CN101762576B - Method for measuring niobium content in tungsten carbide added with niobium or simultaneously added with tantalum and niobium - Google Patents

Method for measuring niobium content in tungsten carbide added with niobium or simultaneously added with tantalum and niobium Download PDF

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CN101762576B
CN101762576B CN2010100345526A CN201010034552A CN101762576B CN 101762576 B CN101762576 B CN 101762576B CN 2010100345526 A CN2010100345526 A CN 2010100345526A CN 201010034552 A CN201010034552 A CN 201010034552A CN 101762576 B CN101762576 B CN 101762576B
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niobium
concentration
solution
tantalum
acid solution
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CN101762576A (en
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胡翼淇
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Jiangxi Rare Earth and Rare Metals Tungsten Group Holding Co Ltd
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Jiangxi Rare Earth and Rare Metals Tungsten Group Holding Co Ltd
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Abstract

The invention relates to a method for measuring a niobium content in tungsten carbide added with niobium or simultaneously added with tantalum and niobium, which comprises the following analytical steps that: after a sample is ground and sieved, the obtained product is melted by sodium peroxide, and the product is leached by hot water; after twice precipitations are carried out on the leached solution by using a coprecipitator to precipitate and using a gallotannic acid to precipitate, niobium or niobium and tantalum are separated from the main tungsten and other impurities, and then tartaric acid solution is prepared; when the prepared tartaric acid solution is in the sulphuric acid medium, the niobium and 5-Br-PADAP form a red chelate, the color depth is in positive proportion to the niobium content, hereby, the niobium content can be measured by photometry according to the working curve of the niobium; and if the sample comprises the niobium and tantalum simultaneously, the interference of tantalum to the measurement of the niobium content is eliminated by a method of adding excessive solution of high-concentration tartaric acid to carry out complexing and screening. The method of the invention has high precipitate recovery rate, simple and convenient operation, small interference, and good accuracy and repeatability.

Description

Add niobium or add the assay method of content of niobium in the tungsten carbide of tantalum and niobium simultaneously
Technical field
The present invention relates to a kind of assay method that adds niobium or add content of niobium in the tungsten carbide of niobium and tantalum simultaneously.
In this manual, term " secondary precipitate " is meant sample after coprecipitator and tannic acid secondary precipitate, and niobium or niobium separate with main body tungsten and other impurity with tantalum.For the first time precipitation is meant that adding coprecipitator lanthanum salt and molysite in alkaline solution makes niobium or niobium and tantalum and its formation co-precipitation.Precipitation has been finished the enrichment of niobium or tantalum and niobium and has been separated with main body tungsten for the first time.Precipitation is meant and adds tannic acid precipitation niobium or niobium and tantalum in acid solution for the second time.For the second time precipitation makes niobium or niobium and tantalum separate with other impurity except that tungsten.Secondary precipitate has greatly improved the antijamming capability of analyzing.
Term " co-precipitation " is meant and adds coprecipitator lanthanum salt and molysite formation co-precipitation that in alkaline solution with enrichment that reaches niobium or niobium and tantalum and the effect of separating with main body tungsten, co-precipitation has greatly improved the recovery of niobium or niobium and tantalum.
Term " water colorimetric " is meant that colorimetric carries out at aqueous phase but not carry out in organic phase.
Background technology
Cemented carbide industry often will be added niobium or be added niobium and tantalum simultaneously in its tungsten carbide powder, wherein the content of niobium and tantalum directly has influence on the performance of wimet.
The analysis of niobium and tantalum itself is exactly a difficult point in the chemical analysis, the chemical property of niobium and tantalum is very similar, the accurate mensuration of niobium and tantalum is just more difficult with chemical method when adding niobium and tantalum simultaneously, and niobium is similar to the chemical property of main body tungsten with tantalum, in the therefore present GB analytical approach, still the chemical analysis detection method of not having niobium when adding niobium in the tungsten carbide or adding tantalum and niobium simultaneously, the assay method that has only the content of niobium in the ore, but this method only is fit to the mensuration of low content niobium, and complex operation, used certain toxic organic compound, result's accuracy and reappearance are undesirable, do not satisfy the mensuration needs of content of niobium in the tungsten carbide of mixing niobium separately or mixing tantalum and niobium simultaneously.
