CN107449854A - A kind of analysis method of aluminium in strong base titration measuring vanadium iron - Google Patents
A kind of analysis method of aluminium in strong base titration measuring vanadium iron Download PDFInfo
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Abstract
The invention discloses a kind of analysis method of the aluminium in strong base titration measuring vanadium iron, and sample to be tested is dissolved with acid, sodium oxide molybdena is hydrogenated with, makes aluminium and Separation of interferential elements, by the solution constant volume containing aluminium element after dissolving, divides and takes the solution after the constant volume of part；Solution after constant volume obtained by second step is adjusted into pH value to 45, then adds excessive disodium ethylene diamine tetraacetate standard liquid, aluminium element contained in the solution after constant volume is coordinated completely with disodium ethylene diamine tetraacetate standard liquid；4th step, again with 1（2 pyridylazos）2 naphthols are indicator, and the solution after titrating in the 3rd step coordination completely with copper sulphate standard liquid is in aubergine being just terminal；According to the addition of various materials in above-mentioned steps, the mass percent of aluminium can be calculated according to the following equation.The analysis method of the present invention can realize the quick inspection and analysis of the aluminium element in vanadium iron.
Description
Technical field
The present invention relates to the measure analysis method field of measure Aluminum in Alloy element, more particularly to a kind of titration of strong base
The analysis method of aluminium in method measure vanadium iron.
Background technology
Vanadium iron is a kind of additive in STEELMAKING PRODUCTION, and aluminium is must to survey one of element.National standard uses chromium day at present
Blue or green S AASs and disodium ethylene diamine tetraacetate（EDTA）Titration, this two methods operation it is cumbersome, analysis time compared with
Long, operation employee is not easy to grasp.What the aluminium in measure vanadium iron was currently mainly used is Chrome azurol s colorimetry and second two
Amine tetraacethyl disodium（EDTA）Titration, simply introduce above two method：
First, Chrome azurol s colorimetry：Sample decomposes through acid, filtering, retains filtrate, after precipitation carries out residue calcination processing, with
Filtrate merges, then is extracted, acid treated, and in the presence of hydroxylamine hydrochloride, pH value, aluminium and chromium are adjusted with hexamethylenetetramine
Reddish black S forms colored complex, and in measuring its dullness on spectrophotometer at 550nm wavelength, aluminium is checked on calibration curve
Quality, the content of aluminium in sample is calculated.
2nd, disodium ethylene diamine tetraacetate（EDTA）Titration：Sample nitric acid, hydrochloric acid decompose, filtering, and retain filtrate,
After precipitation carries out residue calcination processing, merge with filtrate, then carry out precipitation separation, under certain acidity, add excessive second two
Amine tetraacethyl disodium（EDTA）Standard liquid, with 1-（2-pyridylazo）- 2-naphthols（PAN）Indicator, with copper sulphate mark
The titration of quasi- solution, according to the consumption of standard titration solution, the content of aluminium in sample is calculated.
The deficiencies in the prior art：Above two method analysis measurement narrow range, analysis time is longer, and operation is cumbersome to be not easy
Grasped.Therefore, it is necessary to design a kind of analysis method of the aluminium in strong base titration measuring vanadium iron.
The content of the invention
The defects of it is an object of the invention to overcome in the prior art, there is provided a kind of strong base titration measuring vanadium iron closes
The analysis method of aluminium in gold.
The present invention is realized by following proposal：
A kind of analysis method of aluminium in strong base titration measuring vanadium iron, this method comprise the following steps：
The first step, sample to be tested is dissolved with acid, sodium oxide molybdena is hydrogenated with, makes aluminium and Separation of interferential elements；
Second step, by the solution constant volume containing aluminium element after dissolving, divide and take the solution after the constant volume of part；
Then plus excessive ethylenediamine tetra-acetic acid two 3rd step, the solution after the constant volume obtained by second step adjusted into pH value to 4-5,
Sodium standard solution, aluminium element contained in the solution after constant volume is set to be coordinated completely with disodium ethylene diamine tetraacetate standard liquid；
4th step, again with 1-（2- pyridylazos）- beta naphthal is indicator, is titrated with copper sulphate standard liquid in the 3rd step completely
Solution after coordination is in aubergine being just terminal；
According to the addition of various materials in above-mentioned steps, the mass percent of aluminium can be calculated according to the following equation：
In formula：The mass percent of-aluminium；
C-copper sulphate concentration of standard solution, mol/L；
V1- disodium ethylene diamine tetraacetate standard liquid the volume added, ml；
V2The copper sulphate standard liquid volume of-titration consumption, ml；
The quality of m-sample to be tested, g；
The molal weight of 26.98-aluminium, g/mol.
