CN106940357A - Method for detecting bismuth in bismuth slag containing high selenium and tellurium - Google Patents
Method for detecting bismuth in bismuth slag containing high selenium and tellurium Download PDFInfo
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Abstract
The invention relates to a method for detecting bismuth in bismuth slag containing high selenium and tellurium, which comprises the following detection steps: drying and crushing a bismuth slag sample to be detected, and weighing a quantitative sample as an analysis sample; placing the analysis sample in a beaker, adding 5mL of distilled water to wet the sample, adding a plurality of concentrated hydrochloric acid and nitric acid, heating and dissolving the solution by a temperature-controlled electric heating plate until the residual solution is 5mL, preparing a blank sample, and synchronously digesting the blank sample; adding anhydrous sodium sulfite into the analysis sample and the blank sample under a hydrochloric acid medium, heating in a water bath, evaporating the filtrate, smoking with perchloric acid, boiling the nitric acid and distilled water together, cooling and fixing the volume to obtain a sample liquid to be detected and a blank liquid to be detected; preparing and calibrating an EDTA standard solution; and finally converting the content of bismuth in the bismuth slag sample. In a bismuth slag sample with high selenium and tellurium content, selenium and tellurium in the sample are reduced into simple substances while bismuth is continuously remained in the solution, and the selenium, tellurium and bismuth are separated by filtering, so that the end point color in the titration process is obvious.
Description
Technical field
The invention belongs to detection method technical field, it is related to a kind of detection method of bismuth in bismuth slag containing high selen-tellurjum.
Background technology
Bismuth enjoys the metal of the title of " green metal " as one kind, and its purposes is widely.Industrially conventional welding is former
Just contain bismuth metal in material scolding tin.Some antidiarrheal agent medically, osteocomma, eye shadow cream, lipstick all contain fraction of bismuth.Together
When bismuth can also do the additive of alloy, manufacture photoresistance, the hot body of carrier or cooling agent in nucleon reaction heap.At present, the detection side of bismuth
Method mainly has atomic fluorescence spectrometry, inductively coupled plasma spectrum or mass spectrography, a thiocarbamide photometry, atomic absorption spectrography (AAS),
Classical EDTA volumetric methods etc..Generally, atomic fluorescence spectrometry, inductively coupled plasma spectrum or mass spectrography are applied to area
The low content bismuth such as trace element analysis in domain GEOCHEMICAL SURVEY, product（Ppm ranks are lower）Detection；Thiocarbamide photometry,
Atomic absorption method compared with suitable for content be less than 5 percent bismuth detection, if taking dilution measurement to the bismuth of higher amount,
To then bigger detection error be brought；Classical EDTA volumetric methods are applied to the analysis of the Determination of High Content of Bismuth more than 5 percent.With
The increase of the market demand and the exhaustion of mineral resources, bismuth is only refined from ore deposit can not meet needs, such as domestic many to have
Non-ferrous metal smelting enterprise has started to reclaim bismuth from the wet method electrolysis earth of positive pole.Bismuth slag is the wet method to non-ferrous metal, pyrogenic process or phase
The raw material of combined recovery bismuth metal or the general designation of slag charge.The content of bismuth is higher than 5 percent, and wherein impure element in bismuth slag
Species is more, content is high, classical EDTA volumetric methods can not meet bismuth detection demand, especially when in slag charge contain selen-tellurjum
（Selen-tellurjum total amount is more than 0.5%）When, when being titrated during volumetric method Titration of Bismuth, solution becomes brown or brownish black, not only
Influence the regulation of pH value, the mutation of more immediate influence terminal colour, it is impossible to accurately detect the content of bismuth in this kind of slag charge.
Still specially introducing bismuth in this kind of slag charge high containing selen-tellurjum without a kind of national standard method at present, how this detects.
The content of the invention
In order to overcome the disadvantages mentioned above of prior art, the present invention provides a kind of detection side of bismuth in bismuth slag containing high selen-tellurjum
Method, this processing mode Selenium In Some Selenium-rich Biological Samples tellurium is reduced into simple substance and bismuth continues to stay in the solution, is separated selen-tellurjum with bismuth by filtering,
So that terminal colour is obvious in titration process.
