CN105445268B - Analysis method for determining tellurium in high-selenium tellurium slag - Google Patents
Analysis method for determining tellurium in high-selenium tellurium slag Download PDFInfo
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Abstract
The invention provides an analysis method for determining tellurium in high-selenium tellurium slag, which adopts nitric acid and sulfuric acid to dissolve a sample, the sulfuric acid smokes to volatilize selenium in a bromide form for removal, hydrogen chloride in a hydrochloric acid medium of more than 10 mol/L is used for quantitatively reducing high-valence tellurium (VI) into low-valence tellurium (IV), silver sulfate is used for removing the interference of chloride ions in a form of silver chloride precipitation, potassium permanganate is used for quantitatively oxidizing the low-valence tellurium (IV) into high-valence tellurium (VI), and excessive potassium permanganate is reduced by ferrous sulfate, so that the content of tellurium in the sample is indirectly measured.
Description
Technical field
The invention belongs to chemical analysis fields, and in particular to a kind of analysis method for measuring tellurium in high selen-tellurjum slag.
Background technique
Tellurium belongs to dilute scattered nonmetalloid, and the existing associated minerals of tellurium have independent mineral deposit again in nature.It is mainly used for stone
The catalyst of oily cracking, the coloured material of the brightener of electroplate liquid, glass, is added in steel to increase its ductility, is added to
Increase its intensity and corrosion resistance in lead.Tellurium and its compound are a kind of semiconductor material again.It is right by consulting literatures data
The method of tellurium de-termination is more in tellurium dioxide product, or even has relevant national standard, for smelting intermediate product tellurium
The pertinent literature of the chemical analysis method of tellurium is less in slag, tellurium de-termination method especially in the tellurium slag containing high selenium, copper and silver
Almost without；The analysis method of tellurium has atomic absorption spectrophotometry, plasma emission spectrometry, potassium bichromate titrimetric method at present
Deng.
Smelting intermediate product tellurium slag mostlys come from Copper making process, wherein mainly containing the general content of tellurium is a few percent
To tens percent, the general content of selenium is a few percent to more than ten percent, and the general content of copper is a few percent, and silver content is general
For a few percent；Due to containing impurity element selenium in general tellurium slag simultaneously, and it is close with the chemical property of tellurium, therefore leads to tellurium
The content of tellurium is difficult to Accurate Determining in slag；Traditional is taken a long time using the method for potassium dichromate oxidation, it is difficult to quickly be obtained
Result is analyzed to instruct industrial production.
Summary of the invention
In order to solve the above-mentioned problems in the prior art, the present invention provides a kind of points for measuring tellurium in high selen-tellurjum slag
Analysis method.
The technical solution adopted by the present invention is that: sample is dissolved using nitric acid, sulfuric acid, sulfuric acid, which is smoldered, makes selenium with bromination
The volatilization of object form removes, and high price tellurium (VI) is quantitatively reduced to low price tellurium by hydrogen chloride in the hydrochloric acid medium greater than 10mol/L
(IV), silver sulfate removes the interference of chloride ion in the form of silver nitride precipitation, and low price tellurium (IV) is quantitatively oxidized to by potassium permanganate
High price tellurium (VI), ferrous sulfate restore excessive potassium permanganate, to measure the content of tellurium in sample indirectly；Specific steps
It is as follows:
(1) 0.1000 ~ 0.5000g(m is accurately weighed) tellurium slag specimen product in 400mL beaker, rush a small amount of water wetting sample, add
Enter 115mol/L 0 ~ 15mL of concentrated nitric acid, heating is boiled after sample dissolution completely, and 10 ~ 15mL sulfuric acid (1+1) is added and is heated to emitting
Sulfuric acid cigarette, remove it is cooling after, rush a small amount of water dilution, 6.8mol/L hydrobromic acid 10mL be added, continue to be heated to after sulfuric acid cigarette emits to the greatest extent
It removes, is added after 12mol/L hydrochloric acid 10mL heating boils to solution and be steamed near dry, 20mL hydrochloric acid (1+1) bath is added extremely
50g/L silver sulfate solution is added dropwise until there is no silver chlorates to sink in solution in 150mL or so, heated solution to nearly boiling dissolved salts
It forms sediment and generates, filtered with Medium speed filter paper, retain filtrate；
(2) C is added in upper filtrate1=0.01mol/L Standard Potassium Permanganate Solution to solution color in stable purplish red
Color and when not fading after amount 5mL, the volume V for the liquor potassic permanganate that accurate recording is added1, placement is cooled to room temperature,
15mL mixture of sulfuric phosphoric acid is added, uses C2=0.05mol/L ferrous sulfate standard solution is titrated, until the aubergine in solution is complete
It takes off entirely, as titration end-point, and the titration volumes V of accurate recording ferrous sulfate2, substitute into the content that tellurium is calculated in following formula
。
Further, mixture of sulfuric phosphoric acid is 98% (wt) concentrated sulfuric acid: 85% (wt) concentrated phosphoric acid: water by volume 3:3:14 mixing and
At.
