CN105628859A - Method for detecting purity of boron nitride - Google Patents
Method for detecting purity of boron nitride Download PDFInfo
- Publication number
- CN105628859A CN105628859A CN201510983760.3A CN201510983760A CN105628859A CN 105628859 A CN105628859 A CN 105628859A CN 201510983760 A CN201510983760 A CN 201510983760A CN 105628859 A CN105628859 A CN 105628859A
- Authority
- CN
- China
- Prior art keywords
- boron nitride
- solution
- mixed liquor
- highly basic
- standard solution
- 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.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Biochemistry (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention provides a method for detecting the purity of boron nitride. The method particularly comprises the following steps: treating boron nitride by adopting a strong alkali solution and a hydrochloric acid solution to obtain a boron nitride mixed solution, then respectively conducting complexometry and acid-alkali neutralization titration on the boron nitride mixed solution by adopting mannitol and a strong alkali standard solution, acquiring the volume difference of the consumed strong alkali standard solution through a blank contrast test, and then calculating by utilizing an established boron nitride monadic linear quantitative detection model so as to obtain the purity of boron nitride. The provided detecting method is simple in step and high in accuracy of detection results.
Description
Technical field
The present invention relates to the detection method of a kind of chemical field, specifically, relate to a kind of method detecting boron nitride purity.
Background technology
Boron nitride is widely used in the fields such as solid lubrication, casting, composite ceramics, electric insulation, superelevation thermal conductance, instrument plated film and Aero-Space because it has good lubricity, electrical insulating property, heat conductivity and chemical resistance. The purity of boron nitride often affects the quality of product after the quality of converted products and silicon nitride crystal conversion.
At present, the method of detection boron nitride mainly has the means such as X-ray diffraction sign, scanning electron microscope sign, laser particle size analysis and specific area measuring, detection complex procedures and testing cost are high, such as wherein scanning electron microscope characterizes and to treat survey material in advance and carry out making the step such as standard sight sheet, and equipment cost is higher, maintenance requires complexity.
Summary of the invention
Being thered is provided a kind of operating procedure simple by consideration of it, the present invention is necessary, the detection method of the boron nitride purity that testing cost is cheap, to solve the problems referred to above.
For solving the problems referred to above, present invention provide the technical scheme that a kind of method detecting boron nitride purity, specifically include following steps:
Boron nitride is processed prepared boron nitride molten mixture by step one, employing highly basic;
Step 2, described boron nitride molten mixture is added water and dissolves, obtain borate filtrate after filtering;
Step 3, adding indicator and excessive hydrochloric acid solution in described borate filtrate, reaction generates boric acid mixed liquor, then adopts highly basic standard solution that described boric acid mixed liquor is carried out acid base neutralization titration, prepares neutral mixed liquor;
Step 4, initially with mannitol, described neutral mixed liquor is carried out complexometry reaction and generate hydroxo complex mixed liquor, then adopting described highly basic standard solution that described hydroxo complex mixed liquor carries out acid base neutralization titration, the described highly basic standard solution volume that record consumes is V1;
Step 5, acid base neutralization titration step to described hydroxo complex mixed liquor carry out blank test, and the volume recording the described highly basic standard solution consumed in the test of described blank is V2, set up boron nitride unitary linear quantitative detection model, specific formula for calculation is:
,
X in formula1For the mass fraction of the boron nitride that sample records, C is the concentration of highly basic standard solution, and m is the quality of alleged boron nitride.
Based on above-mentioned, described indicator refers to the combination of one or more indicators in C.I. 13020. solution, bromocresol green solution, phenolphthalein solution, thymol blue solution.
Based on above-mentioned, described indicator is to be mixed by the C.I. 13020. solution that mass ratio is 1:3��5:1, bromocresol green solution, phenolphthalein solution, and the mass fraction of described bromocresol green solution, described C.I. 13020. solution and described phenolphthalein solution is 0.1%��1%.
Based on above-mentioned, described step 3 also includes adopting after described boric acid mixed liquor is neutralized titration by highly basic standard solution, then carries out boiling 10��20min, makes the carbonic acid existed in described boric acid mixed liquor be removed.
