CN100356161C - Rapid analysis and detection method for tin element in tungsten smelting - Google Patents
Rapid analysis and detection method for tin element in tungsten smelting Download PDFInfo
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- CN100356161C CN100356161C CNB2004100471006A CN200410047100A CN100356161C CN 100356161 C CN100356161 C CN 100356161C CN B2004100471006 A CNB2004100471006 A CN B2004100471006A CN 200410047100 A CN200410047100 A CN 200410047100A CN 100356161 C CN100356161 C CN 100356161C
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Abstract
The present invention discloses a method for quickly analyzing and detecting a tin element in smelting tungsten, which comprises the following steps: sample solution is added to sodium hydroxide and hydrogen peroxide solution to be heated and pretreated; a pH value is adjusted to 8 to 9 by tartaric acid solution; a tartaric acid complexing agent and a masking agent containing ferric ions are added; the tartaric acid solution is used as a carrying current and is led into a reactor of a generation and separation device of flow injection hydride with potassium borohydride solution at the same time, and the tin element generates SnH4 and escapes; carrying gas mixed by high-purity nitrogen gas and oxygen according to the proportion of 1:0.005 to 0.02 is used for leading the SnH4 into an electric heating quartz pipe furnace to be heated, carrying gas flux is controlled to 150 to 300 ml/min, heating temperature is from 820 to 850 DEG C, and tin ground state atoms are generated by decomposing the SnH4; and an atomic absorption spectrum analyzer is used for measuring the absorption value of the tin ground state atoms, and results are calculated and analyzed. The method quickly measures the tin element, sensitivity is high, an analytical cycle is only 20 minutes, a detection lower limit reaches 0.00001 g/L, the repeatability of the analysis results is good, and the method is suitable for measuring micro and trace tin.
Description
Technical field
The express-analysis that the present invention relates to tin element detects, particularly the rapid analysis and test method of tin element in various sample control analyses and the check analysis in the tungsten smelting process.
Background technology
In existing tin element analyzing detecting method, the more numerous and diverse Chemical Decomposition means of general all employings after making tin element and other interference element separating, are measured again.Because complicated operating process, analytical cycle is longer, is difficult to satisfy the requirement of production run express-analysis, can't realize express-analysis especially for the solution example in matrix and the impurity element variation tungsten smelting process greatly.And chemical analysis method exists also for the mensuration of trace and Determination of Trace Tin that stability is bad, the shortcoming of poor reproducibility.For example: extraction-spectrophotometry tin (standard GB/T4324.3-1984 tungsten chemical analysis method), related step: sample leaches and handles, adjusts potential of hydrogen, complexing processing, extract and separate main body tungsten, washs organic phase, tin replaced into water, complexing shelter impurity, add chromogenic reagent, carry out ultimate analysis by spectrophotometer, analytical cycle reaches four hours, and the detection lower limit of actual sample can only reach 0.0005g/L.
Summary of the invention
The objective of the invention is to overcome the defective that above-mentioned chemical analysis detection method exists, a kind of easy, analysis precision of tin element analyzing detecting method, and raising fast is provided, detect with the express-analysis that adapts to various complex samples in the tungsten smelting process.