Macrotype hard alloy industry generally adopts expensive X-ray fluorescence spectra analyser to measure for the content of niobium that adds in the tungsten carbide powder or tantalum, method quick and precisely, but general medium-sized and small enterprises do not have this equipment more.This method need not special inspecting equipment, cost is low, easy and simple to handle, disturb less, accuracy and favorable reproducibility, can satisfy the mensuration of content of niobium in the tungsten carbide that adds niobium in the cemented carbide industry or add niobium and tantalum simultaneously, the detection method of a kind of practicality of can yet be regarded as fully.
The method of content of niobium is as follows in traditional chloro sulphur phenol S spectrphotometric method for measuring ore:
1, scope: be used for the mensuration of stone ore content of niobium, measurement range: 0.010～0.10%.
2, principle
Sample decomposes through alkali fusion, after the water logging, with phosphoric acid complexing tungsten, in the ammonia solution that has EDTA and oxalic acid to exist, with silicic acid enrichment niobium and tantalum, it is separated with tungsten, molybdenum, manganese, aluminium etc.Precipitation after the calcination, is removed silicon with hydrofluorite after filtration, niobium and tantalum is made tartaric acid solution, in hydrochloric acid medium, with chloro sulphur phenol S spectrphotometric method for measuring content of niobium.
3, reagent
(1) the potassium pyrosulfate analysis is pure, solid; (6) the EDTA liquor analysis is pure;
(2) tartaric acid solution is analyzed pure; (7) hydrochloric acid solution is analyzed pure;
(3) aluminum trichloride solution is analyzed pure; (8) acetone is analyzed pure;
(4) liquor ferri trichloridi is analyzed pure; (9) chloro sulphur phenol S liquor analysis is pure;
(5) the oxammonium hydrochloride liquor analysis is pure; (10) High-purity Niobium standard solution and niobium working curve thereof are drawn.
A. the preparation of standard solution: take by weighing 0.1000g high-purity N b 2O 5In porcelain crucible, add 3～4g potassium pyrosulfate solid, on blowtorch, melt to transparently, take off cooling.With concentration is the tartaric acid solution leaching of 60g/L, is heated to frit and all dissolves, after the cooling solution is moved in the 500mL volumetric flask, and be that the tartaric acid solution of 60g/L is diluted to scale with concentration, mixing is stored in the plastic bottle.This liquid 1mL contains 200 μ g Nb 2O 5Standard solution is that the tartaric acid solution of 60g/L is diluted to and contains Nb with concentration thus again 2O 520 μ g/mL.
B. draw the niobium working curve: the concentration of preparing among the removing step a is the Nb of 20 μ g/mL 2O 5Standard solution 0.00mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL and 5.00mL, place one group of 50mL color comparison tube respectively, the tartaric acid solution that adds concentration respectively and be 60g/L is to 10mL, adding concentration is the aluminum trichloride solution 5mL of 400g/L, concentration is the liquor ferri trichloridi 0.5mL of 5g/L, concentration is the oxammonium hydrochloride solution 3mL of 5g/L, whenever adds the equal mixing of a kind of reagent, puts on boiling water bath 5 minutes, take off cooling, adding concentration is the EDTA solution 1mL of 40g/L, and concentration is the hydrochloric acid solution 14mL of 500g/L, adds 5mL acetone behind the mixing, concentration is the chloro sulphur phenol S solution 3mL of 1g/L, be diluted with water to scale and mixing, put 1 hour, part solution is moved in the 1cm cuvette, 645nm place on 721 type spectrophotometers, with the reagent blank is reference, surveys its absorbance, with Nb 2O 5Amount is ordinate drawing curve for horizontal ordinate with the absorbance.
(11) the sodium peroxide analysis is pure, solid; (16) phenolphthalein solution;
(12) the NaOH analysis is pure, solid; (17) ammoniacal liquor is analyzed pure;
(13) phosphate analysis is pure; (18) sodium silicate solution is analyzed pure;
(14) the ammonium chloride saturated solution is analyzed pure; (19) hydrofluorite is analyzed pure.