In the first step, the acid includes hydrochloric acid and nitric acid.
The interference element includes the vanadium and iron in sample.
Beneficial effects of the present invention are：
The analysis method accuracy of aluminium in a kind of strong base titration measuring vanadium iron of the present invention is high, simple to operate, point
The analysis time is short, and measurement range is wide, it is possible to achieve the quick inspection of the aluminium element in vanadium iron and analysis.
Embodiment
The present invention is further described below：
A kind of analysis method of aluminium in strong base titration measuring vanadium iron, this method comprise the following steps：
The first step, sample to be tested is dissolved with acid, sodium oxide molybdena is hydrogenated with, makes aluminium and Separation of interferential elements；It is described acid include hydrochloric acid and
Nitric acid.The interference element includes the vanadium and iron in sample.
Second step, by the solution constant volume containing aluminium element after dissolving, divide and take the solution after the constant volume of part；
Then plus excessive ethylenediamine tetra-acetic acid two 3rd step, the solution after the constant volume obtained by second step adjusted into pH value to 4-5,
Sodium standard solution, aluminium element contained in the solution after constant volume is set to be coordinated completely with disodium ethylene diamine tetraacetate standard liquid；
4th step, again with 1-（2- pyridylazos）- beta naphthal is indicator, is titrated with copper sulphate standard liquid in the 3rd step completely
Solution after coordination is in aubergine being just terminal；
According to the addition of various materials in above-mentioned steps, the mass percent of aluminium can be calculated according to the following equation：
In formula：The mass percent of-aluminium；
C-copper sulphate concentration of standard solution, mol/L；
V1- disodium ethylene diamine tetraacetate standard liquid the volume added, ml；
V2The copper sulphate standard liquid volume of-titration consumption, ml；
The quality of m-sample to be tested, g；
The molal weight of 26.98-aluminium, g/mol.
The concentration and preparation method of the disodium ethylene diamine tetraacetate standard liquid of the present invention are known technology, here, no longer
Repeat.
Technical scheme is further elaborated with reference to three specific embodiments.
Embodiment 1
The present embodiment analysis vanadium iron standard sample YSBC18681-08 (18608) aluminium content is 0.158%, is comprised the following steps that：
1. weighing 0.5000 ± 0.0001g samples in 300ml beakers, add distilled water 30ml, it is 1.19g/ to add 100ml density
Ml hydrochloric acid and the hydrochloric acid 25ml that mixing is diluted in 100ml distilled water, it is 1.38g/ml nitric acid and 100ml to add 100ml density
The nitric acid 30ml that distilled water diluting mixes.
2. being heated to fluidized state using 180-250 DEG C of electric furnace, kept for 12 minutes, it is 1.19g/ to add 100ml density
Ml hydrochloric acid and the hydrochloric acid 20ml that mixing is diluted in 100ml distilled water, after sample is completely dissolved, reheats 30 seconds, add 50ml to distill
Water is kept for 1-2 minutes to fluidized state, and cooling 2-4 minutes are removed from electric furnace.
3. add the barium chloride solution 10ml that mixing is diluted in 25g barium chlorides and 100ml distilled water in above-mentioned solution, manually
After shaking up, the sodium hydroxide solution 60ml that 500g sodium hydroxides mix with 1000ml distilled water dilutings is added within the 5-10 seconds, extremely
Brown hydroxide sediment occurs.
4. being placed on electric furnace is heated to fluidized state, and is kept for 2 minutes, pours into 250ml volumetric flasks, be cooled to room temperature, add
Enter to distill water management in 250ml graduation mark positions, cover bottle stopper, mixing 50-100 times of turning upside down.
5. after obvious layering occurs in brown hydroxide sediment, filtered to dry in 200ml with fast quantification Filter Paper Dry and held
Measuring bottle, 100ml is drawn from 200ml drying capacity bottles in 500ml drying conical flasks.
