CN105445268A - 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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- CN105445268A CN105445268A CN201510799181.3A CN201510799181A CN105445268A CN 105445268 A CN105445268 A CN 105445268A CN 201510799181 A CN201510799181 A CN 201510799181A CN 105445268 A CN105445268 A CN 105445268A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N21/79—Photometric titration
Abstract
The invention provides an analysis method for determining tellurium in high-selenium tellurium slag, which comprises the steps of dissolving a sample by using nitric acid and sulfuric acid, volatilizing selenium in a bromide form by smoking sulfuric acid, quantitatively reducing high-valence tellurium (VI) into low-valence tellurium (IV) by using hydrogen chloride in a hydrochloric acid medium of which the concentration is more than 10mol/L, removing interference of chloride ions by using silver sulfate in a silver chloride precipitation form, quantitatively oxidizing the low-valence tellurium (IV) into high-valence tellurium (VI) by using potassium permanganate, and reducing excessive potassium permanganate by using ferrous sulfate, thereby indirectly measuring the content of tellurium in the sample; the method for analyzing and determining the tellurium in the high-selenium tellurium slag by adopting the hydrochloric acid as a reducing agent and a complexing agent, the potassium permanganate as an oxidizing agent and the ferrous sulfate for indirect titration solves the problem that the tellurium is difficult to accurately determine when the tellurium in the high-selenium tellurium slag is recycled. The method has the advantages of good separation effect, high recovery rate, good precision and the like.
Description
Technical field
The invention belongs to chemical analysis field, be specifically related to a kind of analytical approach measuring tellurium in high selen-tellurjum slag.
Background technology
Tellurium belongs to rare loose nonmetalloid, has again independently mineral deposit at the existing associated minerals of occurring in nature tellurium.Be mainly used in the catalyzer of cracking of oil, the brightener of electroplate liquid, the coloured material of glass, add in steel to increase its ductility, add in lead the intensity and corrosion stability that increase it to.Tellurium and its compound are again a kind of semiconductor materials.By By consulting literatures data, more for the method for tellurium de-termination in tellurium dioxide product, even existing relevant national standard, less for the pertinent literature of the chemical analysis method of tellurium in smelting intermediate product tellurium slag, not almost not having especially containing tellurium de-termination method in the tellurium slag of high selenium, copper and silver; The analytical approach of current tellurium has atomic absorption spectrophotometry, plasma emission spectrometry, potassium bichromate titrimetric method etc.
Smelting intermediate product tellurium slag mainly comes from Copper making process, wherein mainly containing the general content of tellurium be a few percent to tens percent, the general content of selenium be a few percent to tens percent, the general content of copper is a few percent, and silver content is generally a few percent; Owing to containing impurity element selenium in general tellurium slag simultaneously, and its chemical property with tellurium is close, therefore causes the content of tellurium in tellurium slag to be difficult to Accurate Determining; The method of traditional employing potassium dichromate oxidation is consuming time longer, is difficult to show that analysis result is to instruct commercial production fast.
Summary of the invention
In order to solve the above-mentioned problems in the prior art, the invention provides a kind of analytical approach measuring tellurium in high selen-tellurjum slag.
