CN102721582A - 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 of measuring potassium in the 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, has obtained widespread use at aspects such as Aero-Space, catalysis, battery electrode, photoelectricity converting materials, has also shown fine application prospect.Along with improving constantly of nickel oxide technology of preparing, the purity of quality oxide nickel also improves constantly.The content of potassium, sodium, calcium, silicon, magnesium elements has material impact to the performance of nickel oxide in the nickel oxide.
The analytical approach of analyzing nickel oxide at present has polarography determination trace Cd, Pb element; Atomic fluorescence spectrometry [3] is measured micro-As and Sb in metallic nickel and the nickel oxide; Nickelic content in the complexometric titration nickel oxide; Human co-precipitation ICP-AESs such as Osamu Kujirai are measured seven trace impurities such as Al, As, Cr, Fe, Ti, V, Zr in high-purity metal nickel and the nickel oxide, and inductively coupled plasma emission spectrography of no use (ICP-AES) is analyzed the report of potassium, sodium, calcium, silicon, magnesium in the nickel oxide.
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 have become one of chemico-analytic conventional powerful measure, can analyze the most of impurity elements in the nickel oxide.
Summary of the invention
The present invention is just to above-mentioned prior art situation and design a kind of method of measuring potassium in the nickel oxide, sodium, calcium, silicon, magnesium element content that provides, and its objective is that a kind of molten appearance speed is fast, analysis precision is high, the method for potassium, sodium, calcium, silicon, magnesium element content in easy and simple to handle, the mensuration nickel oxide that efficient is high.
Technical scheme of the present invention utilizes inductively coupled plasma emission spectrography (ICP-AES) to analyze potassium, sodium, calcium, silicon, magnesium in the nickel oxide, method accurately and reliably, easy fast, the analysis efficiency of the nickel oxide that is improved with analyze quality.
The objective of the invention is to realize through following technical scheme:
This kind measured the method for potassium, sodium, calcium, silicon, magnesium element content in the nickel oxide, and it is characterized in that: the reagent that this method is used in the 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 mixed in 1: 1 by volume;
Nitric acid I, density is 1.42g/mL, more than top grade is pure;
Nitric acid II, 1+1, nitric acid I and water mixed in 1: 1 by volume;
NaOH is more than top grade is pure;
Sodium standard solution I, quality-volumetric concentration be 0.10mg/mL, the preparation method accurately takes by weighing 0.1886g sodium chloride; Its massfraction is not less than 99.95%, places the 100mL beaker, is dissolved in water; Move in the 1000mL volumetric flask, be diluted with water to scale, shake up;
Sodium standard solution II, quality-volumetric concentration is 0.01mg/mL, the preparation method pipettes 20mL sodium standard solution I in the 200mL volumetric flask, is diluted with water to scale, shakes up;
Sodium standard solution III, quality-volumetric concentration is 0.001mg/mL, the preparation method pipettes 20mL sodium standard solution II in the 200mL volumetric flask, is diluted with water to scale, shakes up;
Potassium standard solution I, quality-volumetric concentration is 0.10mg/mL, and the preparation method accurately takes by weighing 0.1907g potassium chloride, and its massfraction is not less than 99.95%, places the 100mL beaker, is dissolved in water, and moves in the 1000mL volumetric flask, is diluted with water to scale, shakes up;
Potassium standard solution II, quality-volumetric concentration is 0.01mg/mL, the preparation method pipettes 20mL potassium standard solution I in the 200mL volumetric flask, is diluted with water to scale, shakes up;
Potassium standard solution III, quality-volumetric concentration is 0.001mg/mL, the preparation method pipettes 20mL potassium standard solution II in the 200mL volumetric flask, is diluted with water to scale, shakes up;
Calcium standard solution I, quality-volumetric concentration is 0.10mg/mL, the preparation method is that to take by weighing 0.1249g previously baked (100 ℃～110 ℃ bakings 1～2h) and in exsiccator, be cooled to the lime carbonate of room temperature; Its massfraction is not less than 99.95%, places the 100mL beaker, adds 10～40mL hydrochloric acid II; Low-temperature heat to dissolving moves in the 500mL volumetric flask after the cooling fully, 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, the preparation method pipettes 20.00mL calcium standard solution I in the 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, the preparation method pipettes 20.00mL calcium standard solution II in the 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 the preparation method takes by weighing 0.1000g through levigate monocrystalline silicon or polysilicon, and its massfraction is not less than 99.95%; Place the 100mL polytetrafluoroethylene beaker, add 10～30g NaOH, 50～150mL water; Shake gently, put into boiling water bath, be heated to dissolving fully; The cooling back moves in the 1000mL plastics volumetric flask, is diluted with water to scale, shakes up.
