阅读说明：本技术 一种测定尾矿样品中低含量锑的方法 (Method for determining low-content antimony in tailing sample ) 是由 贺仕军 张新念 刘洋 石文莹 于 2019-11-21 设计创作，主要内容包括：一种测定尾矿样品中低含量锑的方法,包括以下步骤,1)配置并且标定硫酸铈标准溶液；2)样品准备：将尾矿样品溶于硫酸和盐酸的混合溶液中；3)滴定：将步骤<Image he="17" wi="17" file="968805DEST_PATH_IMAGE001.GIF" imgContent="drawing" imgFormat="GIF" orientation="portrait" inline="no"></Image>的溶液继续加热至80-90℃,立即加入0.2%的甲基橙-亚甲基蓝溶液,在不断振荡下,用硫酸铈标准溶液滴定,临近终点时,再将溶液加热至80—90℃,继续滴定至绿色出现为终点。本发明是基于硫酸铈容量法进行的改进,与传统的硫酸铈容量法使用的试剂一致,不需专门购买试剂；也没有使用有毒的有毒试剂；本发明法分析速度快；方法精密度和准确度较高；易被操作人员掌握、不需对操作人员进行另外的培训；对尾矿样品中含量为0.05-0.50%锑的分析均可获得满意的结果。(A method for measuring low-content antimony in a tailing sample comprises the following steps of 1) preparing and calibrating a cerium sulfate standard solution; 2) sample preparation: dissolving a tailing sample in a mixed solution of sulfuric acid and hydrochloric acid; 3) titration: will be described in detail The solution is continuously heated to 80-90 ℃, 0.2 percent methyl orange-methylene blue solution is immediately added, under the condition of continuous oscillation, the solution is titrated by cerous sulfate standard solution, when the end point is approached, the solution is heated to 80-90 ℃, and the titration is continuously carried out until green appears as the end point. The invention is an improvement based on the volumetric method of cerium sulfate, is consistent with the reagent used by the traditional volumetric method of cerium sulfate, and does not need to purchase the reagent specially; no toxic or noxious reagents are used; the method has high analysis speed; the method has high precision and accuracy; the device is easy to master by operators and does not need to carry out additional training on the operators; satisfactory knots can be obtained by analyzing the content of 0.05-0.50% of antimony in the tailing sampleAnd (5) fruit.)

1. A method for determining low-content antimony in a tailing sample is characterized by comprising the following steps: comprises the following steps of (a) carrying out,

1) preparing and calibrating a cerium sulfate standard solution;

2) sample preparation:

adding qualitative filter paper when sulfuric acid smoke begins to emerge from the container, continuing heating until the black carbonized by the filter paper disappears, transferring the container onto a high-temperature furnace, rapidly heating under continuous oscillation to make sulfuric acid white smoke emerge for 3-10 seconds, and taking down;

3) titration: will be described in detail

the percentage of antimony was calculated as follows:

V×T

Sb（%）= ———— ×100

M

in the formula: t is the titer of the cerium sulfate standard solution to antimony, g/ml;

v is the volume of cerium sulfate standard solution consumed in the dripping process, and ml;

m-weight sample, g.

2. The method for determining low content of antimony in tailings samples according to claim 1, wherein the method comprises the following steps: the step 1) of preparing the cerium sulfate standard solution comprises the following steps:

3. The method for determining low content of antimony in tailings samples according to claim 1, wherein the method comprises the following steps: the step 1) of preparing the cerium sulfate standard solution comprises the following steps: 1500ml of the prepared cerium sulfate standard solution with the concentration of 0.003g/ml in antimony measured by the traditional cerium sulfate volumetric method is measured, diluted to about 4500ml by 8 percent sulfuric acid solution and fully shaken up.

4. The method for determining low content of antimony in tailings samples according to claim 1, wherein the method comprises the following steps: step 1) calibrating a cerium sulfate standard solution comprises the following steps:

adding qualitative filter paper when sulfuric acid smoke begins to emerge from the container, continuing heating until the black carbonized by the filter paper disappears, transferring the container onto a high-temperature furnace, rapidly heating under continuous oscillation to make sulfuric acid white smoke emerge for 3-10 seconds, and taking down;

3) calibration: will be described in detail

the titer of the cerium sulfate standard solution to antimony was calculated as follows:

T=c*m/v

in the formula: t-titer of cerium sulfate standard solution to antimony (g/ml)

c-Standard results of control (%)

m-weight of the sample to be weighed (gram)

v-volume of cerium sulfate standard solution consumed (ml).

Technical Field

The invention relates to a method for measuring antimony content, in particular to a method for measuring low-content antimony in a tailing sample.

Background

At present, most of antimony in tailings is analyzed by a traditional cerium sulfate volumetric method (S/T556-2009 antimony concentrate chemical analysis method), but the lower limit of detection of the method is 0.10%, the content of antimony in the tailings is reduced to about 0.06% with the continuous improvement of a beneficiation technology, and the traditional analysis method cannot play a role in guidance of beneficiation production and can not truly reflect the recovery rate of beneficiation.

In order to improve the determination of low-content antimony, the content of antimony in tailings is determined by a potassium iodide colorimetric method (Chenzheng e, Pengqin; determination of antimony content by potassium iodide colorimetric method, JW-17 (quality) 1-2010, enterprise standard of mineral company Limited in Hunan Chengzhou) or a 5-Br-PADAP photometric method (Chenzheng e, Penqin; determination of antimony content by potassium iodide colorimetric method, JW-17 (quality) 1-2010, enterprise standard of mineral company Limited in Hunan Chen). The benzene which is a toxic organic solvent is required to be used for extraction when the photometry is used for determination, the analysis flow is long, and special operators, analysis fields and analysis equipment are required.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provide a method for detecting low-content antimony in a tailing sample, which can detect the low-content antimony in the tailing, and the method has low requirements on personnel and analysis sites.

