CN104655517A - Measurement method of content of molybdenum in Mo-Al alloy - Google Patents
Measurement method of content of molybdenum in Mo-Al alloy Download PDFInfo
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Abstract
The invention relates to a measurement method of the content of molybdenum in an Mo-Al alloy, which comprises following steps: (1) weighing 0.15-0.25 g of a to-be-test Mo-Al alloy as a test sample, adding 30 ml of nitric acid to complete dissolve the test sample, and adding 5 ml of hydrochloric acid and boiling the solution; (2) adding 60 ml water and 15-45 ml of an EDTA solution being 50 g/L in concentration to the boiled solution, adjusting the pH value of the solution to 5-6 by ammonia water, adding an ammonium acetate-acetic acid buffer solution, diluting the solution to 250-350 ml by water and heating the solution; (3) adding dropwisely a 20g/L lead acetate solution to the boiled solution until precipitation occurs, adding dropwisely 50 ml of the 20g/L lead acetate solution, and boiling the solution and allowing the boiled solution to stand; (4) filtering the solution being allowed to stand, washing the precipitation with a hot ammonia nitrate solution with the concentration being 50 g/L; and (5) treating the precipitation and calculating the content of molybdenum. The measurement method can simply, quickly and accurately measure the content of molybdenum in the Mo-Al alloy and is wide in application range.
Description
Technical field
The present invention relates to molybdenum field of aluminum alloys, be specifically related to the assay method of molybdenum content in a kind of molybdenum aluminium alloy.
Background technology
At present, along with the continuous increase of smelting titanium alloy amount, the demand of Mo-contained alloy is constantly increased.Owing to containing a large amount of iron in ferro-molybdenum, the smelting of titanium alloy therefore can not be used for.And molybdenum aluminium alloy can meet the requirement of titanium alloy smelting process well, therefore in titanium alloy smelting process, need to use a large amount of molybdenum aluminium alloy.
In molybdenum aluminium alloy, the content of molybdenum is the important technology index must known during titanium alloy is smelted, and is also the Main Basis of buying clearing simultaneously.But not about the GB analytical approach that molybdenum content in molybdenum aluminium alloy measures in prior art, and the matrix difference of molybdenum aluminium alloy and molybdenum-iron is very large, and in ferro-molybdenum, molybdenum content assay method can not be used for the analysis of molybdenum in molybdenum aluminium alloy.In the case, need to explore the analysis of molybdenum content in molybdenum aluminium alloy and study, determine to measure the optimum test condition of molybdenum, set up the analytical approach of molybdenum in molybdenum aluminium alloy accurately and rapidly.
Summary of the invention
The object of the present invention is to provide the assay method of molybdenum content in a kind of molybdenum aluminium alloy of at least one technical matters that can solve in above multiple technical matters.
According to the assay method of molybdenum content in molybdenum aluminium alloy of the present invention, comprise the following steps: (1) takes molybdenum aluminium alloy 0.15 ~ 0.25g to be measured as test portion, adds the nitric acid that 30mL proportioning is 2+3, after described test portion is dissolved completely, add the hydrochloric acid that 5mL density is 1.19g/mL, boil; (2) the EDTA solution that 60mL water and 15 ~ 40mL concentration are 50g/L is added in the solution after boiling, solution ph is regulated to be 5 ~ 6 with the ammoniacal liquor that density is 0.90g/mL, add ammonium acetate solution and 10mL glacial acetic acid that 10mL concentration is 500g/L, heat after being diluted with water to 250 ~ 300mL, under boil condition, drip concentration is that the lead acetate solution of 20g/L is to appearance precipitation, continue again to drip the lead acetate solution that 50mL concentration is 20g/L, leave standstill after continuing to boil 10 ~ 15min; (3) by leave standstill after solution filter, be the hot ammonium nitrate solution washing precipitation of 50g/L by concentration; (4) precipitation after washing is weighed after charing, calcination, drying, cooling, obtain the quality of lead molybdate precipitation; (5) utilize following formula to calculate the content of molybdenum in described test portion:
M
1be the quality of lead molybdate precipitation in described step (4), unit is g; M is the quality of test portion in described step (1), and unit is g.
