CN102721761A - Method for detecting content of perchlorate in solid media in environment through chromatography of ions and application thereof - Google Patents
Method for detecting content of perchlorate in solid media in environment through chromatography of ions and application thereof Download PDFInfo
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- CN102721761A CN102721761A CN2012102205473A CN201210220547A CN102721761A CN 102721761 A CN102721761 A CN 102721761A CN 2012102205473 A CN2012102205473 A CN 2012102205473A CN 201210220547 A CN201210220547 A CN 201210220547A CN 102721761 A CN102721761 A CN 102721761A
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Abstract
The invention discloses a method for detecting content of perchlorate in solid media in the environment through chromatography of ions and application thereof. The method includes: weighing proper amount of treated solid medium samples in the environment, preparing solution with the solid-to-liquid ratio of 1:10, shaking for 3 hours in a table concentrator, centrifuging for 30 minutes on a centrifugal machine, filtering the supernate, removing metal ions and organic matters in the filtrate through treatment of an RP column and an H column, measuring the peak area of liquid to be measured of the samples under the condition of optimum chromatograph, and calculating the concentration of the liquid to be tested according to a standard curve. The method is used for detecting the content of the perchlorate in the environment and is short in appearance time, and the relative standard deviation is lower than 5%. The method for detecting content of the perchlorate can be widely used in detecting the content of the perchlorate in the solid media in the environment, is particularly suitable for detecting the content of the perchlorate in soil or bottom mud of rivers, has significant meaning in monitoring damage of the perchlorate and can meet the requirement for scientific research and production.
Description
Technical field
The present invention relates to the detection method of the contaminant ion salt content in the solid dielectric in a kind of environment; Particularly relate to the perchlorate content detecting method in the solid dielectric in a kind of environment; Relate to the application of the perchlorate content detecting method in the solid dielectric in a kind of environment simultaneously; Can be used for accurately measuring the content of the perchlorate in the environment, and be used to monitor the harm technical field of perchlorate.
Background technology
Perchlorate is a kind of ubiquitous persistence environmental contaminants that potential hazard is arranged, and it has dynamic stability, ease of solubility, makes it in environment, can steady in a long-termly exist.The perchlorate that commercial production produces can be absorbed, accumulate and pass through food chain by plant and get into human body through approach such as soil, water bodys.Because high chloro acid ion's electric charge and radius and iodide ion are very approaching; Can get into the thyroid gland of mammal and human body with the iodide ion competition, weaken the active function of thyroid body, cause the minimizing of thyroid hormone secretion amount; Cause multiple dysfunction, caused the public's extensive concern thus.
Perchlorate is as the ion salt that high harmfulness is arranged; American National Environmental Protection Agency classifies perchlorate as drinking water pollution phenology and mends list; China is along with the high speed development of space flight, national defence, industrial or agricultural; The pollution of perchlorate is unquestionable, at present the monitoring standard of temporary no perchlorate in China's water quality standard.Therefore, the content of accurately measuring the perchlorate in the environment has great importance to the harm of monitoring perchlorate.
Have many methods can measure the perchlorate in the environment, like ultraviolet-visible spectrophotometry, ISE, Raman spectrum, but this several method detectability is too high, and the mensuration process is complicated, is not easy to implement; Also have methods such as Mass Spectrometer Method in addition; Mass detector has good sensitivity and selectivity; Can the perchlorate that concentration is low to moderate several ng/L be detected, but also weak point is arranged, for example when chromatographic resolution is insufficient; Electro-spray ionization source mass spectrum exists ionization to suppress phenomenon, thereby influences the mensuration of perchlorate.In addition, the complex structure of mass detector is restricted its application with costing an arm and a leg.The most process of the method for the perchlorate in the existing mensuration environment is complicated; Waste time and energy during enforcement; Testing cost is higher, is not suitable for measuring the content of the perchlorate in the environment of variable concentrations scope of a large amount of samples, can not satisfy the needs of research and production well.
Summary of the invention
In order to solve the prior art problem, the objective of the invention is to overcome the defective that prior art exists, provide a kind of chromatography of ions of utilizing to perchlorate content detecting method and application in the solid dielectric in the environment; This method is easy to be easy-to-use; Measure reliable results, time saving and energy saving, be easy to control; Be applicable to the content of the perchlorate in the environment of the variable concentrations scope of measuring a large amount of samples, this method can be widely used in the detection to the perchlorate content in the solid dielectric in the environment.
