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Method for determining easy-to-release cyanide in sulfide-containing based cyanide-containing solid waste

A technology of solid waste and determination method, which is used in the measurement of color/spectral properties, chemical analysis by titration, etc., can solve the problems of low measurement results, poor accuracy, inability to determine, etc. accurate effect

Active Publication Date: 2018-07-20
CHANGCHUN GOLD RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] In the new environmental protection law, cyanide-containing solid waste is listed as a hazardous waste list. Cyanide is a highly toxic substance, and its accurate detection is very important. For example, in the gold production process, the cyanide gold leaching process is one of the very important means. The solid waste produced by the cyanidation gold leaching process contains cyanide, and most of them also contain relatively high sulfide. When the cyanide-containing solid waste containing sulfide is easy to release cyanide, the sulfide ion will enter the absorption liquid during distillation. Affect the measurement results. For example, when the cyanide content in cyanide-containing solid waste is high, when the silver nitrate titration method is used for determination, if the sample contains sulfide, the color of the titration end point cannot be seen and cannot be measured. Cyanide-containing solid waste can develop color normally by colorimetry, but the measurement result is low
[0003] The national standard and the standard of the Ministry of Environmental Protection currently measure the easy-to-release cyanide in water quality, such as HJ 484-2009 "Determination of Water Quality Cyanide by Volumetric Method and Spectrophotometric Method", although the influence of sulfide is considered: if there is a large amount of sulfide , using cadmium carbonate and lead carbonate for pretreatment, but for cyanide-containing solid waste, pretreatment cannot be performed first, and the resulting sulfide precipitation and cyanide-containing solid waste cannot be separated
Secondly, during the first distillation, metal ions that form precipitates with sulfide ions cannot be added. These ions will combine with cyanide, which makes the measurement results of easily released cyanide low and the accuracy is not good.

Method used

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  • Method for determining easy-to-release cyanide in sulfide-containing based cyanide-containing solid waste
  • Method for determining easy-to-release cyanide in sulfide-containing based cyanide-containing solid waste
  • Method for determining easy-to-release cyanide in sulfide-containing based cyanide-containing solid waste

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] (1) Use a balance to weigh 1.00 g of cyanide-containing solid waste containing sulfide, transfer the sample to a distillation flask with distilled water, use distilled water to set the volume to 250 mL, add 5 mL of ethanol, shake the sample, and place in the distillation flask Add several glass beads, add 10mL zinc nitrate solution with a concentration of 100g / L and 10mL tartaric acid solution with a concentration of 150g / L, shake well, connect the distillation device, and add 10mL hydrogen with a concentration of 20g / L into the 100mL receiving bottle Sodium oxide solution is used as the absorption liquid. The upper end of the distillate conduit is connected to the outlet of the condenser tube, and the lower end is inserted into the absorption liquid of the receiving bottle. Check the connection to make it tight. During distillation, the lower end of the distillate conduit should be inserted under the liquid surface of the absorption liquid. , so that the absorption is c...

Embodiment 2

[0081] (1) Use a balance to weigh 1.25 g of cyanide-containing solid waste containing sulfides, transfer the sample to a distillation flask with distilled water, use distilled water to set the volume to 250 mL, add 5 mL of ethanol, shake the sample, and place in the distillation flask Add several glass beads, add 12.5mL of zinc nitrate solution with a concentration of 100g / L and 12.5mL of tartaric acid solution with a concentration of 150g / L, shake well, connect the distillation device, and add 10mL of Sodium hydroxide solution is used as the absorption liquid. The upper end of the distillate conduit is connected to the outlet of the condenser tube, and the lower end is inserted into the absorption liquid of the receiving bottle. Check the connection to make it tight. During distillation, the lower end of the distillate conduit should be inserted into the liquid surface of the absorption liquid. down for complete absorption.

[0082] (2) Stop distillation when the volume of th...

Embodiment 3

[0108] (1) Use a balance to weigh 1.50 g of cyanide-containing solid waste containing sulfide, transfer the sample to a distillation flask with distilled water, use distilled water to set the volume to 250 mL, add 5 mL of ethanol, shake the sample, and place in the distillation flask Add several glass beads, add 15mL zinc nitrate solution with a concentration of 100g / L and 15mL tartaric acid solution with a concentration of 150g / L, shake well, connect the distillation device, and add 10mL hydrogen with a concentration of 20g / L into a 100mL receiving bottle Sodium oxide solution is used as the absorption liquid. The upper end of the distillate conduit is connected to the outlet of the condenser tube, and the lower end is inserted into the absorption liquid of the receiving bottle. Check the connection to make it tight. During distillation, the lower end of the distillate conduit should be inserted under the liquid surface of the absorption liquid. , so that the absorption is com...

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Abstract

The invention relates to a method for determining easy-to-release cyanide in sulfide-containing based cyanide-containing solid waste, and belongs to the technical field of determination of easy-to-release cyanide in solid waste. The method comprises the following steps: selecting sampling weight, adopting ethanol as a dispersing agent and adding distilled water to further increase dispersity of the cyanide-containing solid waste; using zinc nitrate and tartaric acid as pre-distillation reagents for primary distillation, performing secondary distillation according to a determination method of total cyanide, and adding silver nitrate as a masking agent to remove sulfide, wherein determined cyanogen is easy-to-release cyanogen in the sample; performing determination with a silver nitrate titration method when the content of cyanide in the sample is larger than 100 mg / kg, and performing determination with isonicotinic acid-pyrazolone spectrophotometry when the content of cyanide in the sample is smaller than 100 mg / kg. The content of the easy-to-release cyanide in the sulfide-containing based cyanide-containing solid waste can be determined accurately, and sulfide interference is removed by adopting ethanol as the dispersing agent and combining the masking agent by means of two-time distillation.

Description

technical field [0001] The invention belongs to the technical field of measuring easily-released cyanide in solid waste, and in particular relates to a method for measuring easily-released cyanide in sulfide-containing cyanide-containing solid waste. Background technique [0002] In the new environmental protection law, cyanide-containing solid waste is listed as a hazardous waste list. Cyanide is a highly toxic substance, and its accurate detection is very important. For example, in the gold production process, the cyanide gold leaching process is one of the very important means. The solid waste produced by the cyanidation gold leaching process contains cyanide, and most of them also contain relatively high sulfide. When the cyanide-containing solid waste containing sulfide is easy to release cyanide, the sulfide ion will enter the absorption liquid during distillation. Affect the measurement results. For example, when the cyanide content in cyanide-containing solid waste i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16G01N21/31
CPCG01N21/31G01N31/16
Inventor 葛仲义陈永红张灵芝王菊孟宪伟芦新根
Owner CHANGCHUN GOLD RES INST