Wherein, in described step (1), when molybdenum content scope is 45.00 ~ 70.00 quality % in test portion, take described test portion 0.25g; When molybdenum content scope is for being greater than 70.00 quality below % to 90.00 quality % in test portion, take described test portion 0.15g.
Wherein, when taking described test portion 0.25g in described step (1), in described step (2), add EDTA solution described in 40mL; When taking described test portion 0.15g in described step (1), in described step (2), add EDTA solution described in 15mL.
Wherein, in described step (2), solution ph is regulated to be in the process of 5 ~ 6 with the ammoniacal liquor that density is 0.9g/mL, when there is floccus in solution, the hydrochloric acid conditioning solution that proportioning is 1+1 is used to disappear to floccus, adding proportioning is again after the hydrochloric acid 5mL of 1+1, again adds the EDTA solution that 5mL concentration is 50g/L, then is that the ammoniacal liquor of 0.9g/mL regulates solution ph to be 5 ~ 6 with density.
Wherein, in described step (2), the rate of addition of lead acetate solution is controlled to be 7.50 ~ 12.50mL/ minute.
Wherein, in described step (2), described standing process is leave standstill 40 ~ 50min at 60 ~ 80 DEG C.
Wherein, in described step (4), described carburizing temperature is 570 ~ 630 DEG C, and described calcination time is 30 ~ 50min.
The mensuration of molybdenum content in molybdenum aluminium alloy can be completed easy, quickly and accurately by the assay method of molybdenum content in molybdenum aluminium alloy of the present invention.In addition, the scope that this method is applicable to molybdenum content is the detection of the molybdenum aluminium alloy of 45.00 ~ 90.00 quality %, and therefore usable range is extensive.
Embodiment
In molybdenum aluminium alloy of the present invention molybdenum content assay method in, the molybdenum aluminium alloy to be measured as test portion can be pulverized in advance, makes it be Powdered.In step (1), take molybdenum aluminium alloy 0.15 ~ 0.25g to be measured as test portion, add the nitric acid that 30mL proportioning is 2+3, after described test portion is dissolved completely, add the hydrochloric acid that 5mL density is 1.19g/mL, boil the oxides of nitrogen eliminated in solution.Wherein, the amount taking test portion is 0.15 ~ 0.25g, but is preferably the approximate range according to molybdenum content in molybdenum aluminium alloy, weighs, be accurate to 0.0001g according to following table 1.In addition, in test portion, add 30mL proportioning is that the nitric acid of 2+3 carries out in the process of dissolving, and is preferably low-temperature heat and test portion is dissolved completely; Proportioning is that the nitric acid of 2+3 refers to, the volume ratio of red fuming nitric acid (RFNA) and water is the salpeter solution that 2:3 configures.The dust technology of this concentration is adopted to be dissolved completely by test portion fast, up hill and dale.Finally being boiled by solution is oxides of nitrogen in order to eliminate in solution.
