CN105203698A - Method for directly determining aluminum content in aluminum-niobium alloy - Google Patents
Method for directly determining aluminum content in aluminum-niobium alloy Download PDFInfo
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- CN105203698A CN105203698A CN201510688893.8A CN201510688893A CN105203698A CN 105203698 A CN105203698 A CN 105203698A CN 201510688893 A CN201510688893 A CN 201510688893A CN 105203698 A CN105203698 A CN 105203698A
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Abstract
The invention relates to a method for directly determining aluminum content in aluminum-niobium alloy, and belongs to the technical field of chemical analysis and detection of hard alloy. The method comprises the following steps: dissolving a powdered aluminum-niobium alloy test sample in a sulfuric acid and nitric acid solution, adding an EDTA solution and distilled water to reduce the acidity of the solution, complexing aluminum ions and hydrolyzing niobium ions to facilitate the complete precipitation, obtaining a test solution of an Al-EDTA complex containing the niobium hydroxide precipitates, sufficiently releasing the aluminum ions, wherein the niobium hydroxide precipitates are too tiny to absorb the aluminum ions, so that the loss of the aluminum ions is reduced; and determining the aluminum ions in the mixed solution in a titration method, wherein xylenol orange in the titration method is used as an indication agent, NaF is used as a replacement agent, ZnCl2 is a standard solution for the titration, and titrating the replaced EDTA with the quantity equal to that of the aluminum. According to the method, the determination of the aluminum in the aluminum-niobium alloy is changed from an indirect difference method to a direct determination method, so that the detection accuracy is greatly improved, and a feasible method is provided for detecting the aluminum content in the niobium-aluminum alloy.
Description
Technical field
The present invention relates to the method for aluminium content in a kind of direct mensuration aluminium niobium alloy, belong to wimet chemical analysis detection technique field.
Background technology
Aluminium niobium alloy has high-melting-point, low-density feature, is widely used as adjuvant and the aerospace industry of superconductive alloy materials and biomedical devices alloy material.Because the ratio of matrix niobium and aluminium changes greatly according to concrete aluminium niobium alloy product requirement, therefore the impact of matrix group pairwise testing is very important, and the composition of aluminium and content to be smelted and extremely important in use procedure at aluminium niobium alloy.At present, for the mensuration of content of niobium in aluminium niobium alloy, most of enterprise all adopts the tannic acid hydrolysis gravimetric method of comparative maturity, and this method is consuming time longer, has a strong impact on enterprises production efficiency.And aluminum content tests method rarely has report in aluminium niobium alloy.Chemical analysis dissolution mechanism due to aluminium niobium alloy maturation is dissolved in the nitration mixture of hydrofluorite and nitric acid, solution is entered after niobium and fluorine ion (F-) and tartrate anion etc. form complex compound, and F-, tartrate anion cause very large interference to Al-single crystal, causing cannot Accurate Determining aluminium.
At present, indirect minusing is generally adopted for aluminum content tests in aluminium niobium alloy, namely content of niobium in aluminium niobium alloy is first measured, other impurity contents measured by the instruments such as recycling chemistry or inductively coupled plasma atomic emission (ICP) spectrum, then deduct content of niobium with total content and obtain aluminium content with other impurity content.This method needs to measure multiple element, and complex operation, time-consumingly to take a lot of work, and result precision is low, can not provide reliable quality foundation in time to production.
In sum, at present for the chemical detection of aluminium content in aluminium niobium alloy, under the prerequisite ensureing measurement result accuracy, the method fast that there is no directly can be followed.This has badly influenced enterprises production efficiency and profit.
Summary of the invention
For the defect existed in prior art, the object of the present invention is to provide the method for aluminium content in a kind of direct mensuration aluminium niobium alloy, described method can aluminium content directly fast, in Accurate Determining aluminium niobium alloy, and provide reliable quality foundation in time for producing.
For realizing object of the present invention, provide following technical scheme.