For reaching the foregoing invention purpose, the present invention adopts following technical proposals:
A kind of chromatography of ions of utilizing is to the perchlorate content detecting method in the solid dielectric in the environment, and this method may further comprise the steps:
(1) drafting of perchlorate ion's typical curve: the perchlorate solution of selecting at least 5 kinds of variable concentrations of preparation for use is as standard solution feature samples reference system solution; Ion chromatography through to each standard solution feature samples reference system solution detects; Obtain the chromatography of ions standard spectrogram of the perchlorate of standard solution feature samples reference system solution; And carry out ion chromatography; Obtain the perchlorate ion's typical curve in the standard solution feature samples reference system solution: Y=aX+b, wherein Y is a voltage, unit is mV; Wherein X is the time, and unit is min; A and b are all dimensionless factor; Preferred concentration of the present invention is respectively the perchlorate solution of 5 kinds of variable concentrations of 5mg/L, 10mg/L, 20mg/L, 50 mg/L and 100 mg/L as standard solution feature samples reference system solution; The chromatography of ions condition that standard solution feature samples reference system solution of the present invention detects can be selected following testing conditions especially:
A. chromatographic column: METROSEP A SUPP 5 – 250,4mm * 250mm,
B. guard column: Metrosep RP Guard,
C. eluent concentration: 5. 0 mmol/L Na2CO3+20% acetonitrile (percent by volume),
D. leacheate flow velocity: 0.7ml/min,
E. sample size: 10 μ L,
F. post is pressed: 800-1100psi,
G. background conductance: 16-18uS;
(2) produce sample to be tested: get the solid dielectric sample in the environment, after the impurity elimination freeze drying, grind, mix subsequent use excessively behind 100 mesh sieves;
(3) extract perchlorate in the sample to be tested: the subsequent use sample to be tested of preparation in the weighing above-mentioned steps (2) is that the ratio of 1:10 carries out putting into shaking table and shaking after solid-liquid mixes according to the subsequent use sample to be tested and the mass ratio of high purity water; And extraction solution; The solution that is extracted is carried out centrifugal again, get supernatant and use membrane filtration, obtain filter liquor; Remove metallic ion and organic molecule in the filter liquor then, obtain high chlorate extract to be measured; Remove metallic ion and preferably corresponding respectively employing RP post of organic molecule and the processing of H post in the filter liquor; The concussion speed of shaking table is preferably 250r/min, and extraction time is preferably 3 hours; Centrifugal speed is preferably 5000r/min, and centrifugation time is preferably 30min; The pore-size of the filter membrane that filtering supernatant is used is preferably 0.22 μ m;
(4) stratographic analysis of perchlorate extract to be measured test: with above-mentioned steps (1) under the identical chromatography of ions condition of standard solution feature samples reference system solution detection; Draw to extract and pre-service and above-mentioned steps (1) in the perchlorate extract to be measured of sample size equal volume when carrying out the chromatography of ions detection with standard solution feature samples reference system solution; Carry out ion chromatography; Record the peak area of perchlorate ion's curve in the perchlorate extract to be measured; With reference in above-mentioned steps (1), obtaining perchlorate ion's typical curve, convert concentration into perchlorate extract to be measured;
(5) calculating of the perchlorate content in the solid dielectric sample in the environment:
Calculate with following formula (I):
In the formula (I):
M is the perchlorate content in the solid dielectric sample in the environment, and unit is mg/kg;
in above-mentioned steps (4), converting the concentration that obtains perchlorate extract to be measured according to the ion chromatography test data, unit is mg/L;
M is the quality of the solid dielectric sample in the environment that in above-mentioned steps (3), is taken by weighing, and unit is g;
w
H2O Be the water percentage of the solid dielectric sample in the environment that in above-mentioned steps (3), is taken by weighing, unit is a mass percent;
V be with above-mentioned steps (1) in the volume of the perchlorate extract to be measured of standard solution feature samples reference system solution sample size equal volume, unit is ml.
