阅读说明：本技术 锑母粒化学分析方法 (Chemical analysis method for antimony master batch ) 是由 覃事敦 胡邵平 于 2019-10-28 设计创作，主要内容包括：本发明属于化学分析技术领域,具体公开了锑母粒化学分析方法,步骤如下：选取试剂：硫酸钾、硫酸(P1.848/ml)、盐酸(p+1)、甲基橙指示剂(1g/L)、硫酸铈标准滴定溶液(Ce(So<Sub>4</Sub>)2约0.1mol/L),配制：称取40.50g硫酸铈[Ce(So<Sub>4</Sub>)2.4H<Sub>2</Sub>O]置于1000ml烧杯中,加入30ml硫酸搅拌均匀,在电炉上逐渐升温加热溶成糊状,并冒硫酸白烟约20min,取下冷却,加入硫酸(1+160ml),再缓缓加入水600ml,搅拌溶解,冷却后移入1000ml容量瓶中,用水稀释至1000ml摇匀；与现有技术相比,本发明试料用硫酸-硫酸钾分解,在盐酸介质中,以甲基橙作指示剂,在80摄氏度-90摄氏度用硫酸铈标准滴定溶液滴定至溶液红色消失为终点,操作方便,分析率高,试验的平均误差小。(The invention belongs to the technical field of chemical analysis, and particularly discloses a chemical analysis method of antimony master batch, which comprises the following steps: selecting a reagent: potassium sulfate, sulfuric acid (P1.848/ml), hydrochloric acid (P +1), methyl orange indicator (1g/L), cerium sulfate standard titration solution (Ce (So) 4 )2 about 0.1mol/L), preparing: 40.50g of cerium sulfate [ Ce (So) was weighed 4 )2.4H 2 O]Placing in 1000ml beaker, adding 30ml sulfuric acid, stirring well, heating gradually on electric furnace to dissolve into paste, and exhausting sulfuric acid white smoke for about 20min, taking down and cooling, adding sulfuric acid (1+160ml), slowly adding water 600ml, stirring to dissolve, cooling, transferring into 1000ml volumetric flask, diluting with water to 1000ml, shaking well; compared with the prior art, the sample is decomposed by sulfuric acid-potassium sulfate, methyl orange is used as an indicator in a hydrochloric acid medium, and a cerium sulfate standard titration solution is used for titration at 80-90 ℃ until the red color of the solution disappears, so that the method is convenient to operate, high in analysis rate and small in average error of the test.)

1. The antimony master batch chemical analysis method is characterized by comprising the following steps: the method comprises the following steps:

firstly, selecting a reagent:

(1) a potassium sulfate, a potassium salt,

(2) sulfuric acid (P1.848/ml),

(3) hydrochloric acid (p +1) is added,

(4) methyl orange indicator (1g/L),

(5) cerium sulfate Standard titration solution (Ce (So)₄)2 about 0.1 mol/L);

secondly, calibrating the solution:

(1) preparation: 40.50g of cerium sulfate [ Ce (So) was weighed₄)2.4H₂O]Placing in 1000ml beaker, adding 30ml sulfuric acid, stirring well, heating gradually on electric furnace to dissolve into paste, and exhausting sulfuric acid white smoke for about 20min, taking down and cooling, adding sulfuric acid (1+160ml), slowly adding water 600ml, stirring to dissolve, cooling, transferring into 1000ml volumetric flask, diluting with water to 1000ml, shaking well;

(2) calibration: weighing 0.25g of three parts of purified antimony (sb > -99.99%), respectively placing in a 300ml flask, adding a small amount of water for wetting, adding 15ml of sulfuric acid for heating and dissolving, clearing, taking down and cooling, adding 40ml of water, and adding 30ml of hydrochloric acid p +1 solution;

thirdly, carrying out blank test along with calibration:

calculating the actual concentration of the cerium sulfate standard brick titration solution according to the formula (1):

in the formula:

p is the actual concentration of the standard titration solution of cerium sulfate, and the unit is mol per liter;

m-amount of metallic antimony in grams;

V₁titrating the volume of the cerium sulfate standard solution consumed by antimony in milliliters;

V₀calibrating the volume of the hollow solution consumed cerium sulfate standard solution, wherein the volume is milliliter;

121.76-molar amount of antimony in grams per mole;

taking the average value of the three calibration results as the actual concentration of the cerium sulfate standard solution, and calibrating the consumed cerium sulfate standard solution in parallel to ensure that the range of the volume of the consumed cerium sulfate standard solution is not more than 0.10 ml;

fourth, sample:

sample shears or fines;

fifthly, analyzing:

(1) test material

Weighing 0.2-0.3g sample to 0.0001g

(2) Number of measurements

Performing two measurements, and averaging

(3) Blank test

Blank test with the sample

(4) Measurement of

(4.1) placing 0.2g-0.3g of a sample into a 300ml conical flask, adding 2g of potassium sulfate, wetting the sample with water, adding 15ml of sulfuric acid, placing on an electric furnace, heating to evaporate water, covering a watch glass, keeping the solution at a slightly boiling temperature, decoloring the dark red color of the solution for hours, taking down and cooling;

(4.2) adding 40ml of water, shaking 30ml of hydrochloric acid uniformly, boiling, adding two drops of methyl orange indicator, and dropping a cerium sulfate standard solution to the red color of the solution for exactly one hour at the temperature of 80-90 ℃;

sixthly, calculating an analysis result:

the mass fraction wsb of antimony was calculated according to equation (2), and the value is expressed in%

In the formula:

c is the actual concentration of the cerium sulfate standard solution, and the unit is mol per liter;

V₂-the volume of cerium sulfate consumed by the standard solution in milliliters;

V₃-the volume of blank spent cerium sulfate standard solution in milliliters;

121.76 molar mass of antimony, in grams per mole, the results obtained should be expressed to the second decimal place.

