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Sample preprocessing device provided with ion chromatograph and used for detecting anions and use method

An ion chromatograph and sample pretreatment technology, which is applied in the fields of analytical chemistry and sample automatic pretreatment devices, can solve the problems of only one type, complex structure, and difficulty in supporting automation of ion chromatographs, so as to reduce the introduction and selectivity. High, the effect of improving the lower limit of detection

Inactive Publication Date: 2016-10-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The so-called "Yinglan" automatic online sample pretreatment technology developed by well-known foreign manufacturers with the dialysis unit and suppression unit as the core, and the so-called "Principle" automatic online sample pretreatment technology based on ten-way valve switching and solid phase extraction column technology Technology, as their ion chromatography-specific supporting equipment, directly analyzes 'dirty' samples and complex matrix samples, which solves the problem of contamination and purification of ion chromatography columns by the complex matrix of samples, and also greatly improves the measurement results and accuracy of complex matrix samples. The sensitivity of the analytical method is improved, but it is difficult to automate the matching with other manufacturers' ion chromatographs, and the structure is also slightly complicated. Although there are many functions, only one can be used at a time, and the combination still needs to be assembled.

Method used

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  • Sample preprocessing device provided with ion chromatograph and used for detecting anions and use method
  • Sample preprocessing device provided with ion chromatograph and used for detecting anions and use method
  • Sample preprocessing device provided with ion chromatograph and used for detecting anions and use method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Such as figure 1 As shown, a sample pretreatment device for detecting anions with a supporting ion chromatograph, comprising a sample liquid suction pipe (11), an absorption liquid storage bottle (12), a sample liquid peristaltic pump (21), an absorption liquid peristaltic pump (22), A dialysis tank (4) and an ion chromatograph system (5), a hydrophilic membrane (43) is arranged in the dialysis tank (4), and the hydrophilic membrane (43) separates the dialysis tank (4) into an absorption side (41) and a sample side (42), characterized in that: the sample pretreatment device also includes a cation exchanger (8), an absorption liquid storage ring (35), a six-way valve (3), a flushing liquid storage bottle (13) and a flushing liquid injection pump (7), ion chromatograph system (5) comprises sampling six-way valve (6), enrichment column (51), guard column (52), analysis column (53), suppressor (54), conductivity detector ( 55), and a display (56); the design of the dialysi...

Embodiment 2

[0048] Basic method of operation of the device in Example 1:

[0049] (1) System flushing, adjust the six-way valve (3) and the sampling six-way valve (6) to the sample injection state, store ultrapure water in the flushing liquid storage bottle (13) and the absorption liquid storage bottle (12) , put the sample liquid suction tube (11) into the liquid to be tested; start the syringe pump (7), sample liquid peristaltic pump (21) and absorption liquid peristaltic pump (22) at the same time, flush the system pipeline;

[0050] (two) T 1 After a certain time, close the absorption liquid peristaltic pump (22) and the syringe pump (7), and the sample liquid peristaltic pump (21) remains on, T 1 Represents the cleaning time of the system flow path and dialysis tank;

[0051] (three) T 3 After a period of time, the ion concentration on both sides of the dialysis tank (4) hydrophilic membrane (43) reaches equilibrium, the sample liquid peristaltic pump (21) is turned off, the absor...

Embodiment 3

[0057]Preparation of standard solution: Prepare a series of mixed standard solutions, each mixed standard solution contains chloride ions in the concentration range of 1-100ug / L, fluoride ions in the range of 1-100ug / L, nitrate ions in the range of 1-100ug / L, 1- 100ug / L methacryl sulfonate ion, 1~100ug / L phosphate ion, 1~100ug / L sulfate ion and 10~1000μg / L thiocyanate ion; separately prepare 1~100μg / L sub Sulfate standard solution series, calibrated by iodometric method with 1g / L sulfite mother liquor before use, obtained by successive dilution with aqueous solution containing 0.15% triethanolamine + 0.55% formaldehyde; mixed standard solution can simulate the coexistence of various ions The influence of time interaction on the conductivity fully takes into account the influence of the real testing environment on the testing results. Through such a design, the introduction of errors can be minimized to make the testing results more authentic and reliable. Since sulfite is easi...

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Abstract

The invention discloses a sample preprocessing device provided with an ion chromatograph and used for detecting anions and a use method. The device comprises a sample liquid suck-in pipe, an absorption liquid storage bottle, a flushing liquid storage bottle, a sample liquid peristaltic pump, an absorption liquid peristaltic pump, a flushing liquid injection pump, a dialysis pool, an anion exchanger, a six-way valve, an absorption liquid storage ring and the ion chromatograph. The sample liquid peristaltic pump, the absorption liquid peristaltic pump, the ion chromatograph and the flushing liquid injection pump are all connected with a computer terminal. During dialysis, sample liquid flows, and absorption liquid stops flowing; when absorption liquid is transferred to the absorption liquid storage ring, sample liquid stops flowing, and absorption liquid flows; when the six-way valve is switched, the flushing liquid injection pump flushes absorption liquid in the storage ring to an anion enrichment column in the ion chromatograph. The device has the advantages of online removing heavy metal ions, being low in measurement limit, high in sample adaptability, mild in condition and free of toxic reagents, being matched with the ion chromatograph, and being capable of measuring various anions in sewage or acrylic fiber solvent within 20 min.

Description

technical field [0001] The invention belongs to the category of analytical chemistry and includes flow injection technology, membrane dialysis technology, column capture technology and valve switching technology. The invention relates to an automatic sample pretreatment device for an ion chromatograph, which can realize the on-line pretreatment of conventional inorganic anion and acrylic solvent anion tests in wastewater. Background technique [0002] Ion chromatography (IC) has developed rapidly since its advent in the 1970s, and is considered to be the most effective method for analyzing ionic substances, especially suitable for the rapid and simultaneous determination of multi-component inorganic and organic anions and cations. Ion chromatography is also known as the conventional 7 kinds of anions (F - , Cl - , NO 2 - 、Br - , NO 3 - 、PO 4 3- , SO 4 2- ) and some small molecule organic acids (such as CHO 2 - 、CH 3 CO 2 - ) detection method - strong selectiv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/08
CPCG01N30/06G01N30/08
Inventor 陆克平罗骁刘浩吴全法朱四九
Owner CHINA PETROLEUM & CHEM CORP
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