This standard specifies the technical requirements, test methods, inspection rules, packaging, marking, transportation, storage and safety requirements of boron trifluoride products. This standard applies to boron trifluoride produced by thermal decomposition using sodium fluoroborate as raw material. It is mainly used for ion implantation and doping in the production of semiconductor devices and integrated circuits. GB/T 14603-1993 Boron trifluoride gas for electronic industry GB/T14603-1993 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Gases for electronic industry-Boron trifluoride
Gases for electronic industry-Boron trifluoride1Subject content and scope of application
GB/T 14603-93
This standard specifies the technical requirements, test methods, inspection rules, packaging, marking, transportation, storage and safety requirements for boron trifluoride products. This standard applies to boron trifluoride produced by thermal decomposition with sodium fluoroborate as raw material. It is mainly used for ion implantation and doping in the production of semiconductor devices and integrated circuits.
Molecular formula: BF:
Relative molecular mass: 67.805 (according to the international relative atomic mass in 1989) 2 Reference standards
Dangerous goods packaging mark
GB4844
GB4845
GB5274
Ammonia test method
Preparation of mixed gas for gas analysis calibration Weighing method
GB5275
Preparation of mixed gas for gas analysis calibration Permeation method
GB7144 Gas cylinder color marking
GB11640 Aluminum alloy seamless gas cylinder
3 Technical requirements
The quality of boron trifluoride shall meet the technical requirements in the following table. Item
Purity of boron trifluoride, 10-2
Air content, 10~6
Sulfur dioxide content, 106
Silicon tetrafluoride content, 10-5
Sulfate content, 10-6
Note: ①The purity and content in the table are molar fractions. ②The quality assurance period is one year.
4 Test method
4.1 Purity of boron trifluoride
Approved by the State Administration of Technical Supervision on August 26, 1993Superior product
First-class product
Qualified product
Implemented on July 1, 1994
Expressed in molar fraction, calculated according to formula (1). GB/T14603—93
100(+2+ +)× 10-
Wherein: r-
purity of boron trifluoride, 10-2;
x1——air content, 10-,
-sulfur dioxide content, 10-6;
silicon tetrafluoride content, 10-6;
sulfate content, 10-6.
4.2 Determination of air and sulfur dioxide content
4.2.1 Method
Thermal conductivity chromatography is used for determination.
4.2.2 Instrument
Gas chromatograph. The instrument is required to detect the minimum amount of air (oxygen and nitrogen) and sulfur dioxide by about one order of magnitude lower than the content of the sample to be tested. The other technical indicators of the chromatograph should meet the requirements of the instrument manual. 4.2.3 Operation reference conditions
Detector: thermal conductivity cell, cold resistance about 1200, thermal conductivity cell temperature: about 80℃;
Thermal conductivity cell bridge current: about 180mA;
Carrier gas: nitrogen, which should comply with the provisions of GB4844 for first-grade pure nitrogen; carrier gas flow rate: about 30mL/min
Injection volume: 1～3mL,
Chromatographic column temperature: about 90℃;
Chromatographic column: a polytetrafluoroethylene column with a length of 1m and an inner diameter of 2.5mm, and the column is tightly packed with porapakQ of 0.2~～0.15mm; polytetrafluoroethylene tubes are used for sampling and injection pipelines. 4.2.4
Measurement steps
4.2.4.1 Determination
Connect the sample gas to the instrument through the needle valve and the connecting pipe. After sufficient replacement and obtaining a representative sample, inject it into the chromatograph. Record the elution curve of each component to be measured and measure the peak area of ​​each component respectively. Repeat the injection twice. When the relative deviation is not greater than 10%, take the average value A;.
4.2.4.2 Calibration
Prepare a standard air mixture with ammonia as the base gas according to GB5274 or Appendix C of GB4845, and prepare a standard sulfur dioxide mixture with nitrogen as the base gas according to GB5275. The lower limit of the air and sulfur dioxide content in the standard mixture is not less than 50% and the upper limit is not more than 200% compared with the air and sulfur dioxide content in the sample gas. Directly inject the sample under the measurement conditions, and record and measure the peak areas of air and sulfur dioxide in the standard mixture. Repeat the injection twice. When the relative deviation is no more than 10%, take the average value A. 4.2.5 Calculation of results
The content of air and sulfur dioxide in boron trifluoride (mol/mol) is calculated according to formula (2): =
Wherein: —-the content of the measured component in the sample gas, 10-,, the content of the measured component in the standard mixed gas, 10-, A
GB/T14603-93
A-the peak area of ​​the measured component in the sample gas, mm2; A-the peak area of ​​the measured component in the standard mixed gas, mm2. 4.3 Determination of silicon tetrafluoride content
4.3.1 Method and principle
The content is determined by spectrophotometry.
BF: and SiF: react with water in the following manner: BF; + 3H,O = H,BO: + 3HF
3SiF4 + 4H,0 - HSi04 + 2H,SiF H,SiF, + 4H,0H,SiO, + 6HF
Under appropriate acidity, silicate reacts with molybdic acid to form a yellow silicomolybdic acid complex, which is reduced to silicomolybdic blue with ascorbic acid, and its color depth is proportional to the content. Spectrophotometric determination is carried out under the selected conditions 4.3.2 Instruments
Spectrophotometer is used.
4.3.3 Reagents and solutions
4.3.3.1 Sulfuric acid (GB625) solution: high-grade pure. c (H,SO.) m0.5mol/L and 10mol/L. 4.3.3.2 Sodium carbonate (GB639): high-grade pure. 4.3.3.3 Silicon dioxide: spectrally pure.
4.3.3.4 Ammonia (GB631): 1+1 aqueous solution. 4.3.3.5 Ascorbic acid: 0.01 g/mL aqueous solution. 4.3.3.6 Ammonium molybdate (GB657) solution: 0.15 g/mL aqueous solution. 4.3.3.7 p-Nitrophenol solution: 0.01 g/mL aqueous solution. 4.3.3.8 Deionized water.
4.3.4 Determination conditions
Wavelength: 650nm,
Cuvette thickness: 1cm,
Silicon molybdenum yellow color developing acidity: pH 1.1~1.4. 4.3.5 Drawing of standard curve
4.3.5.1 Preparation of series of silicon standard solutions
Weigh 5g of sodium carbonate and 0.2140g of silicon dioxide dried to constant weight at 900℃ in a platinum crucible, melt at 900℃ for 30min, dissolve in deionized water after cooling, transfer to a 1L volumetric flask, dilute to the scale and transfer to a plastic bottle for later use. The silicon concentration of this solution is 0.1 mg/mL.
Accurately measure 0.00, 0.50, 1.00, 1.50, 2.00, 2.50, 3.00, 3.50, 4.00, and 4.50 mL of silicon standard solution and add them to a series of 100 mL volumetric flasks respectively, add two drops of 0.01 g/mL p-nitrophenol, adjust to slightly yellow with 1+1 ammonia water, use a burette to add 6. mL of 0.5 mol/L sulfuric acid (4.3.3.1) and immediately add 3 mL of ammonium chloride solution (4.3.3.6), add 8 mL of 10 mol/L sulfuric acid (4.3.3.1) after color development for 10 minutes, and finally add 6 mL of ascorbic acid (4.3.3.5) and color develop for 30 minutes. 4.3.5.2 Determination of absorbance
According to the spectrophotometer instruction manual, use a colorimetric cell with a wavelength of 650nm and a thickness of 1cm to determine the absorbance of the series of standard solutions after color development.
4.3.5.3 Drawing of standard curve
Use the absorbance of the series of standard solutions as the ordinate and the mass of silicon as the abscissa to draw the standard curve. 4.3.5.4 Sampling
Put 40mL of deionized water in a 50mL stainless steel sampler with a sealing thread, and connect it to the gas cylinder containing boron trifluoride through the high-pressure fine-adjustment valve and pressure gauge as shown in the figure below is
.
