CN103529015A - Method for analyzing and detecting cobalt, nickel, iron, titanium and chromium in tungsten carbide - Google Patents
Method for analyzing and detecting cobalt, nickel, iron, titanium and chromium in tungsten carbide Download PDFInfo
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- CN103529015A CN103529015A CN201210232955.0A CN201210232955A CN103529015A CN 103529015 A CN103529015 A CN 103529015A CN 201210232955 A CN201210232955 A CN 201210232955A CN 103529015 A CN103529015 A CN 103529015A
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Abstract
The invention provides a method for analyzing and detecting cobalt, nickel, iron, titanium and chromium in tungsten carbide. By a basal body matching method, the loss of other detection elements caused by a tungsten removal process is avoided; a sample is dissolved by using ammonium sulfate and sulfuric acid; tungsten produced by dissolving the tungsten carbide is complexed by using a citric acid-ammonia water solution; then ICP (inductively coupled plasma) detection is performed, so that a low detection limit and high recycling rate can be achieved. The method is convenient and quick and can be used for accurately detecting the content of cobalt, nickel, iron, titanium and chromium in the tungsten carbide.
Description
Technical field
The present patent application relates to a kind of analyzing detecting method, and especially a kind of ICP of utilization carries out the method for analyzing and testing to the element cobalt in tungsten carbide, nickel, iron, titanium and chromium.
Background technology
Tungsten carbide (WC) is the primary raw material of manufacturing wimet, is also the important source material powder that field of thermal spray is prepared high abrasion coating.WC hardness is high, and particularly its high temperature hardness is high, can be wetting by metal baths such as Co, Ni, Fe well.Detection for cobalt, nickel, iron, titanium, chromium in tungsten carbide has a lot of methods, comprise atomic emission spectrometry, atomic absorption spectrography (AAS), spectrophotometric method, mass spectroscopy etc., but because tungsten itself has abundant spectrum line, a lot of detection method to the mensuration of many elements, exist background interference or peak position overlapping in various degree just disturbing or negative interference, so all tentatively will be carried out the detection of other elements again after tungsten separation.
But existing detection method, except in the process of tungsten, tends to cause the loss of other detection elements, has caused the inaccurate of testing result, causes detection limit higher simultaneously; In addition, the method also having, AAS method for example, also can be for detection of, but can only detect a kind of element at every turn, and detection efficiency is lower.
Summary of the invention
The present patent application is for existing above-mentioned weak point in the detection method of the metallic elements such as cobalt, nickel, iron, titanium, chromium in current tungsten carbide, provide a kind of convenient and swift, detection efficiency is high, detection limit is lower, the detection method that the recovery is higher.
Described in the present patent application, the detection thinking of method is: by the method for Matrix Match, avoid causing except tungsten process the loss of other detection elements, with ammonium sulfate and sulfuric acid dissolution sample, and the tungsten producing after dissolving with citric acid-ammonia spirit complexing tungsten carbide, then carry out ICP detection, thereby obtain low detection limit and the high recovery.This method is convenient, fast, can accurately detect the content of cobalt in tungsten carbide, nickel, iron, titanium, chromium.
Specifically, the analyzing detecting method of cobalt, nickel, iron, titanium and chromium in tungsten carbide described in the present patent application, comprise following step: with ammonium sulfate and concentrated sulfuric acid solution, dissolve tungsten carbide sample, then the tungsten producing after dissolving with citric acid-ammonia spirit complexing tungsten carbide, the method for recycling ICP detects the content of cobalt, nickel, iron, titanium and chromium in tungsten carbide sample.
ICP is that the English of inductively coupled plasma (inductively coupled plasma) is called for short, and the method for carrying out species analysis detection according to the principle of ICP is called as ICP-AES.The method is after being excited according to gaseous atom in sample material (or ion), and when its outer-shell electron turns back to ground state by excited state, the characteristic radiation energy (different spectrum) that radiation transistion is launched is studied a kind of method of the chemical composition of material.Its theory is: atom is comprised of atomic nucleus placed in the middle and outer-shell electron, outer-shell electron moves at different energy levels around atomic nucleus, the ground state of outer-shell electron in minimum energy generally, when the outer-shell electron of ground state is subject to the lower energy jump that absorbs certain feature of outside energy (as electric arc, electric spark, high-frequency electrical energy etc.) effect to high another stationary state (excited state) of energy, electronics in excited state is also unstable, and about 10
-8second will return to ground state or other lower energy level, and the energy absorbing during by electronic transition discharges with the form of light, the generation principle of common atomic emissions that Here it is, Atomic Emission Spectral Analysis process is mainly divided three steps, excites, light splitting and detection.ICP method has been conventional method during species analysis detects now, for detecting different materials, its difference is mainly the testing conditions of ICP method to arrange, and these testing conditions comprise: RF incident power, plasma gas flow velocity, assisted gas flow velocity, flow rate of carrier gas, spectroscopic temperature, integral time and integral number of times.
