CN104237395B - A kind of glacial water inorganic anion measuring method - Google Patents

A kind of glacial water inorganic anion measuring method Download PDF

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Publication number
CN104237395B
CN104237395B CN201310233606.5A CN201310233606A CN104237395B CN 104237395 B CN104237395 B CN 104237395B CN 201310233606 A CN201310233606 A CN 201310233606A CN 104237395 B CN104237395 B CN 104237395B
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nitrite
chlorion
concentration
inorganic anion
measuring method
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CN104237395A (en
Inventor
王晓香
张海霞
张耀南
崔晓庆
王肖波
李森
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Northwest Institute of Eco Environment and Resources of CAS
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Cold and Arid Regions Environmental and Engineering Research Institute of CAS
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Abstract

The invention discloses a kind of glacial water inorganic anion measuring method, it is characterized in that utilizing the chromatography of ions such as degree such as grade, snow and ice solution is analyzed in conjunction with self-control ion-exchange chromatography, high-concentration chlorine ion and low concentration nitrite chromatographic peak degree of separation are improved greatly, and compared with prior art, equipment price is cheap in the present invention, Measuring Time is short, consumptive material is low-consuming, and testing cost is low, and measuring accuracy is high.

Description

A kind of glacial water inorganic anion measuring method
Technical field
The present invention relates to inorganic anion to measure, specifically refer to a kind of method that glacial water inorganic anion is measured.
Background technology
Snow ice is the storage vault of various material in air, is the indicator of Climate and Environment Variation, is the important information source of global climate environmental change, and avalanche quench research has become the important content of global change research due.Anions and canons in snow ice is the reliability index of reflection climate change and environmental lapse, therefore, study the differentiation that the problems such as the source of anions and canons, transmission mechanism and the secondary change mechanism in snow ice thereof not only can recover Climate and environment, the more important thing is and interactional fresh evidence between geographical ring layer can be provided, particularly to the migration and conversion research important in inhibiting of material between air sphere, lithosphere, hydrosphere, cryosphere and humanity are enclosed.The research of snow ice modern process is the basis rebuilding ice core paleoclimate environment record, and avalanche quench properties study is one of important content of snow ice modern process research.
Snow and ice contains a large amount of chlorion, and because chlorion is close with nitrite polarity, in ion chromatography, appearance time is comparatively near, and what the chlorion of large concentration can mask nitrite usually goes out peak.Existing method mainly utilizes expensive chromatography of ions Gradient Elution Method to be separated detection.This method must adopt quaternary gradient pump, and instrument and equipment is expensive, tests length consuming time, and consumptive material consumption is large, and experimental cost is high.
Summary of the invention
In order to overcome above-mentioned technical deficiency part, the object of the present invention is to provide a kind of glacial water inorganic anion measuring method.The degree ion chromatography measurements such as the method employing go out snow ice water middle and high concentration chlorion and low concentration nitrite.
Object of the present invention and step:
A. configure the chlorion of serial concentration known and the standard solution of nitrite, apply following test condition with conductivity to concentration, draw the standard working curve of chlorion and nitrite standard solution, standard working curve selects quadratic equation to return;
During detection, chromatographic condition is as follows:
I chromatographic column: WW, 4mm × 250mm laboratory self-control; Chromatographic column fixed phase component is degree of crosslinking 5%-12% polystyrene-divinyl;
II eluent concentration: sodium carbonate 1.8-2.8mmol/L-sodium bicarbonate 0.2-0.6mmol/L
III leacheate flow velocity: 0.8-1.2mmol/L
IV sample size: 50 μ L
B. sample tests: under above-mentioned chromatographic condition, gets solution to be measured, carries out ion chromatograph analysis.
The present invention compared with prior art, the advantage had:
The degree sulfate by ion chromatography such as employing of the present invention analyze the detection analysis of snow and ice middle and high concentration chlorion and low concentration nitrite, and equipment price is cheap, and Measuring Time is short, and consumptive material is low-consuming, and testing cost is low, and the degree of separation of chromatographic peak is high, and measuring accuracy is high.
Accompanying drawing explanation
Fig. 1 is chlorion of the present invention and nitrite ion chromatogram.
Fig. 2 is existing chlorion and nitrite ion chromatogram.
Embodiment
A kind of glacial water inorganic anion measuring method, its step comprises:
(1) described detection method comprises the steps:
The preparation of typical curve: respectively by 1g/L chlorion mother liquor dilution preparation 10 μ g/ml, 50 μ g/ml, 200 μ g/ml, the Chloride Solution of 500 μ g/ml, 1mg/L nitrous acid mother liquor dilution preparation 1ng/ml, 3ng/ml, 9ng/ml, the nitrite ion standard solution of 15ng/ml, is adjusted to following chromatographic condition by ion chromatograph, carries out ion chromatograph analysis.
During detection, chromatographic condition is as follows:
I chromatographic column: WW, 4mm × 250mm laboratory self-control; Chromatographic column fixed phase component is degree of crosslinking 5%-12% polystyrene-divinyl;
II eluent concentration: sodium carbonate 1.8-2.8mmol/L-sodium bicarbonate 0.2-0.6mmol/L
III leacheate flow velocity: 0.8-1.2mmol/L
IV sample size: 50 μ L
(2) sample tests: under above-mentioned chromatographic condition, gets solution 50 μ L to be measured, carries out ion chromatograph analysis.
Through ion chromatograph analysis, in snow and ice, chlorion and nitrite chromatogram are shown in Fig. 1 and Fig. 2.Wherein Fig. 1 be the present invention apply self-control chromatographic column and etc. the degree chromatography of ions record chromatogram, Fig. 2 is that conventional method records chromatogram.As can be seen from Fig. 1 and Fig. 2: Fig. 1 chlorion and nitrite chromatographic peak degree of separation high, and Fig. 2 chlorion and nitrite chromatographic peak degree of separation low, cause high-concentration chlorine ion likely can annex nitrite chromatographic peak, cause chlorine ion concentration inaccurate, and nitrite detects not out, and the present invention measures chlorion and nitrite chromatographic peak degree of separation in snow ice water greatly improves, ensure that the Measurement accuracy of two kinds of ions.