In order to solve the technical problems, the technical scheme provided by the invention is as follows: a method for determining low-content antimony in a tailing sample comprises the following steps,

1) preparing and calibrating a cerium sulfate standard solution;

2) sample preparation:

putting 1 weight part of antimony-containing tailing sample into a container, and adding 1-2 weight parts of anhydrous potassium sulfate and sulfuric acid, wherein the amount of the sulfuric acid is 15-18ml per 1 gram of tailing sample; heating the container to remove water;

when sulfuric acid smoke begins to be emitted from the container, adding qualitative filter paper, continuing heating until the black color of the filter paper carbonization disappears, and transferring the container onto a high-temperature furnaceRapidly heating under continuous oscillation to make the sulfuric acid white smoke emit for 3-10 seconds, and taking down;

adding 30-50 parts by weight of pure water, heating to slightly boil, taking down, adding the phosphoric acid solution and the 1+1 hydrochloric acid solution, and shaking up, wherein each part by weight of the tailing sample corresponds to 20-40ml of the 1+1 hydrochloric acid solution and 4-6ml of the phosphoric acid solution;

3) titration: will be described in detail

Continuously heating the solution to 80-90 ℃, immediately adding 0.2% methyl orange-methylene blue solution, titrating with cerium sulfate standard solution under continuous oscillation, heating the solution to 80-900 ℃ when the end point is approached, and continuously titrating until green appears as the end point;

the percentage of antimony was calculated as follows:

V×T

Sb（%）= ———— ×100

M

in the formula: t is the titer of the cerium sulfate standard solution to antimony, g/ml;

v is the volume of cerium sulfate standard solution consumed in the dripping process, and ml;

m-weight sample, g.

In the above method for determining low content of antimony in a tailing sample, preferably, the step 1) of preparing the cerium sulfate standard solution comprises the following steps:weighing 35 g of ceric sulfate in a 1000ml beaker, adding 200ml of sulfuric acid, placing on an electric heating plate for heating, continuously stirring by using a glass rod, gradually heating on the electric heating plate, dissolving into paste, emitting sulfuric acid white smoke for about 20 minutes, and taking down for cooling slightly;

adding 200ml of pre-prepared 1+1 sulfuric acid, and stirring to dissolveRelieving to clear and cool;

transferring into 5000ml reagent bottle containing 2000ml water, washing beaker with 1+1 sulfuric acid 200ml, transferring into 5000ml reagent bottle, adding 2400ml water into 5000ml reagent bottle, shaking thoroughly, and standing for more than 1 month.

In the above method for determining low content of antimony in a tailing sample, preferably, the step 1) of preparing the cerium sulfate standard solution comprises the following steps: 1500ml of the prepared cerium sulfate standard solution with the concentration of 0.003g/ml in antimony measured by the traditional cerium sulfate volumetric method is measured, diluted to about 4500ml by 8 percent sulfuric acid solution and fully shaken up.

In the above method for determining low content of antimony in a tailing sample, preferably, the step 1) of calibrating the cerium sulfate standard solution comprises the following steps:

putting 1 weight part of low-grade antimony management sample into a container, and adding 1-2 weight parts of anhydrous potassium sulfate and sulfuric acid, wherein the amount of the sulfuric acid is 15-18ml per 1g of tailing sample; heating the container to remove water;

adding qualitative filter paper when sulfuric acid smoke begins to emerge from the container, continuing heating until the black carbonized by the filter paper disappears, transferring the container onto a high-temperature furnace, rapidly heating under continuous oscillation to make sulfuric acid white smoke emerge for 3-10 seconds, and taking down;

adding 30-50 parts by weight of pure water, heating to slightly boil, taking down, adding the phosphoric acid solution and the 1+1 hydrochloric acid solution, and shaking up, wherein each part by weight of the tailing sample corresponds to 20-40ml of the 1+1 hydrochloric acid solution and 4-6ml of the phosphoric acid solution;

3) calibration: will be described in detail

Continuously heating the solution to 80-90 ℃, immediately adding 0.2% methyl orange-methylene blue solution, titrating with cerium sulfate standard solution under continuous oscillation, heating the solution to 80-900 ℃ when the end point is approached, and continuously titrating until green appears as the end point;

the titer of the cerium sulfate standard solution to antimony was calculated as follows:

T=c*m/v

in the formula: t-titer of cerium sulfate standard solution to antimony (g/ml)

c-Standard results of control (%)

m-weight of the sample to be weighed (gram)

v-volume of cerium sulfate standard solution consumed (ml).

Compared with the prior art, the invention has the advantages that: the method is improved based on the cerium sulfate volumetric method, does not need to add extra workers, is consistent with the reagent used by the traditional cerium sulfate volumetric method, and does not need to specially purchase the reagent; no toxic or noxious reagents are used; the method has high analysis speed (the analysis time is only 2 hours); the method has high precision and accuracy; the device is easy to master by operators and does not need to carry out additional training on the operators; satisfactory results can be obtained by analyzing the content of 0.05-0.50% of antimony in the tailing sample. Therefore, the method has good popularization and application values.

Detailed Description

In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments described below.

It should be particularly noted that when an element is referred to as being "fixed to, connected to or communicated with" another element, it can be directly fixed to, connected to or communicated with the other element or indirectly fixed to, connected to or communicated with the other element through other intermediate connecting components.

Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.