CN102928364A - 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
- Publication number
- CN102928364A CN102928364A CN2012104124080A CN201210412408A CN102928364A CN 102928364 A CN102928364 A CN 102928364A CN 2012104124080 A CN2012104124080 A CN 2012104124080A CN 201210412408 A CN201210412408 A CN 201210412408A CN 102928364 A CN102928364 A CN 102928364A
- Authority
- CN
- China
- Prior art keywords
- solution
- sample
- standard reserving
- reserving solution
- acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
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 the high-purity boracic acid, magnesium, calcium, iron, lead, remove the boric acid matrix by hydrofluoric acid dissolution heating evaporate to dryness, extract soluble salts with chloroazotic acid, behind the 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.In enamel, gloss and the fastness of ceramics mesoboric acid in order to improve goods, also be one of composition of glaze and pigment simultaneously.In metallurgy industry, be used as adjuvant, the cosolvent produced in the 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, such as sodium borohydride, ammonium hydrogen borate, potassium borohydride etc., also can be used as analytical chemistry reagent with preparation buffer solution.
Limit the quantity of requirement is all arranged for calcium, iron, plumbous each element among the GB/T 628-2011 " chemical reagent boric acid ", see the following form:
| Title | Analyze pure | Chemical pure |
| Calcium (Ca), w/% | ≤0.002 | ≤0.01 |
| Iron (Fe), w/% | ≤0.000 5 | ≤0.002 |
| Plumbous (Pb), w/% | ≤0.001 | ≤0.003 |
And corresponding recommendation method of testing is arranged, but each method pre-treatment step is not quite similar, and can't realize that to multielement simultaneous determination treatment step is comparatively loaded down with trivial details, and need to use a large amount of organic reagent methyl alcohol in the process.
Therefore, exploitation technology a kind of accurately, efficient and that be applicable to trace amounts of sodium in the high-purity boracic acid, magnesium, calcium, iron, plumbous analytical test work has 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 analytical approach for measuring high-purity boracic acid trace impurity sodium, magnesium, calcium, iron, lead, measure except boron, chloroazotic acid extraction, atomic absorption spectrum and inductively coupled plasma spectrometry by hydrofluorite, to realize the Accurate Determining to trace impurity in the high-purity boracic acid.
The present invention has realized above-mentioned purpose, and concrete technology is as follows:
The assay method of sodium, magnesium, calcium, iron, lead in the high-purity boracic acid is characterized in that determination step is as follows:
At first, with in the high-purity boracic acid sample polytetrafluoroethylene (PTFE) crucible to be measured;
Second step adds hydrofluorite (HF) and hydrochloric acid (HCl) in the teflon crucible, the hydrofluorite of adding (HF) is 2:1 with the volume ratio of hydrochloric acid (HCl);
In the 3rd step, the teflon crucible is carried out the evaporate to dryness first time;
The 4th step added and the hydrofluorite (HF) of hydrochloric acid with volume in the teflon crucible of the 3rd step evaporate to dryness, carried out the evaporate to dryness second time, removed the boric acid matrix as far as possible;
The 5th step, be incorporated in the teflon crucible of the 4th step evaporate to dryness hydrochloric acid with the chloroazotic acid (1+1) (volume ratio that is chloroazotic acid and water is 1:1) of volume, with the ultrapure water of hydrofluorite with volume, then be heated to boiling, boil to take off behind the 5min and treat the nature cooling;
The 6th step was settled to the 25ml color-comparison tube with the material in the cooled teflon crucible of the 5th step with ultrapure water, shook up to be measured;
In the 7th step, the material to be measured that utilizes Atomic Absorption Spectrometer (AAS), inductively-coupled plasma spectrometer (ICP-OES) that the 6th step was obtained is measured.
Be that 5% nitric acid soaks to put and spends the night with volume ratio before described teflon crucible and 25 mL color-comparison tubes use, then wash with ultrapure water.
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 among the GB6682-92 " specification and the test method of Experiment of Analytical Chemistry chamber water ".
Described first time, evaporate to dryness, for the second time evaporate to dryness, heating all were that the teflon crucible is operated on the control-temperature electric heating plate.
The instrument condition of work that described the 7th pacing is selected surely 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.
