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Method for detecting content of heavy metals in activated carbon

A heavy metal and activated carbon technology, which is applied in material analysis by observing the influence of chemical indicators, and analysis by chemical reaction of materials, etc., can solve the problems of endangering the quality of API products, interfering with final colorimetry, and high content of heavy metals.

Active Publication Date: 2018-02-09
NORTHEAST PHARMA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

The high content of heavy metals will lead to the introduction of exogenous heavy metals into the raw materials to be decolorized, which will directly endanger the product quality of the raw materials
The inspection methods reported in the literature at present either do not mask the high-valent iron ions in the sample solution, or add the reducing agent VC for masking. The former interferes with the final colorimetry, and the latter VC is very easy to change color in acidic or alkaline solutions, which also leads to Interfering with the final colorimetry, it is difficult to draw objective and accurate detection conclusions

Method used

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  • Method for detecting content of heavy metals in activated carbon
  • Method for detecting content of heavy metals in activated carbon

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Taking the heavy metal index of activated carbon not greater than 30ppm as an example, the determination of heavy metal content in activated carbon samples is illustrated:

[0023] 1) Preparation of the test solution

[0024] Take 1.0g of activated carbon, add 20ml of 3mol / L hydrochloric acid and 5ml of bromine test solution, boil for 5 minutes, filter, wash the filter residue with 50ml of boiling water, combine the filtrate and washing solution, and evaporate to near dryness. Then add 1ml of 1mol / L hydrochloric acid, 20ml of water, 5ml of sulfurous acid, and boil the solution until all SO is removed. 2 . Dilute to 50ml with water. Take 20ml of the above solution, put it in a 50ml colorimetric tube, add water to make 25ml, use a pH meter or short-range pH test paper as an external indicator, adjust the pH to 3.0-4.0 with 1mol / L acetic acid, and dilute to 40ml with water.

[0025] 2) Preparation of standard solution

[0026] Take 1.2ml of 10ppm lead standard solution...

Embodiment 2

[0043] Establishment of methodology

[0044] 1 Choice of different color eliminators

[0045] 1.1 Using VC as masking agent

[0046] Take 1.0g of activated carbon, add 10ml of dilute hydrochloric acid and 5ml of bromine test solution, boil for 5min, filter, wash the filter residue with 35ml of boiling water, combine the filtrate and lotion, add an appropriate amount of water to make 50ml, shake well, take 20ml of the test solution In a 50ml colorimetric tube, add 1 drop of phenolphthalein indicator solution. And add ammonia test solution dropwise until the solution is light red, add 2ml of pH3.5 acetate buffer solution and appropriate amount of water to make 25ml, add 0.5g of vitamin C to dissolve.

[0047] Standard solution: Take 1.2ml of 10ppm lead standard solution, put it in a 50ml colorimetric tube, add 2ml of pH3.5 acetate buffer, add water to dilute to 25ml, add 0.5g of vitamin C to dissolve.

[0048] Monitoring solution: Take 20ml of the test solution and place it i...

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Abstract

The invention belongs to the field of pharmaceutical excipient analysis and relates to a method for detecting the content of heavy metals in activated carbon. The method comprises (1) sample solutionpreparation: adding a sulfite solution into a sample solution, (2) standard solution preparation, (3) monitoring solution preparation, (4) preparation of a thioacetamide-glycerine alkali solution, and(5) determination: respectively adding an acetate buffer solution into the sample solution, the standard solution and the monitoring solution, adding the thioacetamide-glycerine alkali solution intothe mixed solution, diluting the mixed solution with water, carrying out uniform mixing, standing the mixed solution for some time, putting the mixed solution on the white background and carrying outperspective observation from top to bottom, wherein the color of the sample solution is not deeper than that of the standard solution and the color of the standard solution is not deeper than that ofthe monitoring solution. The method can eliminate the color interference of high-valent iron ions and ensure the objective and accurate detection results.

Description

technical field [0001] The invention belongs to the field of pharmaceutical auxiliary material analysis, and in particular relates to a method for detecting heavy metal content in activated carbon. technical background [0002] Activated carbon is an excipient used for decolorization in the production of raw materials. Heavy metal content is an important quality indicator that must be controlled. The high content of heavy metals will lead to the introduction of exogenous heavy metals into the raw materials to be decolorized, which will directly endanger the product quality of the raw materials. The inspection methods reported in the literature at present either do not mask the high-valent iron ions in the sample solution, or add the reducing agent VC to mask. The former interferes with the final colorimetry, and the latter VC is very easy to change color in acidic or alkaline solutions, which also leads to Interfering with the final colorimetry, it is difficult to draw obj...

Claims

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Application Information

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IPC IPC(8): G01N21/78G01N21/82
CPCG01N21/78G01N21/82
Inventor 刘晨芳邵冬梅冯文宇周秀峰任赫陈赟周岩赵明佟雪娄玉涛唐奎山谢丹
Owner NORTHEAST PHARMA GRP
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