CN102928364B - Method for measuring trace impurity elements of sodium, magnesium, calcium, iron and lead in high-purity boric acid - Google Patents
Method for measuring trace impurity elements of sodium, magnesium, calcium, iron and lead in high-purity boric acid Download PDFInfo
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Abstract
The invention discloses a method for measuring trace impurity elements of sodium, magnesium, calcium, iron and lead in high-purity boric acid, which comprises the specific processes of heating hydrofluoric acid and hydrochloric acid to remove boron, extracting soluble salts from aqua regia, fixing the volume of ultrapure water, and measuring by an atomic absorption spectrometer and an inductively coupled plasma emission spectrometer, so that the quantitative enrichment and the analytical measurement of the trace impurity elements in a high-purity boric acid sample are realized; the method removes boron by hydrofluoric acid, has less reagent dosage and low sample blank, removes a boric acid matrix to be beneficial to on-machine analysis of the sample, can realize simultaneous determination of single/multiple elements by using an atomic spectrum comprising an atomic absorption spectrometer and an inductively coupled plasma emission spectrometer, is suitable for the analysis and determination of trace impurity elements in the high-purity boric acid sample, has the advantages of low detection limit, high sensitivity, wide linear range and the like, and has the average processing time of a single high-purity boric acid sample of not more than 2 hours.
Description
Technical field
The present invention relates to the analysis determining technology of trace impurity sodium in high-purity boracic acid, magnesium, calcium, iron, lead, by hydrofluoric acid dissolution, heat evaporate to dryness and remove boric acid matrix, with chloroazotic acid, extract soluble salts, after ultrapure water constant volume, with atomic absorption spectrometry constituent content to be measured.
Background technology
Boric acid is of many uses, can be used for the every profession and trades such as glass, enamel, pottery, metallurgy, chemical industry.In glass (optical glass, acid-resistant glass, pyroceram, insulating material glass fibre) manufacture process, add boric acid, can improve heat-resisting, the properties of transparency of glassware, improve physical strength, shorten the melting time.At enamel, ceramics mesoboric acid, in order to improve gloss and the fastness of goods, be also one of composition of glaze and pigment simultaneously.In metallurgy industry, be used as adjuvant, the cosolvent produced in boron steel, so that boron steel has high rigidity and the good ductility of rolling, can prevent the surface oxidation of metal solder, brazing, cover weldering.In chemical industry, for the production of various borate families, as sodium borohydride, ammonium hydrogen borate, potassium borohydride etc., also can be used as analytical chemistry reagent with preparation buffer solution.
In GB/T 628-2011 < < chemical reagent boric acid > >, for calcium, iron, plumbous each element, limit the quantity of and all have requirement, see the following form:
And have corresponding recommendation method of testing, but each method pre-treatment step is not quite similar, and cannot realize multielement simultaneous determination, and treatment step is comparatively loaded down with trivial details, and in process, needs to use a large amount of organic reagent methyl alcohol.
Therefore, develop a kind of accurately, technology efficient and that be applicable to trace amounts of sodium in high-purity boracic acid, magnesium, calcium, iron, plumbous analytical test work become a current analytical work person difficult problem in the urgent need to address.
Summary of the invention
The object of the invention is to develop a kind of for measuring the analytical approach of high-purity boracic acid trace impurity sodium, magnesium, calcium, iron, lead, by hydrofluorite, remove boron, chloroazotic acid extraction, atomic absorption spectrum and inductively coupled plasma spectrometry and measure, to realize the Accurate Determining to trace impurity in high-purity boracic acid.