6. the phenolphthalein indicator 1-2 drops that 0.10g phenolphthalein mixes with the dilution of 100ml absolute ethyl alcohols are added to add in above-mentioned solution
It is 1.19g/ml hydrochloric acid to enter 7ml density, then to be 1.19g/ml hydrochloric acid mix with dilution in 100ml distilled water with 100ml density
Hydrochloric acid be neutralized to it is colourless, cross plus 100ml density be 1.19g/ml hydrochloric acid dripped with diluting the hydrochloric acid 2 of mixing in 100ml distilled water.
7. in above-mentioned solution add 10ml disodium ethylene diamine tetraacetate standard liquids, add 50g anhydrous sodium acetates,
The mixed solution, in beaker, after being completely dissolved, is poured into 1000ml volumetric flasks and adds distillation water management by 60ml acetic acid with distilled water
In 1000ml graduation mark positions, mixed solution 20ml is drawn.
8. heating the solution to fluidized state, and kept for 2-3 minutes, removed, placed cooling control temperature and be higher than 80
DEG C, add 1-（2- pyridylazos）- beta naphthal metal indicator（PAN）8 drops, it is titrated to just in purple with copper sulphate standard liquid
Red is terminal.
9. according to above-mentioned addition, the mass percent of aluminium can be calculated according to above-mentioned formula.
Determine the difference that analysis result is as shown in table 1 below, and table 2 allows for national standard in aluminium element assay.
Vanadium iron standard sample analysis measurement value in the embodiment 1 of table 1
The national standard tolerance of table 2
| Aluminium content（Mass fraction） | Tolerance |
| 0.50~0.80 | 0.05 |
| ＞ 0.80~1.50 | 0.07 |
| ＞ 1.50~2.50 | 0.10 |
| ＞ 2.50~3.50 | 0.12 |
Standard value using this method analysis vanadium iron standard sample complies with the national standard requirements with measured value absolute error（Related state
Tolerance as defined in family's standard refers to table 2）.
Embodiment 2
The vanadium iron standard sample ZBT377 aluminium contents of the present embodiment analysis are 1.33%, are comprised the following steps that：
1. weighing 0.2500 ± 0.0001g samples in 300ml beakers, add distilled water 30ml, it is 1.19g/ to add 100ml density
Ml hydrochloric acid and the hydrochloric acid 20ml that mixing is diluted in 100ml distilled water, it is 1.38g/ml nitric acid and 100ml to add 100ml density
The nitric acid 25ml that distilled water diluting mixes.
2. being heated to fluidized state using 180-250 DEG C of electric furnace, kept for 10 minutes, it is 1.19g/ to add 100ml density
Ml hydrochloric acid and the hydrochloric acid 15ml that mixing is diluted in 100ml distilled water, after sample is completely dissolved, reheats 30 seconds, add 50ml to distill
Water is kept for 1-2 minutes to fluidized state, and cooling 2-4 minutes are removed from electric furnace.
3. add the barium chloride solution 10ml that mixing is diluted in 25g barium chlorides and 100ml distilled water in above-mentioned solution, manually
After shaking up, the sodium hydroxide solution 55ml that 500g sodium hydroxides mix with 1000ml distilled water dilutings is added within the 5-10 seconds, extremely
Brown hydroxide sediment occurs.
4. being placed on electric furnace is heated to fluidized state, and is kept for 1.5 minutes, pours into 250ml volumetric flasks, be cooled to room temperature,
Distillation water management is added in 250ml graduation mark positions, covers bottle stopper, mixing 50-100 times of turning upside down.
5. after obvious layering occurs in brown hydroxide sediment, filtered to dry in 200ml with fast quantification Filter Paper Dry and held
Measuring bottle, 100ml is drawn from 200ml drying capacity bottles in 500ml drying conical flasks.
6. the phenolphthalein indicator 1-2 drops that 0.10g phenolphthalein mixes with the dilution of 100ml absolute ethyl alcohols are added to add in above-mentioned solution
It is 1.19g/ml hydrochloric acid to enter 6ml density, then to be 1.19g/ml hydrochloric acid mix with dilution in 100ml distilled water with 100ml density
Hydrochloric acid be neutralized to it is colourless, cross plus 100ml density be 1.19g/ml hydrochloric acid dripped with diluting the hydrochloric acid 2 of mixing in 100ml distilled water.
