CN101625321A - Method for testing zinc content in soil - Google Patents

Method for testing zinc content in soil Download PDF

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Publication number
CN101625321A
CN101625321A CN200810012247A CN200810012247A CN101625321A CN 101625321 A CN101625321 A CN 101625321A CN 200810012247 A CN200810012247 A CN 200810012247A CN 200810012247 A CN200810012247 A CN 200810012247A CN 101625321 A CN101625321 A CN 101625321A
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testing sample
soil
hno
zinc content
hclo
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CN200810012247A
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陈欣
王俊
史奕
赵牧秋
郭颖
吴蕊
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Institute of Applied Ecology of CAS
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Institute of Applied Ecology of CAS
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Abstract

The invention relates to environmental protection, in particular to a method for testing zinc content in soil. The method comprises the following steps: neutralizing 0.2000+/-0.0020 gram of a sample to be tested in 8 to 13 milliliters of HNO3-HClO4 or 10 to 30 milliliters of HCL-HNO3-HClO4 for 8 to 15 hours; and then testing the Zn content in solution to be tested after neutralizing through an atomic fluorescence spectrometer. The method uses an atomic fluorescence principle to perform quantitative test on Zn ions and is simple to process the sample, and used for testing the Zn content in the soil, the method has the advantages of simple operation, high sensitivity, good reproducibility, and less element interference.

