CN106404703A - Method for detecting mercury ions in soil - Google Patents

Method for detecting mercury ions in soil Download PDF

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Publication number
CN106404703A
CN106404703A CN201610966755.6A CN201610966755A CN106404703A CN 106404703 A CN106404703 A CN 106404703A CN 201610966755 A CN201610966755 A CN 201610966755A CN 106404703 A CN106404703 A CN 106404703A
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Prior art keywords
temperature
soil
solution
mercury
detection method
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CN201610966755.6A
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Chinese (zh)
Inventor
张根义
胡彬
张进
吴念绮
周朱晨
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100 Olson Jiangsu Food Safety Technology Co Ltd
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100 Olson Jiangsu Food Safety Technology Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/33Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention discloses a method for detecting mercury ions in soil. The method comprises the following steps: grinding soil to be detected, and soaking the soil to be detected with a sulfuric acid solution, a hypochlorous acid solution and an acetic acid solution; then carrying out high-temperature digestion, centrifuging, washing residues by using the hypochlorous acid solution, centrifuging, and merging supernate to obtain a test solution; and measuring the concentration in the test solution. The method is an atomic absorption spectrographic method, standard substances of mercury is respectively prepared into standard solutions, the standard solutions and a measured sample solution are subjected to atomic absorption spectrum measurement, and the content of the mercury in the soil to be detected is calculated according to numerical values. When the soil is subjected to acidolysis, sulfuric acid, hypochlorous acid and acetic acid are added, and dissolution of the mercury ions is promoted effectively. The method is high in accuracy and high in sensitivity, has high detecting efficiency, and has the advantages of good recycling rate, high treatment speed, simplicity and convenience in operation and the like.

