CN109270152A - The visualization of presence detection method of heavy metal arsenic in a kind of environmental water sample - Google Patents
The visualization of presence detection method of heavy metal arsenic in a kind of environmental water sample Download PDFInfo
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- 229910052785 arsenic Inorganic materials 0.000 title claims abstract description 90
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 title claims abstract description 90
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 230000007613 environmental effect Effects 0.000 title claims abstract description 33
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 30
- 238000001514 detection method Methods 0.000 title claims abstract description 17
- 238000012800 visualization Methods 0.000 title claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 104
- 235000014653 Carica parviflora Nutrition 0.000 claims abstract description 35
- 238000001179 sorption measurement Methods 0.000 claims abstract description 28
- 238000010521 absorption reaction Methods 0.000 claims abstract description 20
- GOPYZMJAIPBUGX-UHFFFAOYSA-N [O-2].[O-2].[Mn+4] Chemical class [O-2].[O-2].[Mn+4] GOPYZMJAIPBUGX-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000003869 coulometry Methods 0.000 claims abstract description 4
- 241000243321 Cnidaria Species 0.000 claims abstract 11
- 238000005259 measurement Methods 0.000 claims description 59
- 239000000243 solution Substances 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 17
- 229910052748 manganese Inorganic materials 0.000 claims description 17
- 239000011572 manganese Substances 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 12
- 238000009423 ventilation Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 10
- 238000004090 dissolution Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 230000003647 oxidation Effects 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000008247 solid mixture Substances 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 8
- 238000004364 calculation method Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000002156 adsorbate Substances 0.000 claims description 6
- 239000003463 adsorbent Substances 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 238000010790 dilution Methods 0.000 claims description 4
- 239000012895 dilution Substances 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 claims description 3
- 229910001451 bismuth ion Inorganic materials 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 238000009963 fulling Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- 229910001437 manganese ion Inorganic materials 0.000 claims description 3
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 2
- 241000790917 Dioxys <bee> Species 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 6
- 244000132059 Carica parviflora Species 0.000 description 24
- 238000005516 engineering process Methods 0.000 description 4
- 238000007689 inspection Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000003183 carcinogenic agent Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- GOLCXWYRSKYTSP-UHFFFAOYSA-N arsenic trioxide Inorganic materials O1[As]2O[As]1O2 GOLCXWYRSKYTSP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- -1 compound arsenic trioxide Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 238000001676 hydride generation atomic fluorescence spectroscopy Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000013022 venting Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/42—Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte
- G01N27/423—Coulometry
Abstract
The invention discloses a kind of visualization of presence detection methods of heavy metal arsenic in environmental water sample, this method first passes through modified manganese dioxide and adsorbs to heavy metal arsenic in environmental water sample, second adsorption is carried out to the environmental water sample after primary absorption by modified natural coral again, is then measured using content of the coulometry instrument to arsenic in each sample liquid.By the present invention in that with modified manganese dioxide and modified natural coral, pentavalent arsenic in environmental water sample is adsorbed, while measuring adsorption effect, achievees the purpose that detect heavy metal arsenic in environmental water sample, provide new direction for the detection and removal of arsenic in water body.
Description
Technical field
The invention belongs to a kind of visualization of presence of heavy metal arsenic in technical field of environmental detection more particularly to environmental water sample
Detection method.
Background technique
Arsenic is commonly called as arsenic, is a kind of metalloid element, and arsenic element widely exists in nature, shares hundreds of arsenic minerals
Object has been found that compound arsenic trioxide is referred to as arsenic, is the very strong substance of kind of toxicity, on October 27th, 2017, generation
The carcinogenic substance inventory edit reference that health organization international cancer research institution of boundary announces, arsenic and inorganic arsenic chemicals are in one kind
In carcinogenic substance inventory.
Arsenic and its compound are used in pesticide, herbicide, insecticide and many kinds of alloy, also just because of arsenic
It will be used wider and wider general, content of the arsenic substance in water body and soil caused to increase year by year, harm to the human body is huge,
Therefore, particularly important to the detection of the arsenic in environment water.
The detection method of common arsenic content in water body mainly have spectrophotometry, arsenic spot method, catalytic polarographic method with
And Corn by Hydride Generation Atomic Fluorescence Spectrometry etc., but these methods can only be measured the arsenic content in water body, it can not be in measurement
The minimizing technology and removal effect for studying arsenic in water body simultaneously, limit the development of the minimizing technology of arsenic in water body.