Silicon standard solution II, quality-volumetric concentration is 0.01mg/mL, the preparation method pipettes 20.00mL silicon standard solution I in the 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, the preparation method pipettes 20.00mL silicon standard solution II in the 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, the preparation method takes by weighing the pure magnesium of 0.1000g; Its massfraction is not less than 99.95%, places the 150mL beaker to add 10～30mL hydrochloric acid II, and low-temperature heat to dissolving fully; The cooling back moves in the 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, the preparation method pipettes 20.00mL magnesium standard solution I in the 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, the preparation method pipettes 20.00mL magnesium standard solution II in the 200mL volumetric flask, adds 10～30mL hydrochloric acid II, is diluted with water to scale, shakes up.
The step of the mensuration process of this method is:
⑴ sample carries out the sample circuit sample preparation according to the requirement of GB/T 20066, takes by weighing 0.1 ~ 2.0g sample, is accurate to 0.0001g;
⑵ prepare sample solution
Sample is placed the 100mL beaker, add 10 ~ 30mL nitric acid II, low-temperature heat to dissolving is cooled off the back and is moved into the 50mL volumetric flask fully, is diluted with water to scale, shakes up;
⑶ preparation work curve solution:
In 2 ~ 8 100mL beakers; Add and step ⑵ same amount nitric acid II; Low-temperature heat to dissolving fully; The cooling back moves into several corresponding 50mL volumetric flasks; Content range according to potassium, sodium, calcium, silicon, magnesium in the sample of learning in advance; In each volumetric flask, add sodium standard solution I or sodium standard solution II or the sodium standard solution III of potassium standard solution I or potassium standard solution II or potassium standard solution III, the different volumes number of different volumes number, calcium standard solution I or calcium standard solution II or calcium standard solution III, the silicon standard solution I of different volumes number or magnesium standard solution I or the magnesium standard solution II or the magnesium standard solution III of silicon standard solution II or silicon standard solution III and different volumes number of different volumes number, the content that makes potassium in each volumetric flask, sodium, calcium, silicon, magnesium is 0% ~ 200% of the sample potassium learnt, sodium, calcium, silicon, content of magnesium, is diluted with water to scale; Shake up, as working curve solution;
(4) mass concentration of analytical element potassium, sodium, calcium, silicon, magnesium in the measurement sample solution
Intensity with 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 surveying work curve solution successively; Horizontal ordinate is with the mass concentration of analytical element potassium, sodium, calcium, silicon, magnesium in the working curve solution; Ordinate is with the respective strengths of analytical element potassium, sodium, calcium, silicon, magnesium, the drawing curve;
Measure the intensity of element potassium, sodium, calcium, silicon, magnesium in the sample solution then, on the corresponding work curve, find the mass concentration of corresponding analysis element potassium, sodium, calcium, silicon, magnesium with the intensity of element potassium, sodium, calcium, silicon, magnesium in the sample solution;
(5) calculate measurement result, obtain the percentage composition of potassium in the sample, sodium, calcium, silicon, magnesium,
Be calculated as follows the mass percent w of element potassium, sodium, calcium, silicon, magnesium in the sample, numerical value is represented with %:
In the formula:
The mass concentration of ρ---analytical element in the test solution (potassium, sodium, calcium, silicon, magnesium), unit is every milliliter of microgram (μ g/mL);
V---test solution volume, unit are milliliter (mL);
M---test portion quality, unit is gram (g).
Low temperature described in the said method is meant that heated perimeter is at 50～200 ℃.
The condition of work and the analytical line of inductive coupling plasma emission spectrograph are following: 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 scheme of the present invention is:
1) the method detection limit is low is one of advantage of this patent.This method is through spectrum The Study of Interference and the development test of instrument detection limit, adopts claim kind and the modes of sample concentration more, can measure the content that content in the nickel oxide sample is low to moderate 0.0001% potassium, sodium, calcium, silicon, magnesium elements.
2) contaminated possibly be one of advantage of this patent for a short time.Potassium, sodium, calcium, silicon, magnesium elements all are elements that nature is rich in, and when analyzing trace potassium, sodium, calcium, silicon, magnesium elements, very easily receive the pollution that impurity element is introduced.The working curve of this method is the synthetic work curve of no matrix; Do not add matrix in the working curve solution; Avoided adding contaminating impurity in the matrix that matrix might bring into, adding reagent is top grade is pure, and the impurity element of having avoided reagent to import as far as possible pollutes.