(15) oxalic acid solution is analyzed pure;
4, sample: sample ore through sample grinding machine grind good after the oven dry.
5, analytical procedure
5.1 mensuration quantity: take by weighing two parts of samples and measure.
5.2 sample size: take by weighing sample 0.1～1.0g, accurately to 0.0001g.
5.3 measure
(1) sample is inserted in the 30mL corundum crucible, add sodium peroxide solid 1～2g, sodium hydrate solid 0.5～1.5g, fully stir evenly, fusion is 10 minutes in 600 ℃ of muffle furnaces, takes off cold slightly, crucible is put into the 400mL beaker that fills 30mL hot water leach, wash out crucible.
(2) adding concentration in step (1) gained solution is the EDTA solution 30mL of 100g/L, stir evenly, be heated to and boil 5 minutes, cold slightly, add phosphoric acid 8mL, mixing adds hydrochloric acid 12mL, ammonium chloride saturated solution 50mL, concentration is the oxalic acid solution 30mL of 100g/L, be heated to and boil, adding concentration is the phenolphthalein solution 0.5mL of 10g/L, transfers to red and excessive 4～5mL with ammoniacal liquor, hot water is diluted to about 200mL, be heated to little boiling, dripping concentration while hot is the sodium silicate solution 10mL of 150g/L, fully stirs in 70～80 ℃ of water bath heat preservations 30 minutes.
(3) step (2) gained precipitation being used while hot quick filter paper filtering, is that the thermal chlorination ammonium washing lotion of 100g/L is washed about 8 times with concentration, is that the hydrochloric acid solution of 100g/L washs hot wash 2 times 4 times with concentration again.
(4) step (3) gained precipitation is moved into ashing in the 30mL porcelain crucible together with filter paper, calcination is 30 minutes in 700 ℃ of muffle furnaces, and is cold slightly, and the back thing that will burn carefully moves in the platinum crucible, with water-wet, add 6～8mL hydrofluorite, low-grade fever is steamed to the wet salt shape, and adding concentration is the tartaric acid solution 10mL of 150g/L, low-grade fever leaching 10 minutes, the cooling back moves in the 50mL volumetric flask, and water is rare to scale, mixing.
(5) removing step (4) gained solution 1～5mL is in the 50mL color comparison tube, the tartaric acid solution that with concentration is 60g/L complements to 10mL, adding concentration is the aluminum trichloride solution 5mL of 400g/L, concentration is the liquor ferri trichloridi 0.5mL of 5g/L, concentration is the oxammonium hydrochloride solution 3mL of 5g/L, whenever add a kind of reagent mixing, on boiling water bath, put 5 minutes, take off cooling, adding concentration is the EDTA solution 1mL of 40g/L, and concentration is the hydrochloric acid solution 14mL of 500g/L, add 5mL acetone behind the mixing, concentration is the horizontal phenol S of the chlorination of 1g/L solution 3mL, and water is rare to the scale mixing, places 1 hour.
(6) part solution is moved in the 1cm cuvette, to sentence sample blank be reference to 645nm on 721 type spectrophotometers, surveys its absorbance, finds Nb from working curve 2O 5Amount.Calculate content of niobium by following formula:
Nb ( % ) = ( m 1 - m 0 ) v 0 × 10 - 6 mv 1 × 0.06990 × 100
m 1Nb in the test solution that checks on-the working curve 2O 5Amount (μ g);
m 0Nb in the blank solution that checks on-the working curve 2O 5Amount (μ g);
The m-sample takes by weighing weight (g);
v 0-test solution cumulative volume (mL);
v 1-minute get test solution volume (mL);
0.6990-Nb 2O 5Be scaled the coefficient of Nb.