For realizing that the object of the invention has adopted the tin element that makes in the sample to generate the ground state tin atom, with Atomic Absorption Spectrometer the ground state tin atom that generates is carried out the technical scheme of analyzing and testing then, concrete step comprises:
(1) sample solution is added NaOH and superoxol and carries out heating pretreatment, perhaps to the solid slag specimen with sodium peroxide heating and melting, hydrolysis, be filtered into solution and carry out heating pretreatment;
(2) after the cooling of pre-service sample, adjusting acidity to pH value with tartaric acid solution is 8～9;
(3) will adjust and add the tartrate complexing agent in the solution of pH value and contain the ferric ion screening agent, make tin element and matrix tungsten and separation of foreign elements;
(4) isolated stanniferous sample for determining component content is made current-carrying and solution of potassium borohydride with tartaric acid solution and is imported simultaneously that mobile injection of hydride takes place and the reactor of tripping device, makes element tin generation SnH
4Overflow and separate fully with matrix tungsten and impurity element;
(5) carrier gas that mixes in 1: 0.005～0.02 ratio with high pure nitrogen and oxygen is with the SnH that generates
4Importing is positioned at the electrothermal quartz tube stove heating on the Atomic Absorption Spectrometer burner, and the control carrier gas flux is 150～300ml/min, and the air-flow output pressure is 0.25Mpa, and heating-up temperature is 820～850 ℃, makes SnH
4Decompose and generate the ground state tin atom;
(6) with the light absorption value of measuring the ground state tin atom that atomic absorption spectrometry that light path passes through from the electrothermal quartz tube center generates, Calculation results then.
When the inventive method was implemented, the heating pretreatment naoh concentration was preferably 100g/L, and concentration of hydrogen peroxide is preferably 3%.
When the inventive method is implemented, solid slag specimen heating pretreatment be with sample with sodium peroxide heating and melting, hydrolysis, be filtered into solution, add tartaric acid solution adjustment pH value again.
When the inventive method was implemented, the tartaric acid concentration of adjusting pH value was preferably 100～200g/L.
When the inventive method was implemented, the tartrate complexing agent concentration of adding was preferably 100～200g/L; Contain ferric ion screening agent concentration and be preferably 10～20g/L.
When the inventive method was implemented, the tartaric acid concentration that imports mobile injection of hydride generation and tripping device reactor was preferably 30～50g/L, and potassium borohydride concentration is preferably 15～30g/L.
Implement the analysis detecting data collection of the inventive method and result and calculate substantially that computing method are close as a result with conventional Atomic Absorption Spectrometer data acquisition and conventional analysis, specifically:
Employing has the Atomic Absorption Spectrometer of time-delay reading function computer data processing system, reading adopts continuity method or peak area method during mensuration, and time-delay is 8 seconds when adopting continuity method, 0.5 second integral time, continuous-reading 10 times is got in 10 times full-scale reading by being surveyed light absorption value; Time-delay is 5 seconds during with peak area method, 0.5 second integral time, reads light absorption value.Carrying out blank determination and standard series when measuring sample measures.
Analyzing and testing result calculates:
1. look into standard working curve result of calculation as follows.
In the formula: C represents the Sn concentration (g/L) that checks in sample light absorption value correspondence on the standard working curve.
C
0Represent the Sn concentration (g/L) that checks in blank light absorption value correspondence on the standard working curve.
The volume (L) of solution is measured in the V representative.
The quality (g) of sample is measured in the m representative.
2. the result is calculated and demonstrated to automatic data processing by following linear equation;
Property line equation: [C]=K
1[A]+K
0
C by the concentration of mensuration sample
A is by being surveyed light absorption value
K
1, K
0Be equation coefficient.
Advantage of the present invention is highly sensitive to the fast measuring of tin element in the tungsten smelting process, simple and efficient, analytical cycle reduces greatly, only about 20 minutes, actual sample detects lower limit and reaches 0.00001g/L, be suitable for very much matrix and impurity element in the sub-tungsten smelting process change greatly solution and solid sample in the assay determination of trace and Determination of Trace Tin, and the result is stable, consistent, favorable reproducibility.
Description of drawings
Fig. 1 is the principle of work synoptic diagram of mobile injection of hydride generation of the present invention and tripping device;
Fig. 2 is the standard working curve figure of the present invention with Atomic Absorption Spectrometry.
Embodiment
Below in conjunction with drawings and Examples tin element rapid analysis and test method of the present invention is described in further detail.