The technical solution adopted for the present invention to solve the technical problems is：The detection side of bismuth in a kind of bismuth slag containing high selen-tellurjum
Method, its detecting step is：
1st, by bismuth slag sample drying to be measured, crushing, weigh quantitative sample and be used as analysis sample；
2nd, analysis sample is placed in 250mL beakers, adds distilled water 5 mL wetting sample, it is some to add concentrated hydrochloric acid, nitric acid, control
Warm electric hot plate heating for dissolving is to surplus solution 5mL, while blank sample is prepared, it is also synchronous to be cleared up；
3rd, sample will be analyzed and blank sample will add anhydrous sodium sulfite, heating water bath under hydrochloric acid medium, and evaporated filtrate, increase chloric acid
Smolder, nitric acid, distilled water cool down constant volume after boiling altogether, obtain analyte sample fluid and blank solution to be measured；
4th, the configuration of EDTA standard liquids and demarcation；The configuration (0.01mol/L) of EDTA standard liquids：Weigh 3.8g top pure grades EDTA
It is placed in 500mL beakers, is dissolved in water, move into 1000mL volumetric flasks, mixes；Sodium acetate solution（200g/L）：Weigh acetic acid
Sodium 20.0g, with being transferred to constant volume in 100ml volumetric flasks after water dissolves；Tartaric acid solution（100g/L）：Tartaric acid 10.0g is weighed,
With being transferred to constant volume in 100ml volumetric flasks after water dissolves；Saturation thiourea solution：Thiocarbamide is added into a certain amount of water until thiocarbamide
Not in dissolving；Xylenol orange solution（1g/L）：Xylenol orange 0.1g is weighed, it is fixed with being transferred to after water dissolves in 100ml volumetric flasks
Hold.The demarcation of EDTA standard liquids：Weigh the pure bismuths of 0.2g（Mass fraction is more than 99.99%）, it is placed in 250mL beakers, adds
15mL nitric acid, cap upper surface ware, low-temperature heat is complete to dissolving, and removes and is cooled to room temperature, transfers the solution into 100mL volumetric flasks
In, purging surface plate and wall of cup, and it is settled to scale.Three parts of 25.00mL bismuths standard liquid is pipetted in one group of 500mL conical flask
In, 200mL is added water to, 0.2g ascorbic acid, 5ml saturations thiourea solution, 5ml tartaric acid solutions is added and shakes up, use EDTA standards
Volumetric soiutions are titrated to yellow and shoaled, plus 3-4 drop xylenol orange solution, adjusted with sodium acetate solution to pH value be 1.5-1.7. after
The continuous red that is titrated to is changed into glassy yellow for terminal.EDTA concentration is calculated as follows out:
In formula：
The actual concentrations of C-EDTA standard liquids, unit is mole every milliliter（mol/L）
m1- point take the quality of bismuth standard liquid, unit for gram（g）；
V1The volume of EDTA standard liquids is consumed during-titration, unit is milliliter（mL）；
1000-volume conversion factor；
The molal weight of 209-bismuth, unit is unit for gram every mole（g/mol）；
And be recorded as shown in table 1：
The concentration results of the EDTA standard liquids of table 1
5th, bismuth element is determined：The analyte sample fluid and blank solution to be measured obtained using determination step 3, is obtained with reference to step 4
EDTA concentration of standard solution, titration sample solution and blank solution, according to consumption EDTA volume, and then converse bismuth slag specimen product
In bismuth content.
In step 1, sample comminution is to 160-300 mesh, and it is 0.2g to weigh analysis sample quality（4th is accurate to after decimal point）.
It is 15ml that hydrochloric acid, which adds volume, in step 2, and it is 5 mL that nitric acid, which adds volume, and electric plate temperature is 200 DEG C.
In step 2,3, it is pure that hydrochloric acid, nitric acid, perchloric acid, anhydrous sodium sulfite are analysis.
In step 3, concentration of hydrochloric acid is 1+1, and anhydrous sodium sulfite is 1-2g, and water-bath is 2 hours, and filtrate is evaporated to 10mL,
Perchloric acid is 10mL, and nitric acid is 8mL, and distilled water is 20mL, is settled in 100mL volumetric flasks.