A method for aluminium content in direct mensuration aluminium niobium alloy, described method step is as follows:
(1) mixed with sulfuric acid solution, salpeter solution by granularity >=200 object In Powdered Aluminium niobium alloy sample, then heating is boiled and is dissolved completely to described sample, obtains liquid to be measured after cooling;
Sulfuric acid solution is the solution that analytical pure sulfuric acid and water mix with volume ratio 1:1;
Salpeter solution is the solution that the pure nitric acid of analysis and water mix with volume ratio 1:1;
Aluminium niobium alloy sample, ratio between sulfuric acid solution and salpeter solution are 0.1000g ~ 0.3000g:10mL ~ 20mL:10mL ~ 20mL;
Preferred described sample is by aluminium niobium alloy fragmentation rear mistake 200 mesh standard sieve to be determined, then adopts coning and quartering to carry out division sampling and obtains;
(2) under the continuous stirring condition of room temperature, add disodium ethylene diamine tetraacetate (EDTA) solution, be settled to 150mL ~ 200mL with water in liquid to be measured, then >=2min is boiled in heating, is cooled to room temperature, obtains solid-liquid mixed liquor 1;
EDTA solution is be the solution of 0.04mol/L ~ 0.05mol/L by the concentration that analytically pure EDTA and water configure;
The volume ratio of liquid to be measured and EDTA solution is 1:2 ~ 4;
(3) in solid-liquid mixed liquor 1, add phenolphthalein indicator 0.2mL ~ 0.4mL, shake up, under the condition constantly stirred, adding NaOH solution to there is redness, obtaining solid-liquid mixed liquor 2;
Phenolphthalein indicator is that analytically pure phenolphthalein and absolute ethyl alcohol obtain with solid-to-liquid ratio 1g:100mL configuration;
Preferred NaOH solution is the concentration of analytically pure NaOH and water preparation is the mixed solution of 200g/L;
(4) under the condition constantly stirred, with acid buret, hydrochloric acid solution is added in solid-liquid mixed liquor 2, observe redness and just disappear, and then drip hydrochloric acid solution 0.2mL ~ 0.4mL, obtain solid-liquid mixed liquor 3;
Hydrochloric acid solution is the solution that analytically pure hydrochloric acid and water mix with volume ratio 1:1;
(5) joined in solid-liquid mixed liquor 3 by acetic acid-ammonium acetate buffer solution, heating is boiled, and is cooled to room temperature, under the condition constantly stirred, adds xylenol orange indicator 0.2mL ~ 0.4mL, adds ZnCl subsequently with acid buret
2standard solution is orange red to occurring, obtains solid-liquid mixed liquor 4;
Acetic acid-ammonium acetate buffer solution is, after analytically pure ammonium acetate 7.7g, the 50mL that adds water dissolve, add and analyze pure glacial acetic acid 6mL, is settled to water the mixed solution that 100mL obtains;
Volume ratio between acetic acid-ammonium acetate buffer solution and solid-liquid mixed liquor 3 is 1 ~ 1.5:1;
ZnCl
2standard solution is analytically pure ZnCl
2be dissolved in the water the ZnCl obtained
2concentration is the solution of 0.05mol/L;
Xylenol orange indicator is analytically pure xylenol orange and water is that 0.2g:100mL configuration obtains with solid-to-liquid ratio;
(6) in solid-liquid mixed liquor 4, add NaF saturated aqueous solution, be stirred to orange red disappearance, heating is boiled, and is cooled to room temperature, adds xylenol orange indicator 0.2mL ~ 0.4mL, obtains solid-liquid mixed liquor 5;
Xylenol orange indicator is analytically pure xylenol orange and water is that 0.2g:100mL mixed configuration obtains with solid-to-liquid ratio;
(7) under the condition constantly stirred, ZnCl is dripped with acid buret
2standard solution enters in solid-liquid mixed liquor 5 orange red to occurring, minute book step adds ZnCl
2the volume of standard solution;
ZnCl
2standard solution is by analytically pure ZnCl
2be dissolved in the water the ZnCl obtained
2concentration is the solution of 0.05mol/L;
(8) blank test: granularity >=200 object In Powdered Aluminium niobium alloy sample in step (1) is removed, by sulfuric acid solution and salpeter solution mixing, then heating is boiled, and obtains liquid to be measured, all the other same step (1) ~ (7) after cooling;
(9) mass percentage (W of aluminium in described aluminium niobium alloy sample is calculated
al), adopt following formula (A):
Wherein:
V is the ZnCl that step (7) adds
2the volume of standard solution;
V
0for the ZnCl added when repeating step (7) in step (8)
2the volume of standard solution;
C is ZnCl
2the concentration of standard solution;
M is the quality of described aluminium niobium alloy sample;
M
alfor the molal weight of aluminium;
In the method for the invention, the purity >=distilled water purity of water.