Fixed used standard reserving solution and the standard operation solution of described the 7th pacing is:
1.00 the sodium oxide molybdena standard reserving solution of 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;
Prepare the complex element standard reserving solution that obtains 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, its medium is nitric acid (5+95) (volume ratio that is red fuming nitric acid (RFNA) and water is 5:95);
Obtain the complex element standard operation solution that concentration is respectively 1.00,2.00,5.00,10.00 μ g/mL by the preparation of complex element standard reserving solution stepwise dilution, its medium is nitric acid (5+95) (volume ratio that is red fuming nitric acid (RFNA) and water is 5:95);
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 by the preparation of sodium oxide molybdena standard reserving solution stepwise dilution.
The measurement operation in described the 7th step is as follows:
Atomic Absorption Spectrometer is then lighted a fire sodium hollow cathode lamp preheating 15 ~ 30 min first before using, sequentially determining standard sequence and sample solution after absorbance is stable, and the sample solution measurement result is the sample analysis result after deducting reagent blank;
ICP-OES reaches selected analytical line by the condition of work of setting, sequentially determining standard sequence and sample solution, and the sample solution measurement result is the 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 in the experimentation methyl alcohol volatilization on operating personnel's impact simultaneously;
2. remove the boric acid matrix to reduce sample solution viscosity, eliminate the matrix difference between sample solution and standard operation solution, reduce simultaneously the impact on the instrument sampling system;
3. Atomic Absorption Spectrometer and inductive coupling plasma emission spectrograph are as the inorganic analysis instrument of maturation, be widely used in the fields such as geological and mineral, petrochemical complex, environmental monitoring, the plurality of advantages such as it is strong to have antijamming capability, highly sensitive, and the range of linearity is wide.Measure when using inductive coupling plasma emission spectrograph can realize magnesium, calcium, iron, lead among the present invention, but use Atomic Absorption Spectrometer Accurate Determining sodium, each element method detection limit all is lower than GB/T 628-2011 " chemical reagent boric acid " requirement, satisfies 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.
Description of drawings
Fig. 1 is experiment flow synoptic diagram of the present invention
Embodiment
As shown in Figure 1, the assay method of trace impurity sodium, magnesium, calcium, iron, lead in the high-purity boracic acid provided by the invention, its step is as follows:
Accurately take by weighing 5.000 g high-purity boracic acid sample to be measured, pour in the 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 remove the boric acid matrix can measure to the greatest extent;
In the 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 and boil, take off behind 5 min, until naturally being settled to 25 mL color-comparison tubes with ultrapure water after the cooling, 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 takes by weighing 1.8859 g through the high pure sodium chloride of 500 ~ 600 ℃ of calcination 2 h, places 250 mL beakers, and the water dissolving moves in the 1000 mL volumetric flasks, is diluted with water to scale, shakes up.
Magnesium oxide standard reserving solution ρ (MgO)=1.00 mg/mL takes by weighing rapidly 0.5000 g in the high-purity magnesium oxide (MgO) of 800 ℃ of calcinations, place 250 mL beakers, add 25 mL water, add 20 mL(1+1) HCl, stirring and dissolving, move in the 1000 mL volumetric flasks after the cooling, be diluted with water to scale, shake up.
Calcium oxide standard reserving solution ρ (CaO)=1.00 mg/mL takes by weighing 0.8924 g through the high-purity calcium carbonate (CaCO3) of 120 ℃ of oven dry 2 h, place 400 mL beakers, add 10 mL water, the edge cup is slow of speech and adds slowly 30 mL(1+1 after adding a cover surface plate) HCl, boil 2 min after the dissolving, take off, water flushing surface plate and walls of beaker are cooled to room temperature, move in the 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 by weighing 1.000 g spectroscopic pure di-iron trioxide (Fe
2O
3), place 250 mL beakers, add 20 mL HCl, the low-temperature heat dissolving.Move in the 1000 mL volumetric flasks after the cooling, add 30 mL HCl, be diluted with water to scale, shake up.
Plumbous standard reserving solution ρ (Pb)=1.00 mg/mL takes by weighing 1.000 g high purity leads and [uses in advance (1+9) HNO
3Clean the surface, then distinguish water and absolute ethanol washing, air-dry rear for subsequent use], place 250 mL beakers, add 10 mL HNO
3, cover surface plate.After heating for dissolving is complete, move in the 1000 mL volumetric flasks, be diluted with water to scale, shake up.
Complex element standard reserving solution ρ (B)=100.00 μ g/mL is 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 are by the preparation of 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, by sodium oxide molybdena standard reserving solution stepwise dilution preparation, WATER AS FLOW MEDIUM.
AAS then lights a fire sodium hollow cathode lamp preheating 15 ~ 30 min first before using, sequentially determining standard sequence and sample solution after absorbance is stable, and the sample solution measurement result is the sample analysis result after deducting reagent blank.