7. in above-mentioned solution add 15ml disodium ethylene diamine tetraacetate standard liquids, add 50g anhydrous sodium acetates,
The mixed solution, in beaker, after being completely dissolved, is poured into 1000ml volumetric flasks and adds distillation water management by 60ml acetic acid with distilled water
In 1000ml graduation mark positions, mixed solution 20ml is drawn.
8. heating the solution to fluidized state, and kept for 2-3 minutes, removed, placed cooling control temperature and be higher than 80
DEG C, addition 1-（2-pyridylazo）- 2-naphthols（PAN）Metal indicator 9 drips, and is titrated to just with copper sulphate standard liquid
It is terminal in aubergine.
9. according to above-mentioned addition, the mass percent of aluminium can be calculated according to above-mentioned formula.
It is as shown in table 3 that analysis result is determined in the present embodiment：
Vanadium iron standard sample analysis measurement value in the embodiment 2 of table 3
Standard value using this method analysis vanadium iron standard sample complies with the national standard requirements with measured value absolute error（Related state
Tolerance as defined in family's standard refers to table 2）.
Embodiment 3
The vanadium iron standard sample ZBT376 aluminium contents analyzed in the present embodiment are 6.03%, are comprised the following steps that：
1. weighing 0.2500 ± 0.0001g samples in 300ml beakers, add distilled water 30ml, it is 1.19g/ to add 100ml density
Ml hydrochloric acid and the hydrochloric acid 25ml that mixing is diluted in 100ml distilled water, it is 1.38g/ml nitric acid and 100ml to add 100ml density
The nitric acid 30ml that distilled water diluting mixes.
2. being heated to fluidized state using 180-250 DEG C of electric furnace, kept for 12 minutes, it is 1.19g/ to add 100ml density
Ml hydrochloric acid and the hydrochloric acid 20ml that mixing is diluted in 100ml distilled water, after sample is completely dissolved, reheats 30 seconds, add 50ml to distill
Water is kept for 1-2 minutes to fluidized state, and cooling 2-4 minutes are removed from electric furnace.
3. add 25g barium chlorides to be dissolved in the barium chloride solution 10ml for diluting mixing in 100ml distilled water in above-mentioned solution,
After shaking up manually, the sodium hydroxide solution that 500g sodium hydroxides mix with 1000ml distilled water dilutings is added within the 5-10 seconds
50ml, occur to brown hydroxide sediment.
4. being placed on electric furnace is heated to fluidized state, and is kept for 1 minute, pours into 250ml volumetric flasks, be cooled to room temperature, add
Enter to distill water management in 250ml graduation mark positions, cover bottle stopper, mixing 50-100 times of turning upside down.
5. after obvious layering occurs in brown hydroxide sediment, filtered to dry in 200ml with fast quantification Filter Paper Dry and held
Measuring bottle, 100ml is drawn from 200ml drying capacity bottles in 500ml drying conical flasks.
6. the phenolphthalein indicator 1-2 drops that 0.10g phenolphthalein mixes with the dilution of 100ml absolute ethyl alcohols are added to add in above-mentioned solution
It is 1.19g/ml hydrochloric acid to enter 5ml density, then to be 1.19g/ml hydrochloric acid mix with dilution in 100ml distilled water with 100ml density
Hydrochloric acid be neutralized to it is colourless, cross plus 100ml density be 1.19g/ml hydrochloric acid dripped with diluting the hydrochloric acid 2 of mixing in 100ml distilled water.
7. in above-mentioned solution add 20ml disodium ethylene diamine tetraacetate standard liquids, add 50g anhydrous sodium acetates,
The mixed solution, in beaker, after being completely dissolved, is poured into 1000ml volumetric flasks and adds distillation water management by 60ml acetic acid with distilled water
In 1000ml graduation mark positions, mixed solution 20ml is drawn.
8. heating the solution to fluidized state, and kept for 2-3 minutes, removed, placed cooling control temperature and be higher than 80
DEG C, addition 1-（2-pyridylazo）- 2-naphthols（PAN）Metal indicator 10 drips, and is titrated to just with copper sulphate standard liquid
It is well terminal in aubergine.