Beneficial effect
1. the invention provides the method for aluminium content in a kind of direct mensuration aluminium niobium alloy, described method adopts sulfuric acid solution and salpeter solution heating for dissolving granularity>=200 object In Powdered Aluminium niobium alloy sample, allows aluminium niobium sample fully dissolve; Then add EDTA solution and distilled water, reduce solution acidity, complexing aluminium ion, niobium ion is impelled to be hydrolyzed and to precipitate completely, obtain the test solution of the Al-EDTA complex compound containing niobium hydroxide precipitation, aluminium ion is able to abundant release, and niobium hydroxide precipitation is tiny less to aluminum ions absorption, thus reduce aluminum ions loss, can directly measure aluminium ion in mixed liquor by titrimetry, be the content of aluminium in Nb-Al alloy, in described titrimetry, xylenol orange is indicator, and NaF is displacer, ZnCl
2for titration standard solution, titration is displaced the amount with the EDTA of aluminium equivalent;
2. the invention provides the method for aluminium content in a kind of direct mensuration aluminium niobium alloy, Al-single crystal in aluminium niobium alloy is measured from indirect minusing and becomes direct mensuration by described method, significantly improve detection accuracy, and provide a kind of truly feasible method for the detection of aluminium content in Nb-Al alloy;
3. the invention provides the method for aluminium content in a kind of direct mensuration aluminium niobium alloy, described method can aluminium content in Accurate Determining aluminium niobium alloy, provides reliable quality according to reference for producing.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail more.
Embodiment 1
A method for aluminium content in direct mensuration aluminium niobium alloy, described method step is as follows:
(1) fragmentation is carried out to aluminium niobium alloy to be determined, after broken, cross 200 order stainless steel standard sieves, then adopt coning and quartering to carry out division sampling, obtain granularity >=200 object In Powdered Aluminium niobium alloy sample; Precise granularity >=200 object In Powdered Aluminium niobium alloy sample 0.1000g adds in volumetric flask, measure after sulfuric acid solution 10mL and salpeter solution 10mL to add in volumetric flask mixing respectively with graduated cylinder, being placed on heating on electric furnace boils to treating that described sample dissolves completely, take out volumetric flask and naturally cool to room temperature, obtain liquid to be measured;
Sulfuric acid solution is the solution that analytically pure sulfuric acid and distilled water mix with volume ratio 1:1, and salpeter solution is the solution that analytically pure nitric acid and distilled water mix with volume ratio 1:1;
(2) under the condition constantly stirred in room temperature, add EDTA solution 80mL, and be settled to 200mL with distilled water in liquid to be measured, on electric discharge stove, 2min is boiled in heating, takes off and naturally cools to room temperature, obtain solid-liquid mixed liquor 1;
EDTA solution is be the solution of 0.04mol/L by the concentration that analytically pure EDTA and distilled water configure;
(3) in the volumetric flask being contained with solid-liquid mixed liquor 1, add phenolphthalein indicator 0.4mL, shake up, under the condition constantly stirred, be neutralized to by the NaOH solution of 200g/L and occur red, obtain solid-liquid mixed liquor 2;
