CN102721582B - A method for determining contents of potassium element, sodium element, calcium element, silicon element, and magnesium element in nickel oxide - Google Patents
A method for determining contents of potassium element, sodium element, calcium element, silicon element, and magnesium element in nickel oxide Download PDFInfo
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Abstract
The invention provides a method for determining contents of potassium element, sodium element, calcium element, silicon element and magnesium element in nickel oxide. The method capable of effectively dissolving a nickel oxide sample, is a method which can determine the contents of the potassium element, the sodium element, the calcium element, the silicon element and the magnesium element in the nickel oxide with high speed of sample dissolution, high analysis precision, simple and convenient operation as well as high efficiency. Analytical spectral lines selected by the method are as follows: K766.490 nm, Na588.995 nm, Ca393.366 nm, Si251.611 nm and Mg279.553 nm which are on multiple spectral instruments and are not affected by interference of matrix elements and coexisting elements in the nickel oxide; therefore, this method can be applied to almost all inductively coupled plasma atomic emission spectrometers. The method has a wide measurement range with a measurement lower limit being 0.0001% and a measurement upper limit being 0.5% and can satisfy requirements for analyzing the potassium element, the sodium element, the calcium element, the silicon element and the magnesium element in the nickel oxide.
Description
Technical field
This method is a kind of method measuring potassium in nickel oxide, sodium, calcium, silicon, magnesium element content, belongs to alloying element analysis to measure technical field.
Background technology
Nickel oxide is a kind of transition metal oxide, is widely applied in Aero-Space, catalysis, battery electrode, photoelectric conversion material etc., also show fine application prospect.Along with improving constantly of nickel oxide technology of preparing, the purity of quality oxide nickel also improves constantly.In nickel oxide, the performance of content to nickel oxide of potassium, sodium, calcium, silicon, magnesium elements has material impact.
The analytical approach of present analysis nickel oxide has polarography determination trace Cd, Pb element, atomic fluorescence spectrometry [3] measures micro-As and Sb in metallic nickel and nickel oxide, nickelic content in complexometric titration nickel oxide, the people such as Osamu Kujirai measure seven trace impurities such as Al, As, Cr, Fe, Ti, V, Zr in high-purity metal nickel and nickel oxide with co-precipitation ICP-AES, do not use inductively coupled plasma emission spectrography (ICP-AES) to analyze the report of potassium in nickel oxide, sodium, calcium, silicon, magnesium.
Inductively coupled plasma emission spectrography method (ICP-AES) is low with its detection limit, precision good, good stability, all kinds of interference relatively less, the range of linearity is wide, analysis speed is fast etc., and excellent characteristics has become one of chemico-analytic conventional powerful measure, can analyze the most of impurity elements in nickel oxide.
Summary of the invention
The present invention designs for above-mentioned prior art situation a kind of method measuring potassium in nickel oxide, sodium, calcium, silicon, magnesium element content that provides just, its objective is the method for potassium, sodium, calcium, silicon, magnesium element content in the mensuration nickel oxide that a kind of molten sample speed is fast, analysis precision is high, easy and simple to handle, efficiency is high.
Technical solution of the present invention utilizes inductively coupled plasma emission spectrography (ICP-AES) to analyze potassium in nickel oxide, sodium, calcium, silicon, magnesium, method accurately and reliably, fast easy, be improved nickel oxide analysis efficiency and analyze quality.
The object of the invention is to be achieved through the following technical solutions:
This kind measures the method for potassium, sodium, calcium, silicon, magnesium element content in nickel oxide, it is characterized in that: the reagent that the method uses in mensuration process is:
Hydrochloric acid I, density is 1.19g/mL, more than top grade is pure;
Hydrochloric acid II, 1+1, hydrochloric acid I and water mix by volume at 1: 1;
Nitric acid I, density is 1.42g/mL, more than top grade is pure;
Nitric acid II, 1+1, nitric acid I and water mix by volume at 1: 1;
NaOH, more than top grade is pure;
Sodium standard solution I, quality-volumetric concentration be 0.10mg/mL, preparation method accurately takes 0.1886g sodium chloride, its massfraction is not less than 99.95%, is placed in 100mL beaker, is dissolved in water, move in 1000mL volumetric flask, be diluted with water to scale, shake up;
Sodium standard solution II, quality-volumetric concentration is 0.01mg/mL, and preparation method pipettes 20mL sodium standard solution I in 200mL volumetric flask, is diluted with water to scale, shakes up;
Sodium standard solution III, quality-volumetric concentration is 0.001mg/mL, and preparation method pipettes 20mL sodium standard solution II in 200mL volumetric flask, is diluted with water to scale, shakes up;
Potassium standard solution I, quality-volumetric concentration is 0.10mg/mL, and preparation method accurately takes 0.1907g potassium chloride, and its massfraction is not less than 99.95%, is placed in 100mL beaker, is dissolved in water, and moves in 1000mL volumetric flask, is diluted with water to scale, shakes up;
Potassium standard solution II, quality-volumetric concentration is 0.01mg/mL, and preparation method pipettes 20mL potassium standard solution I in 200mL volumetric flask, is diluted with water to scale, shakes up;
Potassium standard solution III, quality-volumetric concentration is 0.001mg/mL, and preparation method pipettes 20mL potassium standard solution II in 200mL volumetric flask, is diluted with water to scale, shakes up;
Calcium standard solution I, quality-volumetric concentration is 0.10mg/mL, preparation method is the calcium carbonate taking 0.1249g previously baked (at 100 DEG C ~ 110 DEG C baking 1 ~ 2h) and be cooled to room temperature in exsiccator, and its massfraction is not less than 99.95%, is placed in 100mL beaker, add 10 ~ 40mL hydrochloric acid II, low-temperature heat, to dissolving completely, moves in 500mL volumetric flask after cooling, adds 10 ~ 30mL hydrochloric acid II, be diluted with water to scale, shake up.