This method is fit to the mensuration of low content niobium in the ore.The mensuration that applies to the higher independent interpolation niobium of content or add content of niobium in the tungsten carbide of niobium, tantalum simultaneously, accuracy, the reappearance of analysis are undesirable.Because silicic acid is undesirable to the concentration effect of the niobium of high-load and tantalum, the recovery is low, and unstable, causes measurement result on the low side, and reappearance is bad.Filter quite time-consumingly behind silicic acid enrichment niobium or niobium and the tantalum, efficient is low, and causes main body tungsten to be difficult to clean, and residual tungsten is more, easily the mensuration of niobium is produced and disturbs.The easily muddy and sticking container inner wall of the developer chloro sulphur phenol S that uses in the analysis, absorbance shakiness during colorimetric estimation causes that reappearance is bad as a result.Use organism acetone in the analytic process and use a large amount of hydrofluorite, environment and analyst's health are caused certain influence.
Summary of the invention
The purpose of this invention is to provide a kind of assay method that adds niobium or add content of niobium in the tungsten carbide of niobium and tantalum simultaneously.
For this reason, the invention provides a kind of assay method that adds niobium or add content of niobium in the tungsten carbide of niobium and tantalum simultaneously, its concrete steps are:
Sample is after grinding is sieved, and with the sodium peroxide fusion, hot water leaches;
Leach back solution after coprecipitator precipitation and tannic acid precipitate secondary precipitate, niobium or niobium separate with main body tungsten and other impurity with tantalum, and make tartaric acid solution;
The gained tartaric acid solution is in sulfuric acid medium, and niobium and 5-Br-PADAP form red chelate, and its color depth is directly proportional with the niobium amount, measures content of niobium with photometry according to the niobium working curve in view of the above;
If contain niobium and tantalum in the sample simultaneously, then eliminate the interference that tantalum is measured content of niobium by adding the way that excessive high concentration winestone acid solution complexing shelters.
The method according to this invention, be applicable to the mensuration of content of niobium in the tungsten carbide that adds niobium or add niobium and tantalum simultaneously, co-precipitation and secondary precipitate technology have been adopted, adopted the water colorimetric method, the complex operation of having avoided using organic phase and organic phase colorimetric to bring, environmental pollution, shortcoming such as reappearance is bad as a result.The interference of tantalum can adopt the tartrate complexing that adds excessive high concentration to shelter, and does not disturb the colorimetric estimation of niobium.
The method according to this invention, the precipitate recovery rate height, easy and simple to handle, disturb less, accuracy and favorable reproducibility.Measurement range of the present invention: 0.010～2.000%, the method relative error is less than 5%, and precision of analysis and favorable reproducibility can satisfy the requirement to detecting of product and technology.
Embodiment
Describe the method for content of niobium in the tungsten carbide that adopts spectrophotometry interpolation niobium or add niobium and tantalum simultaneously below in detail.
1, accommodation: this method is applicable to the assay of niobium in the tungsten carbide that adds niobium or add niobium, tantalum simultaneously.Measurement range: 0.010～2.000%.
2, principle
Sample after grinding is sieved with the sodium peroxide fusion, hot water leaches, through coprecipitator precipitation and the secondary precipitate of tannic acid precipitation, niobium or niobium separate with main body tungsten and other impurity with tantalum, and after making tartaric acid solution, in sulfuric acid medium, niobium and 5-Br-PADAP form red chelate, its color depth is directly proportional with the niobium amount, measure content of niobium with photometry according to the niobium working curve in view of the above, if also have tantalum in the sample simultaneously, the way elimination that the interference of tantalum is sheltered by adding excessive high concentration winestone acid solution complexing.
3, reagent
(1) the potassium pyrosulfate analysis is pure, solid;
(2) tartaric acid solution is analyzed pure;
(3) the EDTA liquor analysis is pure;
(4) sulfuric acid solution is analyzed pure;
(5) the 5-Br-PADAP liquor analysis is pure;
(6) high-purity N b 2O 5Standard solution preparation and niobium working curve are drawn.
A.Nb 2O 5Standard solution preparation: take by weighing high-purity N b 2O 50.1000g put into porcelain crucible, add potassium pyrosulfate solid 3～4g, on blowtorch, melt to transparently, take off cooling.With concentration is the tartaric acid solution leaching of 60g/L, is heated to frit and all dissolves, after the cooling solution is moved in the 500mL volumetric flask, and be that the tartaric acid solution of 60g/L is diluted to scale with concentration, mixing is stored in the plastic bottle.This liquid 1mL contains 200 μ g Nb 2O 5Standard solution is that the tartaric acid solution of 60g/L is diluted to and contains Nb with concentration thus again 2O 520 μ g/mL.