Phenolphthalein indicator is the ethanolic solution analyzing pure phenolphthalein, and concentration is 1g/100mL;
(4) under the condition constantly stirred, drip hydrochloric acid solution with acid buret and enter in solid-liquid mixed liquor 2, observe redness and just disappear, and then drip hydrochloric acid solution 0.4mL, obtain solid-liquid mixed liquor 3;
Hydrochloric acid solution is the solution that analytically pure hydrochloric acid and distilled water mix with volume ratio 1:1;
(5) measuring acetic acid-ammonium acetate buffer solution 200mL with graduated cylinder joins in solid-liquid mixed liquor 3, and 2min is boiled in heating on the stove that discharges, take off and naturally cool to room temperature, under the condition constantly stirred, add 0.2mL xylenol orange indicator with dropper, add the ZnCl of 0.05mol/L subsequently with acid buret
2standard solution is orange red to occurring, obtains solid-liquid mixed liquor 4;
Acetic acid-ammonium acetate buffer solution, for after analyzing pure ammonium acetate 7.7g, adding distil water 50mL and dissolving, adds and analyzes pure glacial acetic acid 6mL, is settled to that 100mL obtains with distilled water; Xylenol orange indicator is analytically pure xylenol orange and distilled water is that 0.2g:100mL is mixed to get with solid-to-liquid ratio;
ZnCl
2standard solution is for analyzing pure ZnCl
2be dissolved in distilled water and obtain, ZnCl
2concentration is 0.05mol/L;
(6) in solid-liquid mixed liquor 4, NaF saturated aqueous solution 150mL is added, be stirred to orange red disappearance, by hold solid-liquid mixed liquor 4 volumetric flask electric discharge stove on heating boil 4min, take off the volumetric flask holding solid-liquid mixed liquor 4 and naturally cool to room temperature, drip 0.2mL xylenol orange indicator with dropper, obtain solid-liquid mixed liquor 5;
Xylenol orange indicator is analytically pure xylenol orange and distilled water is that 0.2g:100mL prepares with solid-to-liquid ratio;
(7) under the condition constantly stirred, ZnCl is dripped with acid buret
2standard solution enters in solid-liquid mixed liquor 5 orange red to occurring, minute book step adds ZnCl
2the volume of standard solution is 31.27mL;
ZnCl
2standard solution is analytically pure ZnCl
2be dissolved in distilled water and prepare, ZnCl
2concentration is 0.05mol/L;
(8) blank test: in step (1), granularity>=200 object In Powdered Aluminium niobium alloy sample is 0g, measure after sulfuric acid solution 10mL and salpeter solution 10mL to add in volumetric flask mixing respectively with graduated cylinder, be placed on heating on electric furnace to boil, take out volumetric flask and naturally cool to room temperature, obtain liquid to be measured, step adds ZnCl in (7)
2the volume of standard solution is 0.00mL, all the other same step (1) ~ (7);
(9) the quality hundred content (W of aluminium in described aluminium niobium alloy sample is calculated
al), adopt following formula (A):
Wherein:
V is the ZnCl that step (7) adds
2the volume of standard solution;
V
0for the ZnCl added when repeating step (7) in step (8)
2the volume of standard solution;
C is ZnCl
2the concentration of standard solution;
M is the quality of described aluminium niobium alloy sample;
M
alfor the molal weight of aluminium.
The present embodiment has done three parallel laboratory tests to aluminium element content in liquid to be measured, and calculating mean value is measurement result, in table 1.