Description

A kind of method of measuring zinc content in soil
Technical field
The present invention relates to a kind of zinc (Zn) ion and detect detection, relate in particular to a kind of atomic fluorescence (Atomic Fluorescence Spectrometry, i.e. AFS) principle of utilizing and the Zn ion is carried out the method for quantitative measurement.
The detection method of zinc has at present: spectrophotometric method, and utilize complexing agent and heavy metal to form colored complex and carry out colorimetric, but its sensitivity is low, poor reproducibility, and be subject to the iron interference, therefore use extensivelyless; Atomic absorption spectrography (AAS), belong to conventional elemental analysis method, but in real work, reading instability in the time of often can feeling to survey zinc mainly is because in the short wavelength regions about 200nm, the absorption of flame gas is more obvious, in addition, salt grain in the flame causes scattering of light, causes the light intensity instability, influences final reading; Though ICP-AES sensitivity and degree of accuracy are higher, the removing method of interference element is not very satisfactory.
Summary of the invention
In order to solve above-mentioned weak point, the object of the present invention is to provide that a kind of favorable reproducibility, element are disturbed less, are convenient to operate, the method for highly sensitive mensuration zinc content in soil.
For achieving the above object, the technical solution used in the present invention is:
Measure the method for zinc content in soil: with the HNO of 0.2000 ± 0.0020g testing sample through 8-13mL 3-HClO 4Or the HCl-HNO of 10-30mL 3-HClO 4Clear up 8-15h, the solution to be measured after then will clearing up is measured the content of Zn in the liquid to be measured by atomic fluorescence spectrometer.
Described testing sample is through HNO 3-HClO 4When clearing up, add 6-10mLHNO in the testing sample earlier 3Under 160-180 ℃, disappear and boil 1-1.5h, then add 2-3mLHClO 4, temperature is brought up to 280-300 ℃ and is continued to disappear and boil until testing sample in the pasty state.Disappearing at testing sample adds entry before boiling, and makes it wetting.The described testing sample that disappears after boiling is the nitric acid constant volume of 1-5% through mass concentration.
Described testing sample is through HCl-HNO 3-HClO 4When clearing up, adding 6-10mLHCl disappears under 160-180 ℃ and boils in the testing sample, adds 2-15mL HNO when being evaporated to raffinate for 4-8mL 3, continue heating and steam near when thick, (ρ=1.67g/mL), then improve temperature and boil to 280-300 ℃ of continuous disappearing is heated to white cigarette and emits most to add 2-5mL perchloric acid.Described testing sample is through HCl-HNO 3-HClO 4When clearing up, also can add HCl and HNO simultaneously in the testing sample 3, wherein HCl and HNO 3Proportioning according to chloroazotic acid adds.Disappearing at testing sample adds entry before boiling, and makes it wetting.The described testing sample that disappears after boiling is the nitric acid constant volume of 1-5% through mass concentration.
Described atomic fluorescence spectrometer is the SK-2002 model, and its condition determination is photoelectric tube negative high voltage: 300V; Lamp current: 70mA; Integral time: 5s; Combustion gas: 100mL/min; Carrier gas is air: 〉=1600mL/min; Auxilliary gas is air: 800mL/min.
Action principle:
Sample is through atomizing, enter in the quartz atomizer flame of high temperature, the gaseous state free atom absorbs the characteristic radiation of hollow cathode modulation emission, and the outer-shell electron of atom transits to higher energy level, transition is returned ground state or than low-lying level, is launched the fluorescence identical or different with former excitation wavelength simultaneously again then.Fluorescence is material extinction institute's radiation emitted afterwards, thereby fluorescence intensity of solution (I f) light intensity (I that should absorb with this solution a) and the fluorescence quantum yield (Y of this material f) relevant, i.e. I f=2.303 ξ bc * Y f* I a(wherein ξ bc is a constant) can be known by this formula, for the lean solution of certain fluorescent material, under the excitation light irradiation of certain frequency and intensity, the fluorescence intensity of solution of surveying is directly proportional with solution concentration, by Computer Processing, can obtain elements corresponding content.
Embodiment
The present invention is described in more detail below by embodiment.
Embodiment 1:
Measure the method for zinc content in soil: the 0.1992g testing sample is added entry in the teflon crucible, make it wetting.The HNO that then adds 8mL 3-HClO 4Clear up 8h, the supernatant after will clearing up is measured the content of Zn in the liquid to be measured (referring to table 1,1-1) with atomic fluorescence spectrometer (SK-2002, Suokun Technology Development Co., Ltd., Xi'an City).