Based on above-mentioned, described boron nitride is the combination of one or more materials in hexagonal boron nitride, Pedicellus et Pericarpium Trapae side's boron nitride, cubic boron nitride and buergerite boron nitride.
Based on above-mentioned, described highly basic standard solution is concentration is standard solution of sodium hydroxide or the standard potassium hydroxide solution of 0.1��0.5mol/L.
Based on above-mentioned, described hydrochloric acid solution is to be carried out with 4��5 times of water of described hydrochloric acid volume mixing by the hydrochloric acid that mass fraction is 20%��30% preparing.
In experimentation, the chemical bond rupture between described boron nitride can be formed boron nitride fused solution by described highly basic, and described boron nitride fused solution just can be converted into boric acid with hydrochloric acid after being neutralized; In described step 3, dripping excessive hydrochloric acid is to be decomposed by carbonate material that may be present in described boric acid mixed liquor, and then generation gas is removed.
Hinge structure of the present invention has prominent substantive distinguishing features and significant progressive, specifically, the present invention by employing highly basic, boron nitride is carried out process by hydrochloric acid makes boron nitride be converted into boric acid; Then pass through mannitol and carry out complex reaction generation complex acid with described boric acid, highly basic standard solution and described complex acid is finally adopted to carry out acid base neutralization titration, and do the blank test of the described mannitol described highly basic standard solution of consumption, by the highly basic standard solution of calculation consumption difference thus drawing the purity of described boron nitride, detection method test operation step provided by the invention is simple, and testing cost is cheap. Further, process of the test adds blank test portion, get rid of in water or the material affecting complex acid that may be present in highly basic standard solution, the boron nitride unitary linear quantitative detection model set up is to utilize the volume differences of described highly basic standard solution consumed to be calculated so that the purity data of the described boron nitride obtained more accurately, be easy to get.
Detailed description of the invention
Below by detailed description of the invention, technical scheme is described in further detail.
Embodiment 1
The present embodiment provides a kind of method detecting boron nitride purity, specifically includes following steps:
Step one, initially with drying oven, hexagonal boron nitride is baked to constant weight; Then weigh the described hexagonal boron nitride 0.0702g after overbaking and sodium hydroxide 3g successively to be placed in nickel crucible and carry out being mixed to form compound, be adopt Muffle furnace that described compound is carried out melt process under 500 DEG C of conditions to obtain boron nitride fused solution in temperature.
Step 2, in described boron nitride fused solution, add the water of 150mL carry out mixed dissolution, adopt filter to obtain boron nitride filtrate after filtering.
Step 3, in described boron nitride filtrate, add 2mL indicator, wherein said indicator be the bromocresol green of 1% by the mass fraction that volume ratio is 1:3:1, C.I. 13020. and phenolphthalein solution agent mix; Then adopting volume ratio is that described boron nitride filtrate is neutralized to presenting redness by the hydrochloric acid that mass fraction is 30% of 1:5 with the mixed solution of water, reaction generates boric acid mixed liquor, described boric acid mixed liquor is boiled 10min, makes the carbonic acid existed in described boric acid mixed liquor be removed.
Step 4, in boric acid mixed liquor described in 150mL, add mixed indicator described in 2mL and concentration is that 0.5mol/L standard solution of sodium hydroxide to described boric acid mixed liquor presents green successively; Then adding 7g mannitol in described boric acid mixed liquor, reaction generates hydroxo complex mixed liquor; Described hydroxo complex mixed liquor is neutralized to presenting dusty blue by the described standard solution of sodium hydroxide adopting concentration to be 0.5mol/L, and the volume of the described standard solution of sodium hydroxide wherein adding described mannitol post consumption is recorded as V1��
Step 5, first in the water of 150mL, it is sequentially added into mixed indicator described in 2mL and mannitol described in 7g carries out being mixed to form mixed liquor, described mixed liquor is reacted to presenting dusty blue by the described standard solution of sodium hydroxide then adopting concentration to be 0.5mol/L, and the volume of the described standard solution of sodium hydroxide wherein consumed is recorded as V2; Test data is substituted in boron nitride unitary linear quantitative detection model provided by the invention, thus calculating the purity of boron nitride to be measured.