Table 1 embodiment 1 measurement result
Embodiment 2
A method for aluminium content in direct mensuration aluminium niobium alloy, described method step is as follows:
(1) fragmentation is carried out to the aluminium niobium alloy that band measures, after broken, cross 200 order stainless steel standard sieves, then adopt coning and quartering to carry out division sampling, obtain granularity >=200 object In Powdered Aluminium niobium alloy sample; Precise granularity >=200 object In Powdered Aluminium niobium alloy sample 0.2000g adds in volumetric flask, measure after sulfuric acid solution 20mL and salpeter solution 20mL to add in volumetric flask mixing respectively with graduated cylinder, being placed on heating on electric furnace boils to treating that described sample dissolves completely, take out volumetric flask and naturally cool to room temperature, obtain liquid to be measured;
Sulfuric acid solution is the solution that analytical pure sulfuric acid and distilled water mix with volume ratio 1:1, and salpeter solution is the solution that the pure nitric acid of analysis and distilled water mix with volume ratio 1:1;
(2) under the condition constantly stirred in room temperature, the EDTA solution 90mL added in liquid to be measured, and be settled to 150mL with distilled water, on electric discharge stove, 3min is boiled in heating, takes off and naturally cools to room temperature, obtain solid-liquid mixed liquor 1;
EDTA solution is be the solution of 0.05mol/L by the concentration that analytically pure EDTA and distilled water configure;
(3) to being contained with the phenolphthalein indicator 0.3mL added in the volumetric flask of solid-liquid mixed liquor 1, shaking up, under the condition constantly stirred, being neutralized to by the NaOH solution of 200g/L and occurring redness, obtaining solid-liquid mixed liquor 2;
Phenolphthalein indicator is the ethanolic solution analyzing pure phenolphthalein, and concentration is 1g/100mL;
(4) under the condition constantly stirred, drip hydrochloric acid solution with acid buret and enter in solid-liquid mixed liquor 2, observe redness and just disappear, and then drip hydrochloric acid solution 0.3mL, obtain solid-liquid mixed liquor 3;
Hydrochloric acid solution is the solution that analysis pure hydrochloric acid and distilled water mix with volume ratio 1:1;
(5) measuring acetic acid-ammonium acetate buffer solution 200mL with graduated cylinder joins in solid-liquid mixed liquor 3, and 3min is boiled in heating on the stove that discharges, take off and naturally cool to room temperature, under the condition constantly stirred, add 0.3mL xylenol orange indicator with dropper, add the ZnCl of 0.05mol/L subsequently with acid buret
2standard solution is orange red to occurring, obtains solid-liquid mixed liquor 4;
Acetic acid-ammonium acetate buffer solution is for after analysis pure ammonium acetate 7.7g, adding distil water 50mL dissolving, and add and analyze pure glacial acetic acid 6mL, being settled to 100mL with distilled water obtains; Xylenol orange indicator is the pure xylenol orange of analysis and distilled water is that 0.2g:100mL configuration obtains with solid-to-liquid ratio; ZnCl
2standard solution is for analyzing pure ZnCl
2be dissolved in distilled water and obtain, concentration is 0.05mol/L;
(6) in solid-liquid mixed liquor 4, NaF saturated aqueous solution 95mL is added, be stirred to orange red disappearance, by hold solid-liquid mixed liquor 4 volumetric flask electric discharge stove on heating boil 2min, take off the volumetric flask holding solid-liquid mixed liquor 4 and naturally cool to room temperature, drip 0.3mL xylenol orange indicator with dropper, obtain solid-liquid mixed liquor 5;
Xylenol orange indicator is the pure xylenol orange of analysis and distilled water is that 0.2g:100mL configuration obtains with solid-to-liquid ratio;
(7) under the condition constantly stirred, the ZnCl of 0.05mol/L is dripped with acid buret
2standard solution enters in solid-liquid mixed liquor 5 orange red to occurring, minute book step adds ZnCl
2the volume of standard solution is 62.54mL;
ZnCl
2standard solution is analytically pure ZnCl
2be dissolved in distilled water and obtain, concentration is 0.05mol/L;
(8) blank test: in step (1), granularity>=200 object In Powdered Aluminium niobium alloy sample is 0g, measure after sulfuric acid solution 20mL and salpeter solution 20mL to add in volumetric flask mixing respectively with graduated cylinder, be placed on heating on electric furnace to boil, take out volumetric flask and naturally cool to room temperature, obtain liquid to be measured, step adds ZnCl in (7)
2the volume of standard solution is 0.00mL, all the other same step (1) ~ (7);
(9) the quality hundred content (W of aluminium in described aluminium niobium alloy sample is calculated
al), adopt following formula (A):
Wherein:
V is the ZnCl that step (7) adds
2the volume of standard solution;
V
0for the ZnCl added when repeating step (7) in step (8)
2the volume of standard solution;
C is ZnCl
2the concentration of standard solution;
M is the quality of described aluminium niobium alloy sample;
M
alfor the molal weight of aluminium.