The technical solution used in the present invention is: employing nitric acid, sulfuric acid dissolve sample, sulfuric acid is smoldered and is made selenium with bromide form volatilization removing, in the hydrochloric acid medium being greater than 10mol/L, high price tellurium (VI) is quantitatively reduced to tellurium (IV) at a low price by hydrogen chloride, silver sulfate is with the interference of the form of silver nitride precipitation removing chlorion, potassium permanganate will quantitatively be oxidized to high price tellurium (VI) by tellurium (IV) at a low price, ferrous sulphate reduces to excessive potassium permanganate, thus indirectly records the content of tellurium in sample; Concrete steps are as follows:
(1) accurately 0.1000 ~ 0.5000g(m is taken) tellurium slag specimen product are in 400mL beaker, rush a small amount of water-wet sample, add 115mol/L red fuming nitric acid (RFNA) 0 ~ 15mL, heating is boiled after sample dissolution is complete, add 10 ~ 15mL sulfuric acid (1+1) to be heated to emit sulfuric acid cigarette, after taking off cooling, rush the dilution of a small amount of water, add 6.8mol/L hydrobromic acid 10mL, continue to be heated to sulfuric acid cigarette to emit to the greatest extent and take off, add 12mol/L hydrochloric acid 10mL heating to boil after to solution steaming near doing, add 20mL hydrochloric acid (1+1) bath to about 150mL, heated solution is to the dissolved salts that closely boils, drip 50g/L silver sulfate solution until no longer include silver nitride precipitation generation in solution, filter with Medium speed filter paper, retain filtrate,
(2) in upper filtrate, C is added
1after amount 5mL, the volume V of the liquor potassic permanganate that accurate recording adds when=0.01mol/L Standard Potassium Permanganate Solution to the color of solution is stable aubergine and does not fade
1, place and be cooled to room temperature, add 15mL mixture of sulfuric phosphoric acid, use C
2=0.05mol/L ferrous sulphate standard solution carries out titration, until the aubergine in solution is taken off completely, is titration end-point, and the titration volumes V of accurate recording ferrous sulphate
2, substitute into the content calculating tellurium in following formula
。
Further, mixture of sulfuric phosphoric acid is 98% (wt) concentrated sulphuric acid: 85% (wt) strong phosphoric acid: water by volume 3:3:14 mixes.
Compared with prior art there is following advantage in the present invention:
1, the present invention adopts nitric-sulfuric acid to dissolve sample, and hydrobromic acid makes the selenium in sample remove with the volatilization of the form of the bromide of selenium when sulfuric acid is smoldered, and reaches the object that selen-tellurjum is separated; In the hydrochloric acid medium being greater than 10mol/L, high price tellurium (VI) is reduced to tellurium (IV) at a low price by hydrogen chloride, and reduce its reduction potential with its generation chloro-complex, increase the electric potential difference of itself and potassium permanganate, accelerate speed and the completeness of tellurium and potassium permanganate oxidation reduction reaction; Before adding potassium permanganate oxidation, with silver sulfate with the chlorion in the form of silver nitride precipitation removing solution, get rid of chlorion to disturb the reduction of potassium permanganate, ferrous sulphate carries out titration to excessive potassium permanganate, thus indirect calculation goes out the content of tellurium, solve and be difficult to Accurate Determining and traditional volumetric method longer problem consuming time, ensure that the accuracy of result, reliability and ageing.
2, the present invention adopts above-mentioned principle that interference element selenium is effectively separated with elemental tellurium to be measured, with silver sulfate with the chlorion in the form of silver nitride precipitation removing solution, avoid the impact on test of interference element selenium and chlorion, improve the reliability of analysis result and ageing significantly.
3, the invention provides a kind of efficient, reliable analysis test method for tellurium in high selen-tellurjum slag.
4, the present invention adopts hydrochloric acid as reductive agent and complexing agent, potassium permanganate is as oxygenant, the method that ferrous sulphate carries out indirect titration is carried out analysis to the tellurium in high selen-tellurjum slag and is measured, and solve tellurium in high selen-tellurjum slag when recycling, tellurium is difficult to the problem of Accurate Determining.This method has the advantages such as the high and precision of good separating effect, the recovery is good.
Embodiment
Be described further the present invention below in conjunction with embodiment, the method that following example adopts mark-on to reclaim is verified the precision of the method applied in the present invention test result and the recovery.
The condition of work of reagent and instrument:
The chemical reagent used in test method of the present invention is analytical reagent.
25mL, 50mL acid buret, nitric acid (15mol/L); Hydrochloric acid (12mol/L); Sulfuric acid (1+1); Standard Potassium Permanganate Solution (0.01mol/L); Ferrous sulphate standard solution (0.05mol/L); Mixture of sulfuric phosphoric acid (volume ratio 98% (wt) concentrated sulphuric acid: 85% (wt) strong phosphoric acid: water=3:3:14).
