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Method for detecting content of antimony in liquid product

A detection method, liquid technology, applied in the field of chemical analysis, can solve the problems of high cost and complicated operation, and achieve the effect of high selectivity and wide application range

Active Publication Date: 2014-08-06
金浦新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods require relatively complex pre-sample processing and must be equipped with necessary instruments, which have problems such as complex operation and high cost.

Method used

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  • Method for detecting content of antimony in liquid product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042]A. Accurately weigh 0.65g (± 0.0001g) samples of antimony-containing metal passivators (used in catalytic cracking units, antimony is +5, numbered 1#) and place them in three 250ml cones bottle (take two 250ml Erlenmeyer flasks for blank test at the same time), add 20ml 98% sulfuric acid each time to dissolve the sample, control the appropriate temperature (110-115°C), add 3 drops (about 1 g ) 98% nitric acid, shake well for digestion and oxidation, cool to 40°C, add (1.5±0.1) g of urea, shake well, heat until no white smoke is produced, cool to below 40°C, add (0.5±0.1) g of masking agent thiourea , Rinse the wall of the bottle with (10±1)mL of 98% sulfuric acid, shake well and heat until no small bubbles are generated, cool to below 40°C and slowly add (100±1)ml of deionized water and shake slowly, then add (20 ±1)ml 37% hydrochloric acid, shake well, boil and keep boiling slightly for 2-3min, cool to 65-75℃ for test;

[0043] B. Determination of antimony content in s...

Embodiment 2

[0046] A. Accurately weigh 0.75g (± 0.0001g) sample of 4% ethylene glycol antimony ethylene glycol solution (for polyester preparation equipment, antimony is +3 valence, number 2#) mixed uniformly in three In one 250ml conical flask (take two 250ml conical flasks for blank test at the same time), add 20ml of 98% sulfuric acid each time to dissolve the sample, control the appropriate temperature (110-115°C), add 3 drops with a dropper while it is hot (about 1 gram) 98% nitric acid, shake well for digestion and oxidation, cool to 40°C, add (1.5±0.1) g of urea, shake well, heat until no white smoke is produced, cool to below 40°C, add (0.5±0.1) g of urea For the masking agent thiourea, wash the bottle wall with (10±1)mL of 98% sulfuric acid, shake well and heat until no small bubbles are generated, cool to below 40°C, slowly add deionized water (100±1)ml and shake slowly, Then add (20±1)ml 37% hydrochloric acid, shake well, boil and keep boiling slightly for 2-3min, cool to 65-75...

Embodiment 3

[0050] A. Accurately weigh 0.95g (±0.0001g) samples of fireproof coating (containing antimony white powder, antimony is +5, number 3#) and place them in three 250ml conical flasks (take three at the same time) 250ml Erlenmeyer flask for blank test), add 20ml 98% sulfuric acid each time to dissolve the sample, control the appropriate temperature (110-115°C), add 3 drops (about 1 gram) 98% nitric acid with a dropper while it is hot and shake well Digest and oxidize, cool to 40°C, add (1.5±0.1) g of urea, shake well, heat until no white smoke occurs, cool to below 40°C, add (0.5±0.1) g of masking agent thiourea, use (10±1) Rinse the wall of the bottle with 98% sulfuric acid in mL, shake well and heat until there are no small bubbles, cool to below 40°C, slowly add (100±1)ml of deionized water and shake well, then add (20±1)ml of 37% hydrochloric acid to shake Mix well, boil and keep boiling slightly for 2-3 minutes, cool to 65-75°C for testing;

[0051] B. Determination of antim...

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Abstract

The invention discloses a method for detecting the content of antimony in a liquid product. The method comprises the following steps in sequence: A, dissolving and preparing a liquid sample: dissolving the liquid sample by concentrated sulfuric acid, cooling to 35-45 DEG C, adding urea until no white smoke is generated, adding thiourea with the mass using amount which is 0.5-2 times of the mass of the liquid sample under a condition that the temperature is not higher than 40 DEG C, adding water with the adding amount which is 100-500 times of the mass of the liquid sample to realize dilution, adding 37% hydrochloric acid in mass to obtain a solution, boiling the solution, keeping micro-boiling for 2-3 minutes, and cooling to 65-75 DEG C to obtain a solution to be detected; B, detecting the content of the antimony in the liquid sample: dropwise adding 0.1% methyl orange indicating agent into the solution to be detected, keeping the temperature of the solution to be detected at 65-75 DEG C, and titrating the solution to be detected through standard potassium bromate solution until the pink color disappears. According to the detection method disclosed by the invention, no special analyzer is needed; the method is simple, quick, accurate, wide in application range and high in selectivity.

Description

technical field [0001] The invention relates to a method for detecting antimony content in liquid products, which belongs to the quantitative analysis method (volume method) of metal elements in the field of chemical analysis. Background technique [0002] Metal antimony is not a very active element. It only reacts with water to release hydrogen when it is red hot. It will not be oxidized by air at room temperature, but it can combine with fluorine, chlorine, and bromine; it can combine with iodine and other substances when heated. non-metal compound. Antimony is easily soluble in hot nitric acid to form hydrated antimony oxide, which can react with hot sulfuric acid to produce antimony sulfate. Antimony can react with oxygen at high temperature to form antimony trioxide, which is an amphoteric oxide, hardly soluble in water, but soluble in acid and alkali. Antimony is mostly used as a component of other alloys, which can increase its hardness and strength. For example, an...

Claims

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Application Information

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IPC IPC(8): G01N31/16
Inventor 王春柱沙玉英戴宁斌
Owner 金浦新材料股份有限公司
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