The present invention has realized above-mentioned purpose, and concrete technology is as follows:
The assay method of trace impurity sodium, magnesium, calcium, iron, lead in high-purity boracic acid, is characterized in that determination step is as follows:
First, high-purity boracic acid sample to be measured is added in polytetrafluoroethylene (PTFE) crucible;
Second step adds hydrofluorite (HF) and hydrochloric acid (HCl) in teflon crucible, and the hydrofluorite adding (HF) is 2:1 with the volume ratio of hydrochloric acid (HCl);
The 3rd step, carries out evaporate to dryness for the first time by teflon crucible;
The 4th step, the hydrofluorite (HF) toward adding in the teflon crucible of the 3rd step evaporate to dryness with hydrochloric acid same volume, carries out evaporate to dryness for the second time, removes boric acid matrix as far as possible;
The 5th step, toward be incorporated in the teflon crucible of the 4th step evaporate to dryness hydrochloric acid same volume chloroazotic acid (1+1) (volume ratio that is chloroazotic acid and water is 1:1), with the ultrapure water of hydrofluorite same volume, then be heated to boiling, boil after 5min and take off and treat that nature is cooling;
The 6th step, is settled to 25ml color-comparison tube by the material in the cooled teflon crucible of the 5th step with ultrapure water, shakes up to be measured;
The 7th step, the material to be measured that utilizes Atomic Absorption Spectrometer (AAS), inductively-coupled plasma spectrometer (ICP-OES) to obtain the 6th step is measured.
Before described teflon crucible and 25 mL color-comparison tubes are used, by volume ratio, be that 5% nitric acid soaks to put and spends the night, then with ultrapure water, wash.
The purity of described hydrofluorite and hydrochloric acid is electron level (Metal-oxide-semiconductor, MOS level).
Described ultrapure water meets three grades of water requirements in the specification of GB6682-92 < < Experiment of Analytical Chemistry chamber water and test method > >.
Described evaporate to dryness for the first time, evaporate to dryness, heating are for the second time all that teflon crucible is operated on control-temperature electric heating plate.
The instrument condition of work that described the 7th pacing is selected is surely as follows:
Instrument: MK II-M6 type Atomic Absorption Spectrometer, sodium hollow cathode lamp;
Atomic Absorption Spectrometer condition of work: automatic peak-seeking pattern, acetylene flow 1.1 L/min; Air mass flow 1.2 L/min; Lamp current 3 mA;
Instrument: PE 5300V type inductive coupling plasma emission spectrograph;
Inductive coupling plasma emission spectrograph condition of work: RF power 1300 W; Cold gas 15.0 L/min; Atomization gas flow 0.8 L/min; Assisted gas flow 0.2 L/min; Sample introduction flow velocity: 1.5 mL/min; Irrigation flow rate: 2.5 mL/min; Analytical line: Mg 285.213 nm, Ca 317.933 nm, Fe 238.204 nm, Pb 220.353 nm.
Fixed standard reserving solution and the standard operation solution used of described the 7th pacing is:
The sodium oxide molybdena standard reserving solution of 1.00 mg/mL, the magnesium oxide standard reserving solution of 1.00 mg/mL, the calcium oxide standard reserving solution of 1.00 mg/mL, the di-iron trioxide standard reserving solution of 1.00 mg/mL, the plumbous standard reserving solution of 1.00 mg/mL;
The complex element standard reserving solution that is obtained 100.00 μ g/mL by magnesium oxide standard reserving solution, calcium oxide standard reserving solution, di-iron trioxide standard reserving solution, plumbous standard reserving solution combination dilution preparation, its medium is nitric acid (5+95) (volume ratio that is red fuming nitric acid (RFNA) and water is 5:95);
By the preparation of complex element standard reserving solution stepwise dilution, obtain the complex element standard operation solution that concentration is respectively 1.00,2.00,5.00,10.00 μ g/mL, its medium is nitric acid (5+95) (volume ratio that is red fuming nitric acid (RFNA) and water is 5:95);
By the preparation of sodium oxide molybdena standard reserving solution stepwise dilution, obtain the sodium oxide molybdena standard operation solution that concentration is respectively 0.50,1.00,1.50,2.00,2.50 μ g/mL, WATER AS FLOW MEDIUM.
The measurement operation of described the 7th step is as follows:
Atomic Absorption Spectrometer is first then lighted a fire sodium hollow cathode lamp preheating 15 ~ 30 min before using, sequentially determining standard sequence and sample solution after absorbance is stable, and sample solution measurement result is sample analysis result after deducting reagent blank;
ICP-OES presses the condition of work of setting and selected analytical line, sequentially determining standard sequence and sample solution, and sample solution measurement result is sample analysis result after deducting reagent blank.
Advantage of the present invention is as follows:
1. use hydrofluorite to replace methyl alcohol except boron, can greatly reduce reagent dosage, reduce reagent blank, save experimental period, also can avoid the impact of methyl alcohol volatilization on operating personnel in experimentation simultaneously;
2. remove boric acid matrix to reduce sample solution viscosity, eliminate the matrix difference between sample solution and standard operation solution, reduce the impact on instrument sampling system simultaneously;
3. Atomic Absorption Spectrometer and inductive coupling plasma emission spectrograph are as ripe inorganic analysis instrument, be widely used in the fields such as geological and mineral, petrochemical complex, environmental monitoring, there is antijamming capability strong, highly sensitive, the plurality of advantages such as the range of linearity is wide.When using inductive coupling plasma emission spectrograph can realize magnesium, calcium, iron, lead in the present invention, measure, use the Atomic Absorption Spectrometer can Accurate Determining sodium, each element method detection limit all, lower than GB/T 628-2011 < < chemical reagent boric acid > > requirement, meets daily need of production;
4. simplified operational procedure of the present invention, reagent consumption is few, and analysis speed is fast, and the single-piece sample average processing time is no more than 2 hours.
Accompanying drawing explanation
Fig. 1 is experiment flow schematic diagram of the present invention
Embodiment
As shown in Figure 1, the assay method of trace impurity sodium, magnesium, calcium, iron, lead in high-purity boracic acid provided by the invention, its step is as follows:
Accurately take 5.000 g high-purity boracic acid sample to be measured, pour in polytetrafluoroethylene (PTFE) crucible, add 10 mL hydrofluorite (HF) and 5 mL hydrochloric acid (HCl), evaporate to dryness on 200 ℃ of control-temperature electric heating plates;
Add 5 mL HF again evaporate to dryness can measure to the greatest extent, remove boric acid matrix;
In polytetrafluoroethylene (PTFE) crucible, add 1:1(v/v) newly join chloroazotic acid 5 mL, ultrapure water 10 mL, on electric hot plate, be heated to boil, after 5 min, take off, after naturally cooling, with ultrapure water, be settled to 25 mL color-comparison tubes, shake up to be measured;
Selected instrument condition of work is as follows:
Instrument: MK II-M6 type Atomic Absorption Spectrometer (can adopt flame atomic absorption spectrophotometer FAAS), sodium hollow cathode lamp
Atomic Absorption Spectrometer (AAS) condition of work: automatic peak-seeking pattern, acetylene flow 1.1 L/min; Air mass flow 1.2 L/min; Lamp current 3 mA;
Instrument: PE 5300V type inductive coupling plasma emission spectrograph
Inductive coupling plasma emission spectrograph (ICP-OES) condition of work: RF power 1300 W; Cold gas 15.0 L/min; Atomization gas flow 0.8 L/min; Assisted gas flow 0.2 L/min; Sample introduction flow velocity: 1.5 mL/min; Irrigation flow rate: 2.5 mL/min; Analytical line: Mg 285.213 nm, Ca 317.933 nm, Fe 238.204 nm, Pb 220.353 nm.
The preparation of standard series:
Sodium oxide molybdena standard reserving solution ρ (Na
2o)=1.00 mg/mL take 1.8859 g through the high pure sodium chloride of 500 ~ 600 ℃ of calcination 2 h, are placed in 250 mL beakers, and water dissolves, and move in 1000 mL volumetric flasks, are diluted with water to scale, shake up.
Magnesium oxide standard reserving solution ρ (MgO)=1.00 mg/mL takes rapidly 0.5000 g in the high-purity magnesium oxide (MgO) of 800 ℃ of calcinations, be placed in 250 mL beakers, add 25 mL water, add 20 mL(1+1) HCl, stirring and dissolving, in cooling rear immigration 1000 mL volumetric flasks, be diluted with water to scale, shake up.