Embodiment 1
(1) 0.5000g tellurium slag specimen product are accurately taken in 400mL beaker, rush a small amount of water-wet sample, add 15mol/L red fuming nitric acid (RFNA) 15mL, heating is boiled after sample dissolution is complete, add 15mL sulfuric acid (1+1) to be heated to emit sulfuric acid cigarette, after taking off cooling, rush the dilution of a small amount of water, add 6.8mol/L hydrobromic acid 10mL, continue to be heated to sulfuric acid cigarette to emit to the greatest extent and take off, add 12mol/L hydrochloric acid 10mL heating to boil after to solution steaming near doing, add 20mL hydrochloric acid (1+1) bath to about 150mL, heated solution is to the dissolved salts that closely boils, drip 50g/L silver sulfate solution until no longer include silver nitride precipitation generation in solution, filter with Medium speed filter paper, retain filtrate,
(2) in above-mentioned filtrate, add excessive 5mL when 0.01mol/L Standard Potassium Permanganate Solution to the color of solution is stable aubergine and does not fade, the volume of the liquor potassic permanganate that accurate recording adds, placement is cooled to room temperature, add 15mL mixture of sulfuric phosphoric acid, titration is carried out with 0.05mol/L ferrous sulphate standard solution, until the aubergine in solution is taken off completely, be titration end-point.Result of calculation is in table 1.
Table 1 embodiment 1 sample analysis result and recovery of standard addition and precision.
Embodiment 2
(1) 0.4000g tellurium slag specimen product are accurately taken in 400mL beaker, rush a small amount of water-wet sample, add 15mol/L red fuming nitric acid (RFNA) 15mL, heating is boiled after sample dissolution is complete, add 15mL sulfuric acid (1+1) to be heated to emit sulfuric acid cigarette, after taking off cooling, rush the dilution of a small amount of water, add the hydrobromic acid of 10mL6.8mol/L, continue to be heated to sulfuric acid cigarette to emit to the greatest extent and take off, the 10mL hydrochloric acid heating adding 12mol/L is boiled after to solution steaming near doing, add 20mL hydrochloric acid (1+1) bath to about 150mL, heated solution is to the dissolved salts that closely boils, drip the silver sulfate solution of 50g/L until no longer include silver nitride precipitation generation in solution, filter with Medium speed filter paper, retain filtrate,
(2) after amount 5mL when the Standard Potassium Permanganate Solution adding 0.01mol/L in above-mentioned filtrate to the color of solution is stable aubergine and does not fade, the volume of the liquor potassic permanganate that accurate recording adds, placement is cooled to room temperature, add 15mL mixture of sulfuric phosphoric acid, titration is carried out with 0.05mol/L ferrous sulphate standard solution, until the aubergine in solution is taken off completely, be titration end-point.Result of calculation is in table 2.
Table 2 embodiment 2 sample analysis result and recovery of standard addition and precision.
Embodiment 3
(1) 0.3000g tellurium slag specimen product are accurately taken in 400mL beaker, rush a small amount of water-wet sample, add 15mol/L red fuming nitric acid (RFNA) 10mL, heating is boiled after sample dissolution is complete, add 10mL sulfuric acid (1+1) to be heated to emit sulfuric acid cigarette, after taking off cooling, rush the dilution of a small amount of water, add the hydrobromic acid 10mL of 6.8mol/L, continue to be heated to sulfuric acid cigarette to emit to the greatest extent and take off, the hydrochloric acid 10mL heating adding 12mol/L is boiled after to solution steaming near doing, add 20mL hydrochloric acid (1+1) bath to about 150mL, heated solution is to the dissolved salts that closely boils, drip 50g/L silver sulfate solution until no longer include silver nitride precipitation generation in solution, filter with Medium speed filter paper, retain filtrate,
(2) add in above-mentioned filtrate when 0.01mol/L Standard Potassium Permanganate Solution to the color of solution is stable aubergine and does not fade after amount 5mL, the volume of the liquor potassic permanganate that accurate recording adds, placement is cooled to room temperature, add 15mL mixture of sulfuric phosphoric acid, titration is carried out with 0.05mol/L ferrous sulphate standard solution, until the aubergine in solution is taken off completely, be titration end-point.Result of calculation is in table 3.
Table 3 embodiment 3 sample analysis result and recovery of standard addition and precision.