The present embodiment has done three parallel laboratory tests to aluminium element content in liquid to be measured, and calculating mean value is measurement result, in table 2.
Table 2 embodiment 2 measurement result
Embodiment 3
A method for aluminium content in direct mensuration aluminium niobium alloy, described method step is as follows:
(1) fragmentation is carried out to the aluminium niobium alloy that band measures, after broken, cross 200 order stainless steel standard sieves, then adopt coning and quartering to carry out division sampling, obtain granularity >=200 object In Powdered Aluminium niobium alloy sample; Precise granularity >=200 object In Powdered Aluminium niobium alloy sample 0.3000g adds in volumetric flask, measure after sulfuric acid solution 20mL and salpeter solution 20mL to add in volumetric flask mixing respectively with graduated cylinder, being placed on heating on electric furnace boils to treating that described sample dissolves completely, take out volumetric flask and naturally cool to room temperature, obtain liquid to be measured;
Sulfuric acid solution is the solution that analytical pure sulfuric acid and distilled water mix with volume ratio 1:1, and salpeter solution is the solution that the pure nitric acid of analysis and distilled water mix with volume ratio 1:1;
(2) under the condition constantly stirred in room temperature, add EDTA solution 100mL, and be settled to 150mL with distilled water in liquid to be measured, on electric discharge stove, 4min is boiled in heating, takes off and naturally cools to room temperature, obtain solid-liquid mixed liquor 1;
EDTA solution is be the solution of 0.05mol/L by the concentration that analytically pure EDTA and distilled water configure;
(3) in the volumetric flask being contained with solid-liquid mixed liquor 1, add phenolphthalein indicator 0.2mL, shake up, under the condition constantly stirred, be neutralized to by the NaOH solution of 200g/L and occur red, obtain solid-liquid mixed liquor 2;
Phenolphthalein indicator is the ethanolic solution analyzing pure phenolphthalein, and concentration is 1g/100mL;
(4) under the condition constantly stirred, drip hydrochloric acid solution with acid buret and enter in solid-liquid mixed liquor 2, observe redness and just disappear, and then drip hydrochloric acid solution 0.2mL, obtain solid-liquid mixed liquor 3;
Hydrochloric acid solution is the solution that analysis pure hydrochloric acid and distilled water mix with volume ratio 1:1;
(5) measuring acetic acid-ammonium acetate buffer solution 150mL with graduated cylinder joins in solid-liquid mixed liquor 3, and 4min is boiled in heating on the stove that discharges, take off and naturally cool to room temperature, under the condition constantly stirred, add 0.2mL xylenol orange indicator with dropper, add the ZnCl of 0.05mol/L subsequently with acid buret
2standard solution is orange red to occurring, obtains solid-liquid mixed liquor 4;
Acetic acid-ammonium acetate buffer solution is for after analysis pure ammonium acetate 7.7g, adding distil water 50mL dissolving, and add and analyze pure glacial acetic acid 6mL, being settled to 100mL with distilled water obtains; Xylenol orange indicator is the pure xylenol orange of analysis and distilled water is that 0.2g:100mL prepares with solid-to-liquid ratio; ZnCl
2standard solution is for analyzing pure ZnCl
2be dissolved in distilled water and obtain, concentration is 0.05mol/L;
(6) in solid-liquid mixed liquor 4, NaF saturated aqueous solution 100mL is added, be stirred to orange red disappearance, by hold solid-liquid mixed liquor 4 volumetric flask electric discharge stove on heating boil 2min, take off the volumetric flask holding solid-liquid mixed liquor 4 and naturally cool to room temperature, drip 0.2mL xylenol orange indicator with dropper, obtain solid-liquid mixed liquor 5;
Xylenol orange indicator is the pure xylenol orange of analysis and distilled water is that 0.2g:100mL obtains with solid-to-liquid ratio;
(7) under the condition constantly stirred, the ZnCl of 0.05mol/L is dripped with acid buret
2standard solution enters in solid-liquid mixed liquor 5 orange red to occurring, minute book step adds ZnCl
2the volume of standard solution is 98.65mL;
ZnCl
2standard solution is for analyzing pure ZnCl
2be dissolved in distilled water and obtain, concentration is 0.05mol/L;
(8) blank test: in step (1), granularity>=200 object In Powdered Aluminium niobium alloy sample is 0g, measure after sulfuric acid solution 20mL and salpeter solution 20mL to add in volumetric flask mixing respectively with graduated cylinder, be placed on heating on electric furnace to boil, take out volumetric flask and naturally cool to room temperature, obtain liquid to be measured, step adds ZnCl in (7)
2the volume of standard solution is 0.00mL, all the other same step (1) ~ (7);
(9) the quality hundred content (W of aluminium in described aluminium niobium alloy sample is calculated
al), adopt following formula (A):
Wherein:
V is the ZnCl that step (7) adds
2the volume of standard solution;
V
0for the ZnCl added when repeating step (7) in step (8)
2the volume of standard solution;
C is ZnCl
2the concentration of standard solution;
M is the quality of described aluminium niobium alloy sample;
M
alfor the molal weight of aluminium.