The sample weighting amount of table 1 test portion
| The scope (quality %) of molybdenum content in molybdenum aluminium alloy | Sample weighting amount (g) |
| ≥45.00～70.00 | 0.25 |
| ＞70.00～90.00 | 0.15 |
In molybdenum aluminium alloy of the present invention, the step (2) of the assay method of molybdenum content is, the EDTA solution that 60mL water and 15 ~ 40mL concentration are 50g/L is added in solution after boiling, solution ph is regulated to be 5 ~ 6 with the ammoniacal liquor that density is 0.9g/mL, add ammonium acetate solution and 10mL glacial acetic acid that 10mL concentration is 500g/L, heat after being diluted with water to 250 ~ 300mL, under boil condition, drip concentration is that the lead acetate solution of 20g/L is to appearance precipitation, continue again to drip the lead acetate solution that 50mL concentration is 20g/L, leave standstill after continuing to boil 10 ~ 15min.The object adding EDTA is to shelter the coexistence elements such as aluminium, iron, thus eliminates coexisting ion to the interference of Mo determination.In addition, in order to make measurement result more accurate, be preferably and using the ammoniacal liquor that density is 0.9g/mL to regulate solution ph to be in the process of 5 ~ 6, when there is floccus in solution, the hydrochloric acid conditioning solution that proportioning is 1+1 is used to disappear to floccus, adding proportioning is again after the hydrochloric acid 5mL of 1+1, again adds the EDTA solution that 5mL concentration is 50g/L, then is that the ammoniacal liquor of 0.9g/mL regulates solution ph to be 5 ~ 6 with density.Wherein proportioning is that the hydrochloric acid of 1+1 refers to, the volume ratio of concentrated hydrochloric acid and water is the hydrochloric acid solution that 1:1 configures.In addition, using acetic acid and the ammonium acetate solution of above-mentioned specified quantitative, is to form acetic acid-ammonium acetate buffer system, to make the precipitation completely of lead molybdate.The glacial acetic acid used preferably is analyzed pure.Formed in the process of precipitation adding lead acetate, should slowly drip lead acetate solution, in case local concentration is excessive and cause precipitation to carry impurity secretly, and can deposit seed be increased.Be preferably and the rate of addition of lead acetate solution is controlled to be 7.50 ~ 12.50mL/ minute.In addition, the process that leaves standstill is preferably and leaves standstill 40 ~ 50min at 60 ~ 80 DEG C, is fully formed to make precipitation.
In addition, in order to the masking effect making EDTA solution reach best, abundant sheltering the interference ions, being preferably when taking molybdenum content scope in test portion 0.25g(and test portion in above-mentioned steps (1) is 45.00 ~ 70.00 quality %) time, in above-mentioned steps (2), add the EDTA solution that 40mL concentration is 50g/L; When taking in test portion 0.15g(and test portion molybdenum content scope for being greater than 70.00 quality below % to 90.00 quality % in above-mentioned steps (1)) time, in above-mentioned steps (2), add the EDTA solution that 15mL concentration is 50g/L.
In molybdenum aluminium alloy of the present invention, the step (3) of the assay method of molybdenum content is, being filtered by the solution after leaving standstill, is the hot ammonium nitrate solution washing precipitation of 50g/L by concentration.At this, the temperature of hot ammonium nitrate solution can be 50 ~ 80 DEG C.Wherein, the Medium speed filter paper be preferably with filling filter paper pulp filters, and cleans with the glass bar with rubber tip and contain the wall of cup of filtering solution, contains the beaker 5 times of filtering solution, washing precipitation 15 times with the hot ammonium nitrate solution washing that concentration is 50g/L.
In molybdenum aluminium alloy of the present invention the step (4) of the assay method of molybdenum content be by washing after precipitation weigh after charing, calcination, drying, cooling, obtain lead molybdate precipitate quality.Wherein, carburizing temperature 570 ~ 630 DEG C is preferably, calcination time 30 ~ 50min.
Below in conjunction with specific embodiment and reference examples, the present invention is further described.In addition, in the present invention, if no special instructions, mass percent is.
The reagent that embodiment and reference examples use:
Hydrochloric acid (ρ 1.19g/mL);
Hydrochloric acid (1+1): the volume ratio of concentrated hydrochloric acid and water is the hydrochloric acid solution that 1:1 configures;
Nitric acid (ρ 1.42g/mL);
Nitric acid (2+3): the volume ratio of red fuming nitric acid (RFNA) and water is the salpeter solution that 2:3 configures;
Ammoniacal liquor (ρ 0.90g/mL);
Glacial acetic acid (analyzing pure);
Lead acetate solution (20g/L): take 20g lead acetate in beaker, adds 300mL water and makes it dissolve, and adding appropriate glacial acetic acid (analyzing pure) limit edged, to be stirred to solution limpid, be settled to 1000mL mixing, filter for subsequent use;
Ammonium nitrate solution (50g/L);
Ammonium acetate solution (500g/L);
EDTA solution (50g/L);
Sodium hydroxide solution (200g/L);
Pure molybdenum powder (>=99.95%);
Aluminum standard solution (5.0mg/L): take 1.0000g metallic aluminium (99.98%) and be placed in 500mL plastic beaker, add 20mL sodium hydroxide solution (200g/L), neutralize and excessive 20mL with hydrochloric acid (1+1), after boiling solution clarification, cooling, move in 200mL volumetric flask, be diluted with water to scale, mixing.Containing 5.0mg aluminium in this solution of 1mL.
embodiment 1
The mensuration of molybdenum content in molybdenum aluminium alloy is carried out successively according to following steps.
