Method for detecting total cyanide and sulfide through online photolysis-noncontact diffusion-chromatographic separation

A chromatographic separation and sulfide technology, applied in the field of total cyanide and sulfide, can solve the problems of changing ion chromatograph, difficult operation, complicated conversion system, etc., achieving good selectivity, less consumption of reagents and samples, and laboratory costs. improved effect

Active Publication Date: 2014-11-26
ANQING NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The UV photolysis-ion chromatographic separation-voltammetric (ampere) cell determination of cyanide and sulfide in wastewater reported earlier in the literature, the conversion system is relatively complicated, and the internal changes of the ion chromatograph need to be changed, which is difficult to operate
[0004] The present invention detects the method for total cyanide and sulfide in waste water, and it obtains total cyanide under mild condition, and to the protection of reducing sulfide, then there is no report

Method used

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  • Method for detecting total cyanide and sulfide through online photolysis-noncontact diffusion-chromatographic separation
  • Method for detecting total cyanide and sulfide through online photolysis-noncontact diffusion-chromatographic separation
  • Method for detecting total cyanide and sulfide through online photolysis-noncontact diffusion-chromatographic separation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Take no less than 20mL of wastewater from the treatment tank, filter with fast filter paper, the quantitative loop is 100μL, the sample solution flow rate is 1.5mL / min; light source 8w (on), 312nm, narrow wave; spiral ring photolysis tube, hard glass, inner diameter 0.5mm, length 1.1m; light time, 7min (programmable stop flow 1~999s); gas-liquid membrane separation and diffusion unit, hydrophobic membrane φ47mm, pore size 0.55μm; water flow rate in the first peristaltic pump 0.5mL / min, acid The solution flow rate is 0.8mL / min, the composition is a mixture of 0.5mol / L phosphoric acid and 0.1mol / L hypophosphorous acid, containing 0.001mol / L~0.1mol / L sulfamic acid, ascorbic acid, EDTA, citric acid (sulfamic acid The contents of acid, ascorbic acid, EDTA, and citric acid are all greater than 0); the flow rate of the alkaline absorption solution is 0.8 mL / min, and the composition is 0.001 mol / L ethylene diamine and 0.01 mol / L sodium hydroxide. Capture column, IonPac AG7; sepa...

Embodiment 2

[0050] The equipment and operating procedures are the same as in Example 1. Take a certain amount of water sample from the conditioning pool, filter it with fast filter paper, the quantitative loop is 200μL, the sample solution flow rate is 1.3mL / min; the light source is 8w (off), 312nm, narrow wave; spiral ring photolysis Tube, hard glass, inner diameter 0.5mm, length 1.1m; light time, 6min (programmable stop flow 1~999s); gas-liquid membrane separation and diffusion unit, hydrophobic membrane φ47mm, pore size 0.65μm; water in the first peristaltic pump The flow rate is 0.6mL / min, and the acidic solution flow rate is 0.8mL / min. The composition is a mixture of 0.5mol / L phosphoric acid and 0.1mol / L hypophosphorous acid, containing 0.001mo1 / L~0.1mol / L sulfamic acid, ascorbic acid, EDTA, citric acid; the flow rate of the alkaline absorption solution is 0.8mL / min, and the composition is 0.001mol / L ethylenediamine and 0.01mol / L sodium hydroxide. Capture column, Metrosep A PCC 1 HC / 4...

Embodiment 3

[0052] The equipment and operating procedures are as in Example 1. Take a sample of synthetic ammonia water and filter it with fast filter paper. The quantitative loop is 200μL, the sample solution flow rate is 1.3mL / min; the light source is 8w, 312nm, narrow wave; spiral ring photolysis tube, hard glass , Inner diameter 0.5mm, length 1.1m; light time, 8min; gas-liquid membrane separation and diffusion unit, hydrophobic membrane φ47mm, pore size 0.22μm; water flow rate in the first peristaltic pump 0.55mL / min, acid solution flow rate 0.85mL / min, composition It is a mixture of 0.5mol / L phosphoric acid and 0.1mol / L hypophosphorous acid, containing 0.001mol / L~0.1mol / L sulfamic acid, ascorbic acid, EDTA, and citric acid; the flow rate of the alkaline absorption solution is 0.75mL / min , The composition is 0.001mol / L ethylenediamine and 0.01mol / L sodium hydroxide. Capture column, Metrosep A PCC 1 VHC / 4.0; Separation column, AS7; Silver working electrode (Ag), three waveform integral ...

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Abstract

The invention discloses a method for detecting total cyanide and sulfide through online photolysis-noncontact diffusion-chromatographic separation. The method mainly comprises the following steps: in a flowing injection system, absorbing a sample into an acid solution flow to be conveyed into a photolysis device for photolysis so that cyanide in different forms is turned into hydrogen cyanide and sulfide is turned into hydrogen sulfide, passing the solution through an acid canal of a gas-liquid membrane separation diffusion unit to be diffused into an alkali canal on the other side through a hydrophobic membrane in a noncontact manner; keeping the cyanide and the sulfide diffused in an alkaline absorbing solution; by alternately switching a second six-way valve and a third six-way valve, driving a matter to be detected in a buffer pipe through a water solution in an injection pump, trapping the matter to be detected in the buffer pipe through a trapping column in the third six-way valve and locking the matter to be detected; washing the trapping column through leacheate, entering a separation column, discharging the cyanide and the sulfide sequentially and detecting one by one through an ampere detector. The method disclosed by the invention is short in detection time, light in interference, sealed in process, high in sensitivity, low in damage on member, mild in condition and environmental friendly.

Description

Technical field [0001] The invention belongs to the field of analytical chemistry, and relates to a flow injection-ultraviolet photolysis-non-contact dialysis-chromatographic separation of sulfide ion and cyanide ion-pulse amperometric detection of total cyanide and sulfide in wastewater. Background technique [0002] Cyanide and sulfide are two important items in environmental pollution monitoring. At the same time, there are three main points to accurately determine the total cyanide and sulfide in wastewater. One is to convert all the complex cyanide in the sample into free cyanide, the other is the separation of cyanide and sulfide, and the third is to treat cyanide and sulfide in the conversion process. The interference of sulfide is eliminated. The existing standard method for total cyanide is HJ 484-2009, the determination of water quality cyanide (volume method and spectrophotometry), which is mainly distilled under strong acid conditions to convert cyanide into hydrogen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/20G01N30/14
Inventor 张元广陆克平王钧伟秦伟高迎春
Owner ANQING NORMAL UNIV
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