On-line photolysis dialysis/chromatographic separation amperometric detection device and method for total cyanide and sulfide in wastewater

A chromatographic separation and amperometric detection technology, which is applied in the field of online photolysis dialysis/chromatographic separation amperometric detection of total cyanide and sulfide in wastewater, can solve the problems of complicated conversion system and difficult operation, so as to save strong acid distillation treatment and avoid separation Effect of conversion absorption, prevention effect

Active Publication Date: 2017-05-03
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The UV photolysis-ion chromatographic separation-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
"Stop flow" in online dialysis combined with ion chromatography for determination is an analytical technique developed by Metrohm, which is connected with ultraviolet photolysis for the acquisition of total cyanide, but there is no report

Method used

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  • On-line photolysis dialysis/chromatographic separation amperometric detection device and method for total cyanide and sulfide in wastewater
  • On-line photolysis dialysis/chromatographic separation amperometric detection device and method for total cyanide and sulfide in wastewater
  • On-line photolysis dialysis/chromatographic separation amperometric detection device and method for total cyanide and sulfide in wastewater

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Embodiment 1

[0028] Such as figure 1As shown, this embodiment includes an alkali receiving solution container 1, a sample container 2, a first peristaltic pump 3, a second peristaltic pump 4, a filter 5, a photolyzer 6, a dialysis tank 7 and an ion chromatograph 8, the dialysis The pool 7 includes a receiving liquid channel 71 and a sample channel 72, and a hydrophilic membrane 73 is arranged between the receiving liquid channel 71 and the sample channel 72 for separation, and one end of the first peristaltic pump 3 is connected to the alkali receiving solution Container 1, the other end is connected to the receiving liquid channel 71 of the dialysis tank 7, one end of the second peristaltic pump 4 is connected to the sample container 2, and the other end is connected to the filter 5, and the sample container 2 is provided with a stabilizer and an exchange agent for filtering Device 5 links to each other with photolyzer 6, and photolyzer 6 links to each other with the sample channel 72 of ...

Embodiment 2

[0039] The sample in this embodiment is the water sample of the adjustment pool, which is filtered with fast filter paper. The preparation of the sample mixed solution is as follows: first add a grain (tablet) of sodium hydroxide, 0.5 mL of hypophosphorous acid with a mass percentage of 10%, 0.5 mL of an iron-titanium reagent with a mass percentage of 1% and 1% of a mass percentage in a 10 mL volumetric flask. Ascorbic acid 0.5mL, add 5mL sample solution, mix uniformly to make a sample mixed solution. The flow rate of the sample mixed solution in the second peristaltic pump 4 is 0.4mL / min; the light source of the photolysis device 6 is 8w, 312nm, narrow wave, spiral ring photolysis tube, hard glass, inner diameter 0.5mm, length 10m, and light time 9min; After stop-flow dialysis for 9min, enter 100μL quantitative loop 81; transfer time 32s; guard column 84: IonPac AG7; separation column 86: IonPac AS7; amperometric cell potential 0mV; eluent: 0.01min, 0.5mol / L sodium acetate+ ...

Embodiment 3

[0042] The sample of the present embodiment is the total well sewage sample of sodium thiocyanate, which is filtered through fast filter paper. The preparation of the sample mixed solution is as follows: first add a grain (tablet) of sodium hydroxide, 0.5 mL of hypophosphorous acid with a mass percentage of 10%, 0.5 mL of an iron-titanium reagent with a mass percentage of 1% and 1% of a mass percentage in a 10 mL volumetric flask. Add 0.5mL of sulfamic acid to 5mL of sample solution, and mix to obtain a sample mixed solution. The flow rate of the sample mixed solution in the second peristaltic pump 4 is 0.5mL / min; the light source of the photolysis device 6 is 8w, 312nm, narrow wave, spiral ring photolysis tube, hard glass, inner diameter 0.5mm, length 10m, light time 8min; After stop-flow dialysis for 10 minutes, enter 50μL quantitative loop 81; transfer time 32s; guard column 84: Metrosep A Supp 10Guard; separation column 86: Metrosep A Supp 10-100; ampere cell potential 10m...

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Abstract

The invention discloses a device and a method for amperometric detection of the total cyanide and sulfide of wastewater by online photolysis dialysis / chromatographic separation. A first peristaltic pump pumps alkaline in a container into a receiving-liquid cavity channel of a dialysis cell, the excessive solution flows through a quantitative ring in an ion chromatograph, then flows into a waste-liquid bottle and then is stopped; a second peristaltic pump injects a fixed-volume sample solution containing a stabilizing agent and an exchange agent into a filter and a photolysis device continuously to reach a sample cavity channel of the dialysis cell, and after components to be detected are bilaterally balanced by membrane dialysis, the first peristaltic pump is started and conveys received liquid containing the total cyanide and the sulfide into a quantitative ring of a six-way valve in the ion chromatograph; by switching of the six-way valve, leacheate flows through the quantitative ring and is separated from a separating column by a protective column and is detected out by an amperometric detector. The device and the method disclosed by the invention have the advantages that under the mild alkaline condition, all cyanides are converted into alkaline-metal cyanides by narrow-spectrum ultraviolet photolysis, so that not only is the classic process of strong-acid distillation or acidified ultraviolet photolysis and then membrane separation omitted, but also almost no membrane pressure is generated in operation, and the sample treatment is simple.

Description

technical field [0001] The invention relates to a method for measuring total cyanide and sulfide, in particular to an on-line photolysis dialysis / chromatographic separation amperometric detection device and method for total cyanide and sulfide in wastewater. Background technique [0002] Accurate determination of total cyanide and sulfide in wastewater is very important for environmental and industrial applications. For the detection of the two, there are two key points, one is to turn all the complex cyanide in the sample into free cyanide, and the other is to separate the interfering substances such as cyanide and sulfide. The existing standard method for total cyanide is mainly to convert cyanide into hydrogen cyanide by distillation under strongly acidic conditions, add reagents to eliminate interference, and use titration, electrode method and photometric method after lye absorption. These two types of methods have the defects of slow analysis speed, cumbersome operati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 陆克平汪声美姚旺生毕锡斌程泉
Owner CHINA PETROLEUM & CHEM CORP
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