CN103940806A - Analysis method for measuring gallium element in zinc oxide powder - Google Patents
Analysis method for measuring gallium element in zinc oxide powder Download PDFInfo
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Abstract
The invention belongs to an alloy macro element analysis technology, and relates to an analysis method for measuring a gallium element in zinc oxide powder. According to the analysis method disclosed by the invention, the zinc oxide powder is dissolved by diluted hydrochloric acid, and the hydrochloric acid-insoluble part of a test sample is completely dissolved by nitric acid. By carrying out an interference experiment, an optimal analysis spectral line is determined, and the accuracy of measurement is improved; the method is wide in measurement range; by synchronously treating the test sample and preparing a high-standard solution and a low-standard solution for measuring the gallium element, the analysis error is the minimum and the method is good in repeatability; low-content gallium element analysis can obtain a good analysis result by direct measurement; by an internal-standard element measurement method, high-content element analysis can be carried out well, the relative standard deviation is low, and the recovery rate and accuracy are high; standard sample analysis, method re-inspection and comparison of the result with analysis results of other units indicate that the formulated analysis method is good in accuracy, stable, and capable of completely meeting the requirements of trace and macro analysis.
Description
Technical field
The invention belongs to alloy macroelement analytical technology, relate to a kind of analytical approach of measuring gallium element in Zinc oxide powder.
Background technology
Zinc paste is new a kind of oxide, as fields such as a kind of adjuvant widespread use plastics, synthetic rubber, paint, electronic ceramics, cosmetics, chemical fibre and commodity.
Along with new material is constantly released, various excellent performance materials are further strict to the requirement of its composition, and in alloy, the content of various elements is most important on the impact of material property.At present, the analysis of gallium in Zinc oxide powder is not also had to examination criteria method both at home and abroad, the method about gallium that can find mostly is extract and separate rhodamine B photometry, butyl rhodamine b spectrophotometric method, graphite oven atomic absorption etc., these method operation stepss are many, and labour intensity is large, take tediously longly, be unfavorable for Fast Measurement; The inductively coupled plasma mass spectrometry of finding, inductively coupled plasma spectrometry method is respectively for the detection of gallium element in steel and alloy, precious metal alloys, very large with Zinc oxide powder materials variances, if adopt said method need to carry out lot of experiments checking, therefore see that from two aspects existing method is not suitable for the analysis needs of gallium Zinc oxide powder.
The feature that inductively coupled plasma atomic emission spectrometer (ICP) analysis has accurately, quick, multielement is analyzed simultaneously; be widely used in the fields such as geology, metallurgy, machine-building, environmental protection, biomedicine, food; there is good detection limit and analytical precision; matrix disturbs little; linear dynamic range is wide; analytical work person can be mixed with a series of standard with primary standard substance, and the advantage such as sample pretreating easy (than chemical analysis).
The means that gallium element is measured have colourimetry, ICP-AES method (ICP-AES), ICP-MS method (inductively coupled plasma atomic emissions mass spectroscopy), graphite oven atomic absorption etc. conventionally.For the different-alloy trade mark, can find corresponding analytical approach, analysis about gallium in Zinc oxide powder, at present both at home and abroad all without the method for this element of accurate analysis, substantially be all Ni-based, iron-base superalloy, noble metal or other alloy methods of applying mechanically, using method exist dissolved samples not exclusively, the selection of analytical line is uncertain etc. causes the shortcomings such as analytical cycle is long.
Summary of the invention
The object of the invention is: propose that a kind of analytical element content is higher, wide ranges, the analytical approach of gallium element in the mensuration Zinc oxide powder of gallium analysis of can accurately carrying out.
Technical scheme of the present invention is: adopt inductive coupling plasma emission spectrograph, condition of work and the analytical line of instrument are as follows: high frequency frequency: 40.68MHz; Incident power: 0.95～1.1Kw; Reflective power: < 15W; Argon flow amount: cooling gas flow: 12～20L/min; Sheath airshed: 0.1～0.6L/min; Sample lifting capacity: 1.0～1.5ml/min; Integral time: 1～10s;
(1) reagent, using in mensuration process is as follows:
(1.1), hydrochloric acid, ρ 1.19g/mL; Top grade is pure;
(1.2), nitric acid, ρ 1.42g/mL; Top grade is pure;
(1.3), hydrochloric acid, 1+1;
(1.4), aluminum standard solution: 1.00mg/mL; Take 1.0000g; > 99.99% fine aluminium, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to aluminium and dissolves completely, adds 5 nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.5), aluminum standard solution: 0.10mg/mL; Pipette 20.00mL aluminum standard solution (1.4), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.6), iron standard solution: 0.10mg/mL; Take 0.1000g; > 99.99% pure iron, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to iron and dissolves completely, adds 2mL nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.7), iron standard solution: 0.01mg/mL; Pipette 20.00mL iron standard solution (1.6), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.8), calcium standard solution: 0.10mg/mL; Take 0.2497g in advance at 105 ℃ of-110 ℃ of calcium carbonate that are dried to constant weight in 200mL beaker, add 20mL water, drip hydrochloric acid (1.3) to dissolving completely, add 5mL hydrochloric acid (1.3), heating is boiled, in cooling rear immigration 1000mL volumetric flask, be diluted with water to scale, mix;
(1.9), calcium standard solution: 0.01mg/mL; Pipette 20.00mL calcium standard solution (1.8), be placed in 200mL volumetric flask, be diluted with water to scale, shake up;
(1.10), magnesium standard solution: 0.10mg/mL; Take 0.1000g; The pure magnesium of > 99.99%, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to magnesium and dissolves completely, adds 1mL nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.11), magnesium standard solution: 0.01mg/mL; Pipette 20.00mL magnesium standard solution (1.10), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.12), copper standard solution: 0.10mg/mL; Take 0.1000g; > 99.99% fine copper, is placed in 250mL beaker, is blown into 10mL intermediate water, adds 10mL nitric acid (1.2), is heated to copper and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.13), copper standard solution: 0.01mg/mL; Pipette 20.00mL copper standard solution (1.12), be placed in 200mL volumetric flask, add 10mL nitric acid (1.2), be diluted with water to scale, shake up;
(1.14), gallium standard solution: 1.00mg/mL; Take 1.0000g; The pure gallium of > 99.99%, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to gallium and dissolves completely, adds 5 nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.15), gallium standard solution: 0.10mg/mL; Pipette 20.00mL gallium standard solution (1.14), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.16), gallium standard solution: 0.01mg/mL; Pipette 20.00mL gallium standard solution (1.15), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.17), Zinc Matrix solution, 10.0mg/mL; Take 0.500g; The pure zinc of > 99.99%, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), heating for dissolving.Be cooled to room temperature, move in 500mL volumetric flask, be diluted with water to scale, shake up;
(1.18), yttrium inner mark solution, 0.2mg/mL; Take 0.127g, > 99.95% yttria, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), and low-temperature heat, to dissolving completely, in cooling rear immigration 500mL volumetric flask, is diluted with water to scale, shakes up;
(2), sampling and sample preparation; The sample of analyzing use samples and sample preparation according to the requirement of HB/Z205;
(3) element analysis spectrum line is selected:
Prepare serial single solution, 5.0mL Zinc Matrix solution (1.17), 8.0mL Zinc Matrix solution (1.17), 5.0mL aluminum standard solution (1.5), 5.0mL aluminum standard solution (1.4), 5.0mL iron standard solution (1.7), 5.0mL calcium standard solution (1.9), 5.0mL magnesium standard solution (1.11), 5.0mL copper standard solution (1.13), 15mL hydrochloric acid (1.1), 6mL nitric acid (1.2), 2.00mL yttrium inner mark solution (1.18), 0.50mL gallium standard solution (1.16) and 5.00mL gallium standard solution (1.14) are respectively in 100mL volumetric flask, respectively above-mentioned solution is carried out on the analysis spectral line of 5-6 bar gallium to spectrogram scanning, stack, therefrom choose 2 analytic signals strong, Zinc oxide powder matrix coexistence elements disturb minimum analytical line as separated time spectral line,
(4) Zinc oxide powder solubility test
Take three parts, 0.10g sample, add respectively 5mL hydrochloric acid, 10mL hydrochloric acid, 15mL hydrochloric acid to heat on electric furnace, Zinc oxide powder dissolves not exclusively;
Take three parts, 0.10g sample, add respectively 2mL nitric acid, 4mL nitric acid, 6mL nitric acid to heat on electric furnace, Zinc oxide powder does not dissolve;
Take three parts, 0.10g sample, add respectively 5mL hydrochloric acid and 2mL nitric acid, 10mL hydrochloric acid and 4mL nitric acid, 15mL hydrochloric acid and 6mL nitric acid to heat on electric furnace, Zinc oxide powder dissolves completely;
(5) mark consumption test in yttrium
Take 0.10g sample, be accurate to 0.0001g and be placed in 150mL beaker, add 10mL hydrochloric acid (1.3), on electric hot plate, low-grade fever to test portion dissolves; From electric hot plate, take off slightly coldly, add 3mL nitric acid (1.2), low-grade fever on electric hot plate, drives away nitrogen oxides, blows water, and dissolved salts is boiled in heating; Cooling test solution is to room temperature; Move into and accurately add in the 100mL volumetric flask of 1.00mL, 2.00mL, 3.00mL, 4.00mL and 5.00mL yttrium inner mark solution (1.18), be diluted with water to scale, shake up; Research shows, while adding 2.00mL yttrium inner mark solution, measurement result relative standard deviation is minimum, measures the most stable;
(6), analytical procedure is as follows:
(6.1), test portion: take 0.10g sample, be accurate to 0.0001g;
(6.2), prepare sample solution: the test portion of analytical procedure (6.1) is placed in to 150mL beaker, adds 5mL～15mL hydrochloric acid (1.3), on electric hot plate, low-grade fever to test portion dissolves; From electric hot plate, take off slightly coldly, add 3mL～6mL nitric acid (1.2), low-grade fever on electric hot plate, drives away nitrogen oxides, blows water, and dissolved salts is boiled in heating; Cooling test solution is to room temperature; Move into and accurately add in the 100mL volumetric flask of 2.00mL yttrium inner mark solution (1.18), be diluted with water to scale, shake up;
(6.3), preparation calibration solution;
(6.3.1), prepare low mark solution; By zinc impregnation in tested Zinc oxide powder, study the low mark solution of assignment system as follows; In 100mL volumetric flask, add 5mL～15mL hydrochloric acid (1.3), add 3mL～6mL nitric acid (1.2), pipette the Zinc Matrix solution (1.17) close with test portion principal ingredient zinc content, accurately add 2.00mL yttrium inner mark solution (1.18), water is rare to scale, shakes up, as low mark solution;
(6.3.2), prepare high standard solution; By zinc impregnation in tested Zinc oxide powder, study assignment system high standard solution as follows; In 100mL volumetric flask, add 5mL～15mL hydrochloric acid (1.3), add 3mL～6mL nitric acid (1.2), pipette the Zinc Matrix solution (1.17) close with test portion principal ingredient zinc content, the gallium standard solution (1.14), (1.15), (1.16) that add different amounts, accurately add 2.00mL yttrium inner mark solution (1.18) again, and water is rare to scale, shake up, as high standard solution;
(6.4), measure the concentration of gallium in sample solution; Press the selected condition of work of inductively coupled plasma atomic emission spectrometer and analysis spectral line, take yttrium as internal standard element, adopt successively low mark solution and high standard solution to carry out standardization to instrument, then, measure the concentration of gallium in sample solution;
(7), computation and measurement result, obtain the content of gallium;
Be calculated as follows the percentage composition of element to be measured:
In formula: w---the percentage composition of gallium element in test solution, unit: %;
ρ---the mass concentration of gallium element in test solution, unit: μ g/mL;
V---test solution volume during measurement, unit: mL;
M---test portion quality, unit: g.
Advantage of the present invention is:
1) sample preparation technology is one of advantage of this invention, and the present invention adopts and adds 5mL～15mL hydrochloric acid (1.3), and on electric hot plate, low-grade fever to test portion dissolves; From electric hot plate, take off slightly coldly, add 3mL～6mL nitric acid (1.2), heating, dissolves Zinc oxide powder completely.The present invention is dissolved Zinc oxide powder with watery hydrochloric acid, with nitric acid, hydrochloric acid in sample is not dissolved to part sample and dissolves completely.
2) by carrying out interference experiment, determine optimized analysis spectral line, improved the accuracy of measuring;
3) method measurement range is wide, and it is 0.005% that measurement is rolled off the production line, and is limited to 5.0% in measurement;
4) adopt synchronous processing sample and prepare high and low mark solution and measure gallium element, analytical error is minimum, and method is reproducible;
5) low content gallium element is analyzed, and directly measurement can obtain better analysis result;
6) adopt the measuring method of internal standard element, can carry out preferably high-load ultimate analysis;
7) addition 0.005%～0.05%, the recovery 90.0%～105.0%, and relative standard deviation is less than 6.8%, addition 0.05%～5.0%, the recovery 96.0%～101.2%, relative standard deviation is less than 1.5%, and the recovery, precision are better;
8) by analysis, the method for standard model, reviewed and compared and show that made fixed analytical approach accuracy is good with other unit analysis result, method is stable, meets the requirement of trace, macro-analysis completely.
9) the application's method is measured fast, easy and simple to handle, has saved a large amount of man power and materials.
Embodiment
Embodiment mono-
Measure gallium content in Zinc oxide powder, adopt inductive coupling plasma emission spectrograph, condition of work and the analytical line of instrument are as follows: high frequency frequency: 40.68MHz; Incident power: 0.95～1.1Kw; Reflective power: < 15W; Argon flow amount: cooling gas flow: 12～20L/min; Sheath airshed: 0.1～0.6L/min; Sample lifting capacity: 1.0～1.5ml/min; Integral time: 1～10s;
(1) reagent, using in mensuration process is as follows:
(1.1), hydrochloric acid, ρ 1.19g/mL; Top grade is pure;
(1.2), nitric acid, ρ 1.42g/mL; Top grade is pure;
(1.3), hydrochloric acid, 1+1;
(1.4), aluminum standard solution: 1.00mg/mL; Take 1.0000g; > 99.99% fine aluminium, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to aluminium and dissolves completely, adds 5 nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.5), aluminum standard solution: 0.10mg/mL; Pipette 20.00mL aluminum standard solution (1.4), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.6), iron standard solution: 0.10mg/mL; Take 0.1000g; > 99.99% pure iron, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to iron and dissolves completely, adds 2mL nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.7), iron standard solution: 0.01mg/mL; Pipette 20.00mL iron standard solution (1.6), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.8), calcium standard solution: 0.10mg/mL; Take 0.2497g in advance at 105 ℃ of-110 ℃ of calcium carbonate that are dried to constant weight in 200mL beaker, add 20mL water, drip hydrochloric acid (1.3) to dissolving completely, add 5mL hydrochloric acid (1.3), heating is boiled, in cooling rear immigration 1000mL volumetric flask, be diluted with water to scale, mix;
(1.9), calcium standard solution: 0.01mg/mL; Pipette 20.00mL calcium standard solution (1.8), be placed in 200mL volumetric flask, be diluted with water to scale, shake up;
(1.10), magnesium standard solution: 0.10mg/mL; Take 0.1000g; The pure magnesium of > 99.99%, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to magnesium and dissolves completely, adds 1mL nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.11), magnesium standard solution: 0.01mg/mL; Pipette 20.00mL magnesium standard solution (1.10), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.12), copper standard solution: 0.10mg/mL; Take 0.1000g; > 99.99% fine copper, is placed in 250mL beaker, is blown into 10mL intermediate water, adds 10mL nitric acid (1.2), is heated to copper and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.13), copper standard solution: 0.01mg/mL; Pipette 20.00mL copper standard solution (1.12), be placed in 200mL volumetric flask, add 10mL nitric acid (1.2), be diluted with water to scale, shake up;
(1.14), gallium standard solution: 1.00mg/mL; Take 1.0000g; The pure gallium of > 99.99%, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to gallium and dissolves completely, adds 5 nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.15), gallium standard solution: 0.10mg/mL; Pipette 20.00mL gallium standard solution (1.14), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.16), gallium standard solution: 0.01mg/mL; Pipette 20.00mL gallium standard solution (1.15), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.17), Zinc Matrix solution, 10.0mg/mL; Take 0.500g; The pure zinc of > 99.99%, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), heating for dissolving.Be cooled to room temperature, move in 500mL volumetric flask, be diluted with water to scale, shake up;
(1.18), yttrium inner mark solution, 0.2mg/mL; Take 0.127g, > 99.95% yttria, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), and low-temperature heat, to dissolving completely, in cooling rear immigration 500mL volumetric flask, is diluted with water to scale, shakes up;
(2), sampling and sample preparation; The sample of analyzing use samples and sample preparation according to the requirement of HB/Z205;
(3) element analysis spectrum line is selected:
Prepare serial single solution, 5.0mL Zinc Matrix solution (1.17), 8.0mL Zinc Matrix solution (1.17), 5.0mL aluminum standard solution (1.5), 5.0mL aluminum standard solution (1.4), 5.0mL iron standard solution (1.7), 5.0mL calcium standard solution (1.9), 5.0mL magnesium standard solution (1.11), 5.0mL copper standard solution (1.13), 15mL hydrochloric acid (1.1), 6mL nitric acid (1.2), 2.00mL yttrium inner mark solution (1.18), 0.50mL gallium standard solution (1.16) and 5.00mL gallium standard solution (1.14) are respectively in 100mL volumetric flask, respectively above-mentioned solution is carried out on the analysis spectral line of 5-6 bar gallium to spectrogram scanning, stack, therefrom choose 294.36nm as separated time spectral line,
(4) Zinc oxide powder solubility test
Take three parts, 0.10g sample, add respectively 5mL hydrochloric acid, 10mL hydrochloric acid, 15mL hydrochloric acid to heat on electric furnace, Zinc oxide powder dissolves not exclusively;
Take three parts, 0.10g sample, add respectively 2mL nitric acid, 4mL nitric acid, 6mL nitric acid to heat on electric furnace, Zinc oxide powder does not dissolve;
Take three parts, 0.10g sample, add respectively 5mL hydrochloric acid and 2mL nitric acid, 10mL hydrochloric acid and 4mL nitric acid, 15mL hydrochloric acid and 6mL nitric acid to heat on electric furnace, Zinc oxide powder dissolves completely;
(5) mark consumption test in yttrium
Take 0.10g sample, be accurate to 0.0001g and be placed in 150mL beaker, add 10mL hydrochloric acid (1.3), on electric hot plate, low-grade fever to test portion dissolves; From electric hot plate, take off slightly coldly, add 3mL nitric acid (1.2), low-grade fever on electric hot plate, drives away nitrogen oxides, blows water, and dissolved salts is boiled in heating; Cooling test solution is to room temperature; Move into and accurately add in the 100mL volumetric flask of 1.00mL, 2.00mL, 3.00mL, 4.00mL and 5.00mL yttrium inner mark solution (1.18), be diluted with water to scale, shake up; Research shows, while adding 2.00mL yttrium inner mark solution, measurement result relative standard deviation is minimum, measures the most stable;
(6), analytical procedure is as follows:
(6.1), test portion: take 0.10g sample, be accurate to 0.0001g;
(6.2), prepare sample solution: the test portion of analytical procedure (6.1) is placed in to 150mL beaker, adds 5mL hydrochloric acid (1.3), on electric hot plate, low-grade fever to test portion dissolves; From electric hot plate, take off slightly coldly, add 3mL nitric acid (1.2), low-grade fever on electric hot plate, drives away nitrogen oxides, blows water, and dissolved salts is boiled in heating; Cooling test solution is to room temperature; Move into and accurately add in the 100mL volumetric flask of 2.00mL yttrium inner mark solution (1.18), be diluted with water to scale, shake up;
(6.3), preparation calibration solution;
(6.3.1), prepare low mark solution; By zinc impregnation in tested Zinc oxide powder, study the low mark solution of assignment system as follows; In 100mL volumetric flask, add 5mL hydrochloric acid (1.3), add 3mL nitric acid (1.2), pipette the Zinc Matrix solution (1.17) close with test portion principal ingredient zinc content, accurately add 2.00mL yttrium inner mark solution (1.18), water is rare to scale, shake up, as low mark solution;
(6.3.2), prepare high standard solution; By zinc impregnation in tested Zinc oxide powder, study assignment system high standard solution as follows; In 100mL volumetric flask, add 5mL hydrochloric acid (1.3), add 3mL nitric acid (1.2), pipette the Zinc Matrix solution (1.17) close with test portion principal ingredient zinc content, the gallium standard solution (1.14), (1.15), (1.16) that add different amounts, accurately add 2.00mL yttrium inner mark solution (1.18) again, and water is rare to scale, shake up, as high standard solution;
(6.4), measure the concentration of gallium in sample solution; Press the selected condition of work of inductively coupled plasma atomic emission spectrometer and analysis spectral line 294.36nm, take yttrium as internal standard element, adopt successively low mark solution and high standard solution to carry out standardization to instrument, then, measure the concentration of gallium in sample solution;
(7), computation and measurement result, obtain the content of gallium;
Analysis spectral line 294.36nm, gallium content 0.0054%;
Embodiment bis-
Measure gallium content in Zinc oxide powder, adopt inductive coupling plasma emission spectrograph, condition of work and the analytical line of instrument are as follows: high frequency frequency: 40.68MHz; Incident power: 0.95～1.1Kw; Reflective power: < 15W; Argon flow amount: cooling gas flow: 12～20L/min; Sheath airshed: 0.1～0.6L/min; Sample lifting capacity: 1.0～1.5ml/min; Integral time: 1～10s;
(1) reagent, using in mensuration process is as follows:
(1.1), hydrochloric acid, ρ 1.19g/mL; Top grade is pure;
(1.2), nitric acid, ρ 1.42g/mL; Top grade is pure;
(1.3), hydrochloric acid, 1+1;
(1.4), aluminum standard solution: 1.00mg/mL; Take 1.0000g; > 99.99% fine aluminium, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to aluminium and dissolves completely, adds 5 nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.5), aluminum standard solution: 0.10mg/mL; Pipette 20.00mL aluminum standard solution (1.4), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.6), iron standard solution: 0.10mg/mL; Take 0.1000g; > 99.99% pure iron, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to iron and dissolves completely, adds 2mL nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.7), iron standard solution: 0.01mg/mL; Pipette 20.00mL iron standard solution (1.6), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.8), calcium standard solution: 0.10mg/mL; Take 0.2497g in advance at 105 ℃ of-110 ℃ of calcium carbonate that are dried to constant weight in 200mL beaker, add 20mL water, drip hydrochloric acid (1.3) to dissolving completely, add 5mL hydrochloric acid (1.3), heating is boiled, in cooling rear immigration 1000mL volumetric flask, be diluted with water to scale, mix;
(1.9), calcium standard solution: 0.01mg/mL; Pipette 20.00mL calcium standard solution (1.8), be placed in 200mL volumetric flask, be diluted with water to scale, shake up;
(1.10), magnesium standard solution: 0.10mg/mL; Take 0.1000g; The pure magnesium of > 99.99%, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to magnesium and dissolves completely, adds 1mL nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.11), magnesium standard solution: 0.01mg/mL; Pipette 20.00mL magnesium standard solution (1.10), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.12), copper standard solution: 0.10mg/mL; Take 0.1000g; > 99.99% fine copper, is placed in 250mL beaker, is blown into 10mL intermediate water, adds 10mL nitric acid (1.2), is heated to copper and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.13), copper standard solution: 0.01mg/mL; Pipette 20.00mL copper standard solution (1.12), be placed in 200mL volumetric flask, add 10mL nitric acid (1.2), be diluted with water to scale, shake up;
(1.14), gallium standard solution: 1.00mg/mL; Take 1.0000g; The pure gallium of > 99.99%, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to gallium and dissolves completely, adds 5 nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.15), gallium standard solution: 0.10mg/mL; Pipette 20.00mL gallium standard solution (1.14), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.16), gallium standard solution: 0.01mg/mL; Pipette 20.00mL gallium standard solution (1.15), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.17), Zinc Matrix solution, 10.0mg/mL; Take 0.500g; The pure zinc of > 99.99%, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), heating for dissolving.Be cooled to room temperature, move in 500mL volumetric flask, be diluted with water to scale, shake up;
(1.18), yttrium inner mark solution, 0.2mg/mL; Take 0.127g, > 99.95% yttria, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), and low-temperature heat, to dissolving completely, in cooling rear immigration 500mL volumetric flask, is diluted with water to scale, shakes up;
(2), sampling and sample preparation; The sample of analyzing use samples and sample preparation according to the requirement of HB/Z205;
(3) element analysis spectrum line is selected:
Prepare serial single solution, 5.0mL Zinc Matrix solution (1.17), 8.0mL Zinc Matrix solution (1.17), 5.0mL aluminum standard solution (1.5), 5.0mL aluminum standard solution (1.4), 5.0mL iron standard solution (1.7), 5.0mL calcium standard solution (1.9), 5.0mL magnesium standard solution (1.11), 5.0mL copper standard solution (1.13), 15mL hydrochloric acid (1.1), 6mL nitric acid (1.2), 2.00mL yttrium inner mark solution (1.18), 0.50mL gallium standard solution (1.16) and 5.00mL gallium standard solution (1.14) are respectively in 100mL volumetric flask, respectively above-mentioned solution is carried out on the analysis spectral line of 5-6 bar gallium to spectrogram scanning, stack, therefrom choose 417.20nm as separated time spectral line,
(4) Zinc oxide powder solubility test
Take three parts, 0.10g sample, add respectively 5mL hydrochloric acid, 10mL hydrochloric acid, 15mL hydrochloric acid to heat on electric furnace, Zinc oxide powder dissolves not exclusively;
Take three parts, 0.10g sample, add respectively 2mL nitric acid, 4mL nitric acid, 6mL nitric acid to heat on electric furnace, Zinc oxide powder does not dissolve;
Take three parts, 0.10g sample, add respectively 5mL hydrochloric acid and 2mL nitric acid, 10mL hydrochloric acid and 4mL nitric acid, 15mL hydrochloric acid and 6mL nitric acid to heat on electric furnace, Zinc oxide powder dissolves completely;
(5) mark consumption test in yttrium
Take 0.10g sample, be accurate to 0.0001g and be placed in 150mL beaker, add 10mL hydrochloric acid (1.3), on electric hot plate, low-grade fever to test portion dissolves; From electric hot plate, take off slightly coldly, add 3mL nitric acid (1.2), low-grade fever on electric hot plate, drives away nitrogen oxides, blows water, and dissolved salts is boiled in heating; Cooling test solution is to room temperature; Move into and accurately add in the 100mL volumetric flask of 1.00mL, 2.00mL, 3.00mL, 4.00mL and 5.00mL yttrium inner mark solution (1.18), be diluted with water to scale, shake up; Research shows, while adding 2.00mL yttrium inner mark solution, measurement result relative standard deviation is minimum, measures the most stable;
(6), analytical procedure is as follows:
(6.1), test portion: take 0.10g sample, be accurate to 0.0001g;
(6.2), prepare sample solution: the test portion of analytical procedure (6.1) is placed in to 150mL beaker, adds 10mL hydrochloric acid (1.3), on electric hot plate, low-grade fever to test portion dissolves; From electric hot plate, take off slightly coldly, add 5mL nitric acid (1.2), low-grade fever on electric hot plate, drives away nitrogen oxides, blows water, and dissolved salts is boiled in heating; Cooling test solution is to room temperature; Move into and accurately add in the 100mL volumetric flask of 2.00mL yttrium inner mark solution (1.18), be diluted with water to scale, shake up;
(6.3), preparation calibration solution;
(6.3.1), prepare low mark solution; By zinc impregnation in tested Zinc oxide powder, study the low mark solution of assignment system as follows; In 100mL volumetric flask, add 10mL hydrochloric acid (1.3), add 5mL nitric acid (1.2), pipette the Zinc Matrix solution (1.17) close with test portion principal ingredient zinc content, accurately add 2.00mL yttrium inner mark solution (1.18), water is rare to scale, shake up, as low mark solution;
(6.3.2), prepare high standard solution; By zinc impregnation in tested Zinc oxide powder, study assignment system high standard solution as follows; In 100mL volumetric flask, add 10mL hydrochloric acid (1.3), add 5mL nitric acid (1.2), pipette the Zinc Matrix solution (1.17) close with test portion principal ingredient zinc content, the gallium standard solution (1.14), (1.15), (1.16) that add different amounts, accurately add 2.00mL yttrium inner mark solution (1.18) again, and water is rare to scale, shake up, as high standard solution;
(6.4), measure the concentration of gallium in sample solution; Press the selected condition of work of inductively coupled plasma atomic emission spectrometer and analysis spectral line 417.20nm nm, take yttrium as internal standard element, adopt successively low mark solution and high standard solution to carry out standardization to instrument, then, measure the concentration of gallium in sample solution;
(5), computation and measurement result, the content that obtains gallium is 0.014%.
Embodiment tri-
Measure gallium content in Zinc oxide powder, adopt inductive coupling plasma emission spectrograph, condition of work and the analytical line of instrument are as follows: high frequency frequency: 40.68MHz; Incident power: 0.95～1.1Kw; Reflective power: < 15W; Argon flow amount: cooling gas flow: 12～20L/min; Sheath airshed: 0.1～0.6L/min; Sample lifting capacity: 1.0～1.5ml/min; Integral time: 1～10s;
(1) reagent, using in mensuration process is as follows:
(1.1), hydrochloric acid, ρ 1.19g/mL; Top grade is pure;
(1.2), nitric acid, ρ 1.42g/mL; Top grade is pure;
(1.3), hydrochloric acid, 1+1;
(1.4), aluminum standard solution: 1.00mg/mL; Take 1.0000g; > 99.99% fine aluminium, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to aluminium and dissolves completely, adds 5 nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.5), aluminum standard solution: 0.10mg/mL; Pipette 20.00mL aluminum standard solution (1.4), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.6), iron standard solution: 0.10mg/mL; Take 0.1000g; > 99.99% pure iron, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to iron and dissolves completely, adds 2mL nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.7), iron standard solution: 0.01mg/mL; Pipette 20.00mL iron standard solution (1.6), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.8), calcium standard solution: 0.10mg/mL; Take 0.2497g in advance at 105 ℃ of-110 ℃ of calcium carbonate that are dried to constant weight in 200mL beaker, add 20mL water, drip hydrochloric acid (1.3) to dissolving completely, add 5mL hydrochloric acid (1.3), heating is boiled, in cooling rear immigration 1000mL volumetric flask, be diluted with water to scale, mix;
(1.9), calcium standard solution: 0.01mg/mL; Pipette 20.00mL calcium standard solution (1.8), be placed in 200mL volumetric flask, be diluted with water to scale, shake up;
(1.10), magnesium standard solution: 0.10mg/mL; Take 0.1000g; The pure magnesium of > 99.99%, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to magnesium and dissolves completely, adds 1mL nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.11), magnesium standard solution: 0.01mg/mL; Pipette 20.00mL magnesium standard solution (1.10), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.12), copper standard solution: 0.10mg/mL; Take 0.1000g; > 99.99% fine copper, is placed in 250mL beaker, is blown into 10mL intermediate water, adds 10mL nitric acid (1.2), is heated to copper and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.13), copper standard solution: 0.01mg/mL; Pipette 20.00mL copper standard solution (1.12), be placed in 200mL volumetric flask, add 10mL nitric acid (1.2), be diluted with water to scale, shake up;
(1.14), gallium standard solution: 1.00mg/mL; Take 1.0000g; The pure gallium of > 99.99%, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to gallium and dissolves completely, adds 5 nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.15), gallium standard solution: 0.10mg/mL; Pipette 20.00mL gallium standard solution (1.14), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.16), gallium standard solution: 0.01mg/mL; Pipette 20.00mL gallium standard solution (1.15), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.17), Zinc Matrix solution, 10.0mg/mL; Take 0.500g; The pure zinc of > 99.99%, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), heating for dissolving.Be cooled to room temperature, move in 500mL volumetric flask, be diluted with water to scale, shake up;
(2), sampling and sample preparation; The sample of analyzing use samples and sample preparation according to the requirement of HB/Z205;
(3) ultimate analysis line options:
Prepare serial single solution, 5.0mL Zinc Matrix solution (1.17), 8.0mL Zinc Matrix solution (1.17), 5.0mL aluminum standard solution (1.5), 5.0mL aluminum standard solution (1.4), 5.0mL iron standard solution (1.7), 5.0mL calcium standard solution (1.9), 5.0mL magnesium standard solution (1.11), 5.0mL copper standard solution (1.13), 15mL hydrochloric acid (1.1), 6mL nitric acid (1.2), 0.50mL gallium standard solution (1.16) and 5.00mL gallium standard solution (1.14) are respectively in 100mL volumetric flask, respectively above-mentioned solution is carried out on the analysis spectral line of 5-6 bar gallium to spectrogram scanning, stack, therefrom choose 417.20nm as separated time spectral line,
(4) Zinc oxide powder solubility test
Take three parts, 0.10g sample, add respectively 5mL hydrochloric acid, 10mL hydrochloric acid, 15mL hydrochloric acid to heat on electric furnace, Zinc oxide powder dissolves not exclusively;
Take three parts, 0.10g sample, add respectively 2mL nitric acid, 4mL nitric acid, 6mL nitric acid to heat on electric furnace, Zinc oxide powder does not dissolve;
Take three parts, 0.10g sample, add respectively 5mL hydrochloric acid and 2mL nitric acid, 10mL hydrochloric acid and 4mL nitric acid, 15mL hydrochloric acid and 6mL nitric acid to heat on electric furnace, Zinc oxide powder dissolves completely;
(5), analytical procedure is as follows:
(5.1), test portion: take 0.10g sample, be accurate to 0.0001g;
(5.2), prepare sample solution: the test portion of analytical procedure (5.1) is placed in to 150mL beaker, adds 15mL hydrochloric acid (1.3), on electric hot plate, low-grade fever to test portion dissolves; From electric hot plate, take off slightly coldly, add 5mL nitric acid (1.2), low-grade fever on electric hot plate, drives away nitrogen oxides, blows water, and dissolved salts is boiled in heating; Cooling test solution is to room temperature; Move in 100mL volumetric flask, be diluted with water to scale, shake up;
(5.3), preparation calibration solution;
(5.3.1), prepare low mark solution; By zinc impregnation in tested Zinc oxide powder, study the low mark solution of assignment system as follows; In 100mL volumetric flask, add 15mL hydrochloric acid (1.3), add 5mL nitric acid (1.2), pipette the Zinc Matrix solution (1.17) close with test portion principal ingredient zinc content, water is rare to scale, shakes up, as low mark solution;
(5.3.2), prepare high standard solution; By zinc impregnation in tested Zinc oxide powder, study assignment system high standard solution as follows; In 100mL volumetric flask, add 15mL hydrochloric acid (1.3), add 5mL nitric acid (1.2), pipette the Zinc Matrix solution (1.17) close with test portion principal ingredient zinc content, the gallium standard solution (1.14), (1.15), (1.16) that add again different amounts, water is rare to scale, shakes up, as high standard solution;
(6.4), measure the concentration of gallium in sample solution; Press the selected condition of work of inductively coupled plasma atomic emission spectrometer and analytical line 417.20nm nm, adopt successively low mark solution and high standard solution to carry out standardization to instrument, then, measure the concentration of gallium in sample solution;
(5), computation and measurement result, the content that obtains gallium is 1.00%.
Embodiment tetra-
Measure gallium content in Zinc oxide powder, adopt inductive coupling plasma emission spectrograph, condition of work and the analytical line of instrument are as follows: high frequency frequency: 40.68MHz; Incident power: 0.95～1.1Kw; Reflective power: < 15W; Argon flow amount: cooling gas flow: 12～20L/min; Sheath airshed: 0.1～0.6L/min; Sample lifting capacity: 1.0～1.5ml/min; Integral time: 1～10s;
(1) reagent, using in mensuration process is as follows:
(1.1), hydrochloric acid, ρ 1.19g/mL; Top grade is pure;
(1.2), nitric acid, ρ 1.42g/mL; Top grade is pure;
(1.3), hydrochloric acid, 1+1;
(1.4), aluminum standard solution: 1.00mg/mL; Take 1.0000g; > 99.99% fine aluminium, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to aluminium and dissolves completely, adds 5 nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.5), aluminum standard solution: 0.10mg/mL; Pipette 20.00mL aluminum standard solution (1.4), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.6), iron standard solution: 0.10mg/mL; Take 0.1000g; > 99.99% pure iron, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to iron and dissolves completely, adds 2mL nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.7), iron standard solution: 0.01mg/mL; Pipette 20.00mL iron standard solution (1.6), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.8), calcium standard solution: 0.10mg/mL; Take 0.2497g in advance at 105 ℃ of-110 ℃ of calcium carbonate that are dried to constant weight in 200mL beaker, add 20mL water, drip hydrochloric acid (1.3) to dissolving completely, add 5mL hydrochloric acid (1.3), heating is boiled, in cooling rear immigration 1000mL volumetric flask, be diluted with water to scale, mix;
(1.9), calcium standard solution: 0.01mg/mL; Pipette 20.00mL calcium standard solution (1.8), be placed in 200mL volumetric flask, be diluted with water to scale, shake up;
(1.10), magnesium standard solution: 0.10mg/mL; Take 0.1000g; The pure magnesium of > 99.99%, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to magnesium and dissolves completely, adds 1mL nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.11), magnesium standard solution: 0.01mg/mL; Pipette 20.00mL magnesium standard solution (1.10), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.12), copper standard solution: 0.10mg/mL; Take 0.1000g; > 99.99% fine copper, is placed in 250mL beaker, is blown into 10mL intermediate water, adds 10mL nitric acid (1.2), is heated to copper and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.13), copper standard solution: 0.01mg/mL; Pipette 20.00mL copper standard solution (1.12), be placed in 200mL volumetric flask, add 10mL nitric acid (1.2), be diluted with water to scale, shake up;
(1.14), gallium standard solution: 1.00mg/mL; Take 1.0000g; The pure gallium of > 99.99%, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to gallium and dissolves completely, adds 5 nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.15), gallium standard solution: 0.10mg/mL; Pipette 20.00mL gallium standard solution (1.14), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.16), gallium standard solution: 0.01mg/mL; Pipette 20.00mL gallium standard solution (1.15), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.17), Zinc Matrix solution, 10.0mg/mL; Take 0.500g; The pure zinc of > 99.99%, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), heating for dissolving.Be cooled to room temperature, move in 500mL volumetric flask, be diluted with water to scale, shake up;
(1.18), yttrium inner mark solution, 0.2mg/mL; Take 0.127g, > 99.95% yttria, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), and low-temperature heat, to dissolving completely, in cooling rear immigration 500mL volumetric flask, is diluted with water to scale, shakes up;
(2), sampling and sample preparation; The sample of analyzing use samples and sample preparation according to the requirement of HB/Z205;
(3) ultimate analysis line options:
Prepare serial single solution, 5.0mL Zinc Matrix solution (1.17), 8.0mL Zinc Matrix solution (1.17), 5.0mL aluminum standard solution (1.5), 5.0mL aluminum standard solution (1.4), 5.0mL iron standard solution (1.7), 5.0mL calcium standard solution (1.9), 5.0mL magnesium standard solution (1.11), 5.0mL copper standard solution (1.13), 15mL hydrochloric acid (1.1), 6mL nitric acid (1.2), 2.00mL yttrium inner mark solution (1.18), 0.50mL gallium standard solution (1.16) and 5.00mL gallium standard solution (1.14) are respectively in 100mL volumetric flask, respectively above-mentioned solution is carried out on the analysis spectral line of 5-6 bar gallium to spectrogram scanning, stack, therefrom choose 294.36nm as separated time spectral line,
(4) Zinc oxide powder solubility test
Take three parts, 0.10g sample, add respectively 5mL hydrochloric acid, 10mL hydrochloric acid, 15mL hydrochloric acid to heat on electric furnace, Zinc oxide powder dissolves not exclusively;
Take three parts, 0.10g sample, add respectively 2mL nitric acid, 4mL nitric acid, 6mL nitric acid to heat on electric furnace, Zinc oxide powder does not dissolve;
Take three parts, 0.10g sample, add respectively 5mL hydrochloric acid and 2mL nitric acid, 10mL hydrochloric acid and 4mL nitric acid, 15mL hydrochloric acid and 6mL nitric acid to heat on electric furnace, Zinc oxide powder dissolves completely;
(5) mark consumption test in yttrium
Take 0.10g sample, be accurate to 0.0001g and be placed in 150mL beaker, add 10mL hydrochloric acid (1.3), on electric hot plate, low-grade fever to test portion dissolves; From electric hot plate, take off slightly coldly, add 3mL nitric acid (1.2), low-grade fever on electric hot plate, drives away nitrogen oxides, blows water, and dissolved salts is boiled in heating; Cooling test solution is to room temperature; Move into and accurately add in the 100mL volumetric flask of 1.00mL, 2.00mL, 3.00mL, 4.00mL and 5.00mL yttrium inner mark solution (1.18), be diluted with water to scale, shake up; Research shows, while adding 2.00mL yttrium inner mark solution, measurement result relative standard deviation is minimum, measures the most stable;
(6), analytical procedure is as follows:
(6.1), test portion: take 0.10g sample, be accurate to 0.0001g;
(6.2), prepare sample solution: the test portion of analytical procedure (6.1) is placed in to 150mL beaker, adds 15mL hydrochloric acid (1.3), on electric hot plate, low-grade fever to test portion dissolves; From electric hot plate, take off slightly coldly, add 3mL nitric acid (1.2), low-grade fever on electric hot plate, drives away nitrogen oxides, blows water, and dissolved salts is boiled in heating; Cooling test solution is to room temperature; Move into and accurately add in the 100mL volumetric flask of 2.00mL yttrium inner mark solution (1.18), be diluted with water to scale, shake up;
(6.3), preparation calibration solution;
(6.3.1), prepare low mark solution; By zinc impregnation in tested Zinc oxide powder, study the low mark solution of assignment system as follows; In 100mL volumetric flask, add 15mL hydrochloric acid (1.3), add 3mL nitric acid (1.2), pipette the Zinc Matrix solution (1.17) close with test portion principal ingredient zinc content, accurately add 2.00mL yttrium inner mark solution (1.18), water is rare to scale, shake up, as low mark solution;
(6.3.2), prepare high standard solution; By zinc impregnation in tested Zinc oxide powder, study assignment system high standard solution as follows; In 100mL volumetric flask, add 15mL hydrochloric acid (1.3), add 3mL nitric acid (1.2), pipette the Zinc Matrix solution (1.17) close with test portion principal ingredient zinc content, the gallium standard solution (1.14), (1.15), (1.16) that add different amounts, accurately add 2.00mL yttrium inner mark solution (1.18) again, and water is rare to scale, shake up, as high standard solution;
(6.4), measure the concentration of gallium in sample solution; Press the selected condition of work of inductively coupled plasma atomic emission spectrometer and analytical line 294.36nm, take yttrium as internal standard element, adopt successively low mark solution and high standard solution to carry out standardization to instrument, then, measure the concentration of gallium in sample solution;
(7), computation and measurement result, be 4.99%.
Claims (5)
1. an analytical approach of measuring gallium element in Zinc oxide powder, is characterized in that: adopt inductive coupling plasma emission spectrograph, condition of work and the analytical line of instrument are as follows: high frequency frequency: 40.68MHz; Incident power: 0.95～1.1Kw; Reflective power: < 15W; Argon flow amount: cooling gas flow: 12～20L/min; Sheath airshed: 0.1～0.6L/min; Sample lifting capacity: 1.0～1.5ml/min; Integral time: 1～10s;
(1) reagent, using in mensuration process is as follows:
(1.1), hydrochloric acid, ρ 1.19g/mL; Top grade is pure;
(1.2), nitric acid, ρ 1.42g/mL; Top grade is pure;
(1.3), hydrochloric acid, 1+1;
(1.4), aluminum standard solution: 1.00mg/mL; Take 1.0000g; > 99.99% fine aluminium, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to aluminium and dissolves completely, adds 5 nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.5), aluminum standard solution: 0.10mg/mL; Pipette 20.00mL aluminum standard solution (1.4), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.6), iron standard solution: 0.10mg/mL; Take 0.1000g; > 99.99% pure iron, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to iron and dissolves completely, adds 2mL nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.7), iron standard solution: 0.01mg/mL; Pipette 20.00mL iron standard solution (1.6), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.8), calcium standard solution: 0.10mg/mL; Take 0.2497g in advance at 105 ℃ of-110 ℃ of calcium carbonate that are dried to constant weight in 200mL beaker, add 20mL water, drip hydrochloric acid (1.3) to dissolving completely, add 5mL hydrochloric acid (1.3), heating is boiled, in cooling rear immigration 1000mL volumetric flask, be diluted with water to scale, mix;
(1.9), calcium standard solution: 0.01mg/mL; Pipette 20.00mL calcium standard solution (1.8), be placed in 200mL volumetric flask, be diluted with water to scale, shake up;
(1.10), magnesium standard solution: 0.10mg/mL; Take 0.1000g; The pure magnesium of > 99.99%, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to magnesium and dissolves completely, adds 1mL nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.11), magnesium standard solution: 0.01mg/mL; Pipette 20.00mL magnesium standard solution (1.10), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.12), copper standard solution: 0.10mg/mL; Take 0.1000g; > 99.99% fine copper, is placed in 250mL beaker, is blown into 10mL intermediate water, adds 10mL nitric acid (1.2), is heated to copper and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.13), copper standard solution: 0.01mg/mL; Pipette 20.00mL copper standard solution (1.12), be placed in 200mL volumetric flask, add 10mL nitric acid (1.2), be diluted with water to scale, shake up;
(1.14), gallium standard solution: 1.00mg/mL; Take 1.0000g; The pure gallium of > 99.99%, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), is heated to gallium and dissolves completely, adds 5 nitric acid (1.2), in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.15), gallium standard solution: 0.10mg/mL; Pipette 20.00mL gallium standard solution (1.14), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.16), gallium standard solution: 0.01mg/mL; Pipette 20.00mL gallium standard solution (1.15), be placed in 200mL volumetric flask, add 10mL hydrochloric acid (1.3), be diluted with water to scale, shake up;
(1.17), Zinc Matrix solution, 10.0mg/mL; Take 0.500g; The pure zinc of > 99.99%, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), and heating for dissolving, is cooled to room temperature, moves in 500mL volumetric flask, is diluted with water to scale, shakes up;
(1.18), yttrium inner mark solution, 0.2mg/mL; Take 0.127g, > 99.95% yttria, is placed in 250mL beaker, adds 20mL hydrochloric acid (1.3), and low-temperature heat, to dissolving completely, in cooling rear immigration 500mL volumetric flask, is diluted with water to scale, shakes up;
(2), sampling and sample preparation; The sample of analyzing use samples and sample preparation according to the requirement of HB/Z205;
(3) element analysis spectrum line is selected:
Prepare serial single solution, 5.0mL Zinc Matrix solution (1.17), 8.0mL Zinc Matrix solution (1.17), 5.0mL aluminum standard solution (1.5), 5.0mL aluminum standard solution (1.4), 5.0mL iron standard solution (1.7), 5.0mL calcium standard solution (1.9), 5.0mL magnesium standard solution (1.11), 5.0mL copper standard solution (1.13), 15mL hydrochloric acid (1.1), 6mL nitric acid (1.2), 2.00mL yttrium inner mark solution (1.18), 0.50mL gallium standard solution (1.16) and 5.00mL gallium standard solution (1.14) are respectively in 100mL volumetric flask, respectively above-mentioned solution is carried out on the analysis spectral line of 5-6 bar gallium to spectrogram scanning, stack, therefrom choose 2 analytic signals strong, Zinc oxide powder matrix coexistence elements disturb minimum analytical line as separated time spectral line,
(4) Zinc oxide powder solubility test
Take three parts, 0.10g sample, add respectively 5mL hydrochloric acid, 10mL hydrochloric acid, 15mL hydrochloric acid to heat on electric furnace, Zinc oxide powder dissolves not exclusively;
Take three parts, 0.10g sample, add respectively 2mL nitric acid, 4mL nitric acid, 6mL nitric acid to heat on electric furnace, Zinc oxide powder does not dissolve;
Take three parts, 0.10g sample, add respectively 5mL hydrochloric acid and 2mL nitric acid, 10mL hydrochloric acid and 4mL nitric acid, 15mL hydrochloric acid and 6mL nitric acid to heat on electric furnace, Zinc oxide powder dissolves completely;
(5) mark consumption test in yttrium
Take 0.10g sample, be accurate to 0.0001g and be placed in 150mL beaker, add 10mL hydrochloric acid (1.3), on electric hot plate, low-grade fever to test portion dissolves; From electric hot plate, take off slightly coldly, add 3mL nitric acid (1.2), low-grade fever on electric hot plate, drives away nitrogen oxides, blows water, and dissolved salts is boiled in heating; Cooling test solution is to room temperature; Move into and accurately add in the 100mL volumetric flask of 1.00mL, 2.00mL, 3.00mL, 4.00mL and 5.00mL yttrium inner mark solution (1.18), be diluted with water to scale, shake up; Research shows, while adding 2.00mL yttrium inner mark solution, measurement result relative standard deviation is minimum, measures the most stable;
(6), analytical procedure is as follows:
(6.1), test portion: take 0.10g sample, be accurate to 0.0001g;
(6.2), prepare sample solution: the test portion of analytical procedure (6.1) is placed in to 150mL beaker, adds 5mL～15mL hydrochloric acid (1.3), on electric hot plate, low-grade fever to test portion dissolves; From electric hot plate, take off slightly coldly, add 3mL～6mL nitric acid (1.2), low-grade fever on electric hot plate, drives away nitrogen oxides, blows water, and dissolved salts is boiled in heating; Cooling test solution is to room temperature; Move into and accurately add in the 100mL volumetric flask of 2.00mL yttrium inner mark solution (1.18), be diluted with water to scale, shake up;
(6.3), preparation calibration solution;
(6.3.1), prepare low mark solution; By zinc impregnation in tested Zinc oxide powder, study the low mark solution of assignment system as follows; In 100mL volumetric flask, add 5mL～15mL hydrochloric acid (1.3), add 3mL～6mL nitric acid (1.2), pipette the Zinc Matrix solution (1.17) close with test portion principal ingredient zinc content, accurately add 2.00mL yttrium inner mark solution (1.18), water is rare to scale, shakes up, as low mark solution;
(6.3.2), prepare high standard solution; By zinc impregnation in tested Zinc oxide powder, study assignment system high standard solution as follows; In 100mL volumetric flask, add 5mL～15mL hydrochloric acid (1.3), add 3mL～6mL nitric acid (1.2), pipette the Zinc Matrix solution (1.17) close with test portion principal ingredient zinc content, the gallium standard solution (1.14), (1.15), (1.16) that add different amounts, accurately add 2.00mL yttrium inner mark solution (1.18) again, and water is rare to scale, shake up, as high standard solution;
(6.4), measure the concentration of gallium in sample solution; Press the selected condition of work of inductively coupled plasma atomic emission spectrometer and analysis spectral line, take yttrium as internal standard element, adopt successively low mark solution and high standard solution to carry out standardization to instrument, then, measure the concentration of gallium in sample solution;
(7), computation and measurement result, obtain the content of gallium;
Be calculated as follows the percentage composition of element to be measured:
In formula: w---the percentage composition of gallium element in test solution, unit: %;
ρ---the mass concentration of gallium element in test solution, unit: μ g/mL;
V---test solution volume during measurement, unit: mL;
M---test portion quality, unit: g.
2. a kind of method of measuring gallium element in Zinc oxide powder according to claim 1, it is characterized in that, prepare low, high standard solution or use the approaching standard model of chemical composition, after processing according to (6.1)～(6.3), be mixed with needed low, high standard solution.
3. a kind of method of measuring gallium element in Zinc oxide powder according to claim 1, is characterized in that, Matrix Solution adopts pure zinc or zinc paste to carry out Matrix Match, according to (6.3.1)～(6.3.2), is mixed with needed low, high standard calibration solution.
4. a kind of method of measuring gallium element in Zinc oxide powder according to claim 1, it is characterized in that, according to (6.1)～(6.3), process sample solution, low, high standard calibration solution, do not add inner mark solution, with inductively coupled plasma atomic emission spectrometer, measure, delete mark in yttrium and measure.
5. a kind of method of measuring gallium element in Zinc oxide powder according to claim 1, it is characterized in that, according to (6.1)～(6.3), process sample solution, low, high standard calibration solution, with inductively coupled plasma atomic emission spectrometer, measure, delete mark in yttrium and carry out.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104359896A (en) * | 2014-10-23 | 2015-02-18 | 江西稀有稀土金属钨业集团有限公司 | Method for measuring content of major elements in hydrogen storage alloy powder |
| CN106226288A (en) * | 2016-07-12 | 2016-12-14 | 广西壮族自治区分析测试研究中心 | The assay method of gallium content in a kind of copper indium gallium selenium solar photovoltaic cell target |
| CN108362684A (en) * | 2018-01-23 | 2018-08-03 | 中国航发北京航空材料研究院 | The analysis method of gallium element in a kind of measurement rafifinal |
| CN108802011A (en) * | 2018-05-08 | 2018-11-13 | 中国航发北京航空材料研究院 | A method of measuring cadmium copper palladium Zn-ef ficiency in Au82Ni alloys |
| CN114252432A (en) * | 2021-11-19 | 2022-03-29 | 中国科学院金属研究所 | Method for measuring gallium content in antibacterial stainless steel |
| CN114577659A (en) * | 2022-01-26 | 2022-06-03 | 株洲科能新材料股份有限公司 | Method for detecting gallium content in gallium nitride material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0601689B1 (en) * | 1992-12-08 | 1998-07-22 | Director-General Of The Agency Of Industrial Science And Technology | Secondary ion mass spectrometric analysis of metals and method of preparing standard sample therefor |
| CN102735516A (en) * | 2012-07-23 | 2012-10-17 | 武钢集团昆明钢铁股份有限公司 | Method for measuring content of gallium in vanadium slag |
| CN103308509A (en) * | 2013-06-07 | 2013-09-18 | 武钢集团昆明钢铁股份有限公司 | Method for measuring gallium and scandium contents in blast furnace smoke dust |
-
2014
- 2014-04-10 CN CN201410140947.2A patent/CN103940806B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0601689B1 (en) * | 1992-12-08 | 1998-07-22 | Director-General Of The Agency Of Industrial Science And Technology | Secondary ion mass spectrometric analysis of metals and method of preparing standard sample therefor |
| CN102735516A (en) * | 2012-07-23 | 2012-10-17 | 武钢集团昆明钢铁股份有限公司 | Method for measuring content of gallium in vanadium slag |
| CN103308509A (en) * | 2013-06-07 | 2013-09-18 | 武钢集团昆明钢铁股份有限公司 | Method for measuring gallium and scandium contents in blast furnace smoke dust |
Non-Patent Citations (5)
| Title |
|---|
| N. DASKALOVA, G. GENTSHEVA, S. VELICHKOV: "Spectralinterfer ence in the determination of Ho, Tm and Ga as dopants in single crystals of potassium titanylphosphate by inductively coupled plasma atomic emission spectrometry", 《SPECTROCHIMICA ACTA PART B》, vol. 57, no. 8, 31 August 2002 (2002-08-31) * |
| 侯广顺,张丽娜: "电感耦合等离子体原子发射光谱法测定精矿粉中7种伴生元素", 《冶金分析》, vol. 30, no. 10, 31 October 2010 (2010-10-31) * |
| 刘冰冰，王英滨: "电感耦合等离子体-原子发射光谱法测定粉煤灰中的镓", 《光谱实验室》, vol. 29, no. 6, 30 November 2012 (2012-11-30) * |
| 王海舟: "《钢铁及合金分析 第一分册 生铁及铸铁分析》", 31 August 2004, article "CSM 07 01 31 04-2003 生铁及铸铁-镓含量的测定-电感耦合等离子体发射光谱法" * |
| 王海舟: "《钢铁及合金分析 第六分册 金属功能材料分析》", 31 August 2004, article "CSM 07 06 31 04-2003金属功能材料-镓含量的测定-电感耦合等离子体发射光谱法" * |
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