Embodiment 1: the mensuration of tin in the sodium tungstate solution (sample S-1):
Drawing curve or set up linear equation
The metallic tin adding concentrated hydrochloric acid preparation mass concentration of getting purity 99.99% is the tin standard solution of stanniferous 0.01mg/mL; Get pure WO
3(stanniferous＜0.0001%) adds NaOH and hydrochloric acid is prepared mass concentration for containing WO
3The sodium tungstate solution of 100mg/ml is made standard series by the step of the inventive method and is measured and draw atomic absorption spectrum standard working curve (as Fig. 2).Specific operation process is: drawing mass concentration respectively is the tin standard solution 0,0.5,1.0,1.5 of 0.01 mg/ml, and 2.0ml is in the 100ml volumetric flask, and adding mass concentration is the tartrate 20ml of 200g/L, shakes up, and adds mass concentration again for containing WO
3The sodium tungstate solution 5ml of 100mg/ml, mass concentration is the ferric iron solution 5ml of 10g/L, is diluted to 100ml and shakes up, and is every ml and contains Sn 0,0.05, the series standard solution of 0.1,0.15,0.20 μ g.Solution of potassium borohydride, the mass concentration of getting above-mentioned standard solution, mass concentration respectively and be 20g/L are the tartaric acid solution of 30g/L, the input mobile injection of hydride take place and tripping device in.The SnH that the reaction back produces
4Import the ground state atom that decomposes generation tin in the electrothermal quartz tube with carrier gas, light absorption value by atomic absorption spectrometry tinbase attitude atom, light absorption value according to the series standard solution of measuring, with the series standard solution concentration is abscissa, corresponding light absorption value is an ordinate, drawing standard working curve or with series standard solution concentration and corresponding light absorption value is set up aforementioned linear equation.Solution of potassium borohydride is to get a certain amount of potassium borohydride to add mass concentration be NaOH and water-soluble the separating of 100g/L, being diluted to 100ml refilters formulated, with using with joining (the tin standard series is measured and the drawing standard working curve, and compound method following examples of solution of potassium borohydride are all identical).
Sample determination
Get testing sample sodium tungstate solution 2ml in 100ml iron and steel measuring bottle.Adding mass concentration is the sodium hydroxide solution 10ml of 100g/L, adds water 5ml, drips the hydrogen peroxidase 10 .5ml of concentration by volume 3%, boils about 3min, makes the tin in the sample change into tetravalent tin; Be cooled to room temperature after boiling, add water 50ml, drip 1 of 1% phenolphthalein indicator, it is colourless to be with mass concentration that the tartrate of 200g/L is neutralized to, and making pH value is 98; Adding mass concentration then is the tartrate 20ml of 200g/L, and mass concentration is the iron nitrate solution 5ml of 10g/L, and matrix tungsten and impurity element are sheltered in complexing, make tin element and matrix tungsten and separation of foreign elements, is diluted with water to 100ml again and shakes up, to be determined.
Get the above-mentioned solution to be determined for preparing (2 in the accompanying drawing 1), mass concentration and be the tartaric acid solution (3 in the accompanying drawing 1) of 30g/L and solution of potassium borohydride (1 in the accompanying drawing 1) that mass concentration is 20g/L import simultaneously that mobile injection of hydride takes place and the power induction system 5 of tripping device in, 6 of accompanying drawing 1 is the flowmeter measuring device, measure the amount (solution to be determined and solution of potassium borohydride are preferably mensuration 1.5ml/ time, and following examples are all identical) of solution to be determined and solution of potassium borohydride respectively.Solution to be determined is that carrier and solution of potassium borohydride are sent in the reactor 7 by power induction system 5 respectively with the tartaric acid solution, and tin element in the solution to be determined and potassium borohydride react the gaseous state SnH that the back produces in reactor 7
4After gas-liquid separator 8 separated, after the carrier gas 4 that power induction system 5 is sent into imports the heating of electrothermal quartz tube stove, this carrier gas was mixed in 1: 0.01 ratio by high pure nitrogen and oxygen by 9 meterings of the flowmeter measuring device in the accompanying drawing 1.The electrothermal quartz tube stove is the T type quartz ampoule of ф 7 * 140mm, the long 70mm of center admission piece, heat around heating wire, should be placed on the burner of Atomic Absorption Spectrometer, and make the measurement light path of Atomic Absorption Spectrometer pass through (each solution from the electrothermal quartz tube center, reagent, the mobile transport way of carrier gas in generation of injection hydride and tripping device, electrothermal quartz tube stove and position thereof and Atomic Absorption Spectrometer are measured the position of light path, following examples are all identical), the control carrier gas flux is 150ml/min, the air-flow output pressure is 0.25Mpa, heating-up temperature is 820 ℃, makes SnH
4In Sn decompose to generate the ground state atom of tin, the light absorption value of the tinbase attitude atom that generates by atomic absorption spectrometry, measure blank light absorption value simultaneously, other running parameter of Atomic Absorption Spectrometer is for measuring wavelength 286.3nm, lamp current 6mA, high pressure 500V, slit width 0.5nm (other running parameter of Atomic Absorption Spectrometer, following examples are all identical).