In step 5, divide and take supernatant liquor 25mL in 500mL conical flasks, the similarly hereinafter demarcation of EDTA standard liquids；According to consumption
EDTA volumes, can be calculated as follows its content：
In formula：
The actual concentrations of C-EDTA standard liquids, unit is mole every milliliter（mol/L）；
V-sample consumption EDTA volume, unit is milliliter（mL）；
V0 - blank consumes EDTA volume, and unit is milliliter（mL）；
MS The quality of-sample, unit for gram（g）；
The molal weight of 209.0-bismuth, unit is gram every mole（g/mol）；
4-point take volume multiple.
The positive effect of the present invention is：In the bismuth slag specimen higher containing selen-tellurjum, this processing mode Selenium In Some Selenium-rich Biological Samples tellurium is reduced into list
Matter and bismuth continues to stay in the solution, selen-tellurjum is separated with bismuth by filtering, so that terminal colour is obvious in titration process.
Embodiment
With reference to embodiment, the present invention is further described.
The detection method of bismuth in a kind of bismuth slag containing high selen-tellurjum, its detecting step is：
1st, by bismuth slag sample drying to be measured, crushing, weigh quantitative sample and be used as analysis sample；
2nd, analysis sample is placed in 250mL beakers, adds distilled water 5 mL wetting sample, it is some to add concentrated hydrochloric acid, nitric acid, control
Warm electric hot plate heating for dissolving is to surplus solution 5mL, while blank sample is prepared, it is also synchronous to be cleared up；
3rd, sample will be analyzed and blank sample will add anhydrous sodium sulfite, heating water bath under hydrochloric acid medium, and evaporated filtrate, increase chloric acid
Smolder, nitric acid, distilled water cool down constant volume after boiling altogether, obtain analyte sample fluid and blank solution to be measured；
4th, the configuration of EDTA standard liquids and demarcation；The configuration (0.01mol/L) of EDTA standard liquids：Weigh 3.8g top pure grades EDTA
It is placed in 500mL beakers, is dissolved in water, move into 1000mL volumetric flasks, mixes；Sodium acetate solution（200g/L）：Weigh acetic acid
Sodium 20.0g, with being transferred to constant volume in 100ml volumetric flasks after water dissolves；Tartaric acid solution（100g/L）：Tartaric acid 10.0g is weighed,
With being transferred to constant volume in 100ml volumetric flasks after water dissolves；Saturation thiourea solution：Thiocarbamide is added into a certain amount of water until thiocarbamide
Not in dissolving；Xylenol orange solution（1g/L）：Xylenol orange 0.1g is weighed, it is fixed with being transferred to after water dissolves in 100ml volumetric flasks
Hold.The demarcation of EDTA standard liquids：Weigh the pure bismuths of 0.2g（Mass fraction is more than 99.99%）, it is placed in 250mL beakers, adds
15mL nitric acid, cap upper surface ware, low-temperature heat is complete to dissolving, and removes and is cooled to room temperature, transfers the solution into 100mL volumetric flasks
In, purging surface plate and wall of cup, and it is settled to scale.Three parts of 25.00mL bismuths standard liquid is pipetted in one group of 500mL conical flask
In, 200mL is added water to, 0.2g ascorbic acid, 5ml saturations thiourea solution, 5ml tartaric acid solutions is added and shakes up, use EDTA standards
Volumetric soiutions are titrated to yellow and shoaled, plus 3-4 drop xylenol orange solution, adjusted with sodium acetate solution to pH value be 1.5-1.7. after
The continuous red that is titrated to is changed into glassy yellow for terminal.EDTA concentration is calculated as follows out:
In formula：
The actual concentrations of C-EDTA standard liquids, unit is mole every milliliter（mol/L）
m1- point take the quality of bismuth standard liquid, unit for gram（g）；
V1The volume of EDTA standard liquids is consumed during-titration, unit is milliliter（mL）；
1000-volume conversion factor；
The molal weight of 209-bismuth, unit is unit for gram every mole（g/mol）；
And be recorded as shown in table 1：
The concentration results of the EDTA standard liquids of table 1
5th, bismuth element is determined：The analyte sample fluid and blank solution to be measured obtained using determination step 3, is obtained with reference to step 4
EDTA concentration of standard solution, titration sample solution and blank solution, according to consumption EDTA volume, and then converse bismuth slag specimen product
In bismuth content.