The present embodiment has done three parallel laboratory tests to aluminium element content in liquid to be measured, and calculating mean value is measurement result, in table 3.
Table 3 embodiment 3 measurement result
Embodiment 4
Adopt recovery of standard addition experiment to determine the accuracy of the method for aluminium content in a kind of direct mensuration aluminium niobium alloy of the present invention, step is as follows:
(1) Nb-Al alloy being 42.20wt% by known aluminium content carries out fragmentation, crosses 200 order stainless steel standard sieves after broken, then adopts coning and quartering to carry out division sampling, obtains granularity >=200 object In Powdered Aluminium niobium alloy sample;
(2) sample 0.1000g described in precise adds in three volumetric flasks respectively, aluminium powder standard substance 0.1000g, 0.1500g and 0.2000g of precise aluminium content >=99.8wt% add and fill in three volumetric flasks of sample 0.1000g respectively, measure sulfuric acid solution 20mL and salpeter solution 20mL tri-parts respectively with graduated cylinder to add respectively in three volumetric flasks and obtain solid-liquid mixed solution, respectively described three volumetric flasks being placed on heating on electric furnace boils to treating that described sample dissolves completely, naturally cool to room temperature, obtain liquid to be measured;
Described sulfuric acid solution is the solution that analytical pure sulfuric acid and distilled water mix with volume ratio 1:1, and salpeter solution is the solution that the pure nitric acid of analysis and distilled water mix with volume ratio 1:1;
(3) measure aluminium content according to embodiment 1 step (2) to step (9), measurement result is in table 4.
Table 4 measurement result
Known by table 4 data: the recovery, at 100.00wt% ~ 100.07wt%, illustrates the inventive method accurately and reliably thus.
The above, be only section Example of the present invention, be not intended to limit protection scope of the present invention.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (3)
1. directly measure a method for aluminium content in aluminium niobium alloy, it is characterized in that: described method step is as follows:
(1) mixed with sulfuric acid solution, salpeter solution by granularity >=200 object In Powdered Aluminium niobium alloy sample, then heating is boiled and is dissolved completely to described sample, obtains liquid to be measured after cooling;
Sulfuric acid solution is the solution that analytical pure sulfuric acid and water mix with volume ratio 1:1;
Salpeter solution is the solution that the pure nitric acid of analysis and water mix with volume ratio 1:1;
Aluminium niobium alloy sample, ratio between sulfuric acid solution and salpeter solution are 0.1000g ~ 0.3000g:10mL ~ 20mL:10mL ~ 20mL;
(2) under the continuous stirring condition of room temperature, add EDTA solution, be settled to 150mL ~ 200mL with water in liquid to be measured, then >=2min is boiled in heating, is cooled to room temperature, obtains solid-liquid mixed liquor 1;
EDTA solution is be the solution of 0.04mol/L ~ 0.05mol/L by the concentration that analytically pure EDTA and water configure;
The volume ratio of liquid to be measured and EDTA solution is 1:2 ~ 4;
(3) in solid-liquid mixed liquor 1, add phenolphthalein indicator 0.2mL ~ 0.4mL, shake up, under the condition constantly stirred, adding NaOH solution to there is redness, obtaining solid-liquid mixed liquor 2;
Phenolphthalein indicator is that analytically pure phenolphthalein and absolute ethyl alcohol obtain with solid-to-liquid ratio 1g:100mL configuration;