Ground state atom light absorption value according to the tin of measuring, by aforesaid standards curvilinear equation result of calculation or to look into standard working curve result of calculation be that a plurality of analyzing and testing results' of sample sodium tungstate solution the Sn mean value that contains is 0.0102g/L, standard deviation (δ) 0.00023, relative standard deviation 2.3%.
Embodiment 2: the mensuration of tin in the sodium tungstate solution (sample S-2):
Get testing sample sodium tungstate solution 2ml in 100ml iron and steel measuring bottle.Adding mass concentration is the sodium hydroxide solution 10ml of 100g/L, adds water 5ml, drips the hydrogen peroxidase 10 .5ml of concentration by volume 3%, boils about 3min; Being cooled to room temperature after boiling, adding water 50ml, drip 1 of 1% methyl orange indicator, is that the tartrate of 100g/L is neutralized to and occurs redly with mass concentration, and making pH value is 8; Adding mass concentration then is the tartrate 30ml of 100g/L, and mass concentration is the liquor ferri trichloridi 5ml of 200g/L, and matrix tungsten and impurity element are sheltered in complexing, make tin element and matrix tungsten and separation of foreign elements, is diluted with water to 100ml again and shakes up, to be determined.
Getting the above-mentioned solution to be determined for preparing, mass concentration and be the tartaric acid solution of 30g/L and solution of potassium borohydride that mass concentration is 20g/L imports mobile injection of hydride simultaneously and takes place and tripping device, solution to be determined is that carrier and solution of potassium borohydride are sent into respectively in the reactor with the tartaric acid solution, the gaseous state SnH that tin element in the solution to be determined and potassium borohydride reaction back produce
4After gas-liquid separation, import the heating of electrothermal quartz tube stove by high pure nitrogen and oxygen in the carrier gas that 1: 0.005 ratio mixes, the control carrier gas flux is 300ml/min, and the air-flow output pressure is 0.25Mpa, and heating-up temperature is 850 ℃, makes SnH
4In tin decompose to generate the ground state atom of tin, the light absorption value of the tinbase attitude atom that is generated by atomic absorption spectrometry is measured blank light absorption value simultaneously.
Ground state atom light absorption value according to the tin of measuring, by aforesaid standards curvilinear equation result of calculation or look into standard working curve result of calculation and be: a plurality of analyzing and testing results' of sample sodium tungstate solution the Sn mean value that contains is 0.0184g/L, standard deviation (δ) 0.00055, relative standard deviation 3.0%.
Embodiment 3: the mensuration of tin in the ammonium tungstate solution (sample S-3):
Get testing sample ammonium tungstate solution 2ml in 100ml iron and steel measuring bottle.Adding mass concentration is the sodium hydroxide solution 10ml of 100g/L, adds water 5ml, drips the hydrogen peroxidase 10 .5ml of concentration by volume 3%, boils about 3min; Be cooled to room temperature after boiling, add water 50ml, drip 1 of 1% phenolphthalein indicator, it is colourless to be with mass concentration that the tartrate of 100g/L is neutralized to, and making pH value is 9; Adding mass concentration then is the tartrate 20ml of 200g/L, and mass concentration is the liquor ferri trichloridi 5ml of 10g/L, and matrix tungsten and impurity element are sheltered in complexing, make tin element and matrix tungsten and separation of foreign elements, is diluted with water to 100ml again and shakes up, to be determined.
Getting the above-mentioned solution to be determined for preparing, mass concentration and be the tartaric acid solution of 30g/L and solution of potassium borohydride that mass concentration is 15g/L imports mobile injection of hydride simultaneously and takes place and tripping device, solution to be determined is that carrier and solution of potassium borohydride are sent into respectively in the reactor with the tartaric acid solution, the gaseous state SnH that tin element in the solution to be determined and potassium borohydride reaction back produce
4After gas-liquid separation, import the heating of electrothermal quartz tube stove by high pure nitrogen and oxygen in the carrier gas that 1: 0.008 ratio mixes, the control carrier gas flux is 200ml/min, and the air-flow output pressure is 0.25Mpa, and heating-up temperature is 850 ℃, makes SnH
4In Sn decompose to generate the ground state atom of tin, the light absorption value of the tinbase attitude atom that is generated by atomic absorption spectrometry is measured blank light absorption value simultaneously.
Ground state atom light absorption value according to the tin of measuring, by aforesaid standards curvilinear equation result of calculation or look into standard working curve result of calculation and be: a plurality of analyzing and testing results' of sample ammonium tungstate solution the Sn mean value that contains is 0.0024g/L, standard deviation (δ) 0.0001, relative standard deviation 4.16%.
Embodiment 4: the mensuration of tin in the sodium tungstate solution (sample S-4):
Get testing sample sodium tungstate solution 2ml in 100ml iron and steel measuring bottle.Adding mass concentration is the sodium hydroxide solution 10ml of 100g/L, adds water 5ml, drips the hydrogen peroxidase 10 .5ml of concentration by volume 3%, boils about 3min; Be cooled to room temperature after boiling, add water 50ml,, drip 1 of 1% methyl orange indicator, be that the tartrate of 200g/L and boric acid mixed solution (boronic acid containing saturated solution 30%) are neutralized to and occur redly with mass concentration, making pH value is 8; Adding mass concentration then is the tartrate 20ml of 200g/L, and mass concentration is the iron nitrate solution 5ml of 20g/L, and matrix tungsten and impurity element are sheltered in complexing, make tin element and matrix tungsten and separation of foreign elements, is diluted with water to 100ml again and shakes up, to be determined.
Getting the above-mentioned solution to be determined for preparing, mass concentration and be the tartaric acid solution of 50g/L and solution of potassium borohydride that mass concentration is 30g/L imports mobile injection of hydride simultaneously and takes place and tripping device, solution to be determined is that carrier and solution of potassium borohydride are sent into respectively in the reactor with the tartaric acid solution, the gaseous state SnH that tin element in the solution to be determined and potassium borohydride reaction back produce
4After gas-liquid separation, import the heating of electrothermal quartz tube stove by high pure nitrogen and oxygen in the carrier gas that 1: 0.02 ratio mixes, the control carrier gas flux is 150ml/min, and the air-flow output pressure is 0.25Mpa, and heating-up temperature is 820 ℃, makes SnH
4In Sn decompose to generate the ground state atom of tin, the light absorption value of the tinbase attitude atom that is generated by atomic absorption spectrometry is measured blank light absorption value simultaneously.
Ground state atom light absorption value according to the tin of measuring, by aforesaid standards curvilinear equation result of calculation or look into standard working curve result of calculation and be: a plurality of analyzing and testing results' of sample sodium tungstate solution the Sn mean value that contains is 0.0532g/L, standard deviation (δ) 0.00138, relative standard deviation 2.6%.