Further, described ammonium sulfate is analytical pure sulfuric acid ammonium, described ammonium sulfate is analytical pure sulfuric acid ammonium, the described concentrated sulphuric acid is for analyzing the pure concentrated sulphuric acid, in described citric acid-ammonia spirit, the amount of citric acid is 25% of citric acid-ammonia spirit, and the amount of the ammoniacal liquor that concentration is 10-20% is citric acid-ammonia spirit 50%, and all the other compositions of citric acid-ammonia spirit are pure water.
Further, in described method, the mass ratio of tungsten carbide and ammonium sulfate is 2-5:40-50.
Further, in described method, the mass volume ratio of tungsten carbide and the concentrated sulphuric acid is 0.2-0.5g:5-10mL.
Further, in described method, the mass volume ratio of tungsten carbide and citric acid-ammonia spirit is 0.2-0.5g:20-30mL.
Further, the testing conditions of described ICP method is: RF incident power is 1.0-1.4Kw, plasma gas flow velocity is 12.0-16.0L/min, assisted gas flow velocity is 1.0-1.4L/min, flow rate of carrier gas is 0.5-0.9L/min, spectroscopic temperature is 35 ℃-40 ℃, and be 30s-40s integral time, and integral number of times is 2-4 time.
Further, the testing conditions of described ICP method is: RF incident power is 1.2Kw, and plasma gas flow velocity is 14.0L/min, assisted gas flow velocity is 1.2L/min, and flow rate of carrier gas is 0.7L/min, and spectroscopic temperature is 38 ℃, be 35s integral time, and integral number of times is 2 times.
The analyzing detecting method of cobalt, nickel, iron, titanium and chromium in tungsten carbide described in the present patent application, tungsten carbide sample is carried out to pre-service, remove the impact of W elements on testing result, the detection method of recycling ICP detects metallic elements such as cobalt, nickel, iron, titanium and chromium, have convenient and swift, detect advantage accurately.
Embodiment
Below in conjunction with concrete embodiment, the method described in the present patent application is described; the non-restriction to described method; all with identical or approximate principle; the replacement that is equal to each reagent in described method; and the improvement to testing conditions; take and realize same effect as object, all within the present patent application technical scheme required for protection.
Embodiment mono-
The method and the element to be measured that detect cobalt, nickel, iron, titanium and chromium in tungsten carbide sample detect wavelength and detection limit
1. experiment reagent:
The concentrated sulphuric acid (analyze pure, ρ=18.4mol/L);
Ammonium sulfate (analyzing pure);
Citric acid-ammoniacal liquor (25%): take 50g citric acid and add water 50mL, ammoniacal liquor 100mL is to dissolving;
Tungsten carbide (WC, national standard material);
24 elements (Li, Be, Mg, Sr, Ba, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Cd, B, Al, Ga, Tl, Sn, Pb, As, Sb, Bi, national standard material);
2. experimental apparatus and condition of work:
Instrument: adopt ICP-7510 analyser;
Condition of work: RF incident power, 1.2KW; Plasma gas flow velocity, 14.0L/min; Assisted gas flow velocity, 1.2L/min; Flow rate of carrier gas, 0.7L/min; Spectroscopic temperature: 38 ℃; Integral time, 35s; Integral number of times: 2 times;
3. the preparation of typical curve:
Divide the tungsten standard solution (100 μ g/mL) of getting 0.00mL, 0.50mL, 1.00mL, 2.50mL, 5.00mL, be placed in 100mL beaker and add 4g (NH
4)
2sO
4with the 5mL concentrated sulphuric acid, be heated to solution limpid, be cooled to room temperature (18-25 ℃), add 20mL citric acid-ammonia spirit, constant volume, in 250mL volumetric flask, complements to groove with pure water;
4. the detection of sample:
Take tungsten carbide sample 0.25g in 100mL beaker, add 4g (NH
4)
2sO
4with the 10mL concentrated sulphuric acid, add a cover the boiling of heating after surface plate limpid, coolingly use pure water rinsing surface plate afterwards, and then add 30mL citric acid-ammonia spirit limpid to solution, constant volume in 250mL volumetric flask with to be detected;
5. element to be measured detects wavelength and detection limit:
Each element detects wavelength as following table:
Sample blank continuous sample introduction is measured 10 times, with 3 times of standard deviation calculation, is obtained the method detection limit of each element:
Embodiment bis-
The method and the element to be measured that detect cobalt, nickel, iron, titanium and chromium in tungsten carbide sample detect wavelength and detection limit
1, experiment reagent:
The concentrated sulphuric acid (analyze pure, ρ=18.4mol/L);
Ammonium sulfate (analyzing pure);
Citric acid-ammoniacal liquor (25%): take 50g citric acid and add water 50mL, ammoniacal liquor 100mL is to dissolving;
Tungsten carbide (WC, national standard material);
24 elements (Li, Be, Mg, Sr, Ba, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Cd, B, Al, Ga, Tl, Sn, Pb, As, Sb, Bi, national standard material);
2, experimental apparatus and condition of work:
Instrument: adopt ICP-7510 analyser;
Condition of work: RF incident power, 1.0KW; Plasma gas flow velocity, 12.0L/min; Assisted gas flow velocity, 1.0L/min; Flow rate of carrier gas, 0.5L/min; Spectroscopic temperature: 35 ℃; Integral time, 30s; Integral number of times: 3 times;
3, the preparation of typical curve:
Divide the tungsten standard solution (100 μ g/mL) of getting 0.00mL, 0.50mL, 1.00mL, 2.50mL, 5.00mL, be placed in 100mL beaker and add 4g (NH
4)
2sO
4with the 5mL concentrated sulphuric acid, be heated to solution limpid, be cooled to room temperature (18-25 ℃), add 20mL citric acid-ammonia spirit, constant volume, in 250mL volumetric flask, complements to groove with pure water;
4, the detection of sample:
Take tungsten carbide sample 0.20g in 100mL beaker, add 4.50g (NH
4)
2sO
4with the 5mL concentrated sulphuric acid, add a cover the boiling of heating after surface plate limpid, coolingly use pure water rinsing surface plate afterwards, and then add 20mL citric acid-ammonia spirit limpid to solution, constant volume in 250mL volumetric flask with to be detected;
5, element to be measured detects wavelength and detection limit:
Each element detects wavelength as following table:
Sample blank continuous sample introduction is measured 10 times, with 3 times of standard deviation calculation, is obtained the method detection limit of each element:
In this embodiment, in detection method, the change of amount of reagent, does not affect detection wavelength and the detection limit of each element.
Embodiment tri-
The method and the element to be measured that detect cobalt, nickel, iron, titanium and chromium in tungsten carbide sample detect wavelength and detection limit
1, experiment reagent:
The concentrated sulphuric acid (analyze pure, ρ=18.4mol/L);
Ammonium sulfate (analyzing pure);
Citric acid-ammoniacal liquor (25%): take 50g citric acid and add water 50mL, ammoniacal liquor 100mL is to dissolving;
Tungsten carbide (WC, national standard material);
24 elements (Li, Be, Mg, Sr, Ba, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Cd, B, Al, Ga, Tl, Sn, Pb, As, Sb, Bi, national standard material);
2, experimental apparatus and condition of work:
Instrument: adopt ICP-7510 analyser;
Condition of work: RF incident power, 1.4KW; Plasma gas flow velocity, 16.0L/min; Assisted gas flow velocity, 1.4L/min; Flow rate of carrier gas, 0.9L/min; Spectroscopic temperature: 40 ℃; Integral time, 40s; Integral number of times: 4 times;
3, the preparation of typical curve:
Divide the tungsten standard solution (100 μ g/mL) of getting 0.00mL, 0.50mL, 1.00mL, 2.50mL, 5.00mL, be placed in 100mL beaker and add 4g (NH
4)
2sO
4with the 5mL concentrated sulphuric acid, be heated to solution limpid, be cooled to room temperature (18-25 ℃), add 20mL citric acid-ammonia spirit, constant volume, in 250mL volumetric flask, complements to groove with pure water;
4, the detection of sample:
Take tungsten carbide sample 0.50g in 100mL beaker, add 5.0g (NH
4)
2sO
4with the 10mL concentrated sulphuric acid, add a cover the boiling of heating after surface plate limpid, coolingly use pure water rinsing surface plate afterwards, and then add 30mL citric acid-ammonia spirit limpid to solution, constant volume in 250mL volumetric flask with to be detected;
5, element to be measured detects wavelength and detection limit:
Each element detects wavelength as following table:
Sample blank continuous sample introduction is measured 10 times, with 3 times of standard deviation calculation, is obtained the method detection limit of each element:
In this embodiment, in detection method, the change of amount of reagent, does not affect detection wavelength and the detection limit of each element.