(4) under the condition constantly stirred, with acid buret, hydrochloric acid solution is added in solid-liquid mixed liquor 2, observe redness and just disappear, and then drip hydrochloric acid solution 0.2mL ~ 0.4mL, obtain solid-liquid mixed liquor 3;
Hydrochloric acid solution is the solution that analytically pure hydrochloric acid and water mix with volume ratio 1:1;
(5) joined in solid-liquid mixed liquor 3 by acetic acid-ammonium acetate buffer solution, heating is boiled, and is cooled to room temperature, under the condition constantly stirred, adds xylenol orange indicator 0.2mL ~ 0.4mL, adds ZnCl subsequently with acid buret
2standard solution is orange red to occurring, obtains solid-liquid mixed liquor 4;
Acetic acid-ammonium acetate buffer solution is, after analytically pure ammonium acetate 7.7g, the 50mL that adds water dissolve, add and analyze pure glacial acetic acid 6mL, is settled to water the mixed solution that 100mL obtains;
Volume ratio between acetic acid-ammonium acetate buffer solution and solid-liquid mixed liquor 3 is 1 ~ 1.5:1;
(6) in solid-liquid mixed liquor 4, add NaF saturated aqueous solution, be stirred to orange red disappearance, heating is boiled, and is cooled to room temperature, adds xylenol orange indicator 0.2mL ~ 0.4mL, obtains solid-liquid mixed liquor 5;
(7) under the condition constantly stirred, ZnCl is dripped with acid buret
2standard solution enters in solid-liquid mixed liquor 5 orange red to occurring, minute book step adds ZnCl
2the volume of standard solution;
(8) blank test: granularity >=200 object In Powdered Aluminium niobium alloy sample in step (1) is removed, by sulfuric acid solution and salpeter solution mixing, then heating is boiled, and obtains liquid to be measured, all the other same step (1) ~ (7) after cooling;
(9) mass percentage (W of aluminium in described aluminium niobium alloy sample is calculated
al), adopt following formula (A):
Wherein:
V is the ZnCl that step (7) adds
2the volume of standard solution;
V
0for the ZnCl added when repeating step (7) in step (8)
2the volume of standard solution;
C is ZnCl
2the concentration of standard solution;
M is the quality of described aluminium niobium alloy sample;
M
alfor the molal weight of aluminium;
In step (1) ~ (6), the purity >=distilled water purity of water;
Xylenol orange indicator in step (5) and (6) is analytically pure xylenol orange and water is that 0.2g:100mL configuration obtains with solid-to-liquid ratio;
ZnCl in step (5) and (7)
2standard solution is analytically pure ZnCl
2be dissolved in the water the ZnCl obtained
2concentration is the solution of 0.05mol/L.
2. the method for aluminium content in a kind of direct mensuration aluminium niobium alloy according to claim 1, it is characterized in that: sample described in step (1) is by aluminium niobium alloy fragmentation rear mistake 200 mesh standard sieve to be determined, then adopt coning and quartering to carry out division sampling and obtain.
3. the method for aluminium content in a kind of direct mensuration aluminium niobium alloy according to claim 1 and 2, is characterized in that: in step (3), NaOH solution is the concentration of analytically pure NaOH and water preparation is the mixed solution of 200g/L.
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| CN108918754A (en) * | 2018-07-11 | 2018-11-30 | 中国科学院青海盐湖研究所 | Aluminum content tests method in aluminium lithium alloy |
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| CN110057967A (en) * | 2019-05-27 | 2019-07-26 | 南通海星电子股份有限公司 | Aluminum ions quantitative detecting method in a kind of aluminum electric pole foil corrosive liquid |
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