Description

A kind of detection method of mercury in soils ion
Technical field
The present invention relates to technical field of analysis and detection, specifically a kind of detection method of mercury in soils ion.
Background technology
Expansion with city and the development of large-scale industry, heavy metal pollution mouth present in air, soil, water environment Benefit increases.Heavy metal pollution is one of subject matter of water pollution, mining, metal smelt, chemical production wastewater, administration agriculture The artificial pollution such as medicine chemical fertilizer and house refuse, and the natural factor such as geologic erosion, air slaking all can lead to heavy metal with various shapes Formula enters soil.Because heavy metal has that toxicity is big, is difficult in the environment to be metabolized, be easily bioaccumulation and have biomagnification to imitate The features such as answer is so that the heavy metal pollution of soil seriously threatens human health.Particularly hydrargyrum can accumulate in vivo, holds very much Easily absorbed by skin and respiratory tract and digestive tract.Minamata disease is one kind of mercurialism.Hydrargyrum destruction central nervous system, boil on the nape opposite the mouth, Mucosa and tooth have harmful effect.It is exposed to for a long time in high hydrargyrum environment and can lead to brain injury and death.Therefore, mercury in soils Ion concentration be monitored and controlled oneself become be related to environmental conservation, sustainable development and Living consumption improve important asking Topic.
Content of the invention
It is an object of the invention to provide a kind of accuracy is high, sensitivity is high, the response rate is good, processing speed is fast, operation is simple The detection method of mercury in soils ion just, to solve the problems, such as to propose in above-mentioned background technology.
For achieving the above object, the present invention provides following technical scheme:
A kind of detection method of mercury in soils ion, comprises the following steps:
(1)Soil to be measured is ground to the powder of 150-300 mesh, by the soil to be measured sulfuric acid solution of 15wt%-50wt%, The hypochlorite solution of 3wt%-40wt%, the acetum of 10wt%-40wt%, soak 8-15h;
(2)By step(1)Soil to be measured after immersion and acid solution are poured in politef counteracting tank, carry out High-temperature Digestion, first Temperature is risen a height of 150-180 DEG C, High-temperature Digestion 0.8-2h, rise high-temperature to 220-250 DEG C, then High-temperature Digestion 2.5-4h;From The heart, residue is washed with hypochlorite solution, centrifugation, merges supernatant, prepared need testing solution;
(3)Measure the concentration of hydrargyrum in need testing solution, detection method is atomic absorption spectrography (AAS), and the concrete data of detection method is such as Under:
Sclera remodeling wavelength is 323nm, and lamp current is 4-6mA;Slit is 0.4-0.6mm;Heating schedule:Rise high-temperature first extremely dry Dry temperature is 100-120 DEG C, and 1-3min is dried;According still further to 25-33 DEG C/min heating rate rise high-temperature to ashing temperature be 720-800 DEG C, the constant 8-12min of keeping temperature;Heating rate according still further to 18-25 DEG C/min rises high-temperature to atomization temperature For 1350-1450 DEG C, the constant 1-3min of keeping temperature, then rise high-temperature and keep 20s to after 1800 DEG C, cooling;
(4)Respectively the standard substance of hydrargyrum are formulated as standard solution, standard solution and determination sample solution are all carried out Atomic Absorption Spectroscopic assay, and the content according to the hydrargyrum in numerical computations soil to be measured.
As the further scheme of the present invention:Step(1)In, the mass fraction of sulfuric acid solution is 25wt%-40wt%.
As the further scheme of the present invention:Step(1)In, the mass fraction of hypochlorite solution is 5wt%-30wt%.
As the further scheme of the present invention:Step(1)In, the mass fraction of acetum is 20wt%-30wt%.
As the further scheme of the present invention:Step(1)In, soak 10-14h.
As the further scheme of the present invention:Step(2)In, centrifugal speed is 3000-8000r/min, and centrifugation time is 5-30min.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention when acidolysis is carried out to soil, add sulphuric acid, hypochlorous acid, acetic acid, be effectively promoted the molten of mercury ion Go out, detection method accuracy is high, sensitivity is high, has higher detection efficiency, have that the response rate is good, processing speed Hurry up, easy and simple to handle the advantages of.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, Obviously, described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.Based in the present invention Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of not making creative work, all Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of detection method of mercury in soils ion, comprise the following steps:
(1)Soil to be measured is ground to the powder of 150 mesh, will be molten for the hypochlorous acid of the soil to be measured sulfuric acid solution of 15wt%, 3wt% Liquid, the acetum of 10wt%, soak 8h.
(2)By step(1)Soil to be measured after immersion and acid solution are poured in politef counteracting tank, carry out high temperature and disappear Temperature is first risen a height of 150 DEG C by solution, High-temperature Digestion 0.8h, rises high-temperature to 220 DEG C, then High-temperature Digestion 2.5h;Centrifugation, residue Washed with hypochlorite solution, centrifugation, merge supernatant, prepared need testing solution.Centrifugal speed is 3000r/min, centrifugation time For 5min.
(3)Measure the concentration of hydrargyrum in need testing solution, detection method is atomic absorption spectrography (AAS), the concrete data of detection method As follows:
Sclera remodeling wavelength is 323nm, and lamp current is 4mA;Slit is 0.4mm;Heating schedule:Rise high-temperature first to baking temperature For 100 DEG C, 1min is dried;Heating rate liter high-temperature according still further to 25 DEG C/min is 720 DEG C to ashing temperature, and keeping temperature is not Become 8min;Heating rate liter high-temperature according still further to 18 DEG C/min is 1350 DEG C to atomization temperature, the constant 1min of keeping temperature, Rise high-temperature again and keep 20s to after 1800 DEG C, cooling.