Embodiment 5: the mensuration of tin in the solid slag specimen (sample S-5):
Take by weighing sample 0.5000g in the iron crucible that fills the 1g sodium peroxide, topped more above 1g sodium peroxide places 780 ℃ of muffle furnace fusions 5 minutes.Take out coldly slightly, wash the crucible appearance with water, immerse rapidly and fill in the beaker of 150ml water, shake gently, wash crucible after treating to leach fully.Leachate is cooled to move in the 200ml volumetric flask after the room temperature and is diluted to scale, shakes up, with quick filter paper filtering.Draw filtrate 10ml in 100ml iron and steel measuring bottle, add water 50ml, dripping 1 of 1% methyl orange indicator, is that the tartrate of 200g/L is neutralized to red the appearance with mass concentration, and making pH value is 8, adding mass concentration then is the tartrate 20ml of 200g/L, mass concentration is the liquor ferri trichloridi 5ml of 10g/L, and matrix tungsten and impurity element are sheltered in complexing, makes tin element and matrix tungsten and separation of foreign elements, be diluted with water to 100ml again and shake up, to be determined.
Getting the above-mentioned solution to be determined for preparing, mass concentration and be the tartaric acid solution of 30g/L and solution of potassium borohydride that mass concentration is 20g/L imports mobile injection of hydride simultaneously and takes place and tripping device, solution to be determined is that carrier and solution of potassium borohydride are sent into respectively in the reactor with the tartaric acid solution, the gaseous state SnH that tin element in the solution to be determined and potassium borohydride reaction back produce
4After gas-liquid separation, import the heating of electrothermal quartz tube stove by high pure nitrogen and oxygen in the carrier gas that 1: 0.01 ratio mixes, the control carrier gas flux is 150ml/min, and the air-flow output pressure is 0.25Mpa, and heating-up temperature is 820 ℃, makes SnH
4In Sn decompose to generate the ground state atom of tin, the light absorption value of the tinbase attitude atom that is generated by atomic absorption spectrometry is measured blank light absorption value simultaneously.
Ground state atom light absorption value according to the tin of measuring, by aforesaid standards curvilinear equation result of calculation or look into standard working curve result of calculation and be: a plurality of analyzing and testing results' of sample solid slag specimen the Sn mean value that contains is 0.10%, standard deviation (δ) 0.004, relative standard deviation 4.0%.
Embodiment 6: the mensuration (sample S-6) of tin in the ammonium paratungstate (APT):
Get testing sample ammonium paratungstate 1.0000g in 100ml iron and steel measuring bottle, add water 50ml, adding mass concentration after the heating for dissolving again is the sodium hydroxide solution 10ml of 100g/L, drips the hydrogen peroxidase 10 .5ml of concentration by volume 3%, boils about 3min; Be cooled to room temperature after boiling, drip 1 of 1% phenolphthalein indicator, with mass concentration is that the tartrate of 200g/L is neutralized to colourless, making pH value is 9 to add the tartrate 20ml that mass concentration is 200g/L then, mass concentration is the liquor ferri trichloridi 5ml of 20g/L, and matrix tungsten and impurity element are sheltered in complexing, makes tin element and matrix tungsten and separation of foreign elements, be diluted with water to 100ml again and shake up, to be determined.
Getting the above-mentioned solution to be determined for preparing, mass concentration and be the tartaric acid solution of 30g/L and solution of potassium borohydride that mass concentration is 20g/L imports mobile injection of hydride simultaneously and takes place and tripping device, solution to be determined is that carrier and solution of potassium borohydride are sent into respectively in the reactor with the tartaric acid solution, the gaseous state SnH that tin element in the solution to be determined and potassium borohydride reaction back produce
4After gas-liquid separation, import the heating of electrothermal quartz tube stove by high pure nitrogen and oxygen in the carrier gas that 1: 0.01 ratio mixes, the control carrier gas flux is 150ml/min, and the air-flow output pressure is 0.25Mpa, and heating-up temperature is 820 ℃, makes SnH
4In Sn decompose to generate the ground state atom of tin, the light absorption value of the tinbase attitude atom that is generated by atomic absorption spectrometry is measured blank light absorption value simultaneously.