3) the analytical approach measurement range is wide, and measurement lower limit is 0.0001%, is limited to 0.5% in the measurement.
4) this patented method is measured fast, and is easy and simple to handle, practiced thrift a large amount of man power and materials.
Embodiment
Embodiment one
Measure potassium, sodium, calcium, silicon, magnesium elements in high-purity nickel oxide, on following instrument, measure
Adopt JY ULTIMAIIC type inductive coupling plasma emission spectrograph, the following incident power 1050W of the condition of work of instrument and 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), employed reagent is following in the mensuration process:
(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 mixed in 1: 1 by volume;
(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 mixed in 1: 1 by volume;
(1.5), NaOH, more than top grade is pure;
(1.6), quality-volumetric concentration of sodium standard solution I is 0.10mg/mL, the preparation method accurately takes by weighing 0.1886g sodium chloride, its massfraction is not less than 99.95%; Place the 100mL beaker, be dissolved in water, move in the 1000mL volumetric flask; Be diluted with water to scale, shake up;
(1.7), quality-volumetric concentration of sodium standard solution II is 0.01mg/mL, the preparation method pipettes 20mL sodium standard solution I in the 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.8), quality-volumetric concentration of sodium standard solution III is 0.001mg/mL, the preparation method pipettes 20mL sodium standard solution II in the 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.9), quality-volumetric concentration of potassium standard solution I is 0.10mg/mL, the preparation method accurately takes by weighing 0.1907g potassium chloride, its massfraction is not less than 99.95%; Place the 100mL beaker, be dissolved in water, move in the 1000mL volumetric flask; Be diluted with water to scale, shake up;
(1.10), quality-volumetric concentration of potassium standard solution II is 0.01mg/mL, the preparation method pipettes 20mL potassium standard solution I in the 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.11), quality-volumetric concentration of potassium standard solution III is 0.001mg/mL, the preparation method pipettes 20mL potassium standard solution II in the 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.12), quality-volumetric concentration of calcium standard solution I is 0.10mg/mL, the preparation method is the lime carbonate that takes by weighing 0.1249g previously baked (at 110 ℃ of baking 2h) and in exsiccator, be cooled to room temperature, its massfraction is not less than 99.95%; Place the 100mL beaker, add 30mL hydrochloric acid II, low-temperature heat to dissolving fully; The cooling back moves in the 500mL volumetric flask; Add 20mL hydrochloric acid II, be diluted with water to scale, shake up.
(1.13), quality-volumetric concentration of calcium standard solution II is 0.01mg/mL, the preparation method pipettes 20.00mL calcium standard solution I in the 200mL volumetric flask, adds 20mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.14), quality-volumetric concentration of calcium standard solution III is 0.001mg/mL, the preparation method pipettes 20.00mL calcium standard solution II in the 200mL volumetric flask, adds 20mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.15), quality-volumetric concentration of silicon standard solution I is 0.10mg/mL, the preparation method takes by weighing 0.1000g through levigate monocrystalline silicon or polysilicon, its massfraction is not less than 99.95%; Place the 100mL polytetrafluoroethylene beaker, add 20g NaOH, 100mL water; Shake gently, put into boiling water bath, be heated to dissolving fully; The cooling back moves in the 1000mL plastics volumetric flask, is diluted with water to scale, shakes up.
(1.16), quality-volumetric concentration of silicon standard solution II is 0.01mg/mL, the preparation method pipettes 20.00mL silicon standard solution I in the 200mL volumetric flask, adds 20mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.17), quality-volumetric concentration of silicon standard solution III is 0.001mg/mL, the preparation method pipettes 20.00mL silicon standard solution II in the 200mL volumetric flask, adds 20mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.18), quality-volumetric concentration of magnesium standard solution I is 0.10mg/mL, the preparation method takes by weighing the pure magnesium of 0.1000g, its massfraction is not less than 99.95%; Place the 150mL beaker, add 20mL hydrochloric acid II, low-temperature heat to dissolving fully; The cooling back moves in the 1000mL volumetric flask; Add 80mL hydrochloric acid II, be diluted with water to scale, shake up.
(1.19), quality-volumetric concentration of magnesium standard solution II is 0.01mg/mL, the preparation method pipettes 20.00mL magnesium standard solution I in the 200mL volumetric flask, adds 20mL hydrochloric acid II, is diluted with water to scale, shakes up.
