Method for detecting copper, iron and calcium in flash converting furnace slag

Abstract

The invention provides a method for detecting copper, iron and calcium in flash converting furnace slag. The method comprises the following steps: (A) dissolving a flash converting furnace slag test sample with acid to obtain a first solution containing copper ions, iron ions and calcium ions, performing reaction on the first solution, sodium sulfide and sodium hydroxide, and filtering to obtain precipitates and filtrate; (B) dissolving the obtained precipitates with acid to obtain a second solution containing bivalent copper ions and iron ions, masking iron with ammonium bifluoride in the second solution, detecting copper by adopting an iodometry method to obtain the copper content, releasing iron in the solution subjected to copper detection with aluminium trichloride, and detecting iron by adopting the iodometry method to obtain the iron content; (C) titrating the filtrate obtained in the step (A) with edetic acid, thus obtaining the calcium content. The procedures of the detection method provided by the invention are simple, one-step sample weighing is realized, and the contents of three key elements, copper, iron and calcium, in the flash converting furnace slag can be quickly, accurately and continuously measured.

Description

technical field

[0001] The invention relates to the technical field of copper slag detection, in particular to a method for detecting copper, iron and calcium in flash blowing slag. Background technique

[0002] Copper slag contains a large amount of available resources. The analysis and detection of copper, iron and other components in copper smelting slag is of great significance to the smelting process and resource reuse. At present, there are mainly methods for analyzing copper and iron in copper slag concentrate. The determination of copper includes the following two types: the determination of more than 10% copper in copper slag concentrate can use the short iodometric method. Ammonium solution is used to adjust the pH value of the solution to 3.0-4.0. Ammonium bifluoride is used to cover iron, and potassium iodide is added to react with divalent copper. The precipitated iodine is titrated with starch as an indicator and titrated with sodium thiosulfate standard titra...

Examples

Embodiment 1

[0077] Embodiment 1 precision experiment

[0078] (1) Determination of copper:

[0079] Take flash blowing furnace slag as the sample, weigh 0.4000g (m) of the sample and place it in a 250mL conical beaker, add a small amount of water to soak the sample, add 15mL of hydrochloric acid, heat at low temperature and boil for 3 to 5 minutes, cool slightly , then add 10mL of nitric acid and 5mL of sulfuric acid, continue heating until evaporated to dryness, and cool.

[0080]Add 40 mL of water into the above-mentioned conical beaker, heat slowly, and add sulfuric acid solution with a mass concentration of 50%, so that the pH value of the obtained first solution is 2-3. Slightly cool, slowly add 20mL100g / L sodium sulfide solution, slightly boil for 10min. Cool slightly, stir and slowly add dropwise a sodium hydroxide solution with a mass concentration of 20%, until the red precipitate in the solution no longer increases. Cool slightly, let stand for 5 minutes, filter, wash the pre...

Embodiment 2

[0093] Embodiment 2 Accuracy experiment

[0094] 1. Carry out the accuracy test on the flash converting slag samples, namely detect the copper, iron and calcium content in the 3 flash converting slag samples by the method in Example 1. The detection results are shown in Table 2, and Table 2 is the result of the accuracy experiment of the embodiment of the present invention.

[0095] 2. Determination of copper by existing methods: iodometric method

[0096] Weigh 0.3000g sample, place it in a 250mL conical beaker, moisten it with a small amount of water, add 5mL nitric acid and 15mL hydrochloric acid, cover the watch glass, heat at low temperature to dissolve completely, steam until nearly dry, remove and cool slightly. Add 50mL of water and 10mL of sulfuric acid, boil, and slowly add 25mL of 200g / L sodium thiosulfate solution dropwise with stirring until a large amount of precipitation occurs, and filter while hot. Wash the precipitate with hot water for more than 3 times to...

technical field

[0001] The invention relates to the technical field of copper slag detection, in particular to a method for detecting copper, iron and calcium in flash blowing slag. Background technique

[0002] Copper slag contains a large amount of available resources. The analysis and detection of copper, iron and other components in copper smelting slag is of great significance to the smelting process and resource reuse. At present, there are mainly methods for analyzing copper and iron in copper slag concentrate. The determination of copper includes the following two types: the determination of more than 10% copper in copper slag concentrate can use the short iodometric method. Ammonium solution is used to adjust the pH value of the solution to 3.0-4.0. Ammonium bifluoride is used to cover iron, and potassium iodide is added to react with divalent copper. The precipitated iodine is titrated with starch as an indicator and titrated with sodium thiosulfate standard titra...

Examples

Embodiment 1

[0077] Embodiment 1 precision experiment

[0078] (1) Determination of copper:

[0079] Take flash blowing furnace slag as the sample, weigh 0.4000g (m) of the sample and place it in a 250mL conical beaker, add a small amount of water to soak the sample, add 15mL of hydrochloric acid, heat at low temperature and boil for 3 to 5 minutes, cool slightly , then add 10mL of nitric acid and 5mL of sulfuric acid, continue heating until evaporated to dryness, and cool.

[0080]Add 40 mL of water into the above-mentioned conical beaker, heat slowly, and add sulfuric acid solution with a mass concentration of 50%, so that the pH value of the obtained first solution is 2-3. Slightly cool, slowly add 20mL100g / L sodium sulfide solution, slightly boil for 10min. Cool slightly, stir and slowly add dropwise a sodium hydroxide solution with a mass concentration of 20%, until the red precipitate in the solution no longer increases. Cool slightly, let stand for 5 minutes, filter, wash the pre...

Embodiment 2

[0093] Embodiment 2 Accuracy experiment

[0094] 1. Carry out the accuracy test on the flash converting slag samples, namely detect the copper, iron and calcium content in the 3 flash converting slag samples by the method in Example 1. The detection results are shown in Table 2, and Table 2 is the result of the accuracy experiment of the embodiment of the present invention.

[0095] 2. Determination of copper by existing methods: iodometric method

[0096] Weigh 0.3000g sample, place it in a 250mL conical beaker, moisten it with a small amount of water, add 5mL nitric acid and 15mL hydrochloric acid, cover the watch glass, heat at low temperature to dissolve completely, steam until nearly dry, remove and cool slightly. Add 50mL of water and 10mL of sulfuric acid, boil, and slowly add 25mL of 200g / L sodium thiosulfate solution dropwise with stirring until a large amount of precipitation occurs, and filter while hot. Wash the precipitate with hot water for more than 3 times to...

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