The present invention utilizes the chromatography of ions perchlorate content detecting method in the solid dielectric in the environment to be widely used in the perchlorate content that detects in soil or the river bed bed mud.
The present invention has following conspicuous outstanding substantive distinguishing features and remarkable advantage compared with prior art:
Adopt the perchlorate content in the inventive method testing environment, appearance time is fast, and relative standard deviation detects and is limited to 1 μ g/L less than 5%.This shows, the invention of this method, for the content of the perchlorate in the testing environment provides a kind of method of implementing be convenient to reliably, easy to operate, cost is lower, is easy to promote, and can satisfy the needs of research and production.
Description of drawings
Fig. 1 is that the embodiment of the invention one perchlorate ion's concentration is chlorate ion's chromatogram standard spectrogram of the standard solution feature samples reference system solution of 20 μ g/L.
Embodiment
In conjunction with accompanying drawing, details are as follows to the preferred embodiments of the present invention:
Embodiment one:
The precision of the perchlorate content in the bed mud of river bed and the recovery detect, and may further comprise the steps:
(1) drafting of perchlorate ion's typical curve: preparing respectively and selecting concentration for use is that the perchlorate solution of 5 kinds of variable concentrations of 5mg/L, 10mg/L, 20mg/L, 50 mg/L and 100 mg/L is as standard solution feature samples reference system solution; Ion chromatography through to each standard solution feature samples reference system solution detects; Obtain the chromatography of ions standard spectrogram of the perchlorate of standard solution feature samples reference system solution; When carrying out the ion chromatograph analyzing and testing, ion chromatograph is modulated following best chromatographic condition:
A. chromatographic column: METROSEP A SUPP 5 – 250,4mm * 250mm;
B. guard column: Metrosep RP Guard;
C. eluent concentration: 5. 0 mmol/L Na
2CO
3+ 20% acetonitrile (volume fraction);
D. leacheate flow velocity: 0.7ml/min;
E. sample size: 10 μ L;
F. post is pressed: 800-1100psi;
G. background conductance: 16-18 (uS);
Wherein perchlorate ion's concentration is that chlorate ion's chromatogram standard spectrogram of the standard solution feature samples reference system solution of 20 μ g/L is seen Fig. 1.Ion chromatography through to each standard solution feature samples reference system solution detects; Obtain the chromatography of ions standard spectrogram of the perchlorate of standard solution feature samples reference system solution; And carry out ion chromatography; The perchlorate ion's typical curve that obtains in the standard solution feature samples reference system solution is Y=29.374X+0.3538, and its perchlorate ion's typical curve linearly dependent coefficient is R
2＞0.999.
(2) produce sample to be tested: get river bed bed mud sample, after the impurity elimination freeze drying, grind, behind 100 mesh sieves, mix subsequent use excessively.
(3) perchlorate in the bed mud sample of extraction river bed to be measured: the river bed bed mud sample 2.000g that accurately takes by weighing above-mentioned drying is in conical flask; Quantitatively add the 20ml high purity water; Put into shaking table and extract 3h, then solution is transferred in the centrifuge tube the centrifugal 30min of the rotating speed of 5000r/min with the speed jolting of 250r/min; Get supernatant with 0.22 μ m membrane filtration, then filter liquor is handled to remove metallic ion and organism with RP post and H post.
(4) stratographic analysis of perchlorate extract to be measured test: draw and extract and pretreated river bed bed mud sample solution 10 μ l; Under the best ion chromatographic condition in the present embodiment; Carry out perchlorate ion's stratographic analysis; Record the peak area of perchlorate ion's curve in the perchlorate extract to be measured, the perchlorate ion's typical curve in the reference standard solution feature samples reference system solution is Y=29.374X+0.3538, converts the concentration into perchlorate extract to be measured.
(5) calculating of the perchlorate content in the river bed bed mud sample:
Calculate with following formula (I):
（Ⅰ）
In the formula (I):
M is the perchlorate content in the bed mud sample of river bed, and unit is mg/kg;
M is the quality of the river bed bed mud sample that in above-mentioned steps (3), taken by weighing, and unit is g;
w
H2O Be the water percentage of the river bed bed mud sample that takes by weighing in above-mentioned steps (3), unit is a mass percent;
V be with above-mentioned steps (1) in the volume of the perchlorate extract to be measured of standard solution feature samples reference system solution sample size equal volume, unit is ml.