The purity of the hexagonal boron nitride that experiment records the implementation case detection is 99.19%.
Embodiment 2
The present embodiment provides a kind of method detecting boron nitride purity, and concrete steps are roughly the same with described embodiment 1, are different in that:
In described each step, purity materials to be detected is cubic boron nitride;
Described step one adopt 3g potassium hydroxide and 0.0754g cubic boron nitride carry out being mixed to form boric acid dipotassium compound;
Adopting concentration in described step 4 is that 0.3mol/L standard potassium hydroxide solution is neutralized reaction respectively and reacts with mannitol described in 7g;
Described step 5 adopts concentration to be 0.3mol/L standard potassium hydroxide solution with mannitol described in 7g react and carry out blank test.
The purity of the cubic boron nitride that experiment records the implementation case detection is 99.36%.
Embodiment 3
The present embodiment provides a kind of method detecting boron nitride purity, and concrete steps are roughly the same with described embodiment 1, are different in that:
In described each step, purity materials to be detected is Pedicellus et Pericarpium Trapae side's boron nitride;
Adopting concentration in described step 4 is that 0.5mol/L standard potassium hydroxide solution is neutralized reaction respectively and reacts with mannitol described in 7g;
Adopting concentration in described step 5 is that 0.5mol/L standard potassium hydroxide solution carries out blank test with mannitol described in 7g.
The purity of the cubic boron nitride that experiment records the implementation case detection is 99.05%.
Embodiment 4
The present embodiment provide a kind of method detecting boron nitride purity, concrete steps are roughly the same with described embodiment 1, are different in that: the indicator used by the present embodiment is mass fraction be 1% thymol blue solution;
Adopting mass fraction in described step 3 is that described boron nitride filtrate is neutralized to presenting redness by the hydrochloric acid of 30% with the mixed solution of water, reaction generates boric acid mixed liquor, described boric acid mixed liquor is boiled 10min, makes the carbonic acid existed in described boric acid mixed liquor be removed;
Adding thymol blue solution and concentration described in 2mL in described step 4 successively in described boric acid mixed liquor is that 0.5mol/L standard solution of sodium hydroxide to described boric acid mixed liquor presents yellow; Then adding 7g mannitol in described boric acid mixed liquor, reaction generates hydroxo complex mixed liquor; Described hydroxo complex mixed liquor is neutralized to presenting blueness by the described standard solution of sodium hydroxide adopting concentration to be 0.5mol/L, and the volume of the described standard solution of sodium hydroxide wherein adding described mannitol post consumption is recorded as V1��
The purity of the cubic boron nitride that experiment records the implementation case detection is 99.14%.
Finally should be noted that: above example is only in order to illustrate that technical scheme is not intended to limit; Although the present invention being described in detail with reference to preferred embodiment, those of ordinary skill in the field are it is understood that still can modify to the specific embodiment of the present invention or portion of techniques feature carries out equivalent replacement; Without deviating from the spirit of technical solution of the present invention, it all should be encompassed in the middle of the technical scheme scope that the present invention is claimed.
Claims (7)
1. the method detecting boron nitride purity, specifically includes following steps:
Boron nitride is processed prepared boron nitride molten mixture by step one, employing highly basic;
Step 2, described boron nitride molten mixture is added water and dissolves, obtain borate filtrate after filtering;
Step 3, adding indicator and excessive hydrochloric acid solution in described borate filtrate, reaction generates boric acid mixed liquor, then adopts highly basic standard solution that described boric acid mixed liquor is carried out acid base neutralization titration, prepares neutral mixed liquor;
Step 4, initially with mannitol, described neutral mixed liquor is carried out complexometry reaction and generate hydroxo complex mixed liquor, then adopting described highly basic standard solution that described hydroxo complex mixed liquor carries out acid base neutralization titration, the described highly basic standard solution volume that record consumes is V1;
Step 5, acid base neutralization titration step to described hydroxo complex mixed liquor carry out blank test, and the volume recording the described highly basic standard solution consumed in the test of described blank is V2, set up boron nitride unitary linear quantitative detection model, specific formula for calculation is:
,
X in formula1For the mass fraction of the boron nitride that sample records, C is the concentration of highly basic standard solution, and m is the quality of alleged boron nitride.