Calcium oxide standard reserving solution ρ (CaO)=1.00 mg/mL takes 0.8924 g through 120 ℃ of high-purity calcium carbonates (CaCO3) of drying 2 h, be placed in 400 mL beakers, add 10 mL water, after adding a cover surface plate, along cup, be slow of speech and add slowly 30 mL(1+1) HCl, boils 2 min after dissolving, take off, water rinses surface plate and walls of beaker, is cooled to room temperature, moves in 1000 mL volumetric flasks, be diluted with water to scale, shake up.
Di-iron trioxide standard reserving solution ρ (Fe
2o
3)=1.00 mg/mL takes 1.000 g spectroscopic pure di-iron trioxide (Fe
2o
3), be placed in 250 mL beakers, add 20 mL HCl, low-temperature heat is dissolved.In cooling rear immigration 1000 mL volumetric flasks, add 30 mL HCl, be diluted with water to scale, shake up.
Plumbous standard reserving solution ρ (Pb)=1.00 mg/mL takes 1.000 g high purity leads and [uses in advance (1+9) HNO
3clean surface, then distinguish water and absolute ethanol washing, air-dry rear standby], be placed in 250 mL beakers, add 10 mL HNO
3, cover surface plate.After heating for dissolving is complete, move in 1000 mL volumetric flasks, be diluted with water to scale, shake up.
Complex element standard reserving solution ρ (B)=100.00 μ g/mL, by magnesium oxide, calcium oxide, di-iron trioxide, plumbous standard reserving solution combination dilution preparation, medium nitric acid (5+95).
Complex element standard operation solution ρ (B)=1.00,2.00,5.00,10.00 μ g/mL, prepared by complex element standard reserving solution stepwise dilution, medium nitric acid (5+95).
Sodium oxide molybdena standard operation solution ρ (Na
2o)=0.50,1.00,1.50,2.00,2.50 μ g/mL, are prepared WATER AS FLOW MEDIUM by sodium oxide molybdena standard reserving solution stepwise dilution.
AAS first then lights a fire sodium hollow cathode lamp preheating 15 ~ 30 min before using, sequentially determining standard sequence and sample solution after absorbance is stable, and sample solution measurement result is sample analysis result after deducting reagent blank.
ICP-OES presses the condition of work of setting and selected analytical line, sequentially determining standard sequence and sample solution, and sample solution measurement result is sample analysis result after deducting reagent blank.
Use the present invention as follows to the process of Chengdu research institute high-purity boracic acid product sampling analysis:
With reference to impurity estimation content in production procedure sample to be measured, determine sampling amount, with electronic balance, accurately take 2.000 ~ 5.000 g samples, pour in PTFE crucible, add 15 mL HF HCl(2:1, v/v), evaporate to dryness on 200 ℃ of control-temperature electric heating plates, add 5 mL HF evaporate to dryness again, newly joining chloroazotic acid 5 mL, ultrapure water 10 mL boil extraction, are settled to 25 mL color-comparison tubes after cooling, shake up to be measured.
Use AAS and ICP-OES by predefined condition of work, sequentially determining standard sequence and sample solution, acquired results deducts reagent blank and is sample measured result.This batch sample analysis result is as follows: Ca 20.0 ~ 25.8 μ g/g, Mg 1.59 ~ 58.4 μ g/g, Fe 1.87 ~ 5.77 μ g/g, Na 6.93 ~ 360 μ g/g, Pb<1.00 μ g/g.