In step 1, sample comminution is to 160-300 mesh, and it is 0.2g to weigh analysis sample quality（4th is accurate to after decimal point）.
It is 15ml that hydrochloric acid, which adds volume, in step 2, and it is 5 mL that nitric acid, which adds volume, and electric plate temperature is 200 DEG C.
In step 2,3, it is pure that hydrochloric acid, nitric acid, perchloric acid, anhydrous sodium sulfite are analysis.
In step 3, concentration of hydrochloric acid is 1+1, and anhydrous sodium sulfite is 1-2g, and water-bath is 2 hours, and filtrate is evaporated to 10mL,
Perchloric acid is 10mL, and nitric acid is 8mL, and distilled water is 20mL, is settled in 100mL volumetric flasks.
In step 5, divide and take supernatant liquor 25mL in 500mL conical flasks, the similarly hereinafter demarcation of EDTA standard liquids；According to consumption
EDTA volumes, can be calculated as follows its content：
In formula：
The actual concentrations of C-EDTA standard liquids, unit is mole every milliliter（mol/L）；
V-sample consumption EDTA volume, unit is milliliter（mL）；
V0 - blank consumes EDTA volume, and unit is milliliter（mL）；
MS The quality of-sample, unit for gram（g）；
The molal weight of 209.0-bismuth, unit is gram every mole（g/mol）；
4-point take volume multiple.
Example 1：
Certain Guangdong smeltery bismuth slag（Containing selenium 1%, containing tellurium 2%）, bi content is chemically examined, concrete operations are as follows：
1st, take representative bismuth slag specimen product to be measured after 100 DEG C ~ 105 DEG C dry, be crushed to 200 mesh, day is analyzed in analysis
About 0.2g is weighed on flat（4th is accurate to after decimal point）3 parts of sample is as analysis sample；
2nd, analysis sample is placed in 250mL beakers, adds distilled water 5mL wettings sample, analyze pure concentrated hydrochloric acid 15mL, analyze pure
Concentrated nitric acid 5mL, 200 DEG C of heating for dissolving to liquor capacities of electric hot plate are about 5ml, add 40ml hydrochloric acid（1+1）, the anhydrous sulfurous acid of 1g
Sodium, then heating water bath 2 hours, cooled and filtered, filtrate re-evaporation to about 10mL add perchloric acid 10ml to emitting dense white cigarette to cup
Mouthful, room temperature is cooled to, 8mL concentrated nitric acids, 20mL distilled water is added, and rinse wall of cup.Room temperature, constant volume are cooled to after solution is boiled
To 100mL volumetric flasks.Whole process is with experiment blank two.
3rd, divide and take 25mL to analyze liquid and blank solution in 500mL conical flasks, add distilled water to about 200mL, add 0.2g
Ascorbic acid, 5mL saturation thiourea solutions shake up, and being titrated to yellow with EDTA standard titration solutions (0.0102mol/L) shoals, plus
3-4 drop xylenol orange solution, it is 1.5-1.7 to be adjusted with sodium acetate solution to pH value, continues to be titrated to red and is changed into glassy yellow and is
Terminal.The EDTA volumes of consumption are recorded, are calculated as follows:
In formula：
The actual concentrations of C-EDTA standard liquids, unit is mole every milliliter（mol/L）；
V-sample consumption EDTA volume, unit is milliliter（mL）；
V0 - blank consumes EDTA volume, and unit is milliliter（mL）；
MS The quality of-sample, unit for gram（g）；
1000-volume conversion factor；
The molal weight of 209.0-bismuth, unit is gram every mole（g/mol）；
4-point take volume multiple；
As a result such as table 2 is recorded：
Determine trace Bismuth result in the bismuth slag of table 2
4th, accuracy validation
Above-mentioned sample 0.2500g is accurately weighed, the degree of accuracy is verified using the method for mark-on reclaims, 3, recovery are the results are shown in Table
Rate meets needs.