2. the method for detection boron nitride purity according to claim 1, it is characterised in that described indicator refers to the combination of one or more indicators in C.I. 13020. solution, bromocresol green solution, phenolphthalein solution, thymol blue solution.
3. the method for detection boron nitride purity according to claim 1, it is characterized in that, described indicator is to be mixed by the C.I. 13020. solution that mass ratio is 1:3��5:1, bromocresol green solution, phenolphthalein solution, and the mass fraction of described bromocresol green solution, described C.I. 13020. solution and described phenolphthalein solution is 0.1%��1%.
4. the method for the detection boron nitride purity according to Claims 2 or 3, it is characterized in that, described step 3 also includes adopting after described boric acid mixed liquor is neutralized titration by highly basic standard solution, then carries out boiling 10��20min, makes the carbonic acid existed in described boric acid mixed liquor be removed.
5. the method for detection boron nitride purity according to claim 4, it is characterised in that described boron nitride is the combination of one or more materials in hexagonal boron nitride, Pedicellus et Pericarpium Trapae side's boron nitride, cubic boron nitride and buergerite boron nitride.
6. the method for the detection boron nitride purity according to claim 1 or 2 or 5, it is characterised in that described highly basic standard solution is concentration is standard solution of sodium hydroxide or the standard potassium hydroxide solution of 0.1��0.5mol/L.
7. the method for detection boron nitride purity according to claim 6, it is characterised in that described hydrochloric acid solution is to be carried out with 4��5 times of water of described hydrochloric acid volume mixing by the hydrochloric acid that mass fraction is 20%��30% preparing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510983760.3A CN105628859A (en) | 2015-12-24 | 2015-12-24 | Method for detecting purity of boron nitride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510983760.3A CN105628859A (en) | 2015-12-24 | 2015-12-24 | Method for detecting purity of boron nitride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105628859A true CN105628859A (en) | 2016-06-01 |
Family
ID=56043993
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510983760.3A Pending CN105628859A (en) | 2015-12-24 | 2015-12-24 | Method for detecting purity of boron nitride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105628859A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108459136A (en) * | 2018-05-29 | 2018-08-28 | 上海福乐医药科技有限公司 | A kind of method of three boroxane content of titration measuring front three basic ring |
| CN112730143A (en) * | 2020-12-22 | 2021-04-30 | 北京有色金属与稀土应用研究所 | Method for measuring effective chemical components in brazing flux |
| CN114252440A (en) * | 2021-12-31 | 2022-03-29 | 东北大学 | Contrast detection method for determining content of diboron trioxide in metallurgical slag system |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102042982A (en) * | 2010-10-25 | 2011-05-04 | 中国兵器工业集团第五三研究所 | Method for testing content of boron trioxide in glass containing zinc and lead |
| CN102650614A (en) * | 2012-05-18 | 2012-08-29 | 内蒙古包钢钢联股份有限公司 | Method for determining content of boron nitride in steel |
| CN102680564A (en) * | 2012-05-18 | 2012-09-19 | 内蒙古包钢钢联股份有限公司 | Method for determining content of boron nitride in steel |
| CN102830111A (en) * | 2012-07-30 | 2012-12-19 | 沈阳黎明航空发动机(集团)有限责任公司 | Method for rapidly analyzing SiO2 and BN content in aluminum silicon boron nitride powder |
| CN104155267A (en) * | 2014-07-27 | 2014-11-19 | 中国人民解放军第五七一九工厂 | Method for chemically analyzing content of boron nitride in nickel-based powder material |
-
2015
- 2015-12-24 CN CN201510983760.3A patent/CN105628859A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102042982A (en) * | 2010-10-25 | 2011-05-04 | 中国兵器工业集团第五三研究所 | Method for testing content of boron trioxide in glass containing zinc and lead |
| CN102650614A (en) * | 2012-05-18 | 2012-08-29 | 内蒙古包钢钢联股份有限公司 | Method for determining content of boron nitride in steel |
| CN102680564A (en) * | 2012-05-18 | 2012-09-19 | 内蒙古包钢钢联股份有限公司 | Method for determining content of boron nitride in steel |
| CN102830111A (en) * | 2012-07-30 | 2012-12-19 | 沈阳黎明航空发动机(集团)有限责任公司 | Method for rapidly analyzing SiO2 and BN content in aluminum silicon boron nitride powder |
| CN104155267A (en) * | 2014-07-27 | 2014-11-19 | 中国人民解放军第五七一九工厂 | Method for chemically analyzing content of boron nitride in nickel-based powder material |
Non-Patent Citations (2)
| Title |
|---|
| 冯艳春: "前驱物法低温合成六方氮化硼", 《中国优秀硕士学位论文全文数据库（电子期刊）工程科技Ⅰ辑》 * |
| 学百科全书编委会: "《化工百科全书 第12卷》", 30 November 1996, 化学工业出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108459136A (en) * | 2018-05-29 | 2018-08-28 | 上海福乐医药科技有限公司 | A kind of method of three boroxane content of titration measuring front three basic ring |
| CN112730143A (en) * | 2020-12-22 | 2021-04-30 | 北京有色金属与稀土应用研究所 | Method for measuring effective chemical components in brazing flux |
| CN114252440A (en) * | 2021-12-31 | 2022-03-29 | 东北大学 | Contrast detection method for determining content of diboron trioxide in metallurgical slag system |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101135617B (en) | Vanadium-nitrogen alloy resolution method | |
| CN105372386A (en) | Method for measuring content of free boron oxide in boron nitride | |
| CN103149073B (en) | X-ray fluorescence spectra analyzes the MTG YBCO bulk method of ferrosilicon, Si-Ca-Ba, silicomanganese, ferro-aluminum or ferro-titanium sample | |
| CN105628859A (en) | Method for detecting purity of boron nitride | |
| CN102213657A (en) | Digestion method and detection method of Tungsten-base class sample | |
| CN108152444A (en) | Method for detecting content of free nitric acid in bismuth nitrate solution | |
| CN104807813A (en) | Rapid analysis method for content of manganese in ferromanganese iron | |
| CN105241739A (en) | Microwave digestion ICP method for simultaneous determination of contents of multiple elements in synthetic rubber | |
| CN104502298A (en) | Method for determining cadmium and trace lead in iron ore | |
| CN104515766A (en) | Method for measuring impurity elements in graphite slurry | |
| CN109824726A (en) | A kind of preparation method, nonaqueous electrolytic solution and the battery of the double oxalic acid lithium phosphates of difluoro | |
| CN105223307B (en) | A kind of detection method for being used for element silicon volumetric method in vanadium iron | |
| CN104764735A (en) | Method for analyzing phosphorus in ferrochromium | |
| CN106770914A (en) | Boron contents assay method in a kind of boride | |
| CN103868911A (en) | Method for dissolving aluminum oxide and determining trace metal elements in aluminum oxide | |
| CN108459141A (en) | A kind of analysis method of di-oxalate lithium borate product | |
| CN107655886B (en) | Method for measuring silicon dioxide content in phosphorite by potassium fluosilicate volumetric method | |
| CN104330523A (en) | Method for measuring content of sodium malonate containing sodium hydroxide and sodium carbonate impurities | |
| CN106290438B (en) | A kind of method that X-ray fluorescence spectra fusion method measures Calcium Fluoride Content in fluorite | |
| CN104880454B (en) | A kind of method of measuring metal element content in Merlon | |
| CN104034573B (en) | A kind of digestion procedure of nickel-base alloy | |
| CN102967619A (en) | Method for improving precision and accuracy of hydrogen in oxygen-nitrogen-hydrogen combined determination of titanium or titanium alloy | |
| CN105021584B (en) | The assay method of arsenic content in a kind of chrome ore | |
| CN106338510A (en) | Rapid detection method for lead content of halal beef and mutton | |
| CN105606592B (en) | A kind of method of heterogeneous element content in measurement Polycarbosilane |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160601 |