Described testing sample is through HNO 3-HClO 4When clearing up, add 6mLHNO in the testing sample earlier 3(ρ=1.42g/mL) disappears under 160 ℃ and boils 1h, then adds 2mLHClO 4(ρ=1.67g/mL), temperature bring up to 280 ℃ continuous disappear to boil occur minute bubbles continuously until the solution to crucible and overflow, steam and to crucible, melt thing and take off in the pasty state the time, be settled in the 50mL volumetric flask with the nitric acid of mass concentration 1%.
Atomic fluorescence spectrometer instrument start 20 minutes, continuously with standard series 0.00mg/mL standard sample introduction, treat the concentration (ρ of Zn in the stable back of reading bioassay standard series and the testing sample, mg/mL), again by ω (Zn)=(the ÷ m formula of ρ * V) calculate Zn in the soil the quality branch (ω, ug/g).Adopt that series concentration is 0.00,0.05,0.10,0.15, the zinc standard solution of 0.20mg/L in contrast, instrument condition of work: photoelectric tube negative high voltage: 300V lamp current: 70mA; Integral time: 5s; Combustion gas: 100mL/min; Carrier gas (air): 〉=1600mL/min; Auxilliary gas (air): 800mL/min.
ω (Zn)=(÷ m of ρ * V) wherein
In the formula: the massfraction of ω (Zn)-soil Zn, ug/g;
ρ-check in the concentration of Zn, mg/mL by working curve;
The cumulative volume of V-sample solution, mL;
The quality of M-pedotheque, g.
Embodiment 2:
Measure the method for zinc content in soil: the 0.2011g testing sample is added entry in the teflon crucible, make it wetting, then add the HNO of 13mL 3-HClO 4Clear up 15h, the supernatant after will clearing up is measured the content of Zn in the liquid to be measured (referring to table 1,1-2) with atomic fluorescence spectrometer (SK-2002, Suokun Technology Development Co., Ltd., Xi'an City).
Described testing sample is through HNO 3-HClO 4When clearing up, add 10mLHNO in the testing sample earlier 3(ρ=1.42g/mL) disappears under 180 ℃ and boils 1.5h, then adds 3mLHClO 4(ρ=1.67g/mL), temperature bring up to 300 ℃ continuous disappear to boil occur minute bubbles continuously until the solution to crucible and overflow, steam and to crucible, melt thing and take off in the pasty state the time, be settled in the 50mL volumetric flask with the nitric acid of mass concentration 5%.
Embodiment 3:
Measure the method for zinc content in soil: the 0.2001g testing sample is added entry in the teflon crucible, make it wetting, then add the HNO of 10mL 3-HClO 4Clear up 10h, the supernatant after will clearing up is measured the content of Zn in the liquid to be measured (referring to table 1,1-3) with atomic fluorescence spectrometer (SK-2002, Suokun Technology Development Co., Ltd., Xi'an City).
Described testing sample is through HNO 3-HClO 4When clearing up, add 8mLHNO in the testing sample earlier 3(ρ=1.42g/mL) disappears under 170 ℃ and boils 1.2h, then adds 2mLHClO 4(ρ=1.67g/mL), temperature bring up to 290 ℃ continuous disappear to boil occur minute bubbles continuously until the solution to crucible and overflow, steam and to crucible, melt thing and take off in the pasty state the time, be settled in the 50mL volumetric flask with the nitric acid of mass concentration 3%.
Embodiment 4
Measure the method for zinc content in soil: the 0.2002g testing sample is added entry in the teflon crucible, make it wetting, then add the HNO of 12mL 3-HClO 4Clear up 12h, the supernatant after will clearing up is measured the content of Zn in the liquid to be measured (referring to table 1,1-4) with atomic fluorescence spectrometer (SK-2002, Suokun Technology Development Co., Ltd., Xi'an City).
Described testing sample is through HNO 3-HClO 4When clearing up, add 9mLHNO in the testing sample earlier 3(ρ=1.42g/mL) disappears under 165 ℃ and boils 1.3h, then adds 3mLHClO 4(ρ=1.67g/mL), temperature bring up to 285 ℃ continuous disappear to boil occur minute bubbles continuously until the solution to crucible and overflow, steam and to crucible, melt thing and take off in the pasty state the time, be settled in the 50mL volumetric flask with the nitric acid of mass concentration 2%.
Embodiment 5
Measure the method for zinc content in soil: the 0.1998g testing sample is added entry in the teflon crucible, make it wetting, then add the HNO of 11mL 3-HClO 4Clear up 9h, the supernatant after will clearing up is measured the content of Zn in the liquid to be measured (referring to table 1,1-5) with atomic fluorescence spectrometer (SK-2002, Suokun Technology Development Co., Ltd., Xi'an City).
Described testing sample is through HNO 3-HClO 4When clearing up, add 8mLHNO in the testing sample earlier 3(ρ=1.42g/mL) disappears under 175 ℃ and boils 1.1h, then adds 3mLHClO 4(ρ=1.67g/mL), temperature bring up to 295 ℃ continuous disappear to boil occur minute bubbles continuously until the solution to crucible and overflow, steam and to crucible, melt thing and take off in the pasty state the time, be settled in the 50mL volumetric flask with the nitric acid of mass concentration 4%.
Embodiment 6
Measure the method for zinc content in soil: the 0.2g testing sample is added entry in the teflon crucible, make it wetting, then add 10mL HCl-HNO 3-HClO 4Clear up 8h, the supernatant after will clearing up is measured the content of Zn in the liquid to be measured (referring to table 1,2-1) with atomic fluorescence spectrometer (SK-2002, Suokun Technology Development Co., Ltd., Xi'an City).
