electrode as reference electrode as auxiliary electrode；Specific test condition are as follows: the work of enrichment process
Potential is -1.2-1.1V, quiescent time 40s, 300~500s of enrichment time, and scanning speed 10mV/s makes water under agitation
On heavy metal ion enrichment to working electrode in sample；Process in leaching working electrode potential is by -0.8-0.3V forward scan, scanning
Rate 10mV/s dissolves out the heavy metal particle being enriched on working electrode；Register instrument data after measurement is completed, then carry 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, it is more steady to choose measurement result
Fixed, numerical value compares the group data of concentration；It is finally calculated, mainly precision, accuracy and recovery of standard addition is calculated,
Compare the data obtained and calculated result.
Further, in above-mentioned Near Antimony Mine Area soil water termination contaminated stream in heavy metal detection method, HNO in the step (1)3
Concentration be 8~13wt%.
Further, lazy in the step (2) in above-mentioned Near Antimony Mine Area soil water termination contaminated stream in heavy metal detection method
Property gas be nitrogen, nitrogen be passed through the time be 10~15min.
Further, the carboxylic in above-mentioned Near Antimony Mine Area soil water termination contaminated stream in heavy metal detection method, 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
Ratio than 1:1 is added in secondary distilled water, and 30~40min of ultrasonic disperse obtains carboxy methylation graphene suspension；Glass carbon
Electrode is polished in after mirror surface, is successively cleaned by ultrasonic 4min in dehydrated alcohol and secondary distilled water, dries under infrared lamp；
It takes 8~10uL carboxy methylation graphene suspension to be added dropwise with microsyringe to dry under glassy carbon electrode surface, infrared lamp.
Further, in above-mentioned Near Antimony Mine Area soil water termination contaminated stream in heavy metal detection method, the stirring is stirred for magnetic force
It mixes, revolving speed is 200~300rpm.
It is compared in the prior art, the beneficial effects of the present invention are: in soil water termination contaminated stream in Near Antimony Mine Area provided by the invention
Heavy metal element detection method, by based on the sample that Near Antimony Mine Area soil water termination sampled point acquires, using anode voltammetry,
It is tested using three-electrode system using carboxylated graphene modified glass-carbon electrode as working electrode, this method greatly improves
Minute, and precision is high, accuracy is good, and convenient, fast and efficient, detection limit is lower, and measurement sensitivity is higher, fits
Close the Pollution System of this complexity of Near Antimony Mine Area soil-water termination.In addition, the present invention can rapidly detect the degree of pollution, it is
Subsequent improvement maintenance provides help, has great application value and social benefit.
Specific embodiment
The present invention provides heavy metal detection method in a kind of Near Antimony Mine Area soil water termination contaminated stream, the detection method include with
Lower step:
(1) it samples and pre-processes: mining area sampling 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；It is greater than lower seep by force in natural precipitation intensity
When degree generates runoff, each sampled point acquires earth's surface runoff water 0.8~2.5L of sample, and collected liquid is kept in dark place and is taken back；
Institute's water sampling is shaken up before sample preparation, natural subsidence at least 40min, the non-settlement section in siphon upper layer, then with 0.2 μm of membrane filtration,
The HNO that concentration is 8~13wt% is added3PH is acidified between 1.5~3.5, gained water sample is stored refrigerated to post label；
(2) Hyperfrequency waves eliminating stove is then placed in as the dissolved oxygen being passed through in inert gas removing water sample in water sample before test sample
Carry out micro-wave digestion；
(3) test sample: with anodic stripping voltammetry, using carboxylated graphene modified glass-carbon electrode as working electrode, Pt/
Ti electrode is saturated Ag/AgCl electrode as reference electrode as auxiliary electrode；Specific test condition are as follows: the work of enrichment process
Potential is -1.2-1.1V, quiescent time 40s, 300~500s of enrichment time, and scanning speed 10mV/s makes water under agitation
On heavy metal ion enrichment to working electrode in sample；Process in leaching working electrode potential is by -0.8-0.3V forward scan, scanning
Rate 10mV/s dissolves out the heavy metal particle being enriched on working electrode；Register instrument data after measurement is completed, then carry 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, it is more steady to choose measurement result
Fixed, numerical value compares the group data of concentration；It is finally calculated, mainly precision, accuracy and recovery of standard addition is calculated,
Compare the data obtained and calculated result.
Further, lazy in the step (2) in above-mentioned Near Antimony Mine Area soil water termination contaminated stream in heavy metal detection method
Property gas be nitrogen, nitrogen be passed through the time be 10~15min.
Further, the carboxylic in above-mentioned Near Antimony Mine Area soil water termination contaminated stream in heavy metal detection method, 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
Ratio than 1:1 is added in secondary distilled water, and 30~40min of ultrasonic disperse obtains carboxy methylation graphene suspension；Glass carbon
Electrode is polished in after mirror surface, is successively cleaned by ultrasonic 4min in dehydrated alcohol and secondary distilled water, dries under infrared lamp；
It takes 8~10uL carboxy methylation graphene suspension to be added dropwise with microsyringe to dry under glassy carbon electrode surface, infrared lamp.
Further, in above-mentioned Near Antimony Mine Area soil water termination contaminated stream in heavy metal detection method, the stirring is stirred for magnetic force
It mixes, revolving speed is 200~300rpm.
Below in conjunction with specific embodiment, the present invention will be further explained and explanation, but is not intended to limit the present invention
Protection scope.