(4)Respectively the standard substance of hydrargyrum are formulated as standard solution, standard solution and determination sample solution are all carried out atom Absorption spectromtry, and the content according to the hydrargyrum in numerical computations soil to be measured.
Embodiment 2
In the embodiment of the present invention, a kind of detection method of mercury in soils ion, comprise the following steps:
(1)Soil to be measured is ground to the powder of 300 mesh, by the hypochlorous acid of the sulfuric acid solution with 50wt% for the soil to be measured, 40wt% Solution, the acetum of 40wt%, soak 15h.
(2)By step(1)Soil to be measured after immersion and acid solution are poured in politef counteracting tank, carry out high temperature and disappear Temperature is first risen a height of 180 DEG C by solution, High-temperature Digestion 2h, rises high-temperature to 250 DEG C, then High-temperature Digestion 4h;Centrifugation, residue is used secondary Solution chlorate washs, centrifugation, merges supernatant, prepared need testing solution.Centrifugal speed is 8000r/min, and centrifugation time is 30min.
(3)Measure the concentration of hydrargyrum in need testing solution, detection method is atomic absorption spectrography (AAS), the concrete data of detection method As follows:
Sclera remodeling wavelength is 323nm, and lamp current is 6mA;Slit is 0.6mm;Heating schedule:Rise high-temperature first to baking temperature For 120 DEG C, 3min is dried;Heating rate liter high-temperature according still further to 33 DEG C/min is 800 DEG C to ashing temperature, and keeping temperature is not Become 12min;Heating rate liter high-temperature according still further to 25 DEG C/min is 1450 DEG C to atomization temperature, and keeping temperature is constant 3min, then rise high-temperature and keep 20s to after 1800 DEG C, cooling.
(4)Respectively the standard substance of hydrargyrum are formulated as standard solution, standard solution and determination sample solution are all carried out atom Absorption spectromtry, and the content according to the hydrargyrum in numerical computations soil to be measured.
Embodiment 3
In the embodiment of the present invention, a kind of detection method of mercury in soils ion, comprise the following steps:
(1)Soil to be measured is ground to the powder of 200 mesh, will be molten for the hypochlorous acid of the soil to be measured sulfuric acid solution of 25wt%, 5wt% Liquid, the acetum of 20wt%, soak 10h.
(2)By step(1)Soil to be measured after immersion and acid solution are poured in politef counteracting tank, carry out high temperature and disappear Temperature is first risen a height of 160 DEG C by solution, High-temperature Digestion 1h, rises high-temperature to 230 DEG C, then High-temperature Digestion 3h;Centrifugation, residue is used secondary Solution chlorate washs, centrifugation, merges supernatant, prepared need testing solution.Centrifugal speed is 4000r/min, and centrifugation time is 10min.
(3)Measure the concentration of hydrargyrum in need testing solution, detection method is atomic absorption spectrography (AAS), the concrete data of detection method As follows:
Sclera remodeling wavelength is 323nm, and lamp current is 5mA;Slit is 0.5mm;Heating schedule:Rise high-temperature first to baking temperature For 110 DEG C, 2min is dried;Heating rate liter high-temperature according still further to 28 DEG C/min is 760 DEG C to ashing temperature, and keeping temperature is not Become 10min;Heating rate liter high-temperature according still further to 20 DEG C/min is 1400 DEG C to atomization temperature, and keeping temperature is constant 2min, then rise high-temperature and keep 20s to after 1800 DEG C, cooling.
(4)Respectively the standard substance of hydrargyrum are formulated as standard solution, standard solution and determination sample solution are all carried out atom Absorption spectromtry, and the content according to the hydrargyrum in numerical computations soil to be measured.
Embodiment 4
In the embodiment of the present invention, a kind of detection method of mercury in soils ion, comprise the following steps:
(1)Soil to be measured is ground to the powder of 250 mesh, by the hypochlorous acid of the sulfuric acid solution with 40wt% for the soil to be measured, 30wt% Solution, the acetum of 30wt%, soak 14h.
(2)By step(1)Soil to be measured after immersion and acid solution are poured in politef counteracting tank, carry out high temperature and disappear Temperature is first risen a height of 170 DEG C by solution, High-temperature Digestion 1.5h, rises high-temperature to 240 DEG C, then High-temperature Digestion 3.5h;Centrifugation, residue Washed with hypochlorite solution, centrifugation, merge supernatant, prepared need testing solution.Centrifugal speed is 6000r/min, centrifugation time For 20min.
(3)Measure the concentration of hydrargyrum in need testing solution, detection method is atomic absorption spectrography (AAS), the concrete data of detection method As follows:
Sclera remodeling wavelength is 323nm, and lamp current is 5mA;Slit is 0.5mm;Heating schedule:Rise high-temperature first to baking temperature For 110 DEG C, 2min is dried;Heating rate liter high-temperature according still further to 30 DEG C/min is 780 DEG C to ashing temperature, and keeping temperature is not Become 11min;Heating rate liter high-temperature according still further to 22 DEG C/min is 1380 DEG C to atomization temperature, and keeping temperature is constant 2min, then rise high-temperature and keep 20s to after 1800 DEG C, cooling.
(4)Respectively the standard substance of hydrargyrum are formulated as standard solution, standard solution and determination sample solution are all carried out atom Absorption spectromtry, and the content according to the hydrargyrum in numerical computations soil to be measured.
Recording somewhere soil mercury content using said method is 0.028%, and relative standard deviation is in 2.2-4.8%.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie In the case of the spirit or essential attributes of the present invention, the present invention can be realized in other specific forms.Therefore, no matter From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power Profit requires rather than described above limits, it is intended that all in the implication and scope of the equivalency of claim by falling Change is included in the present invention.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each embodiment only wraps Containing an independent technical scheme, only for clarity, those skilled in the art should for this narrating mode of description Using description as an entirety, the technical scheme in each embodiment can also form those skilled in the art through appropriately combined Understandable other embodiment.