Described testing sample is through HCl-HNO 3-HClO 4When clearing up, adding 6mLHCl disappears under 160 ℃ and boils in the testing sample, adds 2mL HNO when being evaporated to residue 5 ± 1mL 3, continue heating and steam near when thick, add 2mL perchloric acid (ρ=1.67g/mL), then improving temperature to 280 ℃ continuous disappearing boils, be heated to white cigarette and emit to the greatest extent, steam and to crucible, melt thing and take off in the pasty state the time, be settled in the 50mL volumetric flask with the nitric acid of mass concentration 4%.
Embodiment 7
Measure the method for zinc content in soil: the 0.2004g testing sample is added entry in the teflon crucible, make it wetting, then add 30mL HCl-HNO 3-HClO 4Clear up 15h, the supernatant after will clearing up is measured the content of Zn in the liquid to be measured (referring to table 1,2-2) with atomic fluorescence spectrometer (SK-2002, Suokun Technology Development Co., Ltd., Xi'an City).
Described testing sample is through HCl-HNO 3-HClO 4When clearing up, adding 10mLHCl disappears under 180 ℃ and boils in the testing sample, adds 15mL HNO when being evaporated to residue 6 ± 1mL 3, continue heating and steam near when thick, add 5mL perchloric acid (ρ=1.67g/mL), then improving temperature to 300 ℃ continuous disappearing boils, be heated to white cigarette and emit to the greatest extent, steam and to crucible, melt thing and take off in the pasty state the time, be settled in the 50mL volumetric flask with the nitric acid of mass concentration 5%.
Embodiment 8
Measure the method for zinc content in soil: the 0.1997g testing sample is added entry in the teflon crucible, make it wetting, then add 20mL HCl-HNO 3-HClO 4Clear up 10h, the supernatant after will clearing up is measured the content of Zn in the liquid to be measured (referring to table 1,2-3) with atomic fluorescence spectrometer (SK-2002, Suokun Technology Development Co., Ltd., Xi'an City).
Described testing sample is through HCl-HNO 3-HClO 4When clearing up, adding 8mLHCl disappears under 165 ℃ and boils in the testing sample, adds 8mL HNO when being evaporated to residue 7 ± 1mL 3, continue heating and steam near when thick, add 4mL perchloric acid (ρ=1.67g/mL), then improving temperature to 285 ℃ continuous disappearing boils, be heated to white cigarette and emit to the greatest extent, steam and to crucible, melt thing and take off in the pasty state the time, be settled in the 50mL volumetric flask with the nitric acid of mass concentration 3%.
Embodiment 9
Measure the method for zinc content in soil: with the 0.2003g testing sample in the teflon crucible
Add entry, make it wetting, then add 15mL HCl-HNO 3-HClO 4Clear up 13h, the supernatant after will clearing up is measured the content of Zn in the liquid to be measured (referring to table 1,2-4) with atomic fluorescence spectrometer (SK-2002, Suokun Technology Development Co., Ltd., Xi'an City).
Described testing sample is through HCl-HNO 3-HClO 4When clearing up, add HCl and HNO in the testing sample simultaneously 3, both are incorporated as 9mLHCl and 3mL HNO according to the proportioning of chloroazotic acid 3, under 175 ℃, disappear and boil, steam near when thick, (ρ=1.67g/mL), then improve temperature to 295 ℃ continuous disappearing and boil is heated to white cigarette and emits to the greatest extent to add 3mL perchloric acid, steam and to crucible, melt thing and take off in the pasty state the time, be settled in the 50mL volumetric flask with the nitric acid of mass concentration 2%.
Embodiment 10
Measure the method for zinc content in soil: the 0.2001g testing sample is added entry in the teflon crucible, make it wetting, then add 26mL HCl-HNO 3-HClO 4Clear up 15h, the supernatant after will clearing up is measured the content of Zn in the liquid to be measured (referring to table 1,2-5) with atomic fluorescence spectrometer (SK-2002, Suokun Technology Development Co., Ltd., Xi'an City).
Described testing sample is through HCl-HNO 3-HClO 4When clearing up, adding 8mLHCl disappears under 165 ℃ and boils in the testing sample, adds 13mL HNO when being evaporated to residue 5 ± 1mL 3, continue heating and steam near when thick, add 5mL perchloric acid (ρ=1.67g/mL), then improving temperature to 285 ℃ continuous disappearing boils, be heated to white cigarette and emit to the greatest extent, steam and to crucible, melt thing and take off in the pasty state the time, be settled in the 50mL volumetric flask with the nitric acid of mass concentration 1%.
The testing result of the different digestion method zinc of table 1
Figure S200810012247XD00051
From the table as can be known: acid mixture HNO 3-HClO 4And HCl-HNO 3-HClO 4Clear up the liquid to be measured after the soil sample, after AFS DETERMINATION, compare (referring to table 1) with national standard soil sample (GSS-3), favorable reproducibility, element disturbs few, is convenient to operation, and is highly sensitive, can be applicable to the detection of environmental area Zn.
Embodiment 11
Clear up the recovery of standard addition experiment that pedotheque carries out 4 concentration levels with two kinds of different digestion methods, result's (seeing Table 2) shows that AFS DETERMINATION result's accuracy is higher, the precision of measurement ideal.
The recovery of standard addition of table 2 pedotheque