B. draw the niobium working curve: the concentration of removing step a preparation is the high-purity N b of 20 μ g/mL 2O 5Standard solution, volume is 0.00mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL and 5.00mL, insert respectively in the 25mL volumetric flask, the tartaric acid solution that with concentration is 60g/L complements to 5mL, successively add the EDTA solution 0.5mL that concentration is 40g/L respectively, concentration is the sulfuric acid solution 1mL of 50g/L, concentration is the 5-Br-PADAP solution 3mL of 5g/L, whenever adding a kind of reagent evenly mixes, water is rare to scale and mixing, boils 5～10 minutes, after the flowing water cooling, with the reagent blank is reference, surveys its absorbance.With Nb 2O 5Amount is ordinate drawing curve for horizontal ordinate with the absorbance.
(7) the sodium peroxide analysis is pure, solid;
(8) the lanthanum salt solusion is analyzed pure;
(9) iron salt solutions is analyzed pure;
(10) sodium hydroxide solution is analyzed pure;
(11) the salt acid analysis is pure;
(12) tannic acid solution is analyzed pure;
(13) hydrofluorite is analyzed pure.
4, sample: in the mortar that does not change sample constituents, pulverize and mistake 0.18mm sieve aperture.
5, analytical procedure
5.1 sample size: take by weighing sample 0.05～0.10g, accurately to 0.0001g.
5.2 measure
(1) sample places 30～50mL corundum crucible or porcelain crucible, go in 600～800 ℃ of muffle furnaces and transform 30～60 minutes, take out cooling, add sodium peroxide solid 2～7g, fully stir evenly, put into 600～800 ℃ of muffle furnace fusions 5～15 minutes, take out cooling, place the 250mL beaker that fills 50～100mL hot water in advance to leach, wash crucible, adding concentration is the lanthanum salt solusion of 50g/L and each 1mL of iron salt solutions that concentration is 50g/L, fully stirs evenly, and low-temperature heat is little boiled several minutes, take off cold slightly, using the middling speed filter paper filtering while hot, is that the hot sodium hydroxide solution of 20g/L washs reusable heat water washing 2～3 times 7～8 times with concentration.
(2) precipitation after the washing is put into former beaker together with filter paper, adds hydrochloric acid 20～30mL, heated and boiled number minute, add boiling water to the nearly 200mL of volume, adding concentration is tannic acid solution and the mixing of 250g/L, continues little the boiling 3～5 minutes of heating, moves in the hot bath and is incubated 0.5～1.5 hour.
(3) step (2) gained precipitation middling speed filter paper filtering, and be the hot tannic acid washing lotion washing 8～10 times of 20g/L with concentration, hot water wash 1～2 time, to precipitate and put into platinum crucible together with filter paper, insert in the muffle furnace after the first ashing again 600～800 ℃ of calcinations 30～60 minutes, take out cold slightly, it is moistening to blow low amounts of water, drip 1～2mL hydrofluorite, the water-bath heating is steamed to the wet salt shape, and adding concentration is tartaric acid solution 20～30mL of 150g/L, water-bath heating leaching 5～15 minutes, take off cooling, water moves in the 50mL volumetric flask and constant volume.
(4) get in step (3) gained solution 1～5mL to the 25mL volumetric flask, the tartaric acid solution of adding concentration and be 60g/L is to 5mL, adding concentration is EDTA solution 0.50mL, the sulfuric acid solution 1mL that concentration is 50g/L, the 5-Br-PADAP solution 3mL that concentration is 5g/L of 40g/L, whenever add the equal mixing of a kind of reagent, be diluted with water to scale and shake up, boil and took off cooling in 5～10 minutes, with the sample blank is reference, 605nm sentences the 1cm cuvette and surveys its absorbance on 721 type spectrophotometers, finds Nb from working curve 2O 5Amount is calculated content of niobium then.