Embodiment
Heavy metal detection method in the soil water termination contaminated stream of Near Antimony Mine Area the following steps are included:
(1) research area is located at the precious Daxing Near Antimony Mine Area of Hunan Lengshuijiang City tinnery, it is located at Lengshuijiang City mine township, tin
At the township Ji Zhonglian, mine office boundary position, south is east longitude 111 ° 25 ' 47 away from 13 km of Lengshuijiang City, geographical coordinate "~
111 ° 31 ' 22 ", 27 ° 49 ' 28 of north latitude "~27 ° 43 ' 05 ".Sampling 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；It is produced in natural precipitation intensity greater than infltration intensity
When raw runoff, each sampled point acquires earth's surface runoff water sample 2.0L, is put into polyethylene bottle and takes 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 layer, then is filtered with 0.2 μm
The HNO that concentration is 10wt% is added in film filtering3It is acidified to pH 2.0, gained water sample is stored refrigerated to post label, carries out sampling note
Record；
(2) Hyperfrequency waves eliminating stove is then placed in as the dissolved oxygen being passed through in inert gas removing water sample in water sample before test sample
Carry out micro-wave digestion；
(3) test sample: with anodic stripping voltammetry, using carboxylated graphene modified glass-carbon electrode as working electrode, Pt/
Ti electrode is saturated Ag/AgCl electrode as reference electrode as auxiliary electrode；Specific test condition are as follows: the work of enrichment process
Potential is -1.2-1.1V, quiescent time 40s, enrichment time 500s, scanning speed 10mV/s, under the conditions of magnetic agitation (revolving speed
200rpm) make on the heavy metal ion enrichment to working electrode in water sample；Process in leaching working electrode potential by -0.8-0.3V just
To scanning, sweep speed 10mV/s dissolves out the heavy metal particle being enriched on working electrode；Register instrument after measurement is completed
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 added in secondary distilled water according to the ratio of solid-to-liquid ratio 1:1, ultrasonic disperse 40min, obtains the carboxylic first of 1mg/mL
Base graphite alkene suspension；Glass-carbon electrode is polished in after mirror surface, is successively cleaned by ultrasonic in dehydrated alcohol and secondary distilled water
4min is dried under infrared lamp；9uL carboxy methylation graphene suspension is taken to be added dropwise in glass-carbon electrode table with microsyringe
Face is dried under infrared lamp；
(4) data processing: data processing is carried out to the content of beary metal in above-mentioned sample, it is more steady to choose measurement result
Fixed, numerical value compares the group data of concentration；It is finally calculated, mainly precision, accuracy and recovery of standard addition is calculated,
Compare the data obtained and calculated result；
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 measures the period as 10min, and precision is up to 0.24%, and the measurement period is short, and precision is accurate, fits
Close native water termination pollution complicated and changeable.
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art, is not being taken off
Under the premise of from structure of the invention, various modifications and improvements can be made, these should also be as being considered as protection scope of the present invention,
These all will not influence the practicability of effect and this patent that the present invention is implemented.
Claims (5)
1. heavy metal detection method in the soil water termination contaminated stream of Near Antimony Mine Area, which is characterized in that detection method includes the following steps for this:
(1) it samples and pre-processes: mining area 2.5~3.0km of sampling area area2, sampled point is evenly distributed in region, oversampling
Degree is 0.03~0.04/km2Point arranges sampled point 125~140 altogether；It is generated in natural precipitation intensity greater than infltration intensity
When runoff, each sampled point acquires earth's surface runoff water 0.8~2.5L of sample, and collected liquid is kept in dark place and is taken back；Before sample preparation
Institute's water sampling is shaken up, natural subsidence at least 40min, the non-settlement section in siphon upper layer, then with 0.2 μm of membrane filtration, is added
HNO3PH is acidified between 1.5~3.5, gained water sample is stored refrigerated to post label；
(2) dissolved oxygen being passed through before test sample into water sample in inert gas removing water sample, is then placed in Hyperfrequency waves eliminating stove progress
Micro-wave digestion；
(3) test sample: with anodic stripping voltammetry, using carboxylated graphene modified glass-carbon electrode as working electrode, Pt/Ti electricity
Pole is saturated Ag/AgCl electrode as reference electrode as auxiliary electrode；Specific test condition are as follows: the work potential of enrichment process
Make water sample under agitation for -1.2~1.1V, quiescent time 40s, 300~500s of enrichment time, scanning speed 10mV/s
In heavy metal ion enrichment to working electrode on；Process in leaching working electrode potential is by -0.8~0.3V forward scan, scanning
Rate 10mV/s dissolves out the heavy metal particle being enriched on working electrode；Register instrument data after measurement is completed, then carry 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, selection measurement result is more stable, counts
Value compares the group data of concentration；It is finally calculated, mainly precision, accuracy and recovery of standard addition is calculated, compared
The data obtained and calculated result.
2. heavy metal detection method in soil water termination contaminated stream in Near Antimony Mine Area according to claim 1, which is characterized in that described
HNO in step (1)3Concentration be 8~13wt%.
3. heavy metal detection method in soil water termination contaminated stream in Near Antimony Mine Area according to claim 1, which is characterized 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 soil water termination contaminated stream in Near Antimony Mine Area according to claim 1, which is characterized 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 added in secondary distilled water according to the ratio of solid-to-liquid ratio 1:1, and 30~40min of ultrasonic disperse obtains carboxymethyl fossil
Black alkene suspension；Glass-carbon electrode is polished to be successively cleaned by ultrasonic 4min in after mirror surface in dehydrated alcohol and secondary distilled water, then
It is dried under infrared lamp；8~10 μ L carboxy methylation graphene suspensions are taken to be added dropwise in glassy carbon electrode surface with microsyringe, it is red
It is dried under outer lamp.
5. heavy metal detection method in soil water termination contaminated stream in Near Antimony Mine Area according to claim 1, which is characterized in that described
Stirring is magnetic agitation, and revolving speed is 200~300rpm.
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