Present embodiment utilizes the chromatography of ions that the precision and the recovery of the perchlorate content detecting method in the bed mud of river bed are detected:
In order to verify that present embodiment utilizes accuracy and the technique effect of the chromatography of ions to the perchlorate content detecting method in the solid dielectric in the environment; The river bed bed mud comparative sample that perchlorate addition in every kilogram of river bed bed mud is respectively three kinds of perchlorate contaminated of 5.0 mg/kg, 10.0 mg/kg and 20.0mg/kg has been prepared in design in addition; Wherein the river bed bed mud comparative sample of every kind of perchlorate contaminated divides the same processing mode of another edition of a book enforcement to obtain 5 parallel river bed bed mud comparative sample again; And respectively these three groups of river bed bed mud comparative sample are carried out ion chromatography; Calculate the perchlorate content of river bed bed mud comparative sample; Compare and analyze with the river bed bed mud comparative sample of pairing three kinds of perchlorate contaminated, obtain the recovery of this enforcement detection method, and calculate relative deviation.Analysis result is seen the precision and the recovery check and analysis result of the perchlorate content in the bed mud of table 1. river bed.
The precision of the perchlorate content in the bed mud of table 1. river bed and recovery check and analysis result
The precision of the perchlorate content in the river bed bed mud from table 1 and recovery check and analysis result can find out, utilize the present embodiment detection method to detect the content of the perchlorate in the bed mud of river bed, and appearance time is fast, and relative standard deviation is less than 5%.This shows that the present embodiment detection method is for the detection of the perchlorate content in the bed mud of river bed, and is time saving and energy saving, measure reliable results, can satisfy the needs of scientific research and production.
Embodiment two:
The precision of the perchlorate content in the soil and the recovery detect, and may further comprise the steps:
(1) drafting of perchlorate ion's typical curve: identical with the step (1) of embodiment one.
(2) produce sample to be tested: the earth sample that fetches earth, after the impurity elimination freeze drying, grind, behind 100 mesh sieves, mix subsequent use excessively.
(3) perchlorate in the extraction pedotheque to be measured: the pedotheque 2.000g that accurately takes by weighing above-mentioned drying is in conical flask; Quantitatively add the 20ml high purity water; Put into shaking table and extract 3h, then solution is transferred in the centrifuge tube the centrifugal 30min of the rotating speed of 5000r/min with the speed jolting of 250r/min; Get supernatant with 0.22 μ m membrane filtration, then filter liquor is handled to remove metallic ion and organism with RP post and H post.
(4) stratographic analysis of perchlorate extract to be measured test: draw and extract and pretreated pedotheque solution 10 μ l; Under the best ion chromatographic condition in the present embodiment; Carry out perchlorate ion's stratographic analysis; Record the peak area of perchlorate ion's curve in the perchlorate extract to be measured, the perchlorate ion's typical curve in the reference standard solution feature samples reference system solution is Y=29.374X+0.3538, converts the concentration into perchlorate extract to be measured.
(5) calculating of the perchlorate content in the pedotheque: calculate with following formula (I):
（Ⅰ）
In the formula (I):
M is the perchlorate content in the pedotheque, and unit is mg/kg;
in above-mentioned steps (4), converting the concentration that obtains perchlorate extract to be measured according to the ion chromatography test data, unit is mg/L;
M is the quality of the pedotheque that in above-mentioned steps (3), taken by weighing, and unit is g;
w
H2O Be the water percentage of the alleged earth sample that fetches earth in above-mentioned steps (3), unit is a mass percent;
V be with above-mentioned steps (1) in the volume of the perchlorate extract to be measured of standard solution feature samples reference system solution sample size equal volume, unit is ml.