Embodiment tetra-
Recovery testu:
Select a tungsten carbide actual sample, quantitatively add the standard solution of element to be measured, carry out recovery testu, testing result is as following table:
Embodiment five
The contrast experiment of ICP and AAS:
ICP and AAS adopt identical tungsten basal body standard solution to carry out the detection of cobalt, nickel, iron, titanium, chromium, and its result is as follows:
As seen from the above table, adopt ICP similar with the result that AAS obtains each detection elements, but AAS method can not detect Ti, therefore there is no testing result; As the table shows, adopt ICP method can detect a plurality of elements simultaneously, convenient and swift, improved detection efficiency.
Claims (7)
1. the analyzing detecting method of cobalt, nickel, iron, titanium and chromium in a tungsten carbide, it is characterized in that, comprise following step: with ammonium sulfate and concentrated sulfuric acid solution, dissolve tungsten carbide sample, then the tungsten producing after dissolving with citric acid-ammonia spirit complexing tungsten carbide, the method for recycling ICP detects the content of cobalt, nickel, iron, titanium and chromium in tungsten carbide sample.
2. described analyzing detecting method according to claim 1, it is characterized in that: described ammonium sulfate is analytical pure sulfuric acid ammonium, the described concentrated sulphuric acid is for analyzing the pure concentrated sulphuric acid, in described citric acid-ammonia spirit, the amount of citric acid is 25% of citric acid-ammonia spirit, concentration is that the amount of the ammoniacal liquor of 10-20% is citric acid-ammonia spirit 50%, and all the other compositions of citric acid-ammonia spirit are pure water.
3. described analyzing detecting method according to claim 1, is characterized in that: in described method, the mass ratio of tungsten carbide and ammonium sulfate is 2-5:40-50.
4. described analyzing detecting method according to claim 1, is characterized in that: in described method, the mass volume ratio of tungsten carbide and the concentrated sulphuric acid is 0.2-0.5g:5-10mL.
5. described analyzing detecting method according to claim 1, is characterized in that: in described method, the mass volume ratio of tungsten carbide and citric acid-ammonia spirit is 0.2-0.5g:20-30mL.
6. according to the analyzing detecting method described in claim 1-5 any one, it is characterized in that: the testing conditions of described ICP method is: RF incident power is 1.0-1.4Kw, plasma gas flow velocity is 12.0-16.0L/min, assisted gas flow velocity is 1.0-1.4L/min, flow rate of carrier gas is 0.5-0.9L/min, spectroscopic temperature is 35 ℃-40 ℃, and be 30s-40s integral time, and integral number of times is 2-4 time.
7. analyzing detecting method according to claim 6, it is characterized in that: in described ICP method, RF incident power is 1.2Kw, plasma gas flow velocity is 14.0L/min, assisted gas flow velocity is 1.2L/min, and flow rate of carrier gas is 0.7L/min, and spectroscopic temperature is 38 ℃, be 35s integral time, and integral number of times is 2 times.
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| CN105823772A (en) * | 2015-01-09 | 2016-08-03 | 自贡硬质合金有限责任公司 | Method for detecting impurity element in tungsten carbide |
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| CN101303307A (en) * | 2008-07-08 | 2008-11-12 | 株洲硬质合金集团有限公司 | Analyses testing method of aluminum, calcium, iron, molybdenum, niobium, titanium, tungsten impurity elements in chromium carbide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105823772A (en) * | 2015-01-09 | 2016-08-03 | 自贡硬质合金有限责任公司 | Method for detecting impurity element in tungsten carbide |
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