9. according to above-mentioned addition, the mass percent of aluminium can be calculated according to above-mentioned formula.
The measure analysis result of the present embodiment is as shown in table 4：
Vanadium iron standard sample analysis measurement value in the embodiment 3 of table 4
Standard value using this method analysis vanadium iron standard sample complies with the national standard requirements with measured value absolute error（Related state
Tolerance as defined in family's standard refers to table 2）.
By vanadium iron standard sample YSBC18681-08 (18608), ZBT377, ZBT376 respectively according to embodiment 1, reality
Apply example 2, the method and steps METHOD FOR CONTINUOUS DETERMINATION of embodiment 3 10 times, by statistical disposition, calculate average value, the standard of aluminium content
Deviation and relative deviation result (being shown in Table 5), meet requirements of the national standard.
Average value, standard deviation and the relative deviation of the vanadium iron standard sample aluminium content of table 5
| Standard sample is numbered | Al standard contents（%） | Average value（%） | Standard deviation（%） | Relative standard deviation（%） |
| YSBC18681-08(18608)（Embodiment 1） | 0.158 | 0.159 | 0.004894 | 3.0741 |
| ZBT377（Embodiment 2） | 1.33 | 1.32 | 0.031358 | 2.3846 |
| ZBT376（Embodiment 3） | 6.03 | 6.00 | 0.062325 | 1.0391 |
The analysis method accuracy of the present invention is high, and simple to operate, analysis time is short, and measurement range is wide, it is possible to achieve vanadium iron
In aluminium quick inspection with analysis.
Although more detailed elaboration is done to technical scheme and has been enumerated, it will be appreciated that for ability
For field technique personnel, modification is made to above-described embodiment or uses equivalent alternative solution, this is to those skilled in the art
It is it is clear that these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to the present invention for member
Claimed scope.
Claims (3)
- A kind of 1. analysis method of the aluminium in strong base titration measuring vanadium iron, it is characterised in that this method include with Lower step：The first step, sample to be tested is dissolved with acid, sodium oxide molybdena is hydrogenated with, makes aluminium and Separation of interferential elements；Second step, by the solution constant volume containing aluminium element after dissolving, divide and take the solution after the constant volume of part；Then plus excessive ethylenediamine tetra-acetic acid two 3rd step, the solution after the constant volume obtained by second step adjusted into pH value to 4-5, Sodium standard solution, aluminium element contained in the solution after constant volume is set to be coordinated completely with disodium ethylene diamine tetraacetate standard liquid；4th step, again with 1-（2- pyridylazos）- beta naphthal is indicator, is titrated with copper sulphate standard liquid in the 3rd step completely Solution after coordination is in aubergine being just terminal；According to the addition of various materials in above-mentioned steps, the mass percent of aluminium can be calculated according to the following equation：In formula：The mass percent of-aluminium；C-copper sulphate concentration of standard solution, mol/L；V1- disodium ethylene diamine tetraacetate standard liquid the volume added, ml；V2The copper sulphate standard liquid volume of-titration consumption, ml；The quality of m-sample to be tested, g；The molal weight of 26.98-aluminium, g/mol.
- 2. the analysis method of the aluminium in a kind of strong base titration measuring vanadium iron according to claim 1, it is special Sign is：In the first step, the acid includes hydrochloric acid and nitric acid.
- 3. the analysis method of the aluminium in a kind of strong base titration measuring vanadium iron according to claim 1, it is special Sign is：The interference element includes the vanadium and iron in sample.
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Cited By (2)
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| CN109596407A (en) * | 2018-11-05 | 2019-04-09 | 包头钢铁（集团）有限责任公司 | A method of aluminium content in measurement molten iron slag gathering agent |
| CN114563528A (en) * | 2022-03-21 | 2022-05-31 | 包头钢铁（集团）有限责任公司 | Method for determining aluminum in high-aluminum high-manganese alloy steel |
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| CN109596407A (en) * | 2018-11-05 | 2019-04-09 | 包头钢铁（集团）有限责任公司 | A method of aluminium content in measurement molten iron slag gathering agent |
| CN114563528A (en) * | 2022-03-21 | 2022-05-31 | 包头钢铁（集团）有限责任公司 | Method for determining aluminum in high-aluminum high-manganese alloy steel |
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