On-line photolysis-non-contact diffusion-chromatographic separation method for detection of total cyanide and sulfide

A chromatographic separation and sulfide technology, which is applied in the field of total cyanide and sulfide, can solve the problems of ion chromatograph changes, difficult operation, complicated transformation system, etc., and achieve good selectivity, low consumption of reagents and samples, and low laboratory costs. improved effect

Active Publication Date: 2016-04-06
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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  • On-line photolysis-non-contact diffusion-chromatographic separation method for detection of total cyanide and sulfide
  • On-line photolysis-non-contact diffusion-chromatographic separation method for detection of total cyanide and sulfide
  • On-line photolysis-non-contact diffusion-chromatographic separation method for detection of total cyanide and sulfide

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Take not less than 20mL of waste water from the treatment pool, filter it with fast filter paper, the quantitative loop is 100μL, the flow rate of the sample solution is 1.5mL / min; the light source is 8w (on), 312nm, narrow wave; the spiral ring photolysis tube, hard glass, inner diameter 0.5mm, length 1.1m; illumination time, 7min (programmable stop flow 1~999s); gas-liquid membrane separation and diffusion unit, hydrophobic membrane φ47mm, pore diameter 0.55μm; water flow rate in the first peristaltic pump 0.5mL / min, acidic The flow rate of the solution is 0.8mL / min, and the composition is a mixture of 0.5mol / L phosphoric acid and 0.1mol / L hypophosphorous acid, which contains 0.001mol / L~0.1mol / L sulfamic acid, ascorbic acid, EDTA, citric acid (sulfamic acid) acid, ascorbic acid, EDTA, and citric acid are all greater than 0); 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. ...

Embodiment 2

[0050] The device and operation procedures are as in Example 1. Take a certain amount of water sample from the adjustment pool, filter it with fast filter paper, the quantitative loop is 200 μL, the flow rate of the sample solution is 1.3mL / min; the light source is 8w (off), 312nm, narrow wave; helical ring photolysis Tube, hard glass, inner diameter 0.5mm, length 1.1m; illumination time, 6min (programmable stop flow 1-999s); gas-liquid membrane separation and diffusion unit, hydrophobic membrane φ47mm, pore diameter 0.65μm; water in the first peristaltic pump The flow rate is 0.6mL / min, the flow rate of the acidic solution 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; the flow rate of alkaline absorption solution is 0.8mL / min, and the composition is 0.001mol / L ethylenediamine and 0.01mol / L sodium hydroxide. Trap column, MetrosepAPCC1HC / 4....

Embodiment 3

[0052] The device and operating procedures are as in Example 1. Take the synthetic ammonia water sample, filter it with fast filter paper, the quantitative loop is 200 μL, the flow rate of the sample solution is 1.3mL / min; the light source is 8w, 312nm, narrow wave; the spiral ring photolysis tube, hard glass , inner diameter 0.5mm, length 1.1m; illumination time, 8min; gas-liquid membrane separation and diffusion unit, hydrophobic membrane φ47mm, pore diameter 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, citric acid; the flow rate of alkaline absorption solution is 0.75mL / min , composed of 0.001mol / L ethylenediamine and 0.01mol / L sodium hydroxide. Trap column, MetrosepAPCC1VHC / 4.0; Separation column, AS7; Silver working electrode (Ag), three-waveform integration pu...

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Abstract

The invention discloses an online photolysis-non-contact diffusion-chromatographic separation method for detecting total cyanide and sulfide. Solution, so that different forms of cyanide into hydrogen cyanide, sulfide into hydrogen sulfide, flow through the acid channel of the gas-liquid membrane separation diffusion unit, non-contact diffusion through the hydrophobic membrane into the other side of the alkali channel; alkaline absorption The liquid will store the diffused cyanide and sulfide in it; through the alternate switching of the second and third six-way valves, the aqueous solution of the syringe pump drives the analyte in the buffer tube, so that the analyte in the buffer tube enters the trapping column in the third six-way valve , to lock the analyte; the eluent washes the trapping column, enters the separation column, cyanide and sulfide flow out in sequence, and are detected one by one by the amperometric detector. The invention has short detection time, less interference, airtight process, high sensitivity, little membrane damage, mild conditions and environmental protection.

Description

technical field [0001] The invention belongs to the field of analytical chemistry and relates to a method for detecting total cyanide and sulfide in wastewater by flow injection-ultraviolet photolysis-non-contact dialysis-chromatographic separation of sulfur ions and cyanide ions-pulse amperometry. Background technique [0002] Cyanide and sulfide are two important items in environmental pollution monitoring. At the same time, there are three key points for accurately determining the total cyanide and sulfide in wastewater. One is to change all complex cyanide in the sample into free cyanide, the other is to separate cyanide from sulfide, and the third is to convert cyanide and sulfide in the conversion process. Sulfide Interference Elimination. Existing total cyanide standard method is HJ484-2009, water quality cyanide determination volumetric method and spectrophotometric method), mainly is to convert cyanide into hydrogen cyanide by distillation under strong acidic condi...

Claims

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Application Information

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Patent Type & Authority Patents(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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