There are following advantages by the present invention compared with prior art:
1, the present invention dissolves sample using nitric-sulfuric acid, and hydrobromic acid makes the selenium in sample when sulfuric acid is smoldered with selenium
Bromide form volatilize remove, achieve the purpose that selen-tellurjum separate；Hydrogen chloride will be high in the hydrochloric acid medium greater than 10mol/L
Valence tellurium (VI) is reduced to low price tellurium (IV), and is generated chloro-complex with it and reduced its reduction potential, itself and potassium permanganate are increased
Potential difference, accelerate the rate and completeness of tellurium Yu potassium permanganate oxidation reduction reaction；Before potassium permanganate oxidation is added,
The chloride ion in solution is removed in the form of silver nitride precipitation with silver sulfate, chloride ion is excluded and the reduction of potassium permanganate is interfered,
Ferrous sulfate titrates excessive potassium permanganate, to calculate the content of tellurium indirectly, solve be difficult to Accurate Determining and
The problem of traditional volumetric method takes a long time ensure that the accuracy, reliability and timeliness of result.
2, the present invention uses above-mentioned principle to efficiently separate interference element selenium with elemental tellurium to be measured, with silver sulfate with chlorination
The form of silver precipitating removes the chloride ion in solution, avoids the influence of interference element selenium and chloride ion to test, significantly mentions
The high reliability and timeliness of analysis result.
3, the present invention provides a kind of efficient, reliable analysis test methods for tellurium in high selen-tellurjum slag.
4, the present invention is using hydrochloric acid as reducing agent and complexing agent, and potassium permanganate is as oxidant, between ferrous sulfate carries out
The method for connecing titration carries out analysis measurement to the tellurium in high selen-tellurjum slag, solves the tellurium in high selen-tellurjum slag and is recycled
When, the problem of tellurium is difficult to Accurate Determining.This method has many advantages, such as that good separating effect, the rate of recovery are high and precision is good.
Specific embodiment
The present invention is further illustrated below with reference to embodiment, following examples are using the method for mark-on reclaims to this
The precision of method test result and the rate of recovery used by inventing are verified.
The operating condition of reagent and instrument:
Chemical reagent used in test method of the present invention is analytical reagents.
25mL, 50mL acid buret, nitric acid (15mol/L)；Hydrochloric acid (12mol/L)；Sulfuric acid (1+1)；Potassium permanganate mark
Quasi- solution (0.01mol/L)；Ferrous sulfate standard solution (0.05mol/L)；Mixture of sulfuric phosphoric acid (volume ratio 98% (wt) concentrated sulfuric acid:
85% (wt) concentrated phosphoric acid: water=3:3:14).
Embodiment 1
(1) 0.5000g tellurium slag specimen product are accurately weighed in 400mL beaker, a small amount of water wetting sample is rushed, 15mol/ is added
L concentrated nitric acid 15mL, heating are boiled after sample dissolution completely, and 15mL sulfuric acid (1+1) is added and is heated to emitting sulfuric acid cigarette, removes cold
But after, a small amount of water dilution is rushed, 6.8mol/L hydrobromic acid 10mL is added, continued to be heated to removing after sulfuric acid cigarette emits to the greatest extent, be added
After 12mol/L hydrochloric acid 10mL heating is boiled to solution and is steamed near dry, 20mL hydrochloric acid (1+1) bath is added to 150mL or so, adds
50g/L silver sulfate solution is added dropwise until using middling speed there is no silver nitride precipitation generation in solution to nearly boiling dissolved salts in hot solution
Filter paper filtering, retains filtrate；
(2) 0.01mol/L Standard Potassium Permanganate Solution is added in above-mentioned filtrate to the color of solution in stable purplish red
Color and excess 5mL when not fading, the volume for the liquor potassic permanganate that accurate recording is added, placement are cooled to room temperature, is added
15mL mixture of sulfuric phosphoric acid is titrated with 0.05mol/L ferrous sulfate standard solution, until the aubergine in solution is taken off completely,
As titration end-point.Calculated result is shown in Table 1.
1 embodiment of table, 1 sample analysis result and recovery of standard addition and precision.