Present embodiment utilizes the chromatography of ions that the precision and the recovery of the perchlorate content detecting method in the soil are detected:
In order to verify that present embodiment utilizes accuracy and the technique effect of the chromatography of ions to the perchlorate content detecting method in the solid dielectric in the environment; The soil comparative sample that perchlorate addition in every kilogram of soil is respectively three kinds of perchlorate contaminated of 5.0 mg/kg, 10.0 mg/kg and 20.0mg/kg has been prepared in design in addition; Wherein the soil comparative sample of every kind of perchlorate contaminated divides the same processing mode of another edition of a book enforcement to obtain 5 parallel soil comparative sample again; And respectively these three groups of soil comparative sample are carried out ion chromatography; Calculate the perchlorate content of soil comparative sample; Compare and analyze with the soil comparative sample of pairing three kinds of perchlorate contaminated, obtain the recovery of this enforcement detection method, and calculate relative deviation.Analysis result is seen the precision and the recovery check and analysis result of the perchlorate content in table 2. soil.
The precision of the perchlorate content in table 2. soil and recovery check and analysis result
The precision of the perchlorate content in the soil from table 2 and recovery check and analysis result can find out, utilize the present embodiment detection method to detect the content of the perchlorate in the soil, and appearance time is fast, and relative standard deviation is also less than 5%.This shows that the present embodiment detection method is for the detection of the perchlorate content in the soil, and is time saving and energy saving, measure reliable results, also can satisfy the needs of scientific research and production.
Combine accompanying drawing that the embodiment of the invention is illustrated above; But the invention is not restricted to the foregoing description; Can also make multiple variation according to the purpose of innovation and creation of the present invention; Change, the modification of making under all spirit and principles according to technical scheme of the present invention, substitute, combination, simplify, all should be the substitute mode of equivalence, as long as goal of the invention according to the invention; Only otherwise deviate from the present invention and utilize know-why and the inventive concept of the chromatography of ions, all belong to protection scope of the present invention to the perchlorate content detecting method in the solid dielectric in the environment.
Claims (7)
1. one kind is utilized the chromatography of ions to the perchlorate content detecting method in the solid dielectric in the environment, it is characterized in that this method may further comprise the steps:
(1) drafting of perchlorate ion's typical curve: the perchlorate solution of selecting at least 5 kinds of variable concentrations of preparation for use is as standard solution feature samples reference system solution; Ion chromatography through to each standard solution feature samples reference system solution detects; Obtain the chromatography of ions standard spectrogram of the perchlorate of standard solution feature samples reference system solution; And carry out ion chromatography; Obtain the perchlorate ion's typical curve in the standard solution feature samples reference system solution: Y=aX+b, wherein Y is a voltage, unit is mV; Wherein X is the time, and unit is min; A and b are all dimensionless factor;
(2) produce sample to be tested: get the solid dielectric sample in the environment, after the impurity elimination freeze drying, grind, mix subsequent use excessively behind 100 mesh sieves;
(3) extract perchlorate in the sample to be tested: the subsequent use sample to be tested of preparation in the weighing above-mentioned steps (2) is that the ratio of 1:10 carries out putting into shaking table and shaking after solid-liquid mixes according to the subsequent use sample to be tested and the mass ratio of high purity water; And extraction solution; The solution that is extracted is carried out centrifugal again, get supernatant and use membrane filtration, obtain filter liquor; Remove metallic ion and organic molecule in the filter liquor then, obtain high chlorate extract to be measured;
(4) stratographic analysis of perchlorate extract to be measured test: with above-mentioned steps (1) under the identical chromatography of ions condition of standard solution feature samples reference system solution detection; Draw to extract and pre-service and above-mentioned steps (1) in the perchlorate extract to be measured of sample size equal volume when carrying out the chromatography of ions detection with standard solution feature samples reference system solution; Carry out ion chromatography; Record the peak area of perchlorate ion's curve in the perchlorate extract to be measured; With reference in above-mentioned steps (1), obtaining perchlorate ion's typical curve, convert concentration into perchlorate extract to be measured;
(5) calculating of the perchlorate content in the solid dielectric sample in the environment:
Calculate with following formula (I):
In the formula (I):
M is the perchlorate content in the solid dielectric sample in the environment, and unit is mg/kg;
M is the quality of the solid dielectric sample in the environment that in above-mentioned steps (3), is taken by weighing, and unit is g;
w
H2O Be the water percentage of the solid dielectric sample in the environment that in above-mentioned steps (3), takes by weighing, unit is a mass percent;
V be with above-mentioned steps (1) in the volume of the perchlorate extract to be measured of standard solution feature samples reference system solution sample size equal volume, unit is ml.
