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Apparatus and method for distillation-free non-color-development detection of trace-amount releasable cyanogens and total cyanogens in water solution

An aqueous solution and trace technology, applied in the field of analytical chemistry, can solve problems such as toxic reagents, reduce use and storage, reduce human operation errors, and eliminate increase or decrease.

Active Publication Date: 2016-07-06
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The fully enclosed distillation, absorption and detection of samples reduces the pollution of cyanide to the environment and the harm to the human body. It has outstanding advantages especially in the detection of large quantities of samples, but the problem of the method itself is still the same. Pyridine, barbituric acid and chloramine-T (a very strong oxidizing agent) in photometry, other interfering substances such as halogens, thiocyanates, thiosulfates, aldehydes and sugars, and nitrogen oxides

Method used

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  • Apparatus and method for distillation-free non-color-development detection of trace-amount releasable cyanogens and total cyanogens in water solution
  • Apparatus and method for distillation-free non-color-development detection of trace-amount releasable cyanogens and total cyanogens in water solution
  • Apparatus and method for distillation-free non-color-development detection of trace-amount releasable cyanogens and total cyanogens in water solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Such as figure 2 As shown, prepare 0-500 μg / L cyanide standard solution series, prepare two sets of standard curves of 0-50 μg / L and 50-500 μg / L on the above device, and save them; different diameter membranes have different standard curves.

[0058] The cyanide-containing wastewater is discharged pool water. Both the quantitative loop and the second quantitative loop are 100 μL, 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, the inner diameter is 0.5mm, and the length is 1.1m; Time, 7min (programmable stop flow 1~999s); membrane separator (set with membrane diffusion separator acid chamber and membrane diffusion separator alkali chamber) (serpentine dialysis tank with upper and lower symmetrical flow channels, diffusion path 100mm, Hydrophobic membrane ); the alkaline solution is 0.001mol / L sodium oxalate+0.01mol / L sodium hydroxide, and the flow rate is 0.8mL / min. Aci...

Embodiment 2

[0066] The device and operating procedures are as in Example 1. Take a certain amount of water sample from the discharge pool, filter it with fast filter paper, the quantitative loop and the second quantitative loop are 200 μL, the flow rate of the sample solution 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; illumination time, 6min (programmable stop-flow 1-999s); membrane separator (set with membrane diffusion separator acid chamber and membrane diffusion Separator alkali chamber) (serpentine dialysis tank with upper and lower symmetrical flow channels, diffusion path 100mm, hydrophobic membrane ); the alkaline solution is 0.001mol / L sodium oxalate+0.02mol / L sodium hydroxide, and the flow rate is 0.7mL / min. Acid solution B is a mixture of 1.0mol / L tartaric acid and 0.3mol / L zinc nitrate, containing 0.001mol / L-0.05mol / L sulfamic acid + ascorbic acid, with a flow rate of 0.8mL / min. T...

Embodiment 3

[0068] The device and operating procedures are as in Example 1, and the cyanide-containing wastewater is a synthetic ammonia water sample. The quantitative loop and the second quantitative loop are 200μL, the flow rate of the sample solution is 1.2mL / min; the light source is 8w (on), 312nm, narrow wave; the spiral ring photolysis tube, hard glass, the inner diameter is 0.5mm, and the length is 1.1m; the light time , 6.5min (programmable stop flow 1 ~ 999s);; Membrane separator (set with membrane diffusion separator acid chamber and membrane diffusion separator alkali chamber); alkali solution is 0.001mol / L sodium oxalate + 0.02mol / L sodium hydroxide, flow rate 0.9mL / min. Acidic solution A is a mixture of 0.4mol / L phosphoric acid and 0.2mol / L hypophosphorous acid, containing 0.001mol / L-0.1mol / L sulfamic acid + ascorbic acid + EDTA + citric acid, with a flow rate of 1.0mL / min. The flow rate of water was 0.6 mL / min. Low-pressure enrichment column, IonPacAG11; CNSolutionFS3100 ...

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Abstract

The invention discloses a device and method for non-distillation-free and non-chromogenic detection of trace amounts of easily-released cyanide and total cyanide in an aqueous solution. The device includes a peristaltic pump, an alkali solution pump tube, an acid solution pump tube, an aqueous solution pump tube, a washing device, and a detection device. The method includes filtering the sample solution, mixing it with an acidic solution, mixing it fully in the mixing tube, and transporting it to the photolysis device for photolysis, so that the different forms of cyanide are converted into simple hydrogen cyanide, and the sulfide is converted into hydrogen sulfide. The alkali chamber of the membrane diffusion separator flows through the low-pressure enrichment column, and the cyanide retained in the low-pressure enrichment column is washed by the eluent in the injection pump, enters the ampere pool, and is detected by DC amperometry. The operating conditions of the present invention are mild , high selectivity, long service life of hydrophobic membrane, safety and environmental protection, high recovery rate and no human error, it can measure easily released cyanide or total cyanide in wastewater within 10 minutes.

Description

technical field [0001] The invention relates to a device and method for non-distillation-free and non-color-developing detection of trace amounts of easily-released cyanide and total cyanide in aqueous solution, belonging to the technical field of analytical chemistry. Background technique [0002] Total cyanide refers to all simple cyanides (mostly cyanides of alkali metals and alkaline earth metals, ammonium cyanides) and most complex cyanides (zinc cyanide complexes, ferricyanides, ferrocyanides, copper cyanides complexes, nickel-cyanide complexes, etc.), excluding cobalt-cyanide complexes. Easy-releasing cyanides include all simple cyanides (mostly alkali metal and alkaline earth metal cyanides) and zinc cyanide complexes, excluding ferricyanide, ferrocyanide, copper cyanide complexes, nickel cyanide complexes, cobalt cyanide complex. [0003] Total cyanide and easily released cyanide in wastewater are two important items in environmental pollution monitoring. Cyanide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/26G01N1/28
Inventor 陆克平黄劲松汪声美郑学根
Owner CHINA PETROLEUM & CHEM CORP
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