Embodiment 2
(1) 0.4000g tellurium slag specimen product are accurately weighed in 400mL beaker, a small amount of water wetting sample is rushed, 15mol/ is added
L concentrated nitric acid 15mL, heating are boiled after sample dissolution completely, and 15mL sulfuric acid (1+1) is added and is heated to emitting sulfuric acid cigarette, removes cooling
Afterwards, a small amount of water dilution is rushed, the hydrobromic acid of 10mL6.8mol/L is added, continues to be heated to removing after sulfuric acid cigarette emits to the greatest extent, be added
After the 10mL hydrochloric acid heating of 12mol/L is boiled to solution and is steamed near dry, 20mL hydrochloric acid (1+1) bath is added to 150mL or so,
The silver sulfate solution of 50g/L is added dropwise until there is no silver nitride precipitation generation, use in solution to nearly boiling dissolved salts in heated solution
Medium speed filter paper filtering, retains filtrate；
(2) color that Standard Potassium Permanganate Solution to the solution of 0.01mol/L are added in above-mentioned filtrate is in stable purple
It is red and when not fading after amount 5mL, the volume for the liquor potassic permanganate that accurate recording is added, placement is cooled to room temperature,
15mL mixture of sulfuric phosphoric acid is added, is titrated with 0.05mol/L ferrous sulfate standard solution, until the aubergine in solution takes off completely
It goes, as titration end-point.Calculated result is shown in Table 2.
2 embodiment of table, 2 sample analysis result and recovery of standard addition and precision.
Embodiment 3
(1) 0.3000g tellurium slag specimen product are accurately weighed in 400mL beaker, a small amount of water wetting sample is rushed, 15mol/ is added
L concentrated nitric acid 10mL, heating are boiled after sample dissolution completely, and 10mL sulfuric acid (1+1) is added and is heated to emitting sulfuric acid cigarette, removes cold
But after, a small amount of water dilution is rushed, the hydrobromic acid 10mL of 6.8mol/L is added, continued to be heated to removing after sulfuric acid cigarette emits to the greatest extent, be added
After the hydrochloric acid 10mL heating of 12mol/L is boiled to solution and is steamed near dry, 20mL hydrochloric acid (1+1) bath is added to 150mL or so,
50g/L silver sulfate solution is added dropwise until there is no silver nitride precipitation generations in solution, in nearly boiling dissolved salts in heated solution
Fast filter paper filtering, retains filtrate；
(2) 0.01mol/L Standard Potassium Permanganate Solution is added in above-mentioned filtrate to the color of solution in stable purplish red
Color and when not fading after amount 5mL, the volume for the liquor potassic permanganate that accurate recording is added, placement is cooled to room temperature, adds
Enter 15mL mixture of sulfuric phosphoric acid, titrated with 0.05mol/L ferrous sulfate standard solution, until the aubergine in solution takes off completely
It goes, as titration end-point.Calculated result is shown in Table 3.
3 embodiment of table, 3 sample analysis result and recovery of standard addition and precision.
Embodiment 4
(1) 0.2000g tellurium slag specimen product are accurately weighed in 400mL beaker, a small amount of water wetting sample is rushed, 15mol/ is added
The concentrated nitric acid 10mL of L, heating are boiled after sample dissolution completely, and 10mL sulfuric acid (1+1) is added and is heated to emitting sulfuric acid cigarette, removes
After cooling, a small amount of water dilution is rushed, the hydrobromic acid 10mL of 6.8mol/L is added, continued to be heated to removing after sulfuric acid cigarette emits to the greatest extent, be added
After the hydrochloric acid 10mL heating of 12mol/L is boiled to solution and is steamed near dry, 20mL hydrochloric acid (1+1) bath is added to 150mL or so,
The silver sulfate solution of 50g/L is added dropwise until there is no silver nitride precipitation generation, use in solution to nearly boiling dissolved salts in heated solution
Medium speed filter paper filtering, retains filtrate；
(2) color that Standard Potassium Permanganate Solution to the solution of 0.01mol/L are added in above-mentioned filtrate is in stable purple
It is red and when not fading after amount 5mL, the volume for the liquor potassic permanganate that accurate recording is added, placement is cooled to room temperature,
15mL mixture of sulfuric phosphoric acid is added, is titrated with the ferrous sulfate standard solution of 0.05mol/L, until the aubergine in solution is complete
It takes off, as titration end-point.Calculated result is shown in Table 4.
4 embodiment of table, 4 sample analysis result and recovery of standard addition and precision.
Above-described is only preferred embodiment of the invention.It should be understood that for those of ordinary skill in the art,
Under technical inspiration provided by the present invention, as the common knowledge of this field, other equivalent modifications and improvement can also be made,
Also it should be regarded as protection scope of the present invention.