(1.20), quality-volumetric concentration of magnesium standard solution III is 0.001mg/mL, the preparation method pipettes 20.00mL magnesium standard solution II in the 200mL volumetric flask, adds 20mL hydrochloric acid II, is diluted with water to scale, shakes up.
(2), sample circuit sample preparation: the sample of analyzing usefulness carries out the sample circuit sample preparation according to the requirement of GB/T 20066;
(3), analytical procedure is following:
(3.1), test portion: take by weighing the 2.0g sample, be accurate to 0.0001g.
(3.2), preparation sample solution: the test portion of analytical procedure (3.1) is placed the 100mL beaker, add 15mL nitric acid II (1.4), low-temperature heat to reaction stops, and the cooling back moves into the 50mL volumetric flask, is diluted with water to scale, shakes up.
(3.3), preparation work curve solution
By two blank reagent solutions of analytical procedure (3.2) preparation; Move in the 50mL volumetric flask; According to the content range of potassium, sodium, calcium, silicon, magnesium in the sample, in second solution, add 2mL potassium standard solution II (1.10), 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), the content that makes potassium, sodium, calcium, silicon, magnesium in first working curve solution is 0 μ g/mL; The content of potassium, sodium, calcium, silicon, magnesium is 0.4 μ g/mL in second working curve solution; Be diluted with water to scale, shake up, as working curve solution;
(3.4), measure the mass concentration (μ g/mL) of potassium, sodium, calcium, silicon, magnesium in the test solution: on inductively coupled plasma atomic emission spectrometer; By selected condition of work; The intensity of analytical element potassium, sodium, calcium, silicon, magnesium in the surveying work curve solution successively; Horizontal ordinate is with the mass concentration (μ g/mL) of potassium, sodium, calcium, silicon, magnesium elements in the working curve solution, the ordinate intensity drawing curve with potassium, sodium, calcium, silicon, magnesium elements; Then; Measure the intensity of potassium, sodium, calcium, silicon, magnesium elements in the sample solution, on working curve, find the mass concentration (μ g/mL) of corresponding potassium, sodium, calcium, silicon, magnesium elements with the intensity of potassium, sodium, calcium, silicon, magnesium elements;
(4), be calculated as follows the massfraction w of analytical element (potassium, sodium, calcium, silicon, magnesium) element, numerical value is represented with %:
In the formula:
The mass concentration of ρ---analytical element in the test solution (potassium, sodium, calcium, silicon, magnesium), unit is every milliliter of microgram (μ g/mL);
V---test solution volume, unit are milliliter (mL);
M---test portion quality, unit is gram (g).
The content that obtains 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 the nickel oxide, on following instrument, measure
Adopt JY ULTIMAIIC type inductive coupling plasma emission spectrograph, the condition of work and the analytical line of instrument are following: 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), employed reagent is following in the mensuration process:
(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 mixed in 1: 1 by volume;
(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 mixed in 1: 1 by volume;
(1.5), NaOH, more than top grade is pure;
(1.6), quality-volumetric concentration of sodium standard solution I is 0.10mg/mL, the preparation method accurately takes by weighing 0.1886g sodium chloride, its massfraction is not less than 99.95%; Place the 100mL beaker, be dissolved in water, move in the 1000mL volumetric flask; Be diluted with water to scale, shake up;
(1.7), quality-volumetric concentration of sodium standard solution II is 0.01mg/mL, the preparation method pipettes 20mL sodium standard solution I in the 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.8), quality-volumetric concentration of sodium standard solution III is 0.001mg/mL, the preparation method pipettes 20mL sodium standard solution II in the 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.9), quality-volumetric concentration of potassium standard solution I is 0.10mg/mL, the preparation method accurately takes by weighing 0.1907g potassium chloride, its massfraction is not less than 99.95%; Place the 100mL beaker, be dissolved in water, move in the 1000mL volumetric flask; Be diluted with water to scale, shake up;
(1.10), quality-volumetric concentration of potassium standard solution II is 0.01mg/mL, the preparation method pipettes 20mL potassium standard solution I in the 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.11), quality-volumetric concentration of potassium standard solution III is 0.001mg/mL, the preparation method pipettes 20mL potassium standard solution II in the 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.12), quality-volumetric concentration of calcium standard solution I is 0.10mg/mL, the preparation method is the lime carbonate that takes by weighing 0.1249g previously baked (at 110 ℃ of baking 2h) and in exsiccator, be cooled to room temperature, its massfraction is not less than 99.95%; Place the 100mL beaker, add 40mL hydrochloric acid II, low-temperature heat to dissolving fully; The cooling back moves in the 500mL volumetric flask; Add 30mL hydrochloric acid II, be diluted with water to scale, shake up.