Claims (1)

1. a glacial water inorganic anion measuring method, is characterized in that:
A. the chlorion of serial concentration known and the standard solution of nitrite is configured, respectively by 1g/L chlorion mother liquor dilution preparation 10 μ g/ml, 50 μ g/ml, 200 μ g/ml, the Chloride Solution of 500 μ g/ml, 1mg/L nitrous acid mother liquor dilution preparation 1ng/ml, the nitrite ion standard solution of 3ng/ml, 9ng/ml, 15ng/ml, ion chromatograph is adjusted to following chromatographic condition, carries out ion chromatograph analysis; Apply following test condition with conductivity to concentration, draw the standard working curve of chlorion and nitrite standard solution, standard working curve selects quadratic equation to return;
During detection, chromatographic condition is as follows:
I chromatographic column: WW, 4mm × 250mm laboratory self-control; Chromatographic column fixed phase component is degree of crosslinking 5%-12% polystyrene-divinyl;
II eluent concentration: sodium carbonate 1.8-2.8mmol/L-sodium bicarbonate 0.2-0.6mmol/L;
III leacheate flow velocity: 0.8-1.2mmol/L;
IV sample size: 50 μ L;
B. sample tests: under above-mentioned chromatographic condition, gets solution to be measured, carries out ion chromatograph analysis.
CN201310233606.5A 2013-06-07 2013-06-07 A kind of glacial water inorganic anion measuring method Active CN104237395B (en)

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CN104655762B (en) * 2015-03-06 2017-01-18 辽宁省分析科学研究院 Method for determining content of anions in cleaning fluid of nuclear pump
CN106226454B (en) * 2016-08-06 2018-06-26 青岛农业大学 The ion chromatographic method of trace chloro ion in a kind of measure trimethyl gallium
CN106338509B (en) * 2016-08-22 2019-03-08 杭州天迈生物科技有限公司 A kind of nitrite in food rapid detection card piece

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CN102507765A (en) * 2011-10-20 2012-06-20 苏州康润医药测试服务有限公司 Method for simultaneously detecting content of trace bromate and nitrite in drinking water

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JPH049758A (en) * 1990-04-27 1992-01-14 Yokogawa Electric Corp Method and apparatus for measuring sulfite ion

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102507765A (en) * 2011-10-20 2012-06-20 苏州康润医药测试服务有限公司 Method for simultaneously detecting content of trace bromate and nitrite in drinking water

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
Determination of major ions in snow and ice cores by ion chromatography;C. F. Buck etal.;《Journal of Chromatography》;19920306;第594卷(第2期);全文 *
DX-300离子色谱测定山地冰川雪冰中的有机酸与无机酸阴离子;周会;《色谱》;20010731;第19卷(第4期);全文 *
ICS-90离子色谱测定雪冰中低分子有机酸和无机阴离子;丁文慈等;《琼州学院学报》;20090428;第16卷(第2期);全文 *
超高含量氯离子基体下痕量亚硝酸盐的检测;刘肖等;《分析实验室》;20071130;第26卷(第11期);第100-103页 *

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Patentee before: Institute of environment and Engineering in cold and dry areas, Chinese Academy of Sciences

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