Claims (9)

1. a method of measuring zinc content in soil is characterized in that: with the HNO of 0.2000 ± 0.0020g testing sample through 8-13mL 3-HClO 4Or the HCl-HNO of 10-30mL 3-HClO 4Clear up 8-15h, the solution to be measured after then will clearing up is measured the content of Zn in the liquid to be measured by atomic fluorescence spectrometer.
2. by the method for the described mensuration zinc content in soil of claim 1, it is characterized in that: described testing sample is through HNO 3-HClO 4When clearing up, add 6-10mLHNO in the testing sample earlier 3Under 160-180 ℃, disappear and boil 1-1.5h, then add 2-3mLHClO 4, temperature is brought up to 280-300 ℃ and is continued to disappear and boil until testing sample in the pasty state.
3. by the method for the described mensuration zinc content in soil of claim 2, it is characterized in that: disappearing at testing sample adds entry before boiling, and makes it wetting.
4. by the method for the described mensuration zinc content in soil of claim 2, it is characterized in that: the described testing sample that disappears after boiling is the nitric acid constant volume of 1-5% through mass concentration.
5. by the method for the described mensuration zinc content in soil of claim 1, it is characterized in that: described testing sample is through HCl-HNO 3-HClO 4When clearing up, adding 6-10mLHCl disappears under 160-180 ℃ and boils in the testing sample, adds 2-15mL HNO when being evaporated to raffinate for 4-8mL 3, continue heating and steam near and when thick, add 2-5mL perchloric acid, then improve temperature and boil to 280-300 ℃ of continuous disappearing, be heated to white cigarette and emit most.
6. by the method for the described mensuration zinc content in soil of claim 5, it is characterized in that: described testing sample is through HCl-HNO 3-HClO 4When clearing up, add HCl and HNO in the testing sample simultaneously 3, wherein HCl and HNO 3Proportioning according to chloroazotic acid adds.
7. by the method for the described mensuration zinc content in soil of claim 5, it is characterized in that: disappearing at testing sample adds entry before boiling, and makes it wetting.
8. by the method for the described mensuration zinc content in soil of claim 5, it is characterized in that: the described testing sample that disappears after boiling is the nitric acid constant volume of 1-5% through mass concentration.
9. by the method for the described mensuration zinc content in soil of claim 1, it is characterized in that: described atomic fluorescence spectrometer is the SK-2002 model, and its condition determination is photoelectric tube negative high voltage: 300V; Lamp current: 70mA; Integral time: 5s; Combustion gas: 100mL/min; Carrier gas: 〉=1600mL/min; Auxilliary gas: 800mL/min.
CN200810012247A 2008-07-09 2008-07-09 Method for testing zinc content in soil Pending CN101625321A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102313706A (en) * 2011-05-30 2012-01-11 广东工业大学 Digestion and determination method of heavy metals in waste dust-collecting bag
CN102507525A (en) * 2011-11-28 2012-06-20 齐齐哈尔大学 Novel method for constructing Zn2+ ratio detecting system by solubilizing fluorescent probe in micelle
CN103196892A (en) * 2013-04-02 2013-07-10 天津虹炎科技有限公司 Method for measuring metallic element mercury in soil
CN105388133A (en) * 2015-10-19 2016-03-09 广州市谱尼测试技术有限公司 Improved method for detecting zinc through atomic fluorescence spectrophotometer
CN108333073A (en) * 2018-02-08 2018-07-27 刘旭飞 The detection device of heavy metal zinc in agricultural soil
CN113418879A (en) * 2021-06-24 2021-09-21 宁夏新龙蓝天科技股份有限公司 Copper chloride solution detection method

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102313706A (en) * 2011-05-30 2012-01-11 广东工业大学 Digestion and determination method of heavy metals in waste dust-collecting bag
CN102313706B (en) * 2011-05-30 2013-02-13 广东工业大学 Digestion and determination method of heavy metals in waste dust-collecting bag
CN102507525A (en) * 2011-11-28 2012-06-20 齐齐哈尔大学 Novel method for constructing Zn2+ ratio detecting system by solubilizing fluorescent probe in micelle
CN103196892A (en) * 2013-04-02 2013-07-10 天津虹炎科技有限公司 Method for measuring metallic element mercury in soil
CN105388133A (en) * 2015-10-19 2016-03-09 广州市谱尼测试技术有限公司 Improved method for detecting zinc through atomic fluorescence spectrophotometer
CN108333073A (en) * 2018-02-08 2018-07-27 刘旭飞 The detection device of heavy metal zinc in agricultural soil
CN113418879A (en) * 2021-06-24 2021-09-21 宁夏新龙蓝天科技股份有限公司 Copper chloride solution detection method

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