(1.13), quality-volumetric concentration of calcium standard solution II is 0.01mg/mL, the preparation method pipettes 20.00mL calcium standard solution I in the 200mL volumetric flask, adds 30mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.14), quality-volumetric concentration of calcium standard solution III is 0.001mg/mL, the preparation method pipettes 20.00mL calcium standard solution II in the 200mL volumetric flask, adds 30mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.15), quality-volumetric concentration of silicon standard solution I is 0.10mg/mL, the preparation method takes by weighing 0.1000g through levigate monocrystalline silicon or polysilicon, its massfraction is not less than 99.95%; Place the 100mL polytetrafluoroethylene beaker, add 30g NaOH, 100mL water; Shake gently, put into boiling water bath, be heated to dissolving fully; The cooling back moves in the 1000mL plastics volumetric flask, is diluted with water to scale, shakes up.
(1.16), quality-volumetric concentration of silicon standard solution II is 0.01mg/mL, the preparation method pipettes 20.00mL silicon standard solution I in the 200mL volumetric flask, adds 30mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.17), quality-volumetric concentration of silicon standard solution III is 0.001mg/mL, the preparation method pipettes 20.00mL silicon standard solution II in the 200mL volumetric flask, adds 30mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.18), quality-volumetric concentration of magnesium standard solution I is 0.10mg/mL, the preparation method takes by weighing the pure magnesium of 0.1000g, its massfraction is not less than 99.95%; Place the 150mL beaker, add 30mL hydrochloric acid II, low-temperature heat to dissolving fully; The cooling back moves in the 1000mL volumetric flask; Add 100mL hydrochloric acid II, be diluted with water to scale, shake up.
(1.19), quality-volumetric concentration of magnesium standard solution II is 0.01mg/mL, the preparation method pipettes 20.00mL magnesium standard solution I in the 200mL volumetric flask, adds 30mL hydrochloric acid II, is diluted with water to scale, shakes up.
(1.20), quality-volumetric concentration of magnesium standard solution III is 0.001mg/mL, the preparation method pipettes 20.00mL magnesium standard solution II in the 200mL volumetric flask, adds 30mL hydrochloric acid II, is diluted with water to scale, shakes up.
(2), sample circuit sample preparation: the sample of analyzing usefulness carries out the sample circuit sample preparation according to the requirement of GB/T 20066;
(3), analytical procedure is following:
(3.1), test portion: take by weighing the 0.1g sample, be accurate to 0.0001g.
(3.2), preparation sample solution: the test portion of analytical procedure (3.1) is placed the 100mL beaker, add 10mL nitric acid (1.4), low-temperature heat to reaction stops, and the cooling back moves into the 50mL volumetric flask, is diluted with water to scale, shakes up.
(3.3), preparation work curve solution
By two blank reagent solutions of analytical procedure (3.2) preparation; Move in the 50mL volumetric flask; According to the content range of potassium, sodium, calcium, silicon, magnesium in the sample, in second solution, add 5mL potassium standard solution I (1.9), 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), the content that makes potassium, sodium, calcium, silicon, magnesium in first working curve solution is 0 μ g/mL; The content of potassium, sodium, calcium, silicon, magnesium is 10.0 μ g/mL in second working curve solution; Be diluted with water to scale, shake up, as working curve solution;
(3.4), measure the mass concentration (μ g/mL) of potassium, sodium, calcium, silicon, magnesium in the test solution: on inductively coupled plasma atomic emission spectrometer; By selected condition of work; The intensity of analytical element potassium, sodium, calcium, silicon, magnesium in the surveying work curve solution successively; Horizontal ordinate is with the mass concentration (μ g/mL) of potassium, sodium, calcium, silicon, magnesium elements in the working curve solution, the ordinate intensity drawing curve with potassium, sodium, calcium, silicon, magnesium elements; Then; Measure the intensity of potassium, sodium, calcium, silicon, magnesium elements in the sample solution, on working curve, find the mass concentration (μ g/mL) of corresponding potassium, sodium, calcium, silicon, magnesium elements with the intensity of potassium, sodium, calcium, silicon, magnesium elements;
(4), be calculated as follows the massfraction w of analytical element (potassium, sodium, calcium, silicon, magnesium) element, numerical value is represented with %:
In the formula:
The mass concentration of ρ---analytical element in the test solution (potassium, sodium, calcium, silicon, magnesium), unit is every milliliter of microgram (μ g/mL);
V---test solution volume, unit are milliliter (mL);
M---test portion quality, unit is gram (g).