Calcium standard solution II, quality-volumetric concentration is 0.01mg/mL, and preparation method pipettes 20.00mL calcium standard solution I in 200mL volumetric flask, adds 10 ~ 30mL hydrochloric acid I, is diluted with water to scale, shakes up.
Calcium standard solution III, quality-volumetric concentration is 0.001mg/mL, and preparation method pipettes 20.00mL calcium standard solution II in 200mL volumetric flask, adds 10 ~ 30mL hydrochloric acid I, is diluted with water to scale, shakes up.
Silicon standard solution I, quality-volumetric concentration is 0.10mg/mL, and preparation method takes 0.1000g through levigate monocrystalline silicon or polysilicon, its massfraction is not less than 99.95%, be placed in 100mL polytetrafluoroethylene beaker, add 10 ~ 30g NaOH, 50 ~ 150mL water, shake gently, put into boiling water bath, be heated to dissolve completely, move in 1000mL plastics volumetric flask after cooling, be diluted with water to scale, shake up.
Silicon standard solution II, quality-volumetric concentration is 0.01mg/mL, and preparation method pipettes 20.00mL silicon standard solution I in 200mL volumetric flask, adds 10 ~ 30mL hydrochloric acid I, is diluted with water to scale, shakes up.
Silicon standard solution III, quality-volumetric concentration is 0.001mg/mL, and preparation method pipettes 20.00mL silicon standard solution II in 200mL volumetric flask, adds 10 ~ 30mL hydrochloric acid I, is diluted with water to scale, shakes up.
Magnesium standard solution I, quality-volumetric concentration is 0.10mg/mL, preparation method takes the pure magnesium of 0.1000g, its massfraction is not less than 99.95%, is placed in 150mL beaker and adds 10 ~ 30mL hydrochloric acid II, and low-temperature heat is to dissolving completely, move into after cooling in 1000mL volumetric flask, add 50 ~ 100mL hydrochloric acid II, be diluted with water to scale, shake up.
Magnesium standard solution II, quality-volumetric concentration is 0.01mg/mL, and preparation method pipettes 20.00mL magnesium standard solution I in 200mL volumetric flask, adds 10 ~ 30mL hydrochloric acid II, is diluted with water to scale, shakes up.
Magnesium standard solution III, quality-volumetric concentration is 0.001mg/mL, and preparation method pipettes 20.00mL magnesium standard solution II in 200mL volumetric flask, adds 10 ~ 30mL hydrochloric acid II, is diluted with water to scale, shakes up.
The step of the mensuration process of the method is:
(1) sample carries out sampling and sample preparation according to the requirement of GB/T 20066, takes 0.1 ~ 2.0g sample, is accurate to 0.0001g;
(2) prepare sample solution
Sample is placed in 100mL beaker, adds 10 ~ 30mL nitric acid II, low-temperature heat, to dissolving completely, moves into 50mL volumetric flask after cooling, is diluted with water to scale, shakes up;
(3) preparation work curve solution:
In 2 ~ 8 100mL beakers, add and step (2) identical amount nitric acid II, low-temperature heat is to dissolving completely, several corresponding 50mL volumetric flask is moved into after cooling, according to potassium in the sample learnt in advance, sodium, calcium, silicon, the content range of magnesium, potassium standard solution I or the potassium standard solution II or potassium standard solution III of different volumes number is added in each volumetric flask, the sodium standard solution I of different volumes number or sodium standard solution II or sodium standard solution III, the calcium standard solution I of different volumes number or calcium standard solution II or calcium standard solution III, the silicon standard solution I of different volumes number or the magnesium standard solution I of silicon standard solution II or silicon standard solution III and different volumes number or magnesium standard solution II or magnesium standard solution III, make the potassium in each volumetric flask, sodium, calcium, silicon, the content of magnesium is the sample potassium learnt, sodium, calcium, silicon, 0% ~ 200% of content of magnesium, be diluted with water to scale, shake up, as working curve solution,
(4) mass concentration of analytical element potassium, sodium, calcium, silicon, magnesium in sample solution is measured
By the intensity of inductively coupled plasma atomic emission spectrometer analytical element potassium, sodium, calcium, silicon, magnesium in spectral line K766.490nm, Na588.995nm, Ca393.366nm, Si251.611nm and Mg279.553nm successively surveying work curve solution, the horizontal ordinate mass concentration of analytical element potassium, sodium, calcium, silicon, magnesium in working curve solution, the respective strengths of ordinate analytical element potassium, sodium, calcium, silicon, magnesium, drawing curve;
Then measure the intensity of Element Potassium, sodium, calcium, silicon, magnesium in sample solution, on corresponding working curve, find the mass concentration of corresponding analysis Element Potassium, sodium, calcium, silicon, magnesium by the intensity of Element Potassium, sodium, calcium, silicon, magnesium in sample solution;
(5) computation and measurement result, obtains the percentage composition of potassium in sample, sodium, calcium, silicon, magnesium,
Be calculated as follows the mass percent w of Element Potassium in sample, sodium, calcium, silicon, magnesium, numerical value represents with %:
In formula:
ρ---the mass concentration of analytical element (potassium, sodium, calcium, silicon, magnesium) in test solution, unit is every milliliter of microgram (μ g/mL);
V---test solution volume, unit is milliliter (mL);
M---test portion quality, unit is gram (g).
Low temperature described in said method refers to that heated perimeter is at 50 ~ 200 DEG C.