ICP-OES reaches selected analytical line by the condition of work of setting, sequentially determining standard sequence and sample solution, and the sample solution measurement result is the 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:
Determine sampling amount with reference to impurity estimation content in the production procedure sample to be measured, accurately take by weighing 2.000 ~ 5.000 g samples with electronic balance, pour in the PTFE crucible, add 15 mL HF HCl(2:1, v/v), evaporate to dryness on 200 ℃ of control-temperature electric heating plates, add again evaporate to dryness of 5 mL HF, with newly join chloroazotic acid 5 mL, ultrapure water 10 mL boil extraction, are settled to 25 mL color-comparison tubes after the 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 deduct reagent blank and are the 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. sodium in the high-purity boracic acid, magnesium, calcium, iron, plumbous assay method is characterized in that determination step is as follows:
At first, with in the high-purity boracic acid sample teflon crucible to be measured;
Second step adds hydrofluorite and hydrochloric acid in the teflon crucible, the hydrofluorite of adding and the volume ratio of hydrochloric acid are 2:1;
In the 3rd step, the teflon crucible is carried out the evaporate to dryness first time;
The 4th step added and the hydrofluorite of hydrochloric acid with volume in the teflon crucible of the 3rd step evaporate to dryness, carried out the evaporate to dryness second time, removed the boric acid matrix as far as possible;
The 5th step, be incorporated in the teflon crucible of the 4th step evaporate to dryness hydrochloric acid with the chloroazotic acid (1+1) of volume, with the ultrapure water of hydrofluorite with volume, then be heated to boiling, boil to take off behind the 5min and treat that nature cools off;
The 6th step was settled to the 25ml color-comparison tube with the material in the cooled teflon crucible of the 5th step with ultrapure water, shook up to be measured;
In the 7th step, the material to be measured that utilizes Atomic Absorption Spectrometer, inductively-coupled plasma spectrometer that the 6th step was obtained is measured.
2. assay method according to claim 1 is characterized in that: be that 5% nitric acid soaks to put and spends the night with volume ratio before described teflon crucible and 25 mL color-comparison tubes use, then wash with ultrapure water.
3. assay method according to claim 1, it 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 first time, evaporate to dryness, for the second time evaporate to dryness, heating all were that the teflon crucible is operated on the control-temperature electric heating plate.
5. assay method according to claim 1 is characterized in that: the instrument condition of work that the mensuration in 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 used standard reserving solution and the standard operation solution of described the 7th pacing is:
1.00 the sodium oxide molybdena standard reserving solution of 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;
Prepare the complex element standard reserving solution that obtains 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, its medium is nitric acid (5+95);
Obtain the complex element standard operation solution that concentration is respectively 1.00,2.00,5.00,10.00 μ g/mL by the preparation of complex element standard reserving solution stepwise dilution, its medium is nitric acid (5+95);
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 by the preparation of sodium oxide molybdena standard reserving solution stepwise dilution.
7. it is characterized in that according to claim 5 or 6 described assay methods: the measurement operation in described the 7th step is as follows:
Atomic Absorption Spectrometer is then lighted a fire sodium hollow cathode lamp preheating 15 ~ 30 min first before using, sequentially determining standard sequence and sample solution after absorbance is stable, and the sample solution measurement result is the sample analysis result after deducting reagent blank;