GB/T 14603—93
Sampling device diagram
1-gas cylinder filled with BF:; 2-high pressure fine-adjusting valve; 3-pressure gauge; 4-mechanical vacuum pump; 5-sampler; 6-cold bath; 7-on/off valve
Put a 10℃ ice salt water cold bath outside the sampler. Use a mechanical vacuum pump to pump to about -0.1MPa, close valve 7, then open the valve of the boron trifluoride gas cylinder and slowly introduce boron trifluoride gas, and absorb it with deionized water for about 30 minutes. The absorption rate is controlled by a pressure gauge and a high-pressure fine-tuning valve. After the absorption is completed, close the valve of the gas cylinder and measure the total volume of the absorption liquid (V). Transfer the absorption liquid into a polytetrafluoroethylene beaker as the sample solution. The sample volume (m) is the difference between the weighing of the absorption liquid before and after absorption. 4.3.6 Determination
Accurately measure 20.00mL of the sample solution in a 100mL volumetric flask, add two drops of 0.01g/mL p-nitrophenol, adjust to slightly yellow with 1+1 ammonia water, add 6mL of 0.5mol/L sulfuric acid with a burette and immediately add 3mL of 0.15g/mL ammonium molybdate solution, add 8mL of 10mol/L sulfuric acid after color development for 10min, and finally add 6mL of 0.01g/mL ascorbic acid to color for 30min. Determine the absorbance. 4.3.7 Calculation of results
The amount of silicon is obtained from the standard curve by the measured absorbance of the sample solution, and the content of silicon tetrafluoride is calculated according to formula (3). Vim
2 = 2 414 Vm
Wherein: 31
The content of SiF in the sample gas, 10-' (mol/mol), the total volume of the absorption solution, mL;
The mass of silicon obtained from the standard curve, mg; V2—the sampling volume of the sample solution during colorimetry, mL; m-
2 414—
-The mass of the sample in the absorption solution, g,
Conversion coefficient.
The arithmetic mean of two parallel determinations is taken as the determination result. 4.4 Determination of sulfate content
4.4.1 Method and principle
The sulfate content is determined by turbidimetry. In an acidic solution, in the presence of a stabilizer, sulfate and barium ions form a uniform barium sulfate suspension, the turbidity of which is proportional to the sulfate ion concentration, and this is used to determine trace amounts of sulfate. 4.4.2 Instruments
Same as 4.3.2.
4.4.3 Reagents
4.4.3.1 Sodium chloride (GB1266);
4.4.3.2 Potassium sulfate (HG3-920);
4.4.3.3 Chloride (GB652);
4.4.3.4 Hydrochloric acid (GB622);
4.4.3.5 Anhydrous ethanol (GB678);
4.4.3.6 Propylene glycol (GB 687);
4.4.3.7 Deionized water.
4.4.4 Solution
GB/T 14603—93
4.4.4.1 Stabilizing solution: Take 15g sodium chloride, add 60mL deionized water, 6mL hydrochloric acid, 10mL propylene glycol, 20mL ethanol, and mix well;
4.4.4.2 Sulfate standard solution: Accurately weigh 0.08710g potassium sulfate, dissolve it in a 1L volumetric flask with deionized water and dilute to the scale. The sulfate concentration of this solution is 5×10-4mol/L; 4.4.4.3 Barium chloride solution: Dissolve 40g barium chloride in deionized water and dilute to 100mL. The concentration of barium chloride in this solution is 400g/1.
4.4.5 Drawing the standard curve
Add 0.00, 1.00, 2.00, 3.00, 4.00, 5.00, 6.00mL of sulfate standard solution to a series of 25mL volumetric flasks, add 2.5mL of stabilizing solution and 5mL of barium chloride solution and dilute to the scale, shake for 1min, and let stand for 5min. Use an absorption cell with a wavelength of 420nm and a thickness of 2cm to measure the absorbance of the series of standard solutions. Use the absorbance as the ordinate and the amount of sulfate (mol) as the abscissa to draw the standard curve. 4.4.6 Sampling
Same as 4.3.5.2.