2. the chromatography of ions of utilizing according to claim 1 is to the perchlorate content detecting method in the solid dielectric in the environment; It is characterized in that: in above-mentioned steps (1), the chromatography of ions condition that standard solution feature samples reference system solution detects is following:
A. chromatographic column: METROSEP A SUPP 5 – 250,4mm * 250mm;
B. guard column: Metrosep RP Guard;
C. eluent concentration: 5. 0 mmol/L Na2CO3+20% acetonitrile (percent by volume);
D. leacheate flow velocity: 0.7ml/min;
E. sample size: 10 μ L;
F. post is pressed: 800-1100psi;
G. background conductance: 16-18uS.
3. the chromatography of ions of utilizing according to claim 1 and 2 is to the perchlorate content detecting method in the solid dielectric in the environment; It is characterized in that: in above-mentioned steps (3), metallic ion and corresponding respectively RP post and the H post of adopting of organic molecule removed in the filter liquor are handled.
4. the chromatography of ions of utilizing according to claim 3 is characterized in that the perchlorate content detecting method in the solid dielectric in the environment: in above-mentioned steps (3), the concussion speed of shaking table is 250r/min, and extraction time is 3 hours; Centrifugal speed is 5000r/min, and centrifugation time is 30min.
5. the chromatography of ions of utilizing according to claim 3 is characterized in that the perchlorate content detecting method in the solid dielectric in the environment: in above-mentioned steps (3), the pore-size of the filter membrane that filtering supernatant is used is 0.22 μ m.
6. the chromatography of ions of utilizing according to claim 1 and 2 is to the perchlorate content detecting method in the solid dielectric in the environment; It is characterized in that: in above-mentioned steps (1), select for use the perchlorate solution of 5 kinds of variable concentrations that concentration is respectively 5mg/L, 10mg/L, 20mg/L, 50 mg/L and 100 mg/L as standard solution feature samples reference system solution.
7. claim 1 or the 2 described application that utilize the chromatography of ions to the perchlorate content detecting method in the solid dielectric in the environment is characterized in that: the perchlorate content that is used for detecting soil or river bed bed mud.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103713017A (en) * | 2013-12-25 | 2014-04-09 | 国核宝钛锆业股份公司 | Method for determining content of chlorine in nuclear-grade zirconium material |
| CN105891386A (en) * | 2016-07-07 | 2016-08-24 | 国家烟草质量监督检验中心 | Measurement of perchlorate ions in smokeless tobacco products |
| CN115436558A (en) * | 2022-08-03 | 2022-12-06 | 浙江衢化氟化学有限公司 | Method for measuring content of chlorine-series oxides by ion chromatography |
-
2012
- 2012-06-29 CN CN2012102205473A patent/CN102721761A/en active Pending
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| J. JACKSON ELLINGTON等: "Determination of perchlorate at parts-per-billion levels in plants by ion chromatography", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| YINXIAN PENG等: "Biodegradation Behavior of Perchlorate in Soils and Sediments", 《ENVIRONMENT AND TRANSPORTATION ENGINEERING（RSETE）》 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103713017A (en) * | 2013-12-25 | 2014-04-09 | 国核宝钛锆业股份公司 | Method for determining content of chlorine in nuclear-grade zirconium material |
| CN103713017B (en) * | 2013-12-25 | 2015-09-23 | 国核宝钛锆业股份公司 | A kind of method measuring content of Cl element in nuclear-grade zirconium material |
| CN105891386A (en) * | 2016-07-07 | 2016-08-24 | 国家烟草质量监督检验中心 | Measurement of perchlorate ions in smokeless tobacco products |
| CN105891386B (en) * | 2016-07-07 | 2018-05-25 | 国家烟草质量监督检验中心 | The measure of perchlorate in smoke-free tobacco product |
| CN115436558A (en) * | 2022-08-03 | 2022-12-06 | 浙江衢化氟化学有限公司 | Method for measuring content of chlorine-series oxides by ion chromatography |
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Application publication date: 20121010 |