Claims (6)

1. a kind of detection method of mercury in soils ion is it is characterised in that comprise the following steps:
(1)Soil to be measured is ground to the powder of 150-300 mesh, by the soil to be measured sulfuric acid solution of 15wt%-50wt%, The hypochlorite solution of 3wt%-40wt%, the acetum of 10wt%-40wt%, soak 8-15h;
(2)By step(1)Soil to be measured after immersion and acid solution are poured in politef counteracting tank, carry out High-temperature Digestion, first Temperature is risen a height of 150-180 DEG C, High-temperature Digestion 0.8-2h, rise high-temperature to 220-250 DEG C, then High-temperature Digestion 2.5-4h;From The heart, residue is washed with hypochlorite solution, centrifugation, merges supernatant, prepared need testing solution;
(3)Measure the concentration of hydrargyrum in need testing solution, detection method is atomic absorption spectrography (AAS), and the concrete data of detection method is such as Under:
Sclera remodeling wavelength is 323nm, and lamp current is 4-6mA;Slit is 0.4-0.6mm;Heating schedule:Rise high-temperature first extremely dry Dry temperature is 100-120 DEG C, and 1-3min is dried;According still further to 25-33 DEG C/min heating rate rise high-temperature to ashing temperature be 720-800 DEG C, the constant 8-12min of keeping temperature;Heating rate according still further to 18-25 DEG C/min rises high-temperature to atomization temperature For 1350-1450 DEG C, the constant 1-3min of keeping temperature, then rise high-temperature and keep 20s to after 1800 DEG C, cooling;
(4)Respectively the standard substance of hydrargyrum are formulated as standard solution, standard solution and determination sample solution are all carried out Atomic Absorption Spectroscopic assay, and the content according to the hydrargyrum in numerical computations soil to be measured.
2. the detection method of mercury in soils ion according to claim 1 is it is characterised in that step(1)In, sulfuric acid solution Mass fraction be 25wt%-40wt%.
3. the detection method of mercury in soils ion according to claim 1 is it is characterised in that step(1)In, hypochlorous acid is molten The mass fraction of liquid is 5wt%-30wt%.
4. the detection method of mercury in soils ion according to claim 1 is it is characterised in that step(1)In, acetum Mass fraction be 20wt%-30wt%.
5. the detection method of mercury in soils ion according to claim 1 is it is characterised in that step(1)In, soak 10- 14h.
6. the detection method of mercury in soils ion according to claim 1 is it is characterised in that step(2)In, centrifugal speed For 3000-8000r/min, centrifugation time is 5-30min.
CN201610966755.6A 2016-10-28 2016-10-28 Method for detecting mercury ions in soil Pending CN106404703A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2810674C1 (en) * 2023-08-22 2023-12-28 Общество с ограниченной ответственностью "Научно-производственное объединение "Метрология" Method for determining mass fraction of total mercury in soils using same standard sample for soils of different composition

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104297172A (en) * 2013-07-18 2015-01-21 上海威正测试技术有限公司 Method for rapid detection of mercury content in soil
CN104406924A (en) * 2014-11-25 2015-03-11 苏州东辰林达检测技术有限公司 Detection method of heavy metal in chitosan
CN104596811A (en) * 2013-10-31 2015-05-06 大连大公环境检测有限公司 Mercury ion detection method
CN105424462A (en) * 2015-12-10 2016-03-23 苏州国环环境检测有限公司 Method of determining mercury in soil through water bath digestion-atomic fluorescence method
CN105784864A (en) * 2016-03-10 2016-07-20 山东五洲检测有限公司 Detection method of heavy metal in soil

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104297172A (en) * 2013-07-18 2015-01-21 上海威正测试技术有限公司 Method for rapid detection of mercury content in soil
CN104596811A (en) * 2013-10-31 2015-05-06 大连大公环境检测有限公司 Mercury ion detection method
CN104406924A (en) * 2014-11-25 2015-03-11 苏州东辰林达检测技术有限公司 Detection method of heavy metal in chitosan
CN105424462A (en) * 2015-12-10 2016-03-23 苏州国环环境检测有限公司 Method of determining mercury in soil through water bath digestion-atomic fluorescence method
CN105784864A (en) * 2016-03-10 2016-07-20 山东五洲检测有限公司 Detection method of heavy metal in soil

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2810674C1 (en) * 2023-08-22 2023-12-28 Общество с ограниченной ответственностью "Научно-производственное объединение "Метрология" Method for determining mass fraction of total mercury in soils using same standard sample for soils of different composition

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