4.4.7 Determination
Accurately pipette 10.00mL of sample solution into a 25mL volumetric flask, add 2.5mL of stabilizing solution and 5mL of barium chloride solution and dilute to the scale. Shake for 1min and let stand for 5min. The absorbance was measured with a wavelength of 420 nm and a 2 cm thick absorption cell. 4.4.8 Calculation of results
According to the measured absorbance of the sample solution, the amount of sulfate was obtained from the standard curve, and the content of sulfate was calculated according to formula (4). x = 67.805 V.m2
?×10%
Wherein: r.—the content of sulfate in the sample gas, 10-6 (mol/mol); V3
the total volume of the absorption solution, ml,
n-—the amount of sulfate obtained from the standard curve, mol; V,—the sampling volume of the sample solution during turbidimetric determination, mL; m2-the mass of the sample in the absorption solution, g;
67.805-the molar mass of boron trifluoride [M(BF,)], g/mol. The arithmetic mean of two parallel measurements was taken as the measurement result. 5 Inspection rules
5.1 The products shall be inspected by the quality supervision department of the manufacturer to ensure that they meet the requirements of this standard. 5.2 Boron trifluoride shall be inspected bottle by bottle. If one of the indicators in the inspection result does not meet the requirements of this standard, the bottle shall be unqualified. s
*（4)
5.3 Users have the right to accept in accordance with the provisions of this standard. GB/T14603-93
5.4 When the supply and demand parties have objections to the quality of the product, they may jointly accept or apply for arbitration. 6 Marking, packaging, transportation and storage
6.1 The use, transportation and storage of gas cylinders shall comply with the relevant provisions of the "Gas Cylinder Safety Supervision Regulations" and the "Dangerous Goods Transportation Regulations". 6.2 The packaging marking shall comply with the provisions of GB1906.3 Gas cylinders filled with boron trifluoride shall comply with the provisions of GB11640. The color marking of gas cylinders shall comply with the provisions of GB7144. 6.4 The valve and bottle neck threaded connection of the gas cylinder filled with boron trifluoride shall not leak. Safety helmets must be worn. 6.5 Gas cylinders (including return gas cylinders) should be heated and evacuated before filling. 6.6 The filling amount of boron trifluoride in the gas cylinder is measured by actual weight, and the filling pressure is 12.0 ± 0.5 MPa at 20°C. 6.7 Gas cylinders filled with boron trifluoride should be stored in a warehouse with a shed and away from heat sources. The ambient temperature should always be kept below 60°C. Gas cylinders in use should be placed in a room with forced ventilation.
6.8 The factory products must be accompanied by a quality analysis result report and a product certificate. The certificate should include: a.
Manufacturer name;
Product name and grade;
c. Gas cylinder number;
Filling quantity (kg), pressure (MPa); d.
This standard code.
7 Safety requirements
7.1 Boron trifluoride is a colorless gas that emits white smoke in humid air. It decomposes with water and has a pungent smell. It is non-flammable, highly toxic, and the wet gas is highly corrosive. When using it, you should wear leather gloves, protective glasses and face protection to prevent contact with boron trifluoride. 7.2 Positive pressure respirators or face respirators with air pipelines should be available near the workplace. 7.3 It is not allowed to transfer gas from one cylinder to another at will, and the cylinders cannot be pressurized at will. 7.4 The maximum allowable content of boron trifluoride in the air of the workplace is 3mg/m2. When discharging boron trifluoride, alkaline aqueous solutions such as caustic potash must be used for absorption and neutralization, and the absorbent and neutralizer must be effective and reliable. Additional notes:
This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Southwest Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Guangming Chemical Research Institute of the Ministry of Chemical Industry. The main drafter of this standard is Li Jingxing.7 Calculation of results
The amount of silicon is obtained from the standard curve by the measured absorbance of the sample solution, and the content of silicon tetrafluoride is calculated according to formula (3). Vim
2 = 2 414 Vm
Wherein: 31
The content of SiF in the sample gas, 10-' (mol/mol), the total volume of the absorption solution, mL;
The mass of silicon obtained from the standard curve, mg; V2—the sampling volume of the sample solution during colorimetry, mL; m-
2 414—
-The mass of the sample in the absorption solution, g,
Conversion coefficient.
The arithmetic mean of two parallel measurements is taken as the determination result. 4.4 Determination of sulfate content
4.4.1 Method and principle
The sulfate content is determined by turbidimetry. In an acidic solution, in the presence of a stabilizer, sulfate and barium ions form a uniform barium sulfate suspension, the turbidity of which is proportional to the sulfate ion concentration, and this is used to determine trace amounts of sulfate. 4.4.2 Instruments
Same as 4.3.2.