The content respectively that obtains 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 the nickel oxide, on following instrument, measure
Adopt JY ULTIMAIIC type inductive coupling plasma emission spectrograph, the condition of work and the analytical line of instrument are following: 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), employed reagent is following in the mensuration process:
(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 mixed in 1: 1 by volume;
(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 mixed in 1: 1 by volume;
(1.5), NaOH, more than top grade is pure;
(1.6), quality-volumetric concentration of sodium standard solution I is 0.10mg/mL, the preparation method accurately takes by weighing 0.1886g sodium chloride, its massfraction is not less than 99.95%; Place the 100mL beaker, be dissolved in water, move in the 1000mL volumetric flask; Be diluted with water to scale, shake up;
(1.7), quality-volumetric concentration of sodium standard solution II is 0.01mg/mL, the preparation method pipettes 20mL sodium standard solution I in the 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.8), quality-volumetric concentration of sodium standard solution III is 0.001mg/mL, the preparation method pipettes 20mL sodium standard solution II in the 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.9), quality-volumetric concentration of potassium standard solution I is 0.10mg/mL, the preparation method accurately takes by weighing 0.1907g potassium chloride, its massfraction is not less than 99.95%; Place the 100mL beaker, be dissolved in water, move in the 1000mL volumetric flask; Be diluted with water to scale, shake up;
(1.10), quality-volumetric concentration of potassium standard solution II is 0.01mg/mL, the preparation method pipettes 20mL potassium standard solution I in the 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.11), quality-volumetric concentration of potassium standard solution III is 0.001mg/mL, the preparation method pipettes 20mL potassium standard solution II in the 200mL volumetric flask, is diluted with water to scale, shakes up;
(1.12), quality-volumetric concentration of calcium standard solution I is 0.10mg/mL, the preparation method is the lime carbonate that takes by weighing 0.1249g previously baked (at 110 ℃ of baking 2h) and in exsiccator, be cooled to room temperature, its massfraction is not less than 99.95%; Place the 100mL beaker, add 20mL hydrochloric acid II, low-temperature heat to dissolving fully; The cooling back moves in the 500mL volumetric flask; Add 10mL hydrochloric acid II, be diluted with water to scale, shake up.
(1.13), quality-volumetric concentration of calcium standard solution II is 0.01mg/mL, the preparation method pipettes 20.00mL calcium standard solution I in the 200mL volumetric flask, adds 10mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.14), quality-volumetric concentration of calcium standard solution III is 0.001mg/mL, the preparation method pipettes 20.00mL calcium standard solution II in the 200mL volumetric flask, adds 10mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.15), quality-volumetric concentration of silicon standard solution I is 0.10mg/mL, the preparation method takes by weighing 0.1000g through levigate monocrystalline silicon or polysilicon, its massfraction is not less than 99.95%; Place the 100mL polytetrafluoroethylene beaker, add 10g NaOH, 100mL water; Shake gently, put into boiling water bath, be heated to dissolving fully; The cooling back moves in the 1000mL plastics volumetric flask, is diluted with water to scale, shakes up.
(1.16), quality-volumetric concentration of silicon standard solution II is 0.01mg/mL, the preparation method pipettes 20.00mL silicon standard solution I in the 200mL volumetric flask, adds 10mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.17), quality-volumetric concentration of silicon standard solution III is 0.001mg/mL, the preparation method pipettes 20.00mL silicon standard solution II in the 200mL volumetric flask, adds 10mL hydrochloric acid I, is diluted with water to scale, shakes up.
(1.18), quality-volumetric concentration of magnesium standard solution I is 0.10mg/mL, the preparation method takes by weighing the pure magnesium of 0.1000g, its massfraction is not less than 99.95%; Place the 150mL beaker, add 10mL hydrochloric acid II, low-temperature heat to dissolving fully; The cooling back moves in the 1000mL volumetric flask; Add 60mL hydrochloric acid II, be diluted with water to scale, shake up.
(1.19), quality-volumetric concentration of magnesium standard solution II is 0.01mg/mL, the preparation method pipettes 20.00mL magnesium standard solution I in the 200mL volumetric flask, adds 10mL hydrochloric acid II, is diluted with water to scale, shakes up.
(1.20), quality-volumetric concentration of magnesium standard solution III is 0.001mg/mL, the preparation method pipettes 20.00mL magnesium standard solution II in the 200mL volumetric flask, adds 10mL hydrochloric acid II, is diluted with water to scale, shakes up.