Condition of work and the analytical line of inductive coupling plasma emission spectrograph are as follows: incident power 0.95 ~ 1.4KW; Reflective power <20W; Cooling gas flow 12 ~ 20L/min; Sample lifting capacity 1.0 ~ 1.5mL/min; Integral time 1 ~ 10s; Ultimate analysis line K766.490nm, Na588.995nm, Ca393.366nm, Si251.611nm and Mg279.553nm.
The advantage of technical solution of the present invention is:
1) method detection limit is low is one of advantage of this patent.This method by spectra1 interfer-research and instrument detection limit development test, employing sample the mode with sample concentration more, can measure content in nickel oxide sample be low to moderate 0.0001% potassium, sodium, calcium, silicon, magnesium elements content.
2) contaminated possibility is little is one of advantage of this patent.Potassium, sodium, calcium, silicon, magnesium elements are all elements that nature is rich in, and are very easily subject to the pollution that impurity element is introduced when analyzing Trace K, sodium, calcium, silicon, magnesium elements.The working curve of this method is the synthetic work curve without matrix, matrix is not added in working curve solution, avoid and add contaminating impurity in matrix that matrix likely brings into, adding reagent is that top grade is pure, avoids the impurity element that reagent imports as far as possible and pollutes.
3) analytical approach measurement range is wide, and measurement lower limit is 0.0001%, and measuring the upper limit is 0.5%.
4) this patented method is measured fast, easy and simple to handle, has saved a large amount of man power and material.
Embodiment
Embodiment one
Measure potassium, sodium, calcium, silicon, magnesium elements in high-purity nickel oxide, following instrument is measured
Adopt JY ULTIMAIIC type inductive coupling plasma emission spectrograph, the condition of work of instrument and the following incident power 1050W of analytical line; Reflective power <10W; Cooling gas flow 15L/min; Sample lifting capacity 1.5mL/min; Integral time 5s; Ultimate analysis line: K766.490nm, Na588.995nm, Ca393.366nm, Si251.611nm and Mg279.553nm.
(1) reagent, used in mensuration process is as follows:
(1.1), hydrochloric acid I, density is 1.19g/mL, more than top grade is pure;
(1.2), hydrochloric acid II, 1+1, hydrochloric acid I and water mix by volume at 1: 1;
(1.3), nitric acid I, density is 1.42g/mL, more than top grade is pure;
(1.4), nitric acid II, 1+1, nitric acid I and water mix by volume at 1: 1;
(1.5), NaOH, more than top grade is pure;
(1.6), the quality-volumetric concentration of sodium standard solution I is 0.10mg/mL, and preparation method accurately takes 0.1886g sodium chloride, and its massfraction is not less than 99.95%, be placed in 100mL beaker, be dissolved in water, move in 1000mL volumetric flask, be diluted with water to scale, shake up;
(1.7), the quality-volumetric concentration of sodium standard solution II is 0.01mg/mL, and preparation method pipettes 20mL sodium standard solution I in 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.8), the quality-volumetric concentration of sodium standard solution III is 0.001mg/mL, and preparation method pipettes 20mL sodium standard solution II in 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.9), the quality-volumetric concentration of potassium standard solution I is 0.10mg/mL, and preparation method accurately takes 0.1907g potassium chloride, and its massfraction is not less than 99.95%, be placed in 100mL beaker, be dissolved in water, move in 1000mL volumetric flask, be diluted with water to scale, shake up;
(1.10), the quality-volumetric concentration of potassium standard solution II is 0.01mg/mL, and preparation method pipettes 20mL potassium standard solution I in 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.11), the quality-volumetric concentration of potassium standard solution III is 0.001mg/mL, and preparation method pipettes 20mL potassium standard solution II in 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.12), the quality-volumetric concentration of calcium standard solution I is 0.10mg/mL, preparation method is the calcium carbonate taking 0.1249g previously baked (at 110 DEG C of baking 2h) and be cooled to room temperature in exsiccator, its massfraction is not less than 99.95%, be placed in 100mL beaker, add 30mL hydrochloric acid II, low-temperature heat is to dissolving completely, move into after cooling in 500mL volumetric flask, add 20mL hydrochloric acid II, be diluted with water to scale, shake up.
(1.13), the quality-volumetric concentration of calcium standard solution II is 0.01mg/mL, and preparation method pipettes 20.00mL calcium standard solution I in 200mL volumetric flask, adds 20mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.14), the quality-volumetric concentration of calcium standard solution III is 0.001mg/mL, and preparation method pipettes 20.00mL calcium standard solution II in 200mL volumetric flask, adds 20mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.15), the quality-volumetric concentration of silicon standard solution I is 0.10mg/mL, preparation method takes 0.1000g through levigate monocrystalline silicon or polysilicon, and its massfraction is not less than 99.95%, is placed in 100mL polytetrafluoroethylene beaker, add 20g NaOH, 100mL water, shakes gently, puts into boiling water bath, be heated to dissolve completely, move into after cooling in 1000mL plastics volumetric flask, be diluted with water to scale, shake up.
(1.16), the quality-volumetric concentration of silicon standard solution II is 0.01mg/mL, and preparation method pipettes 20.00mL silicon standard solution I in 200mL volumetric flask, adds 20mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.17), the quality-volumetric concentration of silicon standard solution III is 0.001mg/mL, and preparation method pipettes 20.00mL silicon standard solution II in 200mL volumetric flask, adds 20mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.18), the quality-volumetric concentration of magnesium standard solution I is 0.10mg/mL, preparation method takes the pure magnesium of 0.1000g, its massfraction is not less than 99.95%, be placed in 150mL beaker, add 20mL hydrochloric acid II, low-temperature heat is to dissolving completely, move into after cooling in 1000mL volumetric flask, add 80mL hydrochloric acid II, be diluted with water to scale, shake up.
