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Method for determining chloride ion content in polyhalite

A technology for chloride ion content and determination method, which is applied in the field of photometric determination of chloride ion content in polyhalite, can solve problems such as large analysis errors and expensive ion chromatography, and achieve high precision, stable results, and wide applicability Effect

Inactive Publication Date: 2015-07-29
BLUESTAR LEHIGH ENG INST CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

As we all know, titration is generally used for the determination of higher levels of ions. For the content of chloride ions below 1%, the determination by titration will inevitably cause large analysis errors; ion chromatography is suitable for lower levels of chloride ions, and ions Chromatography is expensive

Method used

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  • Method for determining chloride ion content in polyhalite
  • Method for determining chloride ion content in polyhalite

Examples

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Embodiment 1

[0018] Embodiment 1, the determination method of chloride ion content in a kind of polyhalite: dissolve polyhalite sample with acid, in acid medium, chloride ion reacts with mercury thiocyanate, thiocyanate ion is replaced, and add The iron III ion in the iron salt of the solution forms a red complex, and the absorbance of the complex in the test solution is measured at 460nm of the spectrophotometer, thereby calculating the content of chloride ion in the polyhalite.

Embodiment 2

[0019] Embodiment 2, a kind of assay method of chloride ion content in polyhalite, its concrete steps are as follows:

[0020] (1) Weigh 0.2g polyhalite sample, accurate to 0.0001g, put it in a 250mL beaker, add 5mL of nitric acid solution, heat and boil to dissolve, and keep for 3min; the nitric acid solution is AR grade, and the nitric acid solution is in a volume ratio of 1: 1 of concentrated nitric acid mixed with water;

[0021] (2) Remove it after cooling, transfer it into a 250mL volumetric flask, release it with water to the mark, and shake well;

[0022] (3) Dispense 5mL of the test solution into a 10mL colorimetric tube with a stopper, add a small amount of water, add 2mL of ferric ammonium sulfate solution, and mix well; add 1mL of mercury thiocyanate-ethanol solution, mix well; leave it at room temperature for 10min; The mass concentration of the described ferric ammonium sulfate solution is 60g / L; the mass concentration of the described mercury thiocyanate-ethano...

Embodiment 3

[0025] Embodiment 3, a kind of assay method of chloride ion content in polyhalite, its concrete steps are as follows:

[0026] (1) Weigh 0.5g of polyhalite sample, accurate to 0.0001g, put it in a 250mL beaker, add 20mL of nitric acid solution, heat and boil to dissolve, and keep for 3-5min; the nitric acid solution is AR grade, and the nitric acid solution is divided by volume. 1:4 concentrated nitric acid mixed with water;

[0027] (2) Remove it after cooling, transfer it into a 250mL volumetric flask, release it with water to the mark, and shake well;

[0028] (3) Dispense 10 mL of the test solution into a 50 mL colorimetric tube with a stopper, add a small amount of water, add 2 mL of ferric ammonium sulfate solution, and mix well; add 1 mL of mercury thiocyanate-ethanol solution, and mix well; leave at room temperature for 30 minutes; The mass concentration of the described ferric ammonium sulfate solution is 60g / L; the mass concentration of the described mercury thiocya...

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Abstract

The invention discloses an analysis method for chloride ion content in polyhalite. The method comprises the following steps: dissolving a polyhalite test sample with acid; reacting chloride ions with mercuric thiocyanate in an acid medium to displace thiocyanate ions out; generating a red complex with iron III ions in ferric salt added into a solution; measuring the light absorption value of the complex in a test solution at the 460-nanometer position of a spectrophotometer in order to calculate the content of chloride ions in the polyhalite. For the content determination of chloride ions less than 1 percent in the polyhalite, the method is simple, convenient, reasonable, rapid and accurate; moreover, results are stable, and the precision is high.

Description

technical field [0001] The invention relates to a content determination method, in particular to a method for photometric determination of chloride ion content in polyhalite. Background technique [0002] Polyhalite is a common potassium magnesium sulfate mineral with a chemical composition of K 2 SO 4 , M 2 SO 4 , 2CaSO 4 ·2H 2 O. It is a low-potassium mineral, often associated with gypsum, and is less soluble than other potassium-magnesium salt minerals. [0003] Because polyhalite is a potassium-magnesium sulfate mineral, the chloride ion content is low, basically below 1%. There is no determination of chloride ion content in polyhalite in the existing method standards, and the determination methods of relevant chloride ions include silver nitrate titration, mercury thiocyanate back titration, ion chromatography and the like. As we all know, the titration method is generally used for the determination of ions with relatively high content. For the content of chlori...

Claims

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Application Information

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IPC IPC(8): G01N21/31
Inventor 张晓梅陈奕徐会会
Owner BLUESTAR LEHIGH ENG INST CO LTD
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