Embodiment 4
(1) 0.2000g tellurium slag specimen product are accurately taken in 400mL beaker, rush a small amount of water-wet sample, add the red fuming nitric acid (RFNA) 10mL of 15mol/L, heating is boiled after sample dissolution is complete, add 10mL sulfuric acid (1+1) to be heated to emit sulfuric acid cigarette, after taking off cooling, rush the dilution of a small amount of water, add the hydrobromic acid 10mL of 6.8mol/L, continue to be heated to sulfuric acid cigarette to emit to the greatest extent and take off, the hydrochloric acid 10mL heating adding 12mol/L is boiled after to solution steaming near doing, add 20mL hydrochloric acid (1+1) bath to about 150mL, heated solution is to the dissolved salts that closely boils, drip the silver sulfate solution of 50g/L until no longer include silver nitride precipitation generation in solution, filter with Medium speed filter paper, retain filtrate,
(2) after amount 5mL when the Standard Potassium Permanganate Solution adding 0.01mol/L in above-mentioned filtrate to the color of solution is stable aubergine and does not fade, the volume of the liquor potassic permanganate that accurate recording adds, placement is cooled to room temperature, add 15mL mixture of sulfuric phosphoric acid, titration is carried out with the ferrous sulphate standard solution of 0.05mol/L, until the aubergine in solution is taken off completely, be titration end-point.Result of calculation is in table 4.
Table 4 embodiment 4 sample analysis result and recovery of standard addition and precision.
Above-described is only preferred embodiment of the present invention.Should be understood that for the person of ordinary skill of the art, under technology enlightenment provided by the present invention, as the common practise of this area, other equivalent modifications and improvement can also be made, also should be considered as protection scope of the present invention.
Claims (2)
1. measure an analytical approach for tellurium in high selen-tellurjum slag, it is characterized in that: specifically comprise the following steps:
(1) accurately 0.1000 ~ 0.5000g(m is taken) tellurium slag specimen product are in 400mL beaker, rush a small amount of water-wet sample, add 15mol/L red fuming nitric acid (RFNA) 10 ~ 15mL, heating is boiled after sample dissolution is complete, add 10 ~ 15mL sulfuric acid (1+1) to be heated to emit sulfuric acid cigarette, after taking off cooling, rush the dilution of a small amount of water, add 6.8mol/L hydrobromic acid 10mL, continue to be heated to sulfuric acid cigarette to emit to the greatest extent and take off, add 12mol/L hydrochloric acid 10mL heating to boil after to solution steaming near doing, add 20mL hydrochloric acid (1+1) bath to 150mL, heated solution is to closely boiling, dissolved salts, drip concentration 50g/L silver sulfate solution until no longer include silver nitride precipitation generation in solution, filter with Medium speed filter paper, retain filtrate,
(2) dripping concentration in the filtrate that step (1) obtains is C
1standard Potassium Permanganate Solution, drips 5mL, the volume V of the liquor potassic permanganate that accurate recording adds when the color be added dropwise in filtrate to Standard Potassium Permanganate Solution is stable aubergine and does not fade again
1, place and be cooled to room temperature, adding 15mL mixture of sulfuric phosphoric acid, is C by concentration
2ferrous sulphate standard solution carry out titration, until the aubergine in solution is taken off completely, be titration end-point, and the titration volumes V of accurate recording ferrous sulphate
2, substitute into the content calculating tellurium in following formula
.
2. a kind of analytical approach measuring tellurium in high selen-tellurjum slag as claimed in claim 1, is characterized in that: mixture of sulfuric phosphoric acid is 98% (wt) concentrated sulphuric acid: 85% (wt) strong phosphoric acid: water by volume 3:3:14 mixes.
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| CN108088842A (en) * | 2018-02-23 | 2018-05-29 | 江西省农业科学院土壤肥料与资源环境研究所 | A kind of system and method for measuring soil with organic matter |
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| CN108088842A (en) * | 2018-02-23 | 2018-05-29 | 江西省农业科学院土壤肥料与资源环境研究所 | A kind of system and method for measuring soil with organic matter |
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