Ground state atom light absorption value according to the tin of measuring, by aforesaid standards curvilinear equation result of calculation or look into standard working curve result of calculation and be: a plurality of analyzing and testing results' of sample ammonium paratungstate the Sn mean value that contains is 0.0001%, standard deviation (δ) 0.000009, relative standard deviation 8.9%.
Claims (5)
1. the rapid analysis and test method of tin element comprised the steps: during a tungsten was smelted
(1) sample solution is added NaOH and superoxol carries out heating pretreatment, perhaps to the solid slag specimen with sodium peroxide heating and melting, hydrolysis, be filtered into solution and carry out heating pretreatment;
(2) after the cooling of pre-service sample, adjust pH value to 8～9 with tartaric acid solution;
(3) in the solution of adjusting pH value, add the tartaric acid solution complexing agent and contain ferric ion solution screening agent, make tin element and matrix tungsten and separation of foreign elements;
(4) isolated stanniferous sample for determining component content is made current-carrying and solution of potassium borohydride with tartaric acid solution and is imported simultaneously that mobile injection of hydride takes place and the reactor of tripping device, makes element tin generation SnH
4Overflow and separate fully with matrix tungsten and impurity element;
(5) the special-purpose carrier gas that mixes in 1: 0.005～0.02 ratio with high pure nitrogen and oxygen is with the SnH that generates
4Importing is positioned at the electrothermal quartz tube stove heating on the Atomic Absorption Spectrometer burner, and the control carrier gas flux is 150～300ml/min, and the air-flow output pressure is 0.25Mpa, and heating-up temperature is 820～850 ℃, makes SnH
4Decompose and generate the ground state tin atom;
(6) with the light absorption value of measuring the ground state tin atom that atomic absorption spectrometry that light path passes through from the electrothermal quartz tube center generates, Calculation results then.
2. rapid analysis and test method according to claim 1, naoh concentration is 100g/L when it is characterized in that heating pretreatment, the concentration by volume of hydrogen peroxide is 3%.
3. rapid analysis and test method according to claim 1, the tartaric acid concentration that it is characterized in that adjusting pH value is 100～200g/L.
4. rapid analysis and test method according to claim 1 is characterized in that the tartaric acid solution complexing agent concentration that adds is 100～200g/L in the solution of adjusting pH value, containing ferric ion screening agent concentration is 10～20g/L.
5. rapid analysis and test method according to claim 1 is characterized in that importing that mobile injection of hydride takes place and the tartaric acid concentration of tripping device reactor is 30～50g/L, and potassium borohydride concentration is 15～30g/L.
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| US5018855A (en) * | 1988-10-26 | 1991-05-28 | Athens Corp. | Atomic absorption process monitoring |
| CN1076278A (en) * | 1992-03-09 | 1993-09-15 | 南开大学 | Flame atomic absorption spectrometry |
| CN1437014A (en) * | 2002-02-04 | 2003-08-20 | 李学璧 | Sample entering method for atomic spectrometer |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5018855A (en) * | 1988-10-26 | 1991-05-28 | Athens Corp. | Atomic absorption process monitoring |
| CN1076278A (en) * | 1992-03-09 | 1993-09-15 | 南开大学 | Flame atomic absorption spectrometry |
| CN1437014A (en) * | 2002-02-04 | 2003-08-20 | 李学璧 | Sample entering method for atomic spectrometer |
Non-Patent Citations (2)
| Title |
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| ICP-AES测定高纯钨中杂质元素 范键等.中南工业大学学报，第30卷第1期 1999 * |
| 氢化物分离SAF-CTMAB光度法测定钨产品中的锡 魏萍.硬质合金，第15卷第3期 1998 * |
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