(2), sample circuit sample preparation: the sample of analyzing usefulness carries out the sample circuit sample preparation according to the requirement of GB/T 20066;
(3), analytical procedure is following:
(3.1), test portion: take by weighing the 0.5g sample, be accurate to 0.0001g.
(3.2), preparation sample solution: the test portion of analytical procedure (3.1) is placed the 100mL beaker, add 20mL nitric acid (1.4), low-temperature heat to reaction stops, and the cooling back moves into the 50mL volumetric flask, is diluted with water to scale, shakes up.
(3.3), preparation work curve solution
By three blank reagent solutions of analytical procedure (3.2) preparation; Move in the 50mL volumetric flask; Content range according to potassium, sodium, calcium, silicon, magnesium in the sample; In second solution, add 5mL potassium standard solution III (1.11), 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 the content of potassium, sodium, calcium, silicon, magnesium in first working curve solution be 0 μ g/mL, the content of potassium, sodium, calcium, silicon, magnesium is 0.1 μ g/mL in second working curve solution; The content of potassium, sodium, calcium, silicon, magnesium is 1.0 μ g/mL in the 3rd working curve solution; Be diluted with water to scale, shake up, as working curve solution;
(3.4), measure the mass concentration (μ g/mL) of potassium, sodium, calcium, silicon, magnesium in the test solution: on inductively coupled plasma atomic emission spectrometer; By selected condition of work; The intensity of analytical element potassium, sodium, calcium, silicon, magnesium in the surveying work curve solution successively; Horizontal ordinate is with the mass concentration (μ g/mL) of potassium, sodium, calcium, silicon, magnesium elements in the working curve solution, the ordinate intensity drawing curve with potassium, sodium, calcium, silicon, magnesium elements; Then; Measure the intensity of potassium, sodium, calcium, silicon, magnesium elements in the sample solution, on working curve, find the mass concentration (μ g/mL) of corresponding potassium, sodium, calcium, silicon, magnesium elements with the intensity of potassium, sodium, calcium, silicon, magnesium elements;
(4), be calculated as follows the massfraction w of analytical element (potassium, sodium, calcium, silicon, magnesium) element, numerical value is represented with %:
In the formula:
The mass concentration of ρ---analytical element in the test solution (potassium, sodium, calcium, silicon, magnesium), unit is every milliliter of microgram (μ g/mL);
V---test solution volume, unit are milliliter (mL);
M---test portion quality, unit is gram (g).
The content that obtains 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: the analytical approach measurement range is wide, and measurement lower limit is 0.0001%, is limited to 0.5% in the measurement, and this method is measured fast, and is easy and simple to handle, practiced thrift a large amount of man power and materials.
Claims (2)
1. method of measuring potassium in the nickel oxide, sodium, calcium, silicon, magnesium element content, it is characterized in that: the reagent that this method is used in the 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 mixed in 1: 1 by volume;
Nitric acid I, density is 1.42g/mL, more than top grade is pure;
Nitric acid II, 1+1, nitric acid I and water mixed in 1: 1 by volume;
NaOH is more than top grade is pure;
Sodium standard solution I, quality-volumetric concentration be 0.10mg/mL, the preparation method accurately takes by weighing 0.1886g sodium chloride; Its massfraction is not less than 99.95%, places the 100mL beaker, is dissolved in water; Move in the 1000mL volumetric flask, be diluted with water to scale, shake up;
Sodium standard solution II, quality-volumetric concentration is 0.01mg/mL, the preparation method pipettes 20mL sodium standard solution I in the 200mL volumetric flask, is diluted with water to scale, shakes up;
Sodium standard solution III, quality-volumetric concentration is 0.001mg/mL, the preparation method pipettes 20mL sodium standard solution II in the 200mL volumetric flask, is diluted with water to scale, shakes up;
Potassium standard solution I, quality-volumetric concentration is 0.10mg/mL, and the preparation method accurately takes by weighing 0.1907g potassium chloride, and its massfraction is not less than 99.95%, places the 100mL beaker, is dissolved in water, and moves in the 1000mL volumetric flask, is diluted with water to scale, shakes up;
Potassium standard solution II, quality-volumetric concentration is 0.01mg/mL, the preparation method pipettes 20mL potassium standard solution I in the 200mL volumetric flask, is diluted with water to scale, shakes up;
Potassium standard solution III, quality-volumetric concentration is 0.001mg/mL, the preparation method pipettes 20mL potassium standard solution II in the 200mL volumetric flask, is diluted with water to scale, shakes up;
Calcium standard solution I, quality-volumetric concentration is 0.10mg/mL, the preparation method is that to take by weighing 0.1249g previously baked (100 ℃～110 ℃ bakings 1～2h) and in exsiccator, be cooled to the lime carbonate of room temperature; Its massfraction is not less than 99.95%, places the 100mL beaker, adds 10～40mL hydrochloric acid II; Low-temperature heat to dissolving moves in the 500mL volumetric flask after the cooling fully, 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, the preparation method pipettes 20.00mL calcium standard solution I in the 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, the preparation method pipettes 20.00mL calcium standard solution II in the 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 the preparation method takes by weighing 0.1000g through levigate monocrystalline silicon or polysilicon, and its massfraction is not less than 99.95%; Place the 100mL polytetrafluoroethylene beaker, add 10～30g NaOH, 50～150mL water; Shake gently, put into boiling water bath, be heated to dissolving fully; The cooling back moves in the 1000mL plastics volumetric flask, is diluted with water to scale, shakes up.