Technical Field

The invention belongs to the technical field of chemical analysis, and particularly relates to a chemical analysis method of antimony master batch.

Background

Antimony, metal element, element symbol Sb, atomic number 51, it is a kind of metal with metallic luster, mainly exist in sulfide mineral stibnite (Sb2S3) in nature, antimony compound is known to be used as cosmetics in ancient times, metallic antimony is also recorded in ancient times, but at that time is mistaken for lead, at about 17 times, it is known that antimony is a chemical element, silver white, glossy, hard and brittle metals (usually made into various shapes such as rod, block and powder), has a flaky crystal structure, gradually loses luster in humid air, burns into white antimony oxide under strong heat, is easy to dissolve in aqua regia, concentrated sulfuric acid, relative density 6.68, melting point 630 ℃, boiling point 1635 ℃, and atomic radius is 51

Electronegativity 2.2.

The existing chemical detection method for the antimony master batch is single, has large error, reduces the detection efficiency of a chemical test, partially stipulates a measurement adaptation method for the amount of antimony in crude antimony oxide of YS/T556, and is suitable for measuring the antimony in the antimony master batch, and the measurement range is 1.0-70%.

Disclosure of Invention

The invention aims to provide a chemical analysis method of antimony master batch, which aims to solve the problems in the background technology.

In order to achieve the purpose, the invention adopts the following technical scheme: the chemical analysis method of the antimony master batch is characterized by comprising the following steps: the method comprises the following steps:

firstly, selecting a reagent:

(1) a potassium sulfate, a potassium salt,

(2) sulfuric acid (P1.848/ml),

(3) hydrochloric acid (p +1) is added,

(4) methyl orange indicator (1g/L),

(5) cerium sulfate Standard titration solution (Ce (So)₄)2 about 0.1 mol/L);

secondly, calibrating the solution:

(1) preparation: 40.50g of cerium sulfate [ Ce (So) was weighed₄)2. 4H₂O]Placing in 1000ml beaker, adding 30ml sulfuric acid, stirring well, heating gradually on electric furnace to dissolve into paste, and exhausting sulfuric acid white smoke for about 20min, taking down and cooling, adding sulfuric acid (1+160ml), slowly adding water 600ml, stirring to dissolve, cooling, transferring into 1000ml volumetric flask, diluting with water to 1000ml, shaking well;

(2) calibration: weighing 0.25g of three parts of purified antimony (sb > -99.99%), respectively placing in a 300ml flask, adding a small amount of water for wetting, adding 15ml of sulfuric acid for heating and dissolving, clearing, taking down and cooling, adding 40ml of water, and adding 30ml of hydrochloric acid p +1 solution;

thirdly, carrying out blank test along with calibration:

calculating the actual concentration of the cerium sulfate standard brick titration solution according to the formula (1):

in the formula:

p is the actual concentration of the standard titration solution of cerium sulfate, and the unit is mol per liter;

m-amount of metallic antimony in grams;

V₁titrating the volume of the cerium sulfate standard solution consumed by antimony in milliliters;

V₀calibrating the volume of the hollow solution consumed cerium sulfate standard solution, wherein the volume is milliliter;

121.76-molar amount of antimony in grams per mole;

taking the average value of the three calibration results as the actual concentration of the cerium sulfate standard solution, and calibrating the consumed cerium sulfate standard solution in parallel to ensure that the range of the volume of the consumed cerium sulfate standard solution is not more than 0.10 ml;

fourth, sample:

sample shears or fines;

fourthly, analyzing:

(1) test material

Weighing 0.2-0.3g sample to 0.0001g

(2) Number of measurements

Performing two measurements, and averaging

(3) Blank test

Blank test with the sample

(4) Measurement of

(4.1) placing 0.2g-0.3g of a sample into a 300ml conical flask, adding 2g of potassium sulfate, wetting the sample with water, adding 15ml of sulfuric acid, placing on an electric furnace, heating to evaporate water, covering a watch glass, keeping the solution at a slightly boiling temperature, decoloring the dark red color of the solution for hours, taking down and cooling;

(4.2) adding 40ml of water, shaking 30ml of hydrochloric acid uniformly, boiling, adding two drops of methyl orange indicator, and dropping a cerium sulfate standard solution to the red color of the solution for exactly one hour at the temperature of 80-90 ℃;

sixthly, calculating an analysis result:

the mass fraction wsb of antimony was calculated according to equation (2), and the value is expressed in%

In the formula:

c is the actual concentration of the cerium sulfate standard solution, and the unit is mol per liter;

V₂-the volume of cerium sulfate consumed by the standard solution in milliliters;

V₃-the volume of blank spent cerium sulfate standard solution in milliliters;

121.76 molar mass of antimony, in grams per mole, the results obtained should be expressed to the second decimal place.

The invention has the technical effects and advantages that: compared with the prior art, the antimony master batch chemical analysis method provided by the invention has the advantages that a sample is decomposed by sulfuric acid-potassium sulfate, methyl orange is used as an indicator in a hydrochloric acid medium, and a cerium sulfate standard titration solution is used for titration at 80-90 ℃ until the red color of the solution disappears as an end point, so that the operation is convenient, the analysis rate is high, and the average error of the test is small.

Detailed Description

The technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. The specific embodiments described herein are merely illustrative of the invention and do not delimit the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.