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A method for direct conversion and detection of total cyanide and sulfide in aqueous solution

An aqueous solution and sulfide technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of difficult operation and complicated transformation system, achieve good selectivity, solve mutual interference of determination, and eliminate the interference of coexisting reducing substances Effect

Active Publication Date: 2017-02-15
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

Method used

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  • A method for direct conversion and detection of total cyanide and sulfide in aqueous solution
  • A method for direct conversion and detection of total cyanide and sulfide in aqueous solution
  • A method for direct conversion and detection of total cyanide and sulfide in aqueous solution

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Embodiment 1

[0025] like figure 1As shown, this embodiment includes a peristaltic pump 1, a first six-way valve 2, a flow-carrying container 3 containing a stabilizer and an exchange agent, an alkaline solution or water container 4, a sample container 5, a three-way valve 6, and an online filter 7 , a mixing tube 8, a photolyzer 9 and an ion chromatograph 10; the inlet of the peristaltic pump 1 is respectively connected to a flow-carrying container 3 containing a stabilizer and an exchanger, an alkaline solution or a water container 4, a sample container 5, and a peristaltic pump 1 The outlets are respectively connected to the first six-way valve 2, three-way valve 6 and online filter 7, the first six-way valve 2 is connected to the mixing pipe 8, and the three-way valve 6 is respectively connected to the flow-carrying container 3 containing stabilizer and exchanger With the first six-way valve 2, the mixing tube 8 is connected to the photolyzer 9, and the photolyzer 9 is connected to the ...

Embodiment 2

[0033] In this embodiment, water samples from the scrubber are taken, and after filtration and adsorption, the sample solution is injected into the quantitative loop 21 manually or by the peristaltic pump 1 . In the device, the volume of the quantitative loop 21 is 100 μL; the flow rate of the stabilizer and the exchanger is 0.4mL / min, and the stabilizer and the exchanger are iron-titanium reagent, sodium citrate and sulfamic acid, and the content is 0.02mol / L; Pure water carrier liquid, flow rate of pure water solvent 0.3mL / min; light source 8w, 312nm, narrow wave; spiral ring photolysis tube, hard glass, inner diameter 0.5mm, length 10m; illumination time, 9min; capture column 101, AG7; separation column 104, AS7; amperometric cell potential, 20mV; eluent, 0.5mol / L sodium acetate + 0.1mol / L sodium hydroxide + 0.5% m / m ethylenediamine; eluent flow rate, 1.0mL / After 9 minutes, change the eluent to 0.1mol / L sodium hydroxide + 5% v / v acetone. DX-500 ion chromatograph 10 system...

Embodiment 3

[0035] In this embodiment, a synthetic ammonia water sample is taken, and after filtration and adsorption, the sample solution is injected into the quantitative loop 21 manually or by a peristaltic pump 1 . In the device, the volume of the quantitative loop 21 is 200 μL; the flow rate of the stabilizer and the exchanger is 0.4mL / min, and the stabilizer and the exchanger are ethylenediaminetetraacetate and hypophosphite with a content of 0.02mol / L; Enter the pure water carrier liquid, the flow rate of pure water solvent is 0.4mL / min; light source 8w, 312nm, narrow wave; spiral ring photolysis tube, hard glass, inner diameter 0.5mm, length 10m; illumination time, 8min; capture column 101 , Metrosep A PCC 1HC / 4.0; separation column 104, Metrosep A Supp 4 separation column 104; amperometric cell potential, 10mV; eluent, 0.1mol / L sodium hydroxide+3.5% acetone v / v; eluent flow rate, 0.01min, 0.8mL / min; 9min later, 1.8mL / min. The sulfide peak and cyanide peak were separated by the 8...

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Abstract

The invention discloses a device and a method for detecting total cyanide and sulfide in a water solution by employing direct conversion. The method comprises the following steps: feeding a sample solution of which the pH is greater than or equal to 11 into a six-way valve quantitative loop to quantify through an online filter, feeding excessive sample solution into a liquid waste bottle; switching a six-way valve, pumping a pure water solvent as a carrying current, pushing out the sample solution, and pumping a water solution containing a stabilizer and an exchanger in advance; after mixing with the sample coming from quantitative loop samples, switching a three-way valve, and refluxing into a storage bottle, further pushing the solution to be mixed evenly in a mixing pipe by virtue of the pure water solvent; entering a photolysis device to carry out photolysis until reaching a capture column in the six-way valve in an ion chromatograph; locking a to-be-detected object, feeding a non-to-be-detected object into the liquid waste bottle; rising the capture column by using an eluting solution, and entering a separation post; sequentially discharging the sulfide and cyanide; and respectively detecting the sulfide and the cyanide by virtue of an ampere detector, and then rinsing the separation column in a reinforcing manner. Compared with an existing national standard method, the method disclosed by the invention is green, safe, environment-friendly, and little in interference; the analysis time, the laboratory safety and the cost are obviously improved; and use of a toxic reagent is also reduced.

Description

technical field [0001] The invention relates to a method for measuring total cyanide and sulfide, in particular to a device and method for direct conversion and detection of total cyanide and sulfide in aqueous solution. Background technique [0002] Total cyanide in wastewater includes free cyanide and complex cyanide, including weak cyanide complexes with low complexation stability constants (such as Cu and Zn) and strong cyanide complexes with high complexation stability constants (such as Fe). Including cyanide complexes with extremely high complex stability constants, such as complexes with Co, Au, and Pt, etc. The existing total cyanide analysis methods are mainly silver nitrate titration method, isonicotinic acid-pyrazolone photometric method and isonicotinic acid-barbituric acid colorimetric method. These three methods all require separation and exclusion of interfering substances. Pretreatment is required, where cyanide is converted to hydrogen cyanide by distillat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/96
Inventor 陆克平夏文兵张元广郑学根宋友陵
Owner CHINA PETROLEUM & CHEM CORP
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