Claims (1)
1. a kind of analysis method for measuring tellurium in high selen-tellurjum slag, it is characterised in that: specifically includes the following steps:
(1) accurately weighing m is 0.1000 ~ 0.5000g tellurium slag specimen product in 400mL beaker, rushes a small amount of water wetting sample, is added
15mol/L 10 ~ 15mL of concentrated nitric acid, heating are boiled after sample dissolution completely, and 10 ~ 15mL sulfuric acid (1+1) is added and is heated to emitting sulphur
Acid fume after removing cooling, rushes a small amount of water dilution, 6.8mol/L hydrobromic acid 10mL is added, and continues to be heated to taking after sulfuric acid cigarette emits to the greatest extent
Under, it is added after 12mol/L hydrochloric acid 10mL heating boils to solution and be steamed near dry, 20mL hydrochloric acid (1+1) bath is added to 150mL,
Concentration 50g/L silver sulfate solution is added dropwise until there is no silver nitride precipitation lifes in solution in heated solution to nearly boiling, dissolved salts
At, filtered with Medium speed filter paper, retain filtrate；
(2) it is C that concentration is added dropwise in the filtrate that step (1) obtains1Standard Potassium Permanganate Solution, until Standard Potassium Permanganate Solution is added dropwise
5mL is added dropwise in stable aubergine and when not fading in the color entered in filtrate again, and the potassium permanganate that accurate recording is added is molten
The volume V of liquid1, placement is cooled to room temperature, and 15mL mixture of sulfuric phosphoric acid is added, is C with concentration2 Ferrous sulfate standard solution dripped
It is fixed, until the aubergine in solution is taken off completely, as titration end-point, and the titration volumes V of accurate recording ferrous sulfate2, generation
Enter to be calculated the content of tellurium in following formula,
The mixture of sulfuric phosphoric acid is the 98%wt concentrated sulfuric acid: 85%wt concentrated phosphoric acid: 3:3:14 is mixed water by volume.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565174A (en) * | 2009-06-05 | 2009-10-28 | 永兴县鑫泰银业有限责任公司 | Method for extracting refined tellurium from tellurium-contained smelting slag |
| CN101844750A (en) * | 2010-06-04 | 2010-09-29 | 中南大学 | Method for preparing high-purity tellurium by material containing tellurium |
| CN101876654A (en) * | 2009-04-30 | 2010-11-03 | 山东松本电源科技有限公司 | Method for determining stibium in aluminum base alloy |
| CN101928834A (en) * | 2010-08-30 | 2010-12-29 | 中南大学 | Method for recovering rare precious metals from solution |
| CN102491287A (en) * | 2011-12-11 | 2012-06-13 | 郴州市金贵银业股份有限公司 | Process for separating and recovering selenium from selenium-containing material |
| CN104034668A (en) * | 2014-06-30 | 2014-09-10 | 锡矿山闪星锑业有限责任公司 | Method for measuring content of tellurium in antimony and antimonous oxide |
| CN104237225A (en) * | 2014-10-16 | 2014-12-24 | 云南驰宏锌锗股份有限公司 | Analyzing method for quickly and precisely measuring tellurium in tellurium smelting process |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508426B (en) * | 2009-03-24 | 2010-12-29 | 中南大学 | Method for separating tellurium from tellurium slag |
-
2015
- 2015-11-18 CN CN201510799181.3A patent/CN105445268B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101876654A (en) * | 2009-04-30 | 2010-11-03 | 山东松本电源科技有限公司 | Method for determining stibium in aluminum base alloy |
| CN101565174A (en) * | 2009-06-05 | 2009-10-28 | 永兴县鑫泰银业有限责任公司 | Method for extracting refined tellurium from tellurium-contained smelting slag |
| CN101844750A (en) * | 2010-06-04 | 2010-09-29 | 中南大学 | Method for preparing high-purity tellurium by material containing tellurium |
| CN101928834A (en) * | 2010-08-30 | 2010-12-29 | 中南大学 | Method for recovering rare precious metals from solution |
| CN102491287A (en) * | 2011-12-11 | 2012-06-13 | 郴州市金贵银业股份有限公司 | Process for separating and recovering selenium from selenium-containing material |
| CN104034668A (en) * | 2014-06-30 | 2014-09-10 | 锡矿山闪星锑业有限责任公司 | Method for measuring content of tellurium in antimony and antimonous oxide |
| CN104237225A (en) * | 2014-10-16 | 2014-12-24 | 云南驰宏锌锗股份有限公司 | Analyzing method for quickly and precisely measuring tellurium in tellurium smelting process |
Non-Patent Citations (3)
| Title |
|---|
| 冶炼产物中碲的容量法测定;李绍荣等;《分析化学》;19741231;第3卷(第3期);全文 * |
| 重铬酸钾容量法分析碲方法的改进;王维;《云南省有色金属学会第七届冶炼技术论文发布会》;20150826;第880页 * |
| 重铬酸钾滴定法测定中和渣中的碲;沈广鑫;《江西冶金》;20081031;第28卷(第5期);全文 * |
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