Summary of the invention
It is an object of the invention to overcome problem above of the existing technology, heavy metal arsenic in a kind of environmental water sample is provided
Visualization of presence detection method, by using modified manganese dioxide and modified natural coral, to the pentavalent arsenic in environmental water sample
It is adsorbed, while measuring adsorption effect, achievees the purpose that detect heavy metal arsenic in environmental water sample, be the inspection of arsenic in water body
It surveys and removal provides new direction.
To realize above-mentioned technical purpose and the technique effect, the invention is realized by the following technical scheme:
The visualization of presence detection method of heavy metal arsenic in a kind of environmental water sample, comprising the following steps:
Step 1: taking in 100mL water sample to be measured to clean reaction vessel, 0.84g titanium dioxide is put into the reaction vessel
Manganese adjusts the pH value of the water sample to be measured to 2-5, after the completion of adjustment, oxygen is passed through into the water sample to be measured, controls gas stream
Amount is 5L/min, and ventilation air is 36 DEG C, duration of ventilation 10min, after the completion of ventilation, water sample after must aoxidizing；
Step 2: adjust the pH value of water sample after the oxidation to 2-5, after the completion of adjustment, to the oxidation after put into water sample
0.10g modified manganese dioxide, as arsenic adsorbent, adsorption time 30min, adsorption temp is 25 DEG C, after the completion of absorption, solid-liquid
Separation obtains sample liquid after arsenic adsorbate and primary absorption；
Step 3: the pH value of sample liquid after the completion of adjustment, uses modified natural coral pair to 2-5 after the adjusting primary absorption
Sample liquid carries out second adsorption after the primary absorption, after the completion of second adsorption, sample liquid after coral and second adsorption after must adsorbing；
Step 4: the arsenic adsorbate being put into the first clean container, 8mol/L is added into first clean container
Hydrochloric acid solution is dissolved, and obtains the first sample liquid, adjusts the first sample liquid pH value to 2-5, sets dissolution time as 10min, molten
After the completion of solution, processing is filtered to first sample liquid, sample liquid one must be measured；
Step 5: coral after the absorption being put into the second clean container, is added into second clean container
8mol/L hydrochloric acid solution is dissolved, and obtains the second sample liquid, adjusts the second sample liquid pH value to 2-5, set dissolution time as
10min after the completion of dissolution, is filtered processing to second sample liquid, must measure sample liquid two；
Step 6: pipetting after the primary absorption of 50mL sample liquid, the measurement sample after sample liquid, the second adsorption respectively
Liquid one and the measurement sample liquid two are sequentially placed and survey into the first measurement container, the second measurement container, third measurement container and the 4th
In constant volume device, 1mL is added into the first measurement container, the second measurement container, third measurement container and the 4th measurement container
40% acidic oxidation stannous and 5mL 15% liquor kalii iodide, after fulling shake, place 10min, obtain the first measurement sample liquid,
Second measurement sample liquid, third measurement sample liquid and the 4th measurement sample liquid；
Step 7: measuring sample liquid and the 4th using the first measurement of coulometry instrument measurement sample liquid, the second measurement sample liquid, third
The content for measuring arsenic in sample liquid, obtains the first arsenic concentration, the second arsenic concentration, third arsenic concentration and the 4th arsenic concentration；
Step 8: measuring the concentration of arsenic in sample liquid and the 4th measurement sample liquid by the second measurement sample liquid, third, changed through analysis
It calculates, obtains the concentration of heavy metal arsenic in environmental water sample；
Step 9: modification is obtained through analytical calculation by the concentration of heavy metal arsenic in comparison third arsenic concentration and environmental water sample
The adsorption rate of manganese dioxide；The suction of modified natural coral is obtained through analytical calculation by the first arsenic concentration of comparison and the 4th arsenic concentration
Attached rate.