(1.19), the quality-volumetric concentration of magnesium standard solution II is 0.01mg/mL, and preparation method pipettes 20.00mL magnesium standard solution I in 200mL volumetric flask, adds 20mL hydrochloric acid II, is diluted with water to scale, shakes up.
(1.20), the quality-volumetric concentration of magnesium standard solution III is 0.001mg/mL, and preparation method pipettes 20.00mL magnesium standard solution II in 200mL volumetric flask, adds 20mL hydrochloric acid II, is diluted with water to scale, shakes up.
(2), sampling and sample preparation: the sample analyzed carries out sampling and sample preparation according to the requirement of GB/T 20066;
(3), analytical procedure is as follows:
(3.1), test portion: take 2.0g sample, be accurate to 0.0001g.
(3.2), prepare sample solution: the test portion of analytical procedure (3.1) is placed in 100mL beaker, add 15mL nitric acid II(1.4), low-temperature heat, to reacting stopping, moving into 50mL volumetric flask after cooling, is diluted with water to scale, shakes up.
(3.3), preparation work curve solution
Two blank reagent solutions are prepared by analytical procedure (3.2), move in 50mL volumetric flask, according to potassium in sample, sodium, calcium, silicon, the content range of magnesium, 2mL potassium standard solution II(1.10 is added) in second solution, 2mL sodium standard solution II(1.7), 2mL calcium standard solution II(1.13), 2mL silicon standard solution II(1.16) and 2mL magnesium standard solution II(1.19), make potassium in first job curve solution, sodium, calcium, silicon, the content of magnesium is 0 μ g/mL, potassium in second working curve solution, sodium, calcium, silicon, the content of magnesium is 0.4 μ g/mL, be diluted with water to scale, shake up, as working curve solution,
(3.4), measure potassium in test solution, sodium, calcium, silicon, the mass concentration (μ g/mL) of magnesium: on inductively coupled plasma atomic emission spectrometer, by selected condition of work, analytical element potassium in surveying work curve solution successively, sodium, calcium, silicon, the intensity of magnesium, horizontal ordinate potassium in working curve solution, sodium, calcium, silicon, the mass concentration (μ g/mL) of magnesium elements, ordinate potassium, sodium, calcium, silicon, the intensity drawing curve of magnesium elements, then, measure potassium in sample solution, sodium, calcium, silicon, the intensity of magnesium elements, with potassium, sodium, calcium, silicon, the intensity of magnesium elements finds corresponding potassium on working curve, sodium, calcium, silicon, the mass concentration (μ g/mL) of magnesium elements,
(4), be calculated as follows the massfraction w of analytical element (potassium, sodium, calcium, silicon, magnesium) element, numerical value represents with %:
In formula:
ρ---the mass concentration of analytical element (potassium, sodium, calcium, silicon, magnesium) in test solution, unit is every milliliter of microgram (μ g/mL);
V---test solution volume, unit is milliliter (mL);
M---test portion quality, unit is gram (g).
The content obtaining potassium, sodium, calcium, silicon, magnesium in this nickel oxide sample is respectively 0.00025%, 0.0045%, 0.0051%, 0.00065%, 0.00084%.
Embodiment two
Measure potassium, sodium, calcium, silicon, magnesium elements in nickel oxide, following instrument is measured
Adopt JY ULTIMAIIC type inductive coupling plasma emission spectrograph, condition of work and the analytical line of instrument are as follows: incident power 950W; Reflective power: <10W; Cooling gas flow: 14L/min; Sample lifting capacity: 1.5mL/min; Integral time: 2s; Ultimate analysis line: K766.490nm, Na 588.995nm, Ca393.366nm, Si251.611nm and Mg279.553nm.
(1) reagent, used in mensuration process is as follows:
(1.1), hydrochloric acid I, density is 1.19g/mL, more than top grade is pure;
(1.2), hydrochloric acid II, 1+1, hydrochloric acid I and water mix by volume at 1: 1;
(1.3), nitric acid I, density is 1.42g/mL, more than top grade is pure;
(1.4), nitric acid II, 1+1, nitric acid I and water mix by volume at 1: 1;
(1.5), NaOH, more than top grade is pure;
(1.6), the quality-volumetric concentration of sodium standard solution I is 0.10mg/mL, and preparation method accurately takes 0.1886g sodium chloride, and its massfraction is not less than 99.95%, be placed in 100mL beaker, be dissolved in water, move in 1000mL volumetric flask, be diluted with water to scale, shake up;
(1.7), the quality-volumetric concentration of sodium standard solution II is 0.01mg/mL, and preparation method pipettes 20mL sodium standard solution I in 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.8), the quality-volumetric concentration of sodium standard solution III is 0.001mg/mL, and preparation method pipettes 20mL sodium standard solution II in 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.9), the quality-volumetric concentration of potassium standard solution I is 0.10mg/mL, and preparation method accurately takes 0.1907g potassium chloride, and its massfraction is not less than 99.95%, be placed in 100mL beaker, be dissolved in water, move in 1000mL volumetric flask, be diluted with water to scale, shake up;
(1.10), the quality-volumetric concentration of potassium standard solution II is 0.01mg/mL, and preparation method pipettes 20mL potassium standard solution I in 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.11), the quality-volumetric concentration of potassium standard solution III is 0.001mg/mL, and preparation method pipettes 20mL potassium standard solution II in 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.12), the quality-volumetric concentration of calcium standard solution I is 0.10mg/mL, preparation method is the calcium carbonate taking 0.1249g previously baked (at 110 DEG C of baking 2h) and be cooled to room temperature in exsiccator, its massfraction is not less than 99.95%, be placed in 100mL beaker, add 40mL hydrochloric acid II, low-temperature heat is to dissolving completely, move into after cooling in 500mL volumetric flask, add 30mL hydrochloric acid II, be diluted with water to scale, shake up.