Silicon standard solution II, quality-volumetric concentration is 0.01mg/mL, the preparation method pipettes 20.00mL silicon standard solution I in the 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, the preparation method pipettes 20.00mL silicon standard solution II in the 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, the preparation method takes by weighing the pure magnesium of 0.1000g; Its massfraction is not less than 99.95%, places the 150mL beaker to add 10～30mL hydrochloric acid II, and low-temperature heat to dissolving fully; The cooling back moves in the 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, the preparation method pipettes 20.00mL magnesium standard solution I in the 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, the preparation method pipettes 20.00mL magnesium standard solution II in the 200mL volumetric flask, adds 10～30mL hydrochloric acid II, is diluted with water to scale, shakes up.
The step of the mensuration process of this method is:
⑴ sample carries out the sample circuit sample preparation according to the requirement of GB/T 20066, takes by weighing 0.1 ~ 2.0g sample, is accurate to 0.0001g;
⑵ prepare sample solution
Sample is placed the 100mL beaker, add 10 ~ 30mL nitric acid II, low-temperature heat to dissolving is cooled off the back and is moved into the 50mL volumetric flask fully, is diluted with water to scale, shakes up;
⑶ preparation work curve solution:
In 2 ~ 8 100mL beakers; Add and step ⑵ same amount nitric acid II; Low-temperature heat to dissolving fully; The cooling back moves into several corresponding 50mL volumetric flasks; Content range according to potassium, sodium, calcium, silicon, magnesium in the sample of learning in advance; In each volumetric flask, add sodium standard solution I or sodium standard solution II or the sodium standard solution III of potassium standard solution I or potassium standard solution II or potassium standard solution III, the different volumes number of different volumes number, calcium standard solution I or calcium standard solution II or calcium standard solution III, the silicon standard solution I of different volumes number or magnesium standard solution I or the magnesium standard solution II or the magnesium standard solution III of silicon standard solution II or silicon standard solution III and different volumes number of different volumes number, the content that makes potassium in each volumetric flask, sodium, calcium, silicon, magnesium is 0% ~ 200% of the sample potassium learnt, sodium, calcium, silicon, content of magnesium, is diluted with water to scale; Shake up, as working curve solution;
(4) mass concentration of analytical element potassium, sodium, calcium, silicon, magnesium in the measurement sample solution
Intensity with 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 surveying work curve solution successively; Horizontal ordinate is with the mass concentration of analytical element potassium, sodium, calcium, silicon, magnesium in the working curve solution; Ordinate is with the respective strengths of analytical element potassium, sodium, calcium, silicon, magnesium, the drawing curve;
Measure the intensity of element potassium, sodium, calcium, silicon, magnesium in the sample solution then, on the corresponding work curve, find the mass concentration of corresponding analysis element potassium, sodium, calcium, silicon, magnesium with the intensity of element potassium, sodium, calcium, silicon, magnesium in the sample solution;
(5) calculate measurement result, obtain the percentage composition of potassium in the sample, sodium, calcium, silicon, magnesium,
Be calculated as follows the mass percent w of element potassium, sodium, calcium, silicon, magnesium in the sample, numerical value is represented with %:
In the 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 are milliliter mL;
M---test portion quality, unit is gram g;
Low temperature described in the said method is meant that heated perimeter is at 50～200 ℃.
2. the method for potassium, sodium, calcium, silicon, content of magnesium in the mensuration nickel oxide according to claim 1 is characterized in that: the condition of work and the analytical line of inductive coupling plasma emission spectrograph are following: 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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