(5) in the sample that adds niobium and tantalum simultaneously, then take following analytical procedure, tantalum does not disturb the mensuration of niobium: in solution 1～5mL to the 25mL volumetric flask of removing step (3) gained, the tartaric acid solution of adding concentration and be 60g/L is to volume 5mL, adding concentration is the EDTA solution 0.5mL of 40g/L, concentration is the tartaric acid solution 5mL of 500g/L, concentration is the sulfuric acid solution 1mL of 50g/L, and concentration is the 5-Br-PADAP solution 3mL of 5g/L, whenever adds a kind of reagent and all need shake up, water is rare to scale and mixing, boiling 5～10 minutes, and took off cooling, is reference with the sample blank, the 605nm place surveys its absorbance on 721 type spectrophotometers, looks into Nb from working curve 2O 5Amount is calculated content of niobium then.
6, the calculating of analysis result
Calculate content of niobium by following formula:
Nb ( % ) = ( m 1 - m 0 ) v 0 × 10 - 6 mv 1 × 0.6990 × 100
m 1Nb in the test solution that checks on-the working curve 2O 5Amount (μ g);
m 0Nb in the blank solution that checks on-the working curve 2O 5Amount (μ g);
The m-sample takes by weighing weight (g);
v 0-test solution cumulative volume (mL);
v 1-minute get test solution volume (mL);
0.6990-Nb 2O 5Be scaled the coefficient of Nb.

Claims (7)

1. assay method that adds niobium or add content of niobium in the tungsten carbide of niobium and tantalum simultaneously is characterized in that analytical procedure comprises:
Sample is after grinding is sieved, and with the sodium peroxide fusion, hot water leaches;
Leach back solution after coprecipitator precipitation and tannic acid precipitate secondary precipitate, niobium or niobium separate with main body tungsten and other impurity with tantalum, and make tartaric acid solution, described coprecipitator is precipitated as and adds lanthanum salt and molysite and niobium or niobium and tantalum formation co-precipitation in alkaline solution, and separate with main body tungsten, eliminate tungsten and disturb;
The gained tartaric acid solution is in sulfuric acid medium, and niobium and 5-Br-PADAP form red chelate, and its color depth is directly proportional with the niobium amount, measures content of niobium with photometry according to the niobium working curve in view of the above.
2. the assay method of content of niobium is characterized in that in the tungsten carbide as claimed in claim 1, when containing niobium and tantalum simultaneously in the sample, eliminates the interference that tantalum is measured content of niobium by adding the way that excessive high concentration winestone acid solution complexing shelters.
3. the assay method of content of niobium is characterized in that in the tungsten carbide as claimed in claim 1, and the drafting of niobium working curve may further comprise the steps:
A.Nb 2O 5The preparation of standard solution: accurately take by weighing 0.1000g high-purity N b 2O 5In porcelain crucible, add 3～4g potassium pyrosulfate solid, on blowtorch, melt to transparently, take off, cooling, with concentration is the tartaric acid solution leaching of 60g/L, is heated to frit and all dissolves, and after the cooling solution is moved in the 500mL volumetric flask, the tartaric acid solution that with concentration is 60g/L is diluted to scale, mixing is stored in the plastic bottle, and this liquid 1mL contains 200 μ g Nb 2O 5, standard solution is that the tartaric acid solution of 60g/L is diluted to and contains Nb with concentration thus again 2O 520 μ g/mL;
B. the drafting of niobium working curve: the concentration of removing step a preparation is the standard solution 0.00mL of 20 μ g/mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL, insert respectively in the 25mL volumetric flask, the tartaric acid solution that with concentration is 60g/L complements to 5mL, successively add the EDTA solution 0.5mL that concentration is 40g/L respectively, concentration is the sulfuric acid solution 1mL of 50g/L, concentration is the 5-Br-PADAP solution 3mL of 5g/L, whenever add the equal mixing of a kind of reagent, water is rare to scale and mixing, boiling 5～10 minutes, after the flowing water cooling, is reference with the reagent blank, survey its absorbance, with Nb 2O 5Amount is horizontal ordinate, is that ordinate is drawn the niobium working curve with the absorbance.