Further, the modified manganese dioxide preparation the following steps are included:
1) the first reaction vessel is taken, 30mL manganese nitrate solution and a certain amount of nitric acid are added into first reaction vessel
Bismuth solution must mix manganese liquid, wherein the molar ratio of manganese ion and bismuth ion is 10 in the mixing manganese liquid；
2) the mixing manganese liquid is diluted, extension rate 5 after the completion of dilution, cools down the mixing manganese liquid, cooling
After the completion, oxygen is continually fed into first reaction vessel, sets gas flow as 10L/min, ventilation air is 5 DEG C, is led to
During gas, sodium hydroxide solution is added dropwise into the mixing manganese liquid, wherein concentration of sodium hydroxide solution 6mol/L is added dropwise
Time is 10min, dripping quantity 100mL, and after being added dropwise to complete, filtering obtains mixture；
3) mixture is rinsed using sulfuric acid solution, after the completion of flushing, be put into vacuum freeze drier into
Row drying sets drying time for 24 hours, after the completion of dry, to obtain modified manganese dioxide.
Further, the modified natural coral preparation the following steps are included:
1) 100g coral sample is taken to sieve with 100 mesh sieve after ground machine grinding, obtain particle coral sample；
2) it takes 50g particle coral sample to be placed in beaker, the ferric chloride solution of 20mL 1.0% is added into the beaker,
Obtain semi-solid mixtures；
3) semi-solid mixtures are put into vacuum freeze drier and are dried, set drying time for 24 hours, to do
After the completion of dry, the semi-solid mixtures are ground, are sieved with 100 mesh sieve, hybrid particles are obtained；
4) it takes in hybrid particles to crucible described in 10g, the crucible is moved into Muffle furnace, sets sintering temperature as 400
DEG C, sintering time 30min after the completion of sintering, obtains high temp samples, and the high temp samples are stood to room temperature, modified natural is obtained
Coral.
The beneficial effects of the present invention are:
The present invention uses modified manganese dioxide and modified natural coral, adsorbs to the pentavalent arsenic in environmental water sample, leads to
It crosses setting modified manganese dioxide and modified natural coral both new adsorbents reaches inspection while measuring adsorption effect
The purpose for surveying heavy metal arsenic in environmental water sample, provides new direction for the detection and removal of arsenic in water body.
Detailed description of the invention
The drawings described herein are used to provide a further understanding of the present invention, constitutes part of this application, this hair
Bright illustrative embodiments and their description are used to explain the present invention, and are not constituted improper limitations of the present invention.In the accompanying drawings:
Fig. 1 is the overhaul flow chart of heavy metal arsenic in environmental water sample provided by the invention；
Fig. 2 is the preparation flow figure of modified manganese dioxide provided by the invention；
Fig. 3 is the preparation flow figure of modified natural coral provided by the invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts all other
Embodiment shall fall within the protection scope of the present invention.
In the description of the present invention, it is to be understood that, term " aperture ", "upper", "lower", " thickness ", "top", " in ",
Indicating positions or the positional relationship such as " length ", "inner", " surrounding ", are merely for convenience of description of the present invention and simplification of the description, without
It is that the component of indication or suggestion meaning or element must have a particular orientation, is constructed and operated in a specific orientation, therefore not
It can be interpreted as limitation of the present invention.
Embodiment
The visualization of presence detection method of heavy metal arsenic in a kind of environmental water sample as shown in Figure 1, comprising the following steps:
Step 1: it takes in 100mL water sample to be measured to clean reaction vessel, 0.84g manganese dioxide is put into reaction vessel,
The pH value of water sample to be measured is adjusted to 2-5, after the completion of adjustment, oxygen is passed through into water sample to be measured, control gas flow is 5L/min,
Ventilation air is 36 DEG C, duration of ventilation 10min, after the completion of ventilation, water sample after must aoxidizing；
Step 2: adjust the pH value of water sample after oxidation to 2-5, after the completion of adjustment, to oxidation after in water sample investment 0.10g change
Property manganese dioxide, as arsenic adsorbent, adsorption time 30min, adsorption temp is 25 DEG C, after the completion of absorption, is separated by solid-liquid separation, and is obtained
Sample liquid after arsenic adsorbate and primary absorption；
Step 3: adjusting the pH value of sample liquid after once adsorbing to 2-5, after the completion of adjustment, using modified natural coral to primary
Sample liquid carries out second adsorption after absorption, after the completion of second adsorption, sample liquid after coral and second adsorption after must adsorbing；
Step 4: arsenic adsorbate being put into the first clean container, 8mol/L hydrochloric acid solution is added into the first clean container