(1.13), the quality-volumetric concentration of calcium standard solution II is 0.01mg/mL, and preparation method pipettes 20.00mL calcium standard solution I in 200mL volumetric flask, adds 30mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.14), the quality-volumetric concentration of calcium standard solution III is 0.001mg/mL, and preparation method pipettes 20.00mL calcium standard solution II in 200mL volumetric flask, adds 30mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.15), the quality-volumetric concentration of silicon standard solution I is 0.10mg/mL, preparation method takes 0.1000g through levigate monocrystalline silicon or polysilicon, and its massfraction is not less than 99.95%, is placed in 100mL polytetrafluoroethylene beaker, add 30g NaOH, 100mL water, shakes gently, puts into boiling water bath, be heated to dissolve completely, move into after cooling in 1000mL plastics volumetric flask, be diluted with water to scale, shake up.
(1.16), the quality-volumetric concentration of silicon standard solution II is 0.01mg/mL, and preparation method pipettes 20.00mL silicon standard solution I in 200mL volumetric flask, adds 30mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.17), the quality-volumetric concentration of silicon standard solution III is 0.001mg/mL, and preparation method pipettes 20.00mL silicon standard solution II in 200mL volumetric flask, adds 30mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.18), the quality-volumetric concentration of magnesium standard solution I is 0.10mg/mL, preparation method takes the pure magnesium of 0.1000g, its massfraction is not less than 99.95%, be placed in 150mL beaker, add 30mL hydrochloric acid II, low-temperature heat is to dissolving completely, move into after cooling in 1000mL volumetric flask, add 100mL hydrochloric acid II, be diluted with water to scale, shake up.
(1.19), the quality-volumetric concentration of magnesium standard solution II is 0.01mg/mL, and preparation method pipettes 20.00mL magnesium standard solution I in 200mL volumetric flask, adds 30mL hydrochloric acid II, is diluted with water to scale, shakes up.
(1.20), the quality-volumetric concentration of magnesium standard solution III is 0.001mg/mL, and preparation method pipettes 20.00mL magnesium standard solution II in 200mL volumetric flask, adds 30mL hydrochloric acid II, is diluted with water to scale, shakes up.
(2), sampling and sample preparation: the sample analyzed carries out sampling and sample preparation according to the requirement of GB/T 20066;
(3), analytical procedure is as follows:
(3.1), test portion: take 0.1g sample, be accurate to 0.0001g.
(3.2), prepare sample solution: the test portion of analytical procedure (3.1) is placed in 100mL beaker, add 10mL nitric acid (1.4), low-temperature heat, to reacting stopping, moving into 50mL volumetric flask after cooling, is diluted with water to scale, shakes up.
(3.3), preparation work curve solution
Two blank reagent solutions are prepared by analytical procedure (3.2), move in 50mL volumetric flask, according to potassium in sample, sodium, calcium, silicon, the content range of magnesium, 5mL potassium standard solution I(1.9 is added) in second solution, 5mL sodium standard solution I(1.6), 5mL calcium standard solution I(1.12), 5mL silicon standard solution I(1.15) and 5mL magnesium standard solution I(1.18), make potassium in first job curve solution, sodium, calcium, silicon, the content of magnesium is 0 μ g/mL, potassium in second working curve solution, sodium, calcium, silicon, the content of magnesium is 10.0 μ g/mL, be diluted with water to scale, shake up, as working curve solution,
(3.4), measure potassium in test solution, sodium, calcium, silicon, the mass concentration (μ g/mL) of magnesium: on inductively coupled plasma atomic emission spectrometer, by selected condition of work, analytical element potassium in surveying work curve solution successively, sodium, calcium, silicon, the intensity of magnesium, horizontal ordinate potassium in working curve solution, sodium, calcium, silicon, the mass concentration (μ g/mL) of magnesium elements, ordinate potassium, sodium, calcium, silicon, the intensity drawing curve of magnesium elements, then, measure potassium in sample solution, sodium, calcium, silicon, the intensity of magnesium elements, with potassium, sodium, calcium, silicon, the intensity of magnesium elements finds corresponding potassium on working curve, sodium, calcium, silicon, the mass concentration (μ g/mL) of magnesium elements,
(4), be calculated as follows the massfraction w of analytical element (potassium, sodium, calcium, silicon, magnesium) element, numerical value represents with %:
In formula:
ρ---the mass concentration of analytical element (potassium, sodium, calcium, silicon, magnesium) in test solution, unit is every milliliter of microgram (μ g/mL);
V---test solution volume, unit is milliliter (mL);
M---test portion quality, unit is gram (g).
The content respectively obtaining potassium, sodium, calcium, silicon, magnesium in this nickel oxide sample is 0.32%, 0.39%, 0.15%, 0.56%, 0.24%.
Embodiment three
Measure potassium, sodium, calcium, silicon, magnesium elements in nickel oxide, following instrument is measured
Adopt JY ULTIMAIIC type inductive coupling plasma emission spectrograph, condition of work and the analytical line of instrument are as follows: incident power 1150W; Reflective power <10W; Cooling gas flow 16L/min; Sample lifting capacity 1.2mL/min; Integral time 10s; Ultimate analysis line: K766.490nm, Na588.995nm, Ca393.366nm, Si251.611nm and Mg279.553nm.
(1) reagent, used in mensuration process is as follows:
(1.1), hydrochloric acid I, density is 1.19g/mL, more than top grade is pure;
(1.2), hydrochloric acid II, 1+1, hydrochloric acid I and water mix by volume at 1: 1;
(1.3), nitric acid I, density is 1.42g/mL, more than top grade is pure;
(1.4), nitric acid II, 1+1, nitric acid I and water mix by volume at 1: 1;
(1.5), NaOH, more than top grade is pure;
(1.6), the quality-volumetric concentration of sodium standard solution I is 0.10mg/mL, and preparation method accurately takes 0.1886g sodium chloride, and its massfraction is not less than 99.95%, be placed in 100mL beaker, be dissolved in water, move in 1000mL volumetric flask, be diluted with water to scale, shake up;
(1.7), the quality-volumetric concentration of sodium standard solution II is 0.01mg/mL, and preparation method pipettes 20mL sodium standard solution I in 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.8), the quality-volumetric concentration of sodium standard solution III is 0.001mg/mL, and preparation method pipettes 20mL sodium standard solution II in 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.9), the quality-volumetric concentration of potassium standard solution I is 0.10mg/mL, and preparation method accurately takes 0.1907g potassium chloride, and its massfraction is not less than 99.95%, be placed in 100mL beaker, be dissolved in water, move in 1000mL volumetric flask, be diluted with water to scale, shake up;
(1.10), the quality-volumetric concentration of potassium standard solution II is 0.01mg/mL, and preparation method pipettes 20mL potassium standard solution I in 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.11), the quality-volumetric concentration of potassium standard solution III is 0.001mg/mL, and preparation method pipettes 20mL potassium standard solution II in 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.12), the quality-volumetric concentration of calcium standard solution I is 0.10mg/mL, preparation method is the calcium carbonate taking 0.1249g previously baked (at 110 DEG C of baking 2h) and be cooled to room temperature in exsiccator, its massfraction is not less than 99.95%, be placed in 100mL beaker, add 20mL hydrochloric acid II, low-temperature heat is to dissolving completely, move into after cooling in 500mL volumetric flask, add 10mL hydrochloric acid II, be diluted with water to scale, shake up.
(1.13), the quality-volumetric concentration of calcium standard solution II is 0.01mg/mL, and preparation method pipettes 20.00mL calcium standard solution I in 200mL volumetric flask, adds 10mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.14), the quality-volumetric concentration of calcium standard solution III is 0.001mg/mL, and preparation method pipettes 20.00mL calcium standard solution II in 200mL volumetric flask, adds 10mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.15), the quality-volumetric concentration of silicon standard solution I is 0.10mg/mL, preparation method takes 0.1000g through levigate monocrystalline silicon or polysilicon, and its massfraction is not less than 99.95%, is placed in 100mL polytetrafluoroethylene beaker, add 10g NaOH, 100mL water, shakes gently, puts into boiling water bath, be heated to dissolve completely, move into after cooling in 1000mL plastics volumetric flask, be diluted with water to scale, shake up.
(1.16), the quality-volumetric concentration of silicon standard solution II is 0.01mg/mL, and preparation method pipettes 20.00mL silicon standard solution I in 200mL volumetric flask, adds 10mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.17), the quality-volumetric concentration of silicon standard solution III is 0.001mg/mL, and preparation method pipettes 20.00mL silicon standard solution II in 200mL volumetric flask, adds 10mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.18), the quality-volumetric concentration of magnesium standard solution I is 0.10mg/mL, preparation method takes the pure magnesium of 0.1000g, its massfraction is not less than 99.95%, be placed in 150mL beaker, add 10mL hydrochloric acid II, low-temperature heat is to dissolving completely, move into after cooling in 1000mL volumetric flask, add 60mL hydrochloric acid II, be diluted with water to scale, shake up.
(1.19), the quality-volumetric concentration of magnesium standard solution II is 0.01mg/mL, and preparation method pipettes 20.00mL magnesium standard solution I in 200mL volumetric flask, adds 10mL hydrochloric acid II, is diluted with water to scale, shakes up.
(1.20), the quality-volumetric concentration of magnesium standard solution III is 0.001mg/mL, and preparation method pipettes 20.00mL magnesium standard solution II in 200mL volumetric flask, adds 10mL hydrochloric acid II, is diluted with water to scale, shakes up.
(2), sampling and sample preparation: the sample analyzed carries out sampling and sample preparation according to the requirement of GB/T 20066;
(3), analytical procedure is as follows:
(3.1), test portion: take 0.5g sample, be accurate to 0.0001g.
(3.2), prepare sample solution: the test portion of analytical procedure (3.1) is placed in 100mL beaker, add 20mL nitric acid (1.4), low-temperature heat, to reacting stopping, moving into 50mL volumetric flask after cooling, is diluted with water to scale, shakes up.