ICP-OES reaches selected analytical line by the condition of work of setting, sequentially determining standard sequence and sample solution, and the sample solution measurement result is the sample analysis result after deducting reagent blank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210412408.0A CN102928364B (en) | 2012-10-25 | 2012-10-25 | Method for measuring trace impurity elements of sodium, magnesium, calcium, iron and lead in high-purity boric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210412408.0A CN102928364B (en) | 2012-10-25 | 2012-10-25 | Method for measuring trace impurity elements of sodium, magnesium, calcium, iron and lead in high-purity boric acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102928364A true CN102928364A (en) | 2013-02-13 |
| CN102928364B CN102928364B (en) | 2014-09-10 |
Family
ID=47643216
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210412408.0A Expired - Fee Related CN102928364B (en) | 2012-10-25 | 2012-10-25 | Method for measuring trace impurity elements of sodium, magnesium, calcium, iron and lead in high-purity boric acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102928364B (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104697986A (en) * | 2015-03-30 | 2015-06-10 | 西部新锆核材料科技有限公司 | Method for measuring lithium content in zirconium and zirconium alloy |
| CN104713873A (en) * | 2013-12-11 | 2015-06-17 | 江南大学 | Trace lead spectrophotometric measuring method |
| CN105319203A (en) * | 2014-07-14 | 2016-02-10 | 广东先导稀材股份有限公司 | Method for measuring trace inorganic impurities in boric acid |
| CN105424681A (en) * | 2015-12-23 | 2016-03-23 | 贵州安吉航空精密铸造有限责任公司 | Assay method of chemical elements in Mg-Zn-Re intermediate alloy |
| CN106932381A (en) * | 2015-12-30 | 2017-07-07 | 中核北方核燃料元件有限公司 | 22 kinds of assay methods of impurity element in the pure level phenolic resin of one seed nucleus |
| WO2018000284A1 (en) * | 2016-06-29 | 2018-01-04 | 深圳市爱诺实业有限公司 | Online monitor for high-purity water trace sodium, online monitoring method and device therefor |
| CN110320202A (en) * | 2019-06-05 | 2019-10-11 | 中核霞浦核电有限公司 | Method that is a kind of while detecting plurality of impurities content in nuclear leve metallic sodium |
| CN111999283A (en) * | 2020-08-14 | 2020-11-27 | 贵州省产品质量检验检测院 | Method for detecting metal ions in methanol fuel |
| CN112362639A (en) * | 2020-11-26 | 2021-02-12 | 三门核电有限公司 | Method for measuring content of trace elements in boron matrix sample |
| CN114993802A (en) * | 2022-06-14 | 2022-09-02 | 滨化集团股份有限公司 | Method for testing content of organic impurities in electronic-grade hydrofluoric acid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1229917A (en) * | 1998-08-25 | 1999-09-29 | 四川省石油管理局地质勘探开发研究院 | Pretreating agent and pretreating process for detecting foreign matter in boracic acid by atomic absorption instrument |
| CN102001675A (en) * | 2010-12-10 | 2011-04-06 | 大连理工大学 | Method for preparing nuclear power-grade high-purity boracic acid |
| CN102644090A (en) * | 2012-05-04 | 2012-08-22 | 大连交通大学 | Method for preparing boric acid from crude boron stone through electroosmosis electrolytic method |
-
2012
- 2012-10-25 CN CN201210412408.0A patent/CN102928364B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1229917A (en) * | 1998-08-25 | 1999-09-29 | 四川省石油管理局地质勘探开发研究院 | Pretreating agent and pretreating process for detecting foreign matter in boracic acid by atomic absorption instrument |
| CN102001675A (en) * | 2010-12-10 | 2011-04-06 | 大连理工大学 | Method for preparing nuclear power-grade high-purity boracic acid |
| CN102644090A (en) * | 2012-05-04 | 2012-08-22 | 大连交通大学 | Method for preparing boric acid from crude boron stone through electroosmosis electrolytic method |
Non-Patent Citations (3)
| Title |
|---|
| 余质坚等: "化学富集―无火焰原子吸收光谱测定高纯硼酸中的微量铁", 《化学试剂》 * |
| 周京霞等: "氢化物-原子荧光光谱法测定高纯硼酸中痕量砷", 《铀矿冶》 * |
| 谷松海等: "X-射线荧光光谱法测定溶样后熔融制样金属硅中铁、铝、钙、钛、磷、铜", 《光谱学与光谱分析》 * |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104713873A (en) * | 2013-12-11 | 2015-06-17 | 江南大学 | Trace lead spectrophotometric measuring method |
| CN105319203B (en) * | 2014-07-14 | 2018-07-06 | 广东先导稀材股份有限公司 | Method for measuring trace inorganic impurities in boric acid |
| CN105319203A (en) * | 2014-07-14 | 2016-02-10 | 广东先导稀材股份有限公司 | Method for measuring trace inorganic impurities in boric acid |
| CN104697986A (en) * | 2015-03-30 | 2015-06-10 | 西部新锆核材料科技有限公司 | Method for measuring lithium content in zirconium and zirconium alloy |
| CN107462567A (en) * | 2015-03-30 | 2017-12-12 | 国核宝钛锆业股份公司 | A kind of method for determining lithium content in zirconium and zircaloy |
| CN107462567B (en) * | 2015-03-30 | 2019-04-09 | 国核宝钛锆业股份公司 | A method of lithium content in measurement zirconium and zircaloy |
| CN105424681A (en) * | 2015-12-23 | 2016-03-23 | 贵州安吉航空精密铸造有限责任公司 | Assay method of chemical elements in Mg-Zn-Re intermediate alloy |