Step (1): sampling, decomposition
Take and record molybdenum aluminium alloy quality m=0.2548g to be measured as test portion, above-mentioned test portion is placed in 500mL beaker, add 30mL nitric acid (2+3) afterwards low-temperature heat dissolve completely to test portion.Add 5mL hydrochloric acid (ρ 1.19g/mL), boil and eliminate oxides of nitrogen.
Step (2): precipitation
60mL water, 40mL EDTA(50g/L is added in solution after above-mentioned boiling) solution, regulate solution ph 5 with ammoniacal liquor (ρ 0.90g/mL).Add 10mL ammonium acetate solution (500g/L), 10mL glacial acetic acid (analyzing pure), is diluted with water to about 250 ~ 300mL.
By the solution heating after dilution, drip lead acetate solution (20g/L) to appearance precipitation under boil condition after, dropwise add 50mL lead acetate solution (20g/L) again, continue to boil 15min, 40min(note is left standstill: will slowly drip when adding lead acetate solution at 60 DEG C, in case local over-concentration and precipitate and carry impurity secretly, deposit seed can be increased simultaneously, at this, rate of addition be controlled as 7.50mL/ minute).
Step (3): precipitation and separation
Filter with the Medium speed filter paper filling a small amount of filter paper pulp, clean wall of cup with the glass bar with rubber tip, wash beaker 5 times with hot ammonium nitrate solution (50g/L), washing precipitation 15 times.
Step (4): precipitation aftertreatment
Precipitation is placed in porcelain crucible together with filter paper, in 570 DEG C of muffle furnaces after charing, then calcination 30min in muffle furnace at this temperature, take out after being placed in exsiccator cooling, weighing results 0.6080g is m1.
Step (5): calculate
By following formula, molybdenum content in molybdenum aluminium alloy is calculated:
In formula: m
1the quality of-lead molybdate precipitation, g;
The quality of m-test portion, g;
0.2613-lead molybdate is scaled the coefficient of molybdenum.
That is, by m=0.2548g, m
1it is 62.35% that=0.6080g substitution above formula calculates molybdenum content w.
Carry out sampling 6 times to same molybdenum aluminium alloy respectively, repeat the operation of above-mentioned steps (1) ~ (5), measurement result charges to table 3.
embodiment 2 ~ 4
According to the method for operating of above-described embodiment 1 within the scope of the setting parameter recorded in the present invention, then measure 3 kinds of different molybdenum aluminium alloys of molybdenum content, as embodiment 2 ~ 4, its measurement result charges to table 3.
embodiment 5
The mensuration of molybdenum content in molybdenum aluminium alloy is carried out successively according to following steps.
Step (1): sampling, decomposition
Take and record molybdenum aluminium alloy quality m=0.1560g to be measured as test portion, above-mentioned test portion is placed in 500mL beaker, add 30mL nitric acid (2+3) afterwards low-temperature heat dissolve completely to test portion.Add 5mL hydrochloric acid (ρ 1.19g/mL), boil and eliminate oxides of nitrogen.
Step (2): precipitation
60mL water, 15mL EDTA(50g/L is added in solution after above-mentioned boiling) solution, regulate solution ph 6 with ammoniacal liquor (ρ 0.90g/mL).Add 10mL ammonium acetate solution (500g/L), 10mL glacial acetic acid (analyzing pure), is diluted with water to about 250 ~ 300mL.
By the solution heating after dilution, slowly drip lead acetate solution (20g/L) to appearance precipitation under boil condition after, slowly dropwise add 50mL lead acetate solution (20g/L) again, continue to boil 10min, 50min (note: will slowly drip when adding lead acetate solution is herein left standstill at 80 DEG C, in case local over-concentration and precipitate and carry impurity secretly, deposit seed can be increased simultaneously, at this, rate of addition be controlled as 12.5mL/ minute).
Step (3): precipitation and separation
Filter with the Medium speed filter paper filling a small amount of filter paper pulp, clean wall of cup with the glass bar with rubber tip, wash beaker 5 times with hot ammonium nitrate solution (50g/L), washing precipitation 15 times.
Step (4): precipitation aftertreatment
Precipitation is placed in porcelain crucible together with filter paper, in 630 DEG C of muffle furnaces after charing, then calcination 50min in muffle furnace at this temperature, take out after being placed in exsiccator cooling, weighing results 0.5200g is m
1.
Step (5): calculate
By following formula, molybdenum content in molybdenum aluminium alloy is calculated as:
In formula: m
1the quality of-lead molybdate precipitation, g;
The quality of m-test portion, g;
0.2613-lead molybdate is scaled the coefficient of molybdenum.
That is, by m=0.1560g, m
1it is 87.10% that=0.5200g substitution above formula calculates molybdenum content w.
Carry out sampling 6 times to same molybdenum aluminium alloy respectively, repeat the operation of above-mentioned steps (1) ~ (5), measurement result charges to table 3.
embodiment 6 ~ 7
According to the method for operating of above-described embodiment 5 within the scope of the setting parameter recorded in the present invention, then measure 2 kinds of different molybdenum aluminium alloys of molybdenum content, as embodiment 6,7, its measurement result charges to table 3.
reference examples 1 ~ 6
According to the addition of following table 2, take a certain amount of pure molybdenum powder (>=99.95%), above-mentioned test portion is placed in 500mL beaker, add 30mL nitric acid (2+3), at 30 DEG C, low temperature is heated to pure molybdenum powder and dissolves completely.Add 5mL hydrochloric acid (ρ 1.19g/mL), boil and eliminate oxides of nitrogen, add a certain amount of aluminum standard solution, the synthetic standard sample 1 ~ 6 of preparation molybdenum aluminium alloy, example 1 ~ 6 in contrast.
The molybdenum content in synthetic standard sample is measured according to step (2) ~ (4) of above-described embodiment 1.Repeatedly measure 6 times to same synthetic standard sample respectively, measurement result charges to table 3.
The preparation of the synthetic standard sample of table 2 molybdenum aluminium alloy
| Numbering | Pure molybdenum powder (g) | Aluminum standard solution (mL) |
| Synthetic standard sample 1 | 0.1150 | 27.00 |
| Synthetic standard sample 2 | 0.1350 | 23.00 |
| Synthetic standard sample 3 | 0.1600 | 18.00 |
| Synthetic standard sample 4 | 0.1125 | 7.50 |
| Synthetic standard sample 5 | 0.1200 | 6.00 |
| Synthetic standard sample 6 | 0.1325 | 3.50 |
Table 3 measurement result
By comparing to the mensuration of synthetic standard sample and theoretical value, fully demonstrate the accuracy of this method.
The tolerance that the present invention measures is as shown in table 4.
Table 4 tolerance
| Molybdenum content, % | Tolerance, % |
| ≥45.00～50.00 | 0.35 |
| >50.00～60.00 | 0.40 |
| >60.00～75.00 | 0.50 |
| >75.00～90.00 | 0.60 |
By the assay method of molybdenum content in molybdenum aluminium alloy provided by the invention, have the following advantages:
(1) dust technology is adopted to be dissolved completely by sample fast, up hill and dale;
(2) shelter the coexistence elements such as aluminium, iron with EDTA, eliminate the mensuration of coexisting ion interference molybdenum content;
(3) control the acidity of solution with acetic acid-ammonium acetate solution, precipitate completely to meet lead molybdate;
(3) difficult problem without corresponding standard substance is solved with synthetic standard sample;
(4) molybdenum content fast, in Accurate Determining in molybdenum aluminium alloy is reached.
Although illustrate and describe the present invention particularly with reference to exemplary embodiment of the present invention, but those skilled in the art will appreciate that, when do not depart from as claims and they equivalent limit the spirit and scope of the present invention, the various changes in form and details can be made at this.Object only in descriptive meaning instead of for restriction should consider embodiment.Therefore, scope of the present invention is not limited by the specific embodiment of the present invention, but is limited by claims, and all differences within the scope of this will be interpreted as comprising in the present invention.
Claims (7)
1. the assay method of molybdenum content in molybdenum aluminium alloy, is characterized in that, said method comprising the steps of:
(1) take molybdenum aluminium alloy 0.15 ~ 0.25g to be measured as test portion, add the nitric acid that 30mL proportioning is 2+3, after described test portion is dissolved completely, add the hydrochloric acid that 5mL density is 1.19g/mL, boil;
(2) the EDTA solution that 60mL water and 15 ~ 40mL concentration are 50g/L is added in the solution after boiling, solution ph is regulated to be 5 ~ 6 with the ammoniacal liquor that density is 0.90g/mL, add ammonium acetate solution and 10mL glacial acetic acid that 10mL concentration is 500g/L, heat after being diluted with water to 250 ~ 300mL, under boil condition, drip concentration is that the lead acetate solution of 20g/L is to appearance precipitation, continue again to drip the lead acetate solution that 50mL concentration is 20g/L, leave standstill after continuing to boil 10 ~ 15min;
(3) by leave standstill after solution filter, be the hot ammonium nitrate solution washing precipitation of 50g/L by concentration;
(4) precipitation after washing is weighed after charing, calcination, drying, cooling, obtain the quality of lead molybdate precipitation;
(5) utilize following formula to calculate the content of molybdenum in described test portion:
Wherein, m
1be the quality of lead molybdate precipitation in described step (4), unit is g; M is the quality of test portion in described step (1), and unit is g.
2. method according to claim 1, is characterized in that, in described step (1), when molybdenum content scope is 45.00 ~ 70.00 quality % in test portion, takes described test portion 0.25g; When molybdenum content scope is for being greater than 70.00 quality below % to 90.00 quality % in test portion, take described test portion 0.15g.
3. method according to claim 2, is characterized in that, when taking described test portion 0.25g in described step (1), in described step (2), adds EDTA solution described in 40mL; When taking described test portion 0.15g in described step (1), in described step (2), add EDTA solution described in 15mL.
4. method according to claim 1, it is characterized in that, in described step (2), solution ph is regulated to be in the process of 5 ~ 6 with the ammoniacal liquor that density is 0.90g/mL, when floccus appears in solution, hydrochloric acid conditioning solution disappears to floccus to use proportioning to be 1+1, then to add proportioning be after the hydrochloric acid 5mL of 1+1, again add the EDTA solution that 5mL concentration is 50g/L, then be that the ammoniacal liquor of 0.90g/mL regulates solution ph to be 5 ~ 6 with density.
5. method according to claim 1, is characterized in that, in described step (2), is controlled to be 7.50 ~ 12.50mL/ minute by the rate of addition of lead acetate solution.
6. method according to claim 1, is characterized in that, in described step (2), described standing process is leave standstill 40 ~ 50min at 60 ~ 80 DEG C.
7. method according to claim 1, is characterized in that, in described step (4), described carburizing temperature is 570 ~ 630 DEG C, and described calcination time is 30 ~ 50min.
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| CN108663283A (en) * | 2018-06-06 | 2018-10-16 | 新兴铸管股份有限公司 | The method of molybdenum content in lead molybdate gravimetric detemination molybdenum-iron |
| CN109613169A (en) * | 2018-12-29 | 2019-04-12 | 中国第重型机械股份公司 | A kind of method of lead molybdate precipitating in ferro-molybdenum chemical analysis |
| CN110146405A (en) * | 2019-06-05 | 2019-08-20 | 核工业北京地质研究院 | The measuring method of boron carbide mass fraction in a kind of aluminum-based boron carbide neutron absorber material |
| CN111307786A (en) * | 2020-03-19 | 2020-06-19 | 河北四通新型金属材料股份有限公司 | Method for detecting molybdenum element in molybdenum niobium aluminum silicon titanium alloy |
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