4. the assay method of niobium is characterized in that in the tungsten carbide as claimed in claim 1, and sample concrete analysis step comprises:
(1) sample size: take by weighing and grind the back sample 0.0500～0.1000g that sieves;
(2) measure
The first step, sample is placed 30～50mL corundum crucible or porcelain crucible, go in 600～800 ℃ of muffle furnaces and transform 30～60 minutes, take out cooling, add sodium peroxide solid 2～7g, fully stir evenly, put into 600～800 ℃ of muffle furnace fusions 5～15 minutes, take out cooling, place the 250mL beaker that fills 50～100mL hot water in advance to leach, wash crucible, adding concentration is the lanthanum salt solusion of 50g/L and each 1mL of iron salt solutions that concentration is 50g/L, fully stir evenly, low-temperature heat is little boiled several minutes, took off coldly slightly, used the middling speed filter paper filtering while hot, with concentration the hot sodium hydroxide solution washing 7～8 times of 20g/L, reusable heat water washing 2～3 times;
Second step, above-mentioned steps gained precipitation is put into former beaker together with filter paper, add hydrochloric acid 20～30mL, heated and boiled number minute, add boiling water to the nearly 200mL of volume, adding concentration is tannic acid solution and the mixing of 250g/L, continues little the boiling 3～5 minutes of heating, moves in the hot bath and is incubated 0.5～1.5 hour;
The 3rd step, use the middling speed filter paper filtering, and be the hot tannic acid washing lotion washing 8～10 times of 20g/L with concentration, hot water wash 1～2 time, to precipitate and put into platinum crucible together with filter paper, insert in the muffle furnace after the first ashing again 600～800 ℃ of calcinations 30～60 minutes, take out cold slightly, it is moistening to blow low amounts of water, drips hydrofluorite 1～2mL, and water-bath is heated to the wet salt shape, adding concentration is tartaric acid solution 20～30mL of 150g/L, cooling is taken off in water-bath heating leaching 5～15 minutes, and water moves in the 50mL volumetric flask and constant volume;
The 4th step, pipette the above-mentioned solution of 1～5mL to the 25mL volumetric flask, the tartaric acid solution of adding concentration and be 60g/L is to 5ml, adding concentration is EDTA solution 0.50mL, the sulfuric acid solution 1mL that concentration is 50g/L, the 5-Br-PADAP solution 3mL that concentration is 5g/L of 40g/L, whenever add the equal mixing of a kind of reagent, be diluted with water to scale and shake up, boil and took off cooling in 5～10 minutes, with the sample blank is reference, and 605nm sentences the 1cm cuvette and surveys its absorbance on 721 type spectrophotometers;
In the 5th step, find Nb from the niobium working curve 2O 5Amount is calculated content of niobium then.
5. the assay method of content of niobium is characterized in that in the tungsten carbide as claimed in claim 4,
For the sample that adds niobium and tantalum simultaneously, then the 4th step was:
Pipette in 1～5mL to the 25mL volumetric flask, the tartaric acid solution of adding concentration and be 60g/L is to volume 5mL, adding concentration respectively is the EDTA solution 0.5mL of 40g/L, concentration is the tartaric acid solution 5mL of 500g/L, concentration is the sulfuric acid solution 1mL of 50g/L, concentration is the 5-Br-PADAP solution 3mL of 5g/L, whenever adding a kind of reagent all need shake up, water is rare to scale and mixing, boiled 5～10 minutes, taking off cooling, is reference with the sample blank, and 605nm sentences the 1cm cuvette and surveys its absorbance on 721 type spectrophotometers.
6. the assay method of content of niobium is characterized in that in the tungsten carbide as claimed in claim 1, and described tannic acid is precipitated as in acid medium and adds tannic acid and make niobium or niobium and tantalum separate with other impurity except that tungsten, eliminates its interference.
7. the assay method of content of niobium is characterized in that in the tungsten carbide as claimed in claim 1, and described colourimetry is meant at aqueous phase carries out spectrphotometric method for measuring, has avoided carrying out in organic phase spectrphotometric method for measuring.
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CN103185697A (en) * 2011-12-27 2013-07-03 北京有色金属研究总院 Measurement method for content of niobium in iron-based amorphous alloy
CN103185698A (en) * 2011-12-27 2013-07-03 北京有色金属研究总院 Measurement method for content of copper in iron-based amorphous alloy
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