(3.3), preparation work curve solution
Prepare three blank reagent solutions by analytical procedure (3.2), move in 50mL volumetric flask, according to potassium in sample, sodium, calcium, silicon, the content range of magnesium, adds 5mL potassium standard solution III(1.11 in second solution), 5mL sodium standard solution III(1.8), 5mL calcium standard solution III(1.14), 5mL silicon standard solution III(1.17) and 5mL magnesium standard solution III(1.20), in the 3rd solution, add 5mL potassium standard solution II(1.10), 5mL sodium standard solution II(1.7), 5mL calcium standard solution II(1.13), 5mL silicon standard solution II(1.16) and 5mL magnesium standard solution II(1.19), make potassium in first job curve solution, sodium, calcium, silicon, the content of magnesium is 0 μ g/mL, potassium in second working curve solution, sodium, calcium, silicon, the content of magnesium is 0.1 μ g/mL, potassium in the 3rd working curve solution, sodium, calcium, silicon, the content of magnesium is 1.0 μ g/mL, is diluted with water to scale, shakes up, as working curve solution,
(3.4), measure potassium in test solution, sodium, calcium, silicon, the mass concentration (μ g/mL) of magnesium: on inductively coupled plasma atomic emission spectrometer, by selected condition of work, analytical element potassium in surveying work curve solution successively, sodium, calcium, silicon, the intensity of magnesium, horizontal ordinate potassium in working curve solution, sodium, calcium, silicon, the mass concentration (μ g/mL) of magnesium elements, ordinate potassium, sodium, calcium, silicon, the intensity drawing curve of magnesium elements, then, measure potassium in sample solution, sodium, calcium, silicon, the intensity of magnesium elements, with potassium, sodium, calcium, silicon, the intensity of magnesium elements finds corresponding potassium on working curve, sodium, calcium, silicon, the mass concentration (μ g/mL) of magnesium elements,
(4), be calculated as follows the massfraction w of analytical element (potassium, sodium, calcium, silicon, magnesium) element, numerical value represents with %:
In formula:
ρ---the mass concentration of analytical element (potassium, sodium, calcium, silicon, magnesium) in test solution, unit is every milliliter of microgram (μ g/mL);
V---test solution volume, unit is milliliter (mL);
M---test portion quality, unit is gram (g).
The content obtaining potassium, sodium, calcium, silicon, magnesium in this nickel oxide sample is respectively 0.0081%, 0.0032%, 0.0015%, 0.0019%, 0.0056%.
Compared with prior art, advantage of the present invention is: analytical approach measurement range is wide, and measurement lower limit is 0.0001%, and measuring the upper limit is 0.5%, and the method is measured fast, easy and simple to handle, has saved a large amount of man power and material.
Claims (2)
1. measure a method for potassium in nickel oxide, sodium, calcium, silicon, magnesium element content, it is characterized in that: the reagent that the method uses in mensuration process is:
Hydrochloric acid I, density is 1.19g/mL, more than top grade is pure;
Hydrochloric acid II, 1+1, hydrochloric acid I and water mix by volume at 1: 1;
Nitric acid I, density is 1.42g/mL, more than top grade is pure;
Nitric acid II, 1+1, nitric acid I and water mix by volume at 1: 1;
NaOH, more than top grade is pure;
Sodium standard solution I, quality-volumetric concentration be 0.10mg/mL, preparation method accurately takes 0.1886g sodium chloride, its massfraction is not less than 99.95%, is placed in 100mL beaker, is dissolved in water, move in 1000mL volumetric flask, be diluted with water to scale, shake up;
Sodium standard solution II, quality-volumetric concentration is 0.01mg/mL, and preparation method pipettes 20mL sodium standard solution I in 200mL volumetric flask, is diluted with water to scale, shakes up;
Sodium standard solution III, quality-volumetric concentration is 0.001mg/mL, and preparation method pipettes 20mL sodium standard solution II in 200mL volumetric flask, is diluted with water to scale, shakes up;
Potassium standard solution I, quality-volumetric concentration is 0.10mg/mL, and preparation method accurately takes 0.1907g potassium chloride, and its massfraction is not less than 99.95%, is placed in 100mL beaker, is dissolved in water, and moves in 1000mL volumetric flask, is diluted with water to scale, shakes up;
Potassium standard solution II, quality-volumetric concentration is 0.01mg/mL, and preparation method pipettes 20mL potassium standard solution I in 200mL volumetric flask, is diluted with water to scale, shakes up;
Potassium standard solution III, quality-volumetric concentration is 0.001mg/mL, and preparation method pipettes 20mL potassium standard solution II in 200mL volumetric flask, is diluted with water to scale, shakes up;
Calcium standard solution I, quality-volumetric concentration is 0.10mg/mL, and preparation method is that to take 0.1249g previously baked, 1 ~ 2h is toasted at 100 DEG C ~ 110 DEG C, and in exsiccator, being cooled to the calcium carbonate of room temperature, its massfraction is not less than 99.95%, is placed in 100mL beaker, add 10 ~ 40mL hydrochloric acid II, low-temperature heat, to dissolving completely, moves in 500mL volumetric flask after cooling, adds 10 ~ 30mL hydrochloric acid II, be diluted with water to scale, shake up;
Calcium standard solution II, quality-volumetric concentration is 0.01mg/mL, and preparation method pipettes 20.00mL calcium standard solution I in 200mL volumetric flask, adds 10 ~ 30mL hydrochloric acid I, is diluted with water to scale, shakes up;
Calcium standard solution III, quality-volumetric concentration is 0.001mg/mL, and preparation method pipettes 20.00mL calcium standard solution II in 200mL volumetric flask, adds 10 ~ 30mL hydrochloric acid I, is diluted with water to scale, shakes up;
Silicon standard solution I, quality-volumetric concentration is 0.10mg/mL, and preparation method takes 0.1000g through levigate monocrystalline silicon or polysilicon, its massfraction is not less than 99.95%, be placed in 100mL polytetrafluoroethylene beaker, add 10 ~ 30g NaOH, 50 ~ 150mL water, shake gently, put into boiling water bath, be heated to dissolve completely, move in 1000mL plastics volumetric flask after cooling, be diluted with water to scale, shake up;
Silicon standard solution II, quality-volumetric concentration is 0.01mg/mL, and preparation method pipettes 20.00mL silicon standard solution I in 200mL volumetric flask, adds 10 ~ 30mL hydrochloric acid I, is diluted with water to scale, shakes up;
Silicon standard solution III, quality-volumetric concentration is 0.001mg/mL, and preparation method pipettes 20.00mL silicon standard solution II in 200mL volumetric flask, adds 10 ~ 30mL hydrochloric acid I, is diluted with water to scale, shakes up;
Magnesium standard solution I, quality-volumetric concentration is 0.10mg/mL, preparation method takes the pure magnesium of 0.1000g, its massfraction is not less than 99.95%, is placed in 150mL beaker and adds 10 ~ 30mL hydrochloric acid II, and low-temperature heat is to dissolving completely, move into after cooling in 1000mL volumetric flask, add 50 ~ 100mL hydrochloric acid II, be diluted with water to scale, shake up;
Magnesium standard solution II, quality-volumetric concentration is 0.01mg/mL, and preparation method pipettes 20.00mL magnesium standard solution I in 200mL volumetric flask, adds 10 ~ 30mL hydrochloric acid II, is diluted with water to scale, shakes up;
Magnesium standard solution III, quality-volumetric concentration is 0.001mg/mL, and preparation method pipettes 20.00mL magnesium standard solution II in 200mL volumetric flask, adds 10 ~ 30mL hydrochloric acid II, is diluted with water to scale, shakes up;
The step of the mensuration process of the method is:
(1) sample carries out sampling and sample preparation according to the requirement of GB/T 20066, takes 0.1 ~ 2.0g sample, is accurate to 0.0001g;
(2) prepare sample solution
Sample is placed in 100mL beaker, adds 10 ~ 30mL nitric acid II, low-temperature heat, to dissolving completely, moves into 50mL volumetric flask after cooling, is diluted with water to scale, shakes up;
(3) preparation work curve solution:
In 2 ~ 8 100mL beakers, add and step (2) identical amount nitric acid II, low-temperature heat is to dissolving completely, several corresponding 50mL volumetric flask is moved into after cooling, according to potassium in the sample learnt in advance, sodium, calcium, silicon, the content range of magnesium, potassium standard solution I or the potassium standard solution II or potassium standard solution III of different volumes number is added in each volumetric flask, the sodium standard solution I of different volumes number or sodium standard solution II or sodium standard solution III, the calcium standard solution I of different volumes number or calcium standard solution II or calcium standard solution III, the silicon standard solution I of different volumes number or the magnesium standard solution I of silicon standard solution II or silicon standard solution III and different volumes number or magnesium standard solution II or magnesium standard solution III, make the potassium in each volumetric flask, sodium, calcium, silicon, the content of magnesium is the sample potassium learnt, sodium, calcium, silicon, 0% ~ 200% of content of magnesium, be diluted with water to scale, shake up, as working curve solution,
(4) mass concentration of analytical element potassium, sodium, calcium, silicon, magnesium in sample solution is measured
By the intensity of inductively coupled plasma atomic emission spectrometer analytical element potassium, sodium, calcium, silicon, magnesium in spectral line K766.490nm, Na588.995nm, Ca393.366nm, Si251.611nm and Mg279.553nm successively surveying work curve solution, the horizontal ordinate mass concentration of analytical element potassium, sodium, calcium, silicon, magnesium in working curve solution, the respective strengths of ordinate analytical element potassium, sodium, calcium, silicon, magnesium, drawing curve;
Then measure the intensity of Element Potassium, sodium, calcium, silicon, magnesium in sample solution, on corresponding working curve, find the mass concentration of corresponding analysis Element Potassium, sodium, calcium, silicon, magnesium by the intensity of Element Potassium, sodium, calcium, silicon, magnesium in sample solution;
(5) computation and measurement result, obtains the percentage composition of potassium in sample, sodium, calcium, silicon, magnesium,
Be calculated as follows the mass percent w of Element Potassium in sample, sodium, calcium, silicon, magnesium, numerical value represents with %:
In formula:
The mass concentration of analytical element potassium, sodium, calcium, silicon, magnesium in ρ-test solution, unit is every milliliter of microgram μ g/mL;
V---test solution volume, unit is milliliter mL;
M---test portion quality, unit is a gram g;
Low temperature described in said method refers to that heated perimeter is at 50 ~ 200 DEG C.
2. the method for potassium, sodium, calcium, silicon, magnesium element content in mensuration nickel oxide according to claim 1, is characterized in that: condition of work and the analytical line of inductive coupling plasma emission spectrograph are as follows: incident power 0.95 ~ 1.4KW; Reflective power <20W; Cooling gas flow 12 ~ 20L/min; Sample lifting capacity 1.0 ~ 1.5mL/min; Integral time 1 ~ 10s; Ultimate analysis line K766.490nm, Na 588.995nm, Ca393.366nm, Si251.611nm and Mg279.553nm.
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| CN103257136A (en) * | 2013-04-12 | 2013-08-21 | 中国航空工业集团公司北京航空材料研究院 | Determination method for calcium, cobalt, chromium and iron in tungsten carbide |
| CN103217413B (en) * | 2013-04-15 | 2015-07-22 | 攀钢集团攀枝花钢铁研究院有限公司 | Analysis method for determining potassium in potassium metavanadate and/or sodium in sodium metavanadate |
| CN103234958B (en) * | 2013-04-15 | 2015-08-26 | 攀钢集团攀枝花钢铁研究院有限公司 | Measure the method for Determination of Potassium in the vanadium wastewater in vanadium oxide production technology |
| CN103940650B (en) * | 2014-04-10 | 2016-08-17 | 中国航空工业集团公司北京航空材料研究院 | A kind of measure the method for ferrum nickel in high density tungsten basigamy pouring weight |
| CN104048951B (en) * | 2014-07-04 | 2017-02-15 | 武钢集团昆明钢铁股份有限公司 | Method for measuring contents of silicon, calcium and aluminum in additives and co-solvents of permanent magnetic ferrites through ICP (Inductively Coupled Plasma) emission spectroscopy |
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