| CN106932381A (en) * | 2015-12-30 | 2017-07-07 | 中核北方核燃料元件有限公司 | 22 kinds of assay methods of impurity element in the pure level phenolic resin of one seed nucleus |
| CN107636448A (en) * | 2016-06-29 | 2018-01-26 | 深圳市爱诺实业有限公司 | High purity water trace amounts of sodium on-line computing model and its on-line monitoring method and device |
| WO2018000284A1 (en) * | 2016-06-29 | 2018-01-04 | 深圳市爱诺实业有限公司 | Online monitor for high-purity water trace sodium, online monitoring method and device therefor |
| US10788474B2 (en) | 2016-06-29 | 2020-09-29 | Shenzhen Ener-Chemistry Industrial Co., Ltd. | Online monitor for trace sodium in high-purity water, and online monitoring method and device thereof |
| CN110320202A (en) * | 2019-06-05 | 2019-10-11 | 中核霞浦核电有限公司 | Method that is a kind of while detecting plurality of impurities content in nuclear leve metallic sodium |
| CN111999283A (en) * | 2020-08-14 | 2020-11-27 | 贵州省产品质量检验检测院 | Method for detecting metal ions in methanol fuel |
| CN112362639A (en) * | 2020-11-26 | 2021-02-12 | 三门核电有限公司 | Method for measuring content of trace elements in boron matrix sample |
| CN114993802A (en) * | 2022-06-14 | 2022-09-02 | 滨化集团股份有限公司 | Method for testing content of organic impurities in electronic-grade hydrofluoric acid |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102928364B (en) | 2014-09-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102928364B (en) | Method for measuring trace impurity elements of sodium, magnesium, calcium, iron and lead in high-purity boric acid | |
| CN102998303B (en) | Applied microwave clears up the detection method that-ICP-AES measures Niobium in Steel, tantalum content | |
| CN103175824B (en) | Inductively coupled plasma spectrometry transmitter measures the method for Silicon in Ferromanganese phosphorus content | |
| Meisel et al. | Determination of rare earth elements, Y, Th, Zr, Hf, Nb and Ta in geological reference materials G‐2, G‐3, SCo‐1 and WGB‐1 by sodium peroxide sintering and inductively coupled plasma‐mass spectrometry | |
| CN102253030B (en) | Method for determining impurity content in high-titanium slag | |
| Fedyunina et al. | Investigation of the efficiency of the sample pretreatment stage for the determination of the Rare Earth Elements in rock samples by inductively coupled plasma mass spectrometry technique | |
| CN101776607B (en) | Method for analyzing total arsenic in glass | |
| CN107024468A (en) | The assay method of iron, aluminium, manganese, calcium, titanium, silicon, magnesium in covering slag | |
| CN107976481B (en) | Method for detecting scandium content in traditional Chinese medicinal materials | |
| Suoranta et al. | Comparison of digestion methods for the determination of ruthenium in catalyst materials | |
| CN110514643B (en) | Method for measuring trace elements in high-purity magnesium-based oxide by inductively coupled plasma emission spectrometry | |
| CN102353637B (en) | Method of determining silver content in rock minerals | |
| CN102879372A (en) | Method for determining arsenic, antimony and bismuth content of pure chromium by using atomic fluorescence spectrometry | |
| CN102621090A (en) | Method for measuring iron content in kaolin through using spectrophotometer | |
| CN102393371B (en) | Sample processing method for detecting boron in industrial silicon with graphite furnace atomic absorption spectrometry | |
| CN105548150A (en) | Method for determining zirconium content in glass | |
| CN102830109A (en) | Determining method of contents of other elements in titanium and titanium alloy | |
| CN102128737A (en) | Method for detecting and pretreating silica sample | |
| CN103698317A (en) | Method for measuring contents of silicon, magnesium and aluminum in coal combustion-supporting agent | |
| CN102393386A (en) | Method for measuring content of calcium, magnesium and silicon in aluminum-based compound deoxidizing slagging constituent | |
| CN103698176A (en) | Determination method of total aluminum content in steel and alloy | |
| CN109632771A (en) | A method of measurement coal, sludge, dedusting ash, sodium oxide molybdena in covering slag | |
| CN104777062A (en) | Method for measuring silicon dioxide content in rare earth concentrate | |
| CN104807806A (en) | Method for measuring content of phosphorus in sintered flux | |
| CN111257097A (en) | Vanadium carbide sample to be tested manufacturing method and impurity content analysis method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140910 Termination date: 20181025 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |