CN111307869A - Method for measuring content of elemental boron in boron powder - Google Patents
Method for measuring content of elemental boron in boron powder Download PDFInfo
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- CN111307869A CN111307869A CN202010231224.9A CN202010231224A CN111307869A CN 111307869 A CN111307869 A CN 111307869A CN 202010231224 A CN202010231224 A CN 202010231224A CN 111307869 A CN111307869 A CN 111307869A
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910052796 boron Inorganic materials 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 33
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 76
- 239000000523 sample Substances 0.000 claims abstract description 42
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 26
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 21
- 238000005303 weighing Methods 0.000 claims abstract description 21
- 239000012496 blank sample Substances 0.000 claims abstract description 13
- 238000009835 boiling Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical class [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 132
- 238000004448 titration Methods 0.000 claims description 43
- 238000005406 washing Methods 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 16
- 239000011521 glass Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 9
- 229930195725 Mannitol Natural products 0.000 claims description 9
- 239000000594 mannitol Substances 0.000 claims description 9
- 235000010355 mannitol Nutrition 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 8
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 229960001484 edetic acid Drugs 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims 1
- 238000005868 electrolysis reaction Methods 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000003513 alkali Substances 0.000 abstract description 2
- 238000007500 overflow downdraw method Methods 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract description 2
- 238000007796 conventional method Methods 0.000 abstract 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 48
- 229910052697 platinum Inorganic materials 0.000 description 24
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 10
- 239000013558 reference substance Substances 0.000 description 6
- 239000001569 carbon dioxide Substances 0.000 description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 description 5
- 238000003556 assay Methods 0.000 description 4
- ZOXJGFHDIHLPTG-BJUDXGSMSA-N Boron-10 Chemical compound [10B] ZOXJGFHDIHLPTG-BJUDXGSMSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- BDOYKFSQFYNPKF-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetic acid;sodium Chemical compound [Na].[Na].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O BDOYKFSQFYNPKF-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000002479 acid--base titration Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- -1 hydrogen ions Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
-
- 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
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Electrochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for measuring the content of elemental boron in boron powder, which aims to solve the problems in the conventional method for measuring the content of elemental boron. The method comprises the following specific steps: step one, pretreatment; step two, weighing a sample; step three, adding anhydrous sodium carbonate; step four, blank control; step five, high-temperature treatment; dissolving a sample; step seven, neutralizing the excessive hydrochloric acid; step eight, heating and boiling; step nine, neutralizing the hydrochloric acid again; step ten, adding a reagent for treatment; step eleven, titrating a sample; step twelve, measuring a blank sample; and thirteen, calculating the content. The invention successfully establishes the method for measuring the content of the elemental boron in the boron powder prepared by the molten salt electrolysis method by the alkali fusion method, can accurately measure the content of the elemental boron in the boron powder by using the experimental conditions listed in the invention content, obtains accurate detection data, has the precision superior to 0.01 percent, is accurate and reliable, and effectively cooperates with the production in a workshop.
Description
Technical Field
The invention relates to the field of boron content determination, in particular to a method for determining the content of elemental boron in boron powder.
Background
At present, research reports about the content measurement of elemental boron (the abundance of boron-10 is more than 85%) are rare, and boron-10 has strong radiation protection and neutron absorption functions and has wide application in the technical fields of nuclear energy, national defense industry, medicine and science. In the nuclear industry, boron-10 can be used as a neutron absorber or shielding material for reactors.
Known related chemical analysis methods comprise a curcumin-spectrophotometry method, an ICP-AES method and an ICP-MS method, wherein the curcumin-spectrophotometry method can only be used for qualitatively detecting boron element and cannot be used for quantitatively detecting boron element; the CP-AES method and the ICP-MS method need expensive ICP, can only measure trace elements and cannot accurately measure high-purity boron elements. The content of boron in GB/T35871-.
Disclosure of Invention
An object of an embodiment of the present invention is to provide a method for determining the content of elemental boron in boron powder, so as to solve the problems mentioned in the background art.
In order to achieve the above purpose, the embodiments of the present invention provide the following technical solutions:
a method for measuring the content of elemental boron in boron powder comprises the following specific steps:
step one, pretreatment: sequentially grinding boron powder (the granularity is less than 100 mu m), acid washing, water washing, alcohol washing and vacuum drying;
step two, weighing a sample: weighing a boron powder sample with the mass of 0.1g in a crucible, accurately weighing the boron powder sample to 0.0001g, and weighing 5 samples in parallel;
step three, adding anhydrous sodium carbonate: 2.0g of anhydrous sodium carbonate is added into the crucible again, and the mixture is stirred uniformly by a glass rod;
step four, blank control: adding 2.0g of anhydrous sodium carbonate into an empty crucible, stirring by using a glass rod, and making a blank control;
step five, high-temperature treatment: covering a crucible cover, putting the crucible into a muffle furnace, keeping the temperature of 850-900 ℃ for 20min, cooling, and performing high-temperature treatment to react single boron with sodium carbonate to generate sodium borate;
step six, dissolving a sample: placing the cooled crucible and the cooled crucible cover into a 500ml beaker filled with dilute hydrochloric acid to dissolve the sample, washing the crucible and the crucible cover for a plurality of times, then washing with hot water, and pouring the washing liquid back to the beaker;
step seven, neutralizing the excessive hydrochloric acid: adding 30ml of saturated sodium hydroxide solution, neutralizing excessive hydrochloric acid by using 0.1mol/L sodium hydroxide solution, and adjusting the pH to 7.0;
step eight, heating and boiling treatment: then adding 5ml of 0.1mol/L hydrochloric acid, heating and boiling for three minutes to remove carbon dioxide completely, and then cooling in a water bath;
step nine, neutralizing the hydrochloric acid again: neutralizing excessive hydrochloric acid with 0.1mol/L sodium hydroxide solution, and adjusting the pH to 7.0;
step ten, adding a reagent for treatment: adding 9g of mannitol, adding 0.5g of ethylene diamine tetraacetic acid, uniformly stirring, and adding mannitol to combine boric acid and hydroxyl in mannitol to ionize hydrogen ions so as to prepare for next acid-base titration;
step eleven, titrating a sample: titrating the solution to an end point by using 0.1mol/L sodium hydroxide titration solution on a full-automatic potentiometric titrator; recording the dosage of the sodium hydroxide titration solution used in the titration as V1;
step twelve, blank sample determination: making a blank sample under the same condition, and recording the dosage of the sodium hydroxide titration solution used in the titration as V2;
step thirteen, calculating the content: the content of the simple substance boron in the boron powder is calculated by the following formula:
b% -the mass percentage of the simple substance boron in the boron powder, the unit is;
c, the concentration of 0.1mol/L sodium hydroxide titration solution is mol/L;
v1-the volume of sodium hydroxide solution consumed by titrating a sample by a full-automatic potentiometric titrator, and the unit is ml;
v2-volume of sodium hydroxide solution consumed in the blank in ml;
m-total mass of the boron powder sample, unit is g;
0.01082-mass of boron expressed in grams equivalent to sodium hydroxide titration.
As a further scheme of the embodiment of the invention: in the third step and the fifth step, the dried glass rod is used for stirring, and the sample is not required to be stuck on the glass rod so as to avoid quality loss and inaccurate result.
As a further scheme of the embodiment of the invention: the preparation method of the dilute hydrochloric acid in the sixth step is concentrated hydrochloric acid: the volume ratio of water is 1: 1, mixing.
As a further scheme of the embodiment of the invention: in step ten, mannitol and disodium edetate are purchased.
As a further scheme of the embodiment of the invention: in the eleventh step, the signal collected by the automatic titrator in the titration process is 0.1mV, and the minimum feed of the automatic titrator is 0.0025 ml.
As a further scheme of the embodiment of the invention: the determination of the content of the simple substance boron needs to be carried out for 2-3 times in parallel, and an average value is taken.
Compared with the prior art, the embodiment of the invention has the beneficial effects that:
the invention successfully establishes the method for measuring the content of the elemental boron in the boron powder prepared by the molten salt electrolysis method by the alkali fusion method, can accurately measure the content of the elemental boron in the boron powder by using the experimental conditions listed in the invention content, obtains accurate detection data, has the precision superior to 0.01 percent, is accurate and reliable, and effectively cooperates with the production in a workshop.
Detailed Description
The technical solution of the present patent will be described in further detail with reference to the following embodiments.
Example 1
(1) Pretreatment of electrolytic product boron powder prepared in workshop
Sequentially grinding 20200110 batches of boron powder (the granularity is less than 100um), acid washing, water washing, alcohol washing and vacuum drying;
(2) weighing boron powder sample
Weighing an electrolysis product sample with the boron powder mass of 0.10g in a platinum crucible, and accurately measuring the sample to 0.0001 g; weighing 5 parallel samples in parallel;
(3) adding anhydrous sodium carbonate
2.0g of anhydrous sodium carbonate is added into the platinum crucible again, and the mixture is stirred uniformly by a glass rod;
(4) blank control
Adding 2.0g of anhydrous sodium carbonate into an empty platinum crucible, stirring by using a glass rod, and making a blank control;
(5) high temperature treatment
Covering a crucible cover, putting the platinum crucible into a muffle furnace, keeping the temperature at 880 ℃ for 20min, and then cooling;
(6) dissolving the sample
Putting the cooled platinum crucible and the cooled cover into a 500ml beaker filled with dilute hydrochloric acid to dissolve a sample, washing the platinum crucible and the cooled cover for a plurality of times, then washing with hot water, and pouring the washing liquid back to the beaker;
(7) neutralizing excess hydrochloric acid
Adding 30ml of saturated sodium hydroxide solution, then neutralizing excess hydrochloric acid by using 0.1mol/L sodium hydroxide solution, and adjusting the pH value to 7.0;
(8) heating and boiling treatment
Then adding 5ml of 0.1mol/L hydrochloric acid, heating and boiling for three minutes to remove carbon dioxide completely, and then cooling in a water bath;
(9) neutralizing the hydrochloric acid again
Neutralizing the excessive hydrochloric acid by using 0.1mol/L sodium hydroxide solution, and adjusting the pH value to be 7.0;
(10) adding reagent for treatment
Adding 9g of mannitol, adding 0.5g of ethylene diamine tetraacetic acid, and uniformly stirring;
(11) titration of samples
Titrating the solution to an end point by using 0.1mol/L sodium hydroxide titration solution on a full-automatic potentiometric titrator; recording the dosage of the sodium hydroxide titration solution used in the titration as V1;
(12) blank sample assay
Making a blank sample under the same condition, and recording the dosage of the sodium hydroxide titration solution used in the titration as V2;
example 2
(1) Pretreatment of electrolytic product boron powder prepared in workshop
Sequentially grinding 20200111 batches of boron powder (the granularity is less than 80um), acid washing, water washing, alcohol washing and vacuum drying;
(2) weighing boron powder sample
Weighing an electrolysis product sample with the boron powder mass of 0.11g in a platinum crucible, and accurately measuring the sample to 0.0001 g; weighing 5 parallel samples in parallel;
(3) adding anhydrous sodium carbonate
Adding 1.6g of anhydrous sodium carbonate into the platinum crucible again, and stirring uniformly by using a glass rod;
(4) blank control
Adding 1.6g of anhydrous sodium carbonate into an empty platinum crucible, stirring by using a glass rod, and making a blank control;
(5) high temperature treatment
Covering a crucible cover, putting the platinum crucible into a muffle furnace, keeping the temperature at 890 ℃ for 15min, and cooling;
(6) dissolving the sample
Putting the cooled platinum crucible and the cooled cover into a 500ml beaker filled with dilute hydrochloric acid to dissolve a sample, washing the platinum crucible and the cooled cover for a plurality of times, then washing with hot water, and pouring the washing liquid back to the beaker;
(7) neutralizing excess hydrochloric acid
Adding 30ml of saturated sodium hydroxide solution, then neutralizing excess hydrochloric acid by using 0.1mol/L sodium hydroxide solution, and adjusting the pH value to 7.0;
(8) heating and boiling treatment
Then adding 5ml of 0.1mol/L hydrochloric acid, heating and boiling for three minutes to remove carbon dioxide completely, and then cooling in a water bath;
(9) neutralizing the hydrochloric acid again
Neutralizing the excessive hydrochloric acid by using 0.1mol/L sodium hydroxide solution, and adjusting the pH value to be 7.0;
(10) adding reagent for treatment
Adding 10g of mannitol, adding 1.0g of ethylene diamine tetraacetic acid disodium and stirring uniformly;
(11) titration of samples
Titrating the solution to an end point by using 0.1mol/L sodium hydroxide titration solution on a full-automatic potentiometric titrator; recording the dosage of the sodium hydroxide titration solution used in the titration as V1;
(12) blank sample assay
Making a blank sample under the same condition, and recording the dosage of the sodium hydroxide titration solution used in the titration as V2;
example 3
(1) Pretreatment of electrolytic product boron powder prepared in workshop
Sequentially grinding 20200112 batches of boron powder (the granularity is less than 40um), acid washing, water washing, alcohol washing and vacuum drying;
(2) weighing boron powder sample
Weighing an electrolysis product sample with the boron powder mass of 0.12g in a platinum crucible, and accurately measuring the sample to 0.0001 g; weighing 5 parallel samples in parallel;
(3) adding anhydrous sodium carbonate
2.0g of anhydrous sodium carbonate is added into the platinum crucible again, and the mixture is stirred uniformly by a glass rod;
(4) blank control
Adding 2.0g of anhydrous sodium carbonate into an empty platinum crucible, stirring by using a glass rod, and making a blank control;
(5) high temperature treatment
Covering a crucible cover, putting the platinum crucible into a muffle furnace, keeping the temperature at 850-900 ℃ for 20min, and cooling;
(6) dissolving the sample
Putting the cooled platinum crucible and the cooled cover into a 500ml beaker filled with dilute hydrochloric acid to dissolve a sample, washing the platinum crucible and the cooled cover for a plurality of times, then washing with hot water, and pouring the washing liquid back to the beaker;
(7) neutralizing excess hydrochloric acid
Adding 30ml of saturated sodium hydroxide solution, then neutralizing excess hydrochloric acid by using 0.1mol/L sodium hydroxide solution, and adjusting the pH value to 7.0;
(8) heating and boiling treatment
Then adding 5ml of 0.1mol/L hydrochloric acid, heating and boiling for three minutes to remove carbon dioxide completely, and then cooling in a water bath;
(9) neutralizing the hydrochloric acid again
Neutralizing the excessive hydrochloric acid by using 0.1mol/L sodium hydroxide solution, and adjusting the pH value to be 7.0;
(10) adding reagent for treatment
Adding 8.5g of mannitol, adding 0.8g of ethylene diamine tetraacetic acid, and uniformly stirring;
(11) titration of samples
Titrating the solution to an end point by using 0.1mol/L sodium hydroxide titration solution on a full-automatic potentiometric titrator; recording the dosage of the sodium hydroxide titration solution used in the titration as V1;
(12) blank sample assay
Making a blank sample under the same condition, and recording the dosage of the sodium hydroxide titration solution used in the titration as V2;
comparative example 1
(1) Weighing a reference boron powder (with the content of simple substance boron being 99%) sample purchased from the national Standard center
Weighing an electrolysis product sample with the reference substance boron powder mass of 0.15g in a platinum crucible, and accurately measuring the sample to 0.0001 g; weighing 5 parallel samples in parallel;
(2) adding anhydrous sodium carbonate
Adding 1.8g of anhydrous sodium carbonate into the platinum crucible again, and stirring uniformly by using a glass rod;
(3) blank control
Adding 1.8g of anhydrous sodium carbonate into an empty platinum crucible, stirring by using a glass rod, and making a blank control;
(4) high temperature treatment
Covering a crucible cover, putting the platinum crucible into a muffle furnace, keeping the temperature at 850-900 ℃ for 20min, and cooling;
(5) dissolving the sample
Putting the cooled platinum crucible and the cooled cover into a 500ml beaker filled with dilute hydrochloric acid to dissolve a sample, washing the platinum crucible and the cooled cover for a plurality of times, then washing with hot water, and pouring the washing liquid back to the beaker;
(6) neutralizing excess hydrochloric acid
Adding 30ml of saturated sodium hydroxide solution, then neutralizing excess hydrochloric acid by using 0.1mol/L sodium hydroxide solution, and adjusting the pH value to 7.0;
(7) heating and boiling treatment
Then adding 5ml of 0.1mol/L hydrochloric acid, heating and boiling for three minutes to remove carbon dioxide completely, and then cooling in a water bath;
(8) neutralizing the hydrochloric acid again
Neutralizing the excessive hydrochloric acid by using 0.1mol/L sodium hydroxide solution, and adjusting the pH value to be 7.0;
(9) adding reagent for treatment
Adding 12g of mannitol, adding 0.9g of ethylene diamine tetraacetic acid, and uniformly stirring;
(10) titration of samples
Titrating the solution to an end point by using 0.1mol/L sodium hydroxide titration solution on a full-automatic potentiometric titrator; recording the dosage of the sodium hydroxide titration solution used in the titration as V1;
(11) blank sample assay
Making a blank sample under the same condition, and recording the dosage of the sodium hydroxide titration solution used in the titration as V2;
the content of the simple substance boron in the boron powder is calculated by the following formula in the above embodiment and the comparative example:
b% -the mass percentage of the simple substance boron in the boron powder, the unit is;
c, the concentration of 0.1mol/L sodium hydroxide titration solution is mol/L;
v1-the volume of sodium hydroxide solution consumed by titrating a sample by a full-automatic potentiometric titrator, and the unit is ml;
v2-volume of sodium hydroxide solution consumed in the blank in ml;
m-total mass of the boron powder sample, unit is g;
0.01082-mass of boron expressed in grams equivalent to sodium hydroxide titration.
The method disclosed by the invention is used for measuring the boron content in 3 batches of boron powder produced in a certain workshop, and the results of measuring the boron content in the same batch of purchased reference boron powder by using the method disclosed by the invention and GB/T35871-.
TABLE 1
As can be seen from Table 1, the content of the three samples in a certain workshop is measured to be 98.323%, 98.485% and 98.414% by the method of the invention, the content of the measured reference substance is 99.020%, while the content of the reference substance measured by the method GB/T35871 2018 is 93.878%, because the content of the purchased reference substance is 99%, the result measured by the method of the invention is consistent with that of the reference substance, and the result measured by the method GB/T35871 2018 is greatly different from that of the reference substance; the standard deviation and the relative standard deviation of the two methods are different, which shows that the method of the invention has higher precision than the GB/T35871-. Thus, the method of the present invention was used to measure high-purity boron.
The experimental conditions listed in the content of the invention can be used for accurately measuring the content of the elemental boron in the prepared product boron powder, accurate detection data is reported, the production is effectively matched, the detection data of the detection method is accurate, and the precision is better than 0.01%. The method is accurate and reliable, and meets the technical index requirements of the project analysis.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (7)
1. A method for measuring the content of elemental boron in boron powder is characterized by comprising the following specific steps:
step one, pretreatment: sequentially carrying out grinding, acid washing, water washing, alcohol washing and vacuum drying treatment on boron powder;
step two, weighing a sample: weighing a boron powder sample with the mass of 0.1g in a crucible, accurately weighing the boron powder sample to 0.0001g, and weighing 5 samples in parallel;
step three, adding anhydrous sodium carbonate: 2.0g of anhydrous sodium carbonate is added into the crucible again, and the mixture is stirred uniformly;
step four, blank control: adding 2.0g of anhydrous sodium carbonate into an empty crucible, stirring, and performing blank control;
step five, high-temperature treatment: covering a crucible cover, putting the crucible into a muffle furnace, keeping the temperature of the muffle furnace at 850-900 ℃ for 20min, and cooling the crucible;
step six, dissolving a sample: placing the cooled crucible and the cooled crucible cover into a 500ml beaker filled with dilute hydrochloric acid to dissolve the sample, washing the crucible and the crucible cover for a plurality of times, then washing with hot water, and pouring the washing liquid back to the beaker;
step seven, neutralizing the excessive hydrochloric acid: adding 30ml of saturated sodium hydroxide solution, neutralizing excessive hydrochloric acid by using 0.1mol/L sodium hydroxide solution, and adjusting the pH to 7.0;
step eight, heating and boiling treatment: then adding 5ml of 0.1mol/L hydrochloric acid, heating and boiling for three minutes, and then cooling in a water bath;
step nine, neutralizing the hydrochloric acid again: neutralizing excessive hydrochloric acid with 0.1mol/L sodium hydroxide solution, and adjusting the pH to 7.0;
step ten, adding a reagent for treatment: adding 9g of mannitol, then adding 0.5g of ethylene diamine tetraacetic acid, and uniformly stirring;
step eleven, titrating a sample: titrating by using 0.1mol/L sodium hydroxide titration solution to an end point; recording the dosage of the sodium hydroxide titration solution used in the titration as V1;
step twelve, blank sample determination: making a blank sample under the same condition, and recording the dosage of the sodium hydroxide titration solution used in the titration as V2;
step thirteen, calculating the content: the content of the simple substance boron in the boron powder is calculated by the following formula:
b% -the mass percentage of the simple substance boron in the boron powder, the unit is;
c, the concentration of 0.1mol/L sodium hydroxide titration solution is mol/L;
v1-volume of sodium hydroxide solution consumed by titration of a sample in ml;
v2-volume of sodium hydroxide solution consumed in the blank in ml;
m-total mass of the boron powder sample, unit is g;
0.01082-mass of boron expressed in grams equivalent to sodium hydroxide titration.
2. The method for determining the content of elemental boron in boron powder according to claim 1, wherein the particle size after grinding in the first step is less than 100 μm.
3. The method for measuring the content of elemental boron in boron powder according to claim 1 or 2, characterized in that in the third step and the fifth step, a dried glass rod is used for stirring.
4. The method for determining the content of elemental boron in boron powder according to claim 1, wherein the method for preparing the dilute hydrochloric acid in the sixth step is concentrated hydrochloric acid: the volume ratio of water is 1: 1, mixing.
5. The method according to claim 1, wherein in step eleven, an automatic titrator is used for titrating to an end point.
6. The method according to claim 5, wherein in the eleventh step, the signal collected by the auto-titrator in the titration process is 0.1mV, and the minimum feed of the auto-titrator is 0.0025 ml.
7. The method for determining the content of elemental boron in boron powder according to claim 1, wherein the determination of the content of elemental boron is performed in parallel 2-3 times, and an average value is taken.
Priority Applications (1)
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| CN112557449A (en) * | 2020-12-11 | 2021-03-26 | 湖北三江航天江河化工科技有限公司 | Method for measuring boron content in bonding agent |
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