It is dissolved, obtains the first sample liquid, adjust the first sample liquid pH value to 2-5, set dissolution time as 10min, after the completion of dissolution, to the
One sample liquid is filtered processing, must measure sample liquid one；
Step 5: coral after absorption being put into the second clean container, it is molten that 8mol/L hydrochloric acid is added into the second clean container
Liquid is dissolved, and obtains the second sample liquid, adjusts the second sample liquid pH value to 2-5, sets dissolution time as 10min, right after the completion of dissolution
Second sample liquid is filtered processing, must measure sample liquid two；
Step 6: pipetting after the primary absorption of 50mL sample liquid, measurement sample liquid one and measurement sample after sample liquid, second adsorption respectively
Liquid two is sequentially placed in the first measurement container, the second measurement container, third measurement container and the 4th measurement container, to first
Measure container, second measurement container, third measurement container and the 4th measurement container in be added 1mL 40% acidic oxidation stannous and
15% liquor kalii iodide of 5mL after fulling shake, places 10min, obtains the first measurement sample liquid, the second measurement sample liquid, third measurement
Sample liquid and the 4th measurement sample liquid；
Step 7: measuring sample liquid and the 4th using the first measurement of coulometry instrument measurement sample liquid, the second measurement sample liquid, third
The content for measuring arsenic in sample liquid, obtains the first arsenic concentration, the second arsenic concentration, third arsenic concentration and the 4th arsenic concentration；
Step 8: measuring the concentration of arsenic in sample liquid and the 4th measurement sample liquid by the second measurement sample liquid, third, changed through analysis
It calculates, obtains the concentration of heavy metal arsenic in environmental water sample, in the process, the sum of the content of heavy metal in three kinds of measurement sample liquids is
The content of heavy metal arsenic in environmental water sample.
Step 9: modification is obtained through analytical calculation by the concentration of heavy metal arsenic in comparison third arsenic concentration and environmental water sample
The adsorption rate of manganese dioxide；The suction of modified natural coral is obtained through analytical calculation by the first arsenic concentration of comparison and the 4th arsenic concentration
Attached rate in detecting environmental water sample while the content of heavy metal arsenic, can more pass through two kinds of different modified suctions by this design
The calculating of the attached dose of adsorption rate to heavy metal arsenic, research select the heavy metal arsenic in suitable adsorbent removal environmental water sample, are
It carries out providing new direction while the detection and removal of heavy metal arsenic in environmental water sample.
The calculation formula of adsorption rate is as follows:
R (%)=(c1-c2)/c1*100%
In formula: c1 is the concentration (μ g/L) of heavy metal arsenic in environmental water sample before adsorbing, and c2 is heavy metal in solution after absorption
The concentration (μ g/L) of arsenic.
As shown in Fig. 2, the preparation of modified manganese dioxide the following steps are included:
1) the first reaction vessel is taken, 30mL manganese nitrate solution is added into the first reaction vessel and a certain amount of bismuth nitrate is molten
Liquid must mix manganese liquid, wherein the molar ratio of manganese ion and bismuth ion is 10 in mixing manganese liquid；
2) dilution mixing manganese liquid, extension rate 5 after the completion of dilution, cool down mixing manganese liquid, after the completion of cooling,
Oxygen is continually fed into the first reaction vessel, sets gas flow as 10L/min, ventilation air is 5 DEG C, in venting process, to
It mixes and sodium hydroxide solution is added dropwise in manganese liquid, wherein concentration of sodium hydroxide solution 6mol/L, time for adding 10min are added dropwise
Amount is 100mL, and after being added dropwise to complete, filtering obtains mixture；
3) mixture is rinsed using sulfuric acid solution, after the completion of flushing, is put into vacuum freeze drier and is done
It is dry, drying time is set as 8h, after the completion of dry, obtains modified manganese dioxide.
As shown in figure 3, the preparation of modified natural coral the following steps are included:
1) 100g coral sample is taken to sieve with 100 mesh sieve after ground machine grinding, obtain particle coral sample；
2) it takes 50g particle coral sample to be placed in beaker, the ferric chloride solution of 20mL 1.0% is added into beaker, obtain half
Solid mixture；
3) semi-solid mixtures are put into vacuum freeze drier and are dried, set drying time for 24 hours, to have dried
Cheng Hou grinds semi-solid mixtures, sieves with 100 mesh sieve, obtain hybrid particles；
4) it takes in 10g hybrid particles to crucible, crucible is moved into Muffle furnace, set sintering temperature as 400 DEG C, when sintering
Between be 30min, after the completion of sintering, obtain high temp samples, the high temp samples stood to room temperature, obtain modified natural coral.
In the present invention, modified manganese dioxide and modified natural coral, adsorb the pentavalent arsenic in environmental water sample, lead to
It crosses setting modified manganese dioxide and modified natural coral both new adsorbents reaches inspection while measuring adsorption effect
The purpose for surveying heavy metal arsenic in environmental water sample, provides new direction for the detection and removal of arsenic in water body.
In the description of this specification, the description of reference term " one embodiment ", " example ", " specific example " etc. means
Particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one implementation of the invention
In example or example.In the present specification, schematic expression of the above terms may not refer to the same embodiment or example.
Moreover, particular features, structures, materials, or characteristics described can be in any one or more of the embodiments or examples to close
Suitable mode combines.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.
Claims (3)
1. the visualization of presence detection method of heavy metal arsenic in a kind of environmental water sample, it is characterised in that: the following steps are included:
Step 1: it takes in 100mL water sample to be measured to clean reaction vessel, 0.84g manganese dioxide is put into the reaction vessel,
The pH value of the water sample to be measured is adjusted to 2-5, after the completion of adjustment, oxygen is passed through into the water sample to be measured, controls gas flow
For 5L/min, ventilation air is 36 DEG C, duration of ventilation 10min, after the completion of ventilation, water sample after must aoxidizing；
Step 2: adjust the pH value of water sample after the oxidation to 2-5, after the completion of adjustment, to the oxidation after put into water sample
0.10g modified manganese dioxide, as arsenic adsorbent, adsorption time 30min, adsorption temp is 25 DEG C, after the completion of absorption, solid-liquid
Separation obtains sample liquid after arsenic adsorbate and primary absorption；
Step 3: the pH value of sample liquid is to 2-5 after the adjusting primary absorption, after the completion of adjustment, using modified natural coral to described
Sample liquid carries out second adsorption after primary absorption, after the completion of second adsorption, sample liquid after coral and second adsorption after must adsorbing；
Step 4: the arsenic adsorbate being put into the first clean container, 8mol/L hydrochloric acid is added into first clean container
Solution is dissolved, and the first sample liquid is obtained, and is adjusted the first sample liquid pH value to 2-5, is set dissolution time as 10min, dissolved
Cheng Hou is filtered processing to first sample liquid, must measure sample liquid one；
Step 5: coral after the absorption being put into the second clean container, 8mol/L salt is added into second clean container
Acid solution is dissolved, and the second sample liquid is obtained, and is adjusted the second sample liquid pH value to 2-5, is set dissolution time as 10min, dissolve
After the completion, processing is filtered to second sample liquid, sample liquid two must be measured；
Step 6: pipetting after the primary absorption of 50mL sample liquid, the measurement sample liquid one after sample liquid, the second adsorption respectively
With the measurement sample liquid two, it is sequentially placed and holds into the first measurement container, the second measurement container, third measurement container and the 4th measurement
In device, it is added 1mL's into the first measurement container, the second measurement container, third measurement container and the 4th measurement container
15% liquor kalii iodide of 40% acidic oxidation stannous and 5mL after fulling shake, places 10min, obtains the first measurement sample liquid, the
Two measurement sample liquids, third measurement sample liquid and the 4th measurement sample liquid；
Step 7: using the first measurement of coulometry instrument measurement sample liquid, the second measurement sample liquid, third measurement sample liquid and the 4th measurement
The content of arsenic in sample liquid obtains the first arsenic concentration, the second arsenic concentration, third arsenic concentration and the 4th arsenic concentration；
Step 8: measuring the concentration of arsenic in sample liquid and the 4th measurement sample liquid by the second measurement sample liquid, third, convert, obtain through analysis
The concentration of heavy metal arsenic in environmental water sample；
Step 9: modified dioxy is obtained through analytical calculation by the concentration of heavy metal arsenic in comparison third arsenic concentration and environmental water sample
Change the adsorption rate of manganese；The absorption of modified natural coral is obtained through analytical calculation by the first arsenic concentration of comparison and the 4th arsenic concentration
Rate.
2. the visualization of presence detection method of heavy metal arsenic, feature exist in a kind of environmental water sample according to claim 1
In: the modified manganese dioxide preparation the following steps are included:
1) the first reaction vessel is taken, 30mL manganese nitrate solution is added into first reaction vessel and a certain amount of bismuth nitrate is molten
Liquid must mix manganese liquid, wherein the molar ratio of manganese ion and bismuth ion is 10 in the mixing manganese liquid；
2) the mixing manganese liquid is diluted, extension rate 5 after the completion of dilution, cools down the mixing manganese liquid, cooling to complete
Afterwards, oxygen is continually fed into first reaction vessel, sets gas flow as 10L/min, ventilation air is 5 DEG C, is ventilated
Sodium hydroxide solution is added dropwise into the mixing manganese liquid, wherein concentration of sodium hydroxide solution 6mol/L, time for adding in Cheng Zhong
For 10min, dripping quantity 100mL, after being added dropwise to complete, filtering obtains mixture；
3) mixture is rinsed using sulfuric acid solution, after the completion of flushing, is put into vacuum freeze drier and is done
It is dry, drying time is set for 24 hours, after the completion of dry, to obtain modified manganese dioxide.
3. the visualization of presence detection method of heavy metal arsenic, feature exist in a kind of environmental water sample according to claim 1
In: the modified natural coral preparation the following steps are included:
1) 100g coral sample is taken to sieve with 100 mesh sieve after ground machine grinding, obtain particle coral sample；
2) it takes 50g particle coral sample to be placed in beaker, the ferric chloride solution of 20mL 1.0% is added into the beaker, obtain half
Solid mixture；
3) semi-solid mixtures are put into vacuum freeze drier and are dried, set drying time for 24 hours, to have dried
Cheng Hou grinds the semi-solid mixtures, sieves with 100 mesh sieve, obtains hybrid particles；
4) it takes in hybrid particles to crucible described in 10g, the crucible is moved into Muffle furnace, set sintering temperature as 400 DEG C, burn
The knot time is 30min, after the completion of sintering, obtains high temp samples, the high temp samples are stood to room temperature, obtain modified natural coral.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040121676A1 (en) * | 2002-12-11 | 2004-06-24 | Japan Atomic Energy Research Institute | Method of synthesizing zirconium-loaded fibrous adsorbent materials having phosphoryl groups and removal of objectionable substances using the adsorbents |
| CN1751783A (en) * | 2005-07-20 | 2006-03-29 | 上海自来水市北科技有限公司 | Composite absorption material for removing arsenic from water and its prepn. method |
| CN103708587A (en) * | 2014-01-03 | 2014-04-09 | 长沙皓龙环保科技有限公司 | Preparation method of composite electrode for removing arsenic in water based on electro-adsorption and method for removing arsenic |
| CN107983300A (en) * | 2016-10-27 | 2018-05-04 | 湖南大学 | Biological carbon composite of manganese dioxide modification and its preparation method and application |
-
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040121676A1 (en) * | 2002-12-11 | 2004-06-24 | Japan Atomic Energy Research Institute | Method of synthesizing zirconium-loaded fibrous adsorbent materials having phosphoryl groups and removal of objectionable substances using the adsorbents |
| CN1751783A (en) * | 2005-07-20 | 2006-03-29 | 上海自来水市北科技有限公司 | Composite absorption material for removing arsenic from water and its prepn. method |
| CN103708587A (en) * | 2014-01-03 | 2014-04-09 | 长沙皓龙环保科技有限公司 | Preparation method of composite electrode for removing arsenic in water based on electro-adsorption and method for removing arsenic |
| CN107983300A (en) * | 2016-10-27 | 2018-05-04 | 湖南大学 | Biological carbon composite of manganese dioxide modification and its preparation method and application |
Non-Patent Citations (2)
| Title |
|---|
| SHIGERU MAEDA ET.AL: "Selective Adsorption of Arsenic(V)Ion by Use of Iron(III) Hydroxide-Loaded Coral Limestone", 《SEPARATION SCIENCE AND TECHNOLOGY》 * |
| 王忺: "不同形态二氧化锰对重金属离子吸附行为的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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