Claims (7)
1. trace impurity sodium in high-purity boracic acid, magnesium, calcium, iron, plumbous assay method, is characterized in that determination step is as follows:
First, high-purity boracic acid sample to be measured is put into teflon crucible;
Second step adds hydrofluorite and hydrochloric acid in teflon crucible, and the hydrofluorite adding and the volume ratio of hydrochloric acid are 2:1;
The 3rd step, carries out evaporate to dryness for the first time by teflon crucible;
The 4th step, the hydrofluorite toward adding in the teflon crucible of the 3rd step evaporate to dryness with hydrochloric acid same volume, carries out evaporate to dryness for the second time, removes boric acid matrix as far as possible;
The 5th step, toward be incorporated in the teflon crucible of the 4th step evaporate to dryness hydrochloric acid same volume chloroazotic acid (1+1), with the ultrapure water of hydrofluorite same volume, be then heated to boiling, boil after 5min and take off and treat that nature is cooling;
The 6th step, is settled to 25ml color-comparison tube by the material in the cooled teflon crucible of the 5th step with ultrapure water, shakes up to be measured;
The 7th step, the material to be measured that utilizes Atomic Absorption Spectrometer, inductively-coupled plasma spectrometer to obtain the 6th step is measured.
2. assay method according to claim 1, is characterized in that: before described teflon crucible and 25 mL color-comparison tubes are used, by volume ratio, be that 5% nitric acid soaks to put and spends the night, then with ultrapure water, wash.
3. assay method according to claim 1, is characterized in that: the purity of described hydrofluorite and hydrochloric acid is electron level.
4. assay method according to claim 1, is characterized in that: described evaporate to dryness for the first time, evaporate to dryness, heating are for the second time all that teflon crucible is operated on control-temperature electric heating plate.
5. assay method according to claim 1, is characterized in that: the instrument condition of work that the mensuration of described the 7th step is selected is as follows:
Instrument: MK II-M6 type Atomic Absorption Spectrometer, sodium hollow cathode lamp; Atomic Absorption Spectrometer condition of work: automatic peak-seeking pattern, acetylene flow 1.1 L/min; Air mass flow 1.2 L/min; Lamp current 3 mA;
Instrument: PE 5300V type inductive coupling plasma emission spectrograph; Inductive coupling plasma emission spectrograph condition of work: RF power 1300 W; Cold gas 15.0 L/min; Atomization gas flow 0.8 L/min; Assisted gas flow 0.2 L/min; Sample introduction flow velocity: 1.5 mL/min; Irrigation flow rate: 2.5 mL/min; Analytical line: Mg 285.213 nm, Ca 317.933 nm, Fe 238.204 nm, Pb 220.353 nm.
6. assay method according to claim 5, is characterized in that: fixed standard reserving solution and the standard operation solution used of described the 7th pacing is:
The sodium oxide molybdena standard reserving solution of 1.00 mg/mL, the magnesium oxide standard reserving solution of 1.00 mg/mL, the calcium oxide standard reserving solution of 1.00 mg/mL, the di-iron trioxide standard reserving solution of 1.00 mg/mL, the plumbous standard reserving solution of 1.00 mg/mL;
The complex element standard reserving solution that is obtained 100.00 μ g/mL by magnesium oxide standard reserving solution, calcium oxide standard reserving solution, di-iron trioxide standard reserving solution, plumbous standard reserving solution combination dilution preparation, its medium is nitric acid (5+95);
By the preparation of complex element standard reserving solution stepwise dilution, obtain the complex element standard operation solution that concentration is respectively 1.00,2.00,5.00,10.00 μ g/mL, its medium is nitric acid (5+95);
By the preparation of sodium oxide molybdena standard reserving solution stepwise dilution, obtain the sodium oxide molybdena standard operation solution that concentration is respectively 0.50,1.00,1.50,2.00,2.50 μ g/mL, WATER AS FLOW MEDIUM.
7. according to the assay method described in claim 5 or 6, it is characterized in that: the measurement operation of described the 7th step is as follows:
Atomic Absorption Spectrometer is first then lighted a fire sodium hollow cathode lamp preheating 15 ~ 30 min before using, sequentially determining standard sequence and sample solution after absorbance is stable, and sample solution measurement result is sample analysis result after deducting reagent blank;
ICP-OES presses the condition of work of setting and selected analytical line, sequentially determining standard sequence and sample solution, and sample solution measurement result is sample analysis result after deducting reagent blank.
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| CN114993802B (en) * | 2022-06-14 | 2024-03-22 | 大晟芯材料科技(山东)有限公司 | Method for testing content of organic impurities in electronic-grade hydrofluoric acid |
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