The recovery of standard addition result of table 3
| Sample number | Measured value ω/% | Addition m/mg | Measured quantity m/mg | The rate of recovery/% |
| 1 | 24.06 | 40.0 | 100.55 | 101 |
Example 2：
Certain Hunan smeltery bismuth slag（Containing selenium 2%, containing tellurium 2%）, bi content is chemically examined, concrete operations are as follows：
1st, take representative bismuth slag specimen product to be measured after 100 DEG C ~ 105 DEG C dry, be crushed to 200 mesh, day is analyzed in analysis
About 0.2g is weighed on flat（4th is accurate to after decimal point）3 parts of sample is as analysis sample；
2nd, analysis sample is placed in 250mL beakers, adds distilled water 5mL wettings sample, analyze pure concentrated hydrochloric acid 15mL, analyze pure
Concentrated nitric acid 5mL, 200 DEG C of heating for dissolving to liquor capacities of electric hot plate are about 5ml, add 40ml hydrochloric acid（1+1）, the anhydrous sulfurous acid of 1g
Sodium, then heating water bath 2 hours, cooled and filtered, filtrate re-evaporation to about 10mL add perchloric acid 10ml to emitting dense white cigarette to cup
Mouthful, room temperature is cooled to, 8mL concentrated nitric acids, 20mL distilled water is added, and rinse wall of cup.Room temperature, constant volume are cooled to after solution is boiled
To 100mL volumetric flasks.Whole process is with experiment blank two.
3rd, divide and take 25mL to analyze liquid and blank solution in 500mL conical flasks, add distilled water to about 200mL, add 0.2g
Ascorbic acid, 5mL saturation thiourea solutions shake up（, it is titrated to yellow with EDTA standard titration solutions (0.0102mol/L) and shoals,
Plus 3-4 drop xylenol orange solution）, it is 1.5-1.7 to be adjusted with sodium acetate solution to pH value, continues to be titrated to red and is changed into glassy yellow
For terminal.The EDTA volumes of consumption are recorded, are calculated as follows:
In formula：
The actual concentrations of C-EDTA standard liquids, unit is mole every milliliter（mol/L）；
V-sample consumption EDTA volume, unit is milliliter（mL）；
V0 - blank consumes EDTA volume, and unit is milliliter（mL）；
MS The quality of-sample, unit for gram（g）；
1000-volume conversion factor；
The molal weight of 209.0-bismuth, unit is gram every mole（g/mol）；
4-point take volume multiple；
As a result such as table 4 is recorded：
Determine trace Bismuth result in the bismuth slag of table 4
4th, accuracy validation
Above-mentioned sample 0.2500g is accurately weighed, the degree of accuracy is verified using the method for mark-on reclaims, 5, recovery are the results are shown in Table
Rate meets needs.
The recovery of standard addition result of table 5
| Sample number | Measured value ω/% | Addition m/mg | Measured quantity m/mg | The rate of recovery/% |
| 2 | 30.23 | 60 | 134.23 | 97.76 |
Claims (6)
1. the detection method of bismuth in a kind of bismuth slag containing high selen-tellurjum, it is characterised in that detecting step is：
1st, by bismuth slag sample drying to be measured, crushing, weigh quantitative sample and be used as analysis sample；
2nd, analysis sample is placed in 250mL beakers, adds distilled water 5 mL wetting sample, it is some to add concentrated hydrochloric acid, nitric acid, control
Warm electric hot plate heating for dissolving is to surplus solution 5mL, while blank sample is prepared, it is also synchronous to be cleared up；
3rd, sample will be analyzed and blank sample will add anhydrous sodium sulfite, heating water bath under hydrochloric acid medium, and evaporated filtrate, increase chloric acid
Smolder, nitric acid, distilled water cool down constant volume after boiling altogether, obtain analyte sample fluid and blank solution to be measured；
4th, the configuration of EDTA standard liquids and demarcation；The configuration (0.01mol/L) of EDTA standard liquids：Weigh 3.8g top pure grades EDTA
It is placed in 500mL beakers, is dissolved in water, move into 1000mL volumetric flasks, mixes；Sodium acetate solution（200g/L）：Weigh acetic acid
Sodium 20.0g, with being transferred to constant volume in 100ml volumetric flasks after water dissolves；Tartaric acid solution（100g/L）：Tartaric acid 10.0g is weighed,
With being transferred to constant volume in 100ml volumetric flasks after water dissolves；Saturation thiourea solution：Thiocarbamide is added into a certain amount of water until thiocarbamide
Not in dissolving；Xylenol orange solution（1g/L）：Xylenol orange 0.1g is weighed, it is fixed with being transferred to after water dissolves in 100ml volumetric flasks
Hold；The demarcation of EDTA standard liquids：Weigh the pure bismuths of 0.2g（Mass fraction is more than 99.99%）, it is placed in 250mL beakers, adds
15mL nitric acid, cap upper surface ware, low-temperature heat is complete to dissolving, and removes and is cooled to room temperature, transfers the solution into 100mL volumetric flasks
In, purging surface plate and wall of cup, and it is settled to scale；Three parts of 25.00mL bismuths standard liquid is pipetted in one group of 500mL conical flask
In, 200mL is added water to, 0.2g ascorbic acid, 5ml saturations thiourea solution, 5ml tartaric acid solutions is added and shakes up, use EDTA standards
Volumetric soiutions are titrated to yellow and shoaled, plus 3-4 drop xylenol orange solution, adjusted with sodium acetate solution to pH value be 1.5-1.7. after
The continuous red that is titrated to is changed into glassy yellow for terminal；
EDTA concentration is calculated as follows out:
In formula：
The actual concentrations of C-EDTA standard liquids, unit is mole every milliliter（mol/L）
m1- point take the quality of bismuth standard liquid, unit for gram（g）；
V1The volume of EDTA standard liquids is consumed during-titration, unit is milliliter（mL）；
1000-volume conversion factor；
The molal weight of 209-bismuth, unit is unit for gram every mole（g/mol）；
And be recorded as shown in table 1：
The concentration results of the EDTA standard liquids of table 1
5th, bismuth element is determined：The analyte sample fluid and blank solution to be measured obtained using determination step 3, is obtained with reference to step 4
EDTA concentration of standard solution, titration sample solution and blank solution, according to consumption EDTA volume, and then converse bismuth slag specimen product
In bismuth content.
2. the detection method of bismuth in the bismuth slag as claimed in claim 1 containing high selen-tellurjum, it is characterised in that：In step 1, sample comminution
To 160-300 mesh, it is 0.2g to weigh analysis sample quality（4th is accurate to after decimal point）.
3. the detection method of bismuth in the bismuth slag as claimed in claim 1 containing high selen-tellurjum, it is characterised in that：Hydrochloric acid is added in step 2
Volume is 15ml, and it is 5 mL that nitric acid, which adds volume, and electric plate temperature is 200 DEG C.
4. the detection method of bismuth in the bismuth slag as claimed in claim 1 containing high selen-tellurjum, it is characterised in that：In step 2,3, hydrochloric acid,
It is pure that nitric acid, perchloric acid, anhydrous sodium sulfite are analysis.
5. the detection method of bismuth in the bismuth slag as claimed in claim 1 containing high selen-tellurjum, it is characterised in that：In step 3, concentration of hydrochloric acid
For 1+1, anhydrous sodium sulfite is 1-2g, and water-bath is 2 hours, and filtrate is evaporated to 10mL, and perchloric acid is 10mL, and nitric acid is 8mL, is steamed
Distilled water is 20mL, is settled in 100mL volumetric flasks.
6. the detection method of bismuth in the bismuth slag as claimed in claim 1 containing high selen-tellurjum, it is characterised in that：In step 5, divide and take upper strata
Clear liquid 25mL is in 500mL conical flasks, the similarly hereinafter demarcation of EDTA standard liquids；According to the EDTA volumes of consumption, it can count as the following formula
Calculate its content：
In formula：
The actual concentrations of C-EDTA standard liquids, unit is mole every milliliter（mol/L）；
V-sample consumption EDTA volume, unit is milliliter（mL）；
V0 - blank consumes EDTA volume, and unit is milliliter（mL）；
MS The quality of-sample, unit for gram（g）；
The molal weight of 209.0-bismuth, unit is gram every mole（g/mol）；
4-point take volume multiple.
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| CN112067493A (en) * | 2020-09-16 | 2020-12-11 | 百杰瑞(荆门)新材料有限公司 | Water content detection method of anhydrous lithium iodide |
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