4.4.3 Reagents
4.4.3.1 Sodium chloride (GB1266);
4.4.3.2 Potassium sulfate (HG3-920);
4.4.3.3 Chloride (GB652);
4.4.3.4 Hydrochloric acid (GB622);
4.4.3.5 Anhydrous ethanol (GB678);
4.4.3.6 Propylene glycol (GB 687);
4.4.3.7 Deionized water.
4.4.4 Solution
GB/T 14603—93
4.4.4.1 Stabilizing solution: Take 15g sodium chloride, add 60mL deionized water, 6mL hydrochloric acid, 10mL propylene glycol, 20mL ethanol, and mix well;
4.4.4.2 Sulfate standard solution: Accurately weigh 0.08710g potassium sulfate, dissolve it in a 1L volumetric flask with deionized water and dilute to the scale. The sulfate concentration of this solution is 5×10-4mol/L; 4.4.4.3 Barium chloride solution: Dissolve 40g barium chloride in deionized water and dilute to 100mL. The concentration of barium chloride in this solution is 400g/1.
4.4.5 Drawing the standard curve
Add 0.00, 1.00, 2.00, 3.00, 4.00, 5.00, 6.00mL of sulfate standard solution to a series of 25mL volumetric flasks, add 2.5mL of stabilizing solution and 5mL of barium chloride solution and dilute to the scale, shake for 1min, and let stand for 5min. Use an absorption cell with a wavelength of 420nm and a thickness of 2cm to measure the absorbance of the series of standard solutions. Use the absorbance as the ordinate and the amount of sulfate (mol) as the abscissa to draw the standard curve. 4.4.6 Sampling
Same as 4.3.5.2.
4.4.7 Determination
Accurately pipette 10.00mL of sample solution into a 25mL volumetric flask, add 2.5mL of stabilizing solution and 5mL of barium chloride solution and dilute to the scale. Shake for 1min and let stand for 5min. The absorbance was measured with a wavelength of 420 nm and a 2 cm thick absorption cell. 4.4.8 Calculation of results
According to the measured absorbance of the sample solution, the amount of sulfate was obtained from the standard curve, and the content of sulfate was calculated according to formula (4). x = 67.805 V.m2
?×10%
Wherein: r.—the content of sulfate in the sample gas, 10-6 (mol/mol); V3
the total volume of the absorption solution, ml,
n-—the amount of sulfate obtained from the standard curve, mol; V,—the sampling volume of the sample solution during turbidimetric determination, mL; m2-the mass of the sample in the absorption solution, g;
67.805-the molar mass of boron trifluoride [M(BF,)], g/mol. The arithmetic mean of two parallel measurements was taken as the measurement result. 5 Inspection rules
5.1 The products shall be inspected by the quality supervision department of the manufacturer to ensure that they meet the requirements of this standard. 5.2 Boron trifluoride shall be inspected bottle by bottle. If one of the indicators in the inspection result does not meet the requirements of this standard, the bottle shall be unqualified. s
*（4)
5.3 Users have the right to accept in accordance with the provisions of this standard. GB/T14603-93
5.4 When the supply and demand parties have objections to the quality of the product, they may jointly accept or apply for arbitration. 6 Marking, packaging, transportation and storage
6.1 The use, transportation and storage of gas cylinders shall comply with the relevant provisions of the "Gas Cylinder Safety Supervision Regulations" and the "Dangerous Goods Transportation Regulations". 6.2 The packaging marking shall comply with the provisions of GB1906.3 Gas cylinders filled with boron trifluoride shall comply with the provisions of GB11640. The color marking of gas cylinders shall comply with the provisions of GB7144. 6.4 The valve and bottle neck threaded connection of the gas cylinder filled with boron trifluoride shall not leak. Safety helmets must be worn. 6.5 Gas cylinders (including return gas cylinders) should be heated and evacuated before filling. 6.6 The filling amount of boron trifluoride in the gas cylinder is measured by actual weight, and the filling pressure is 12.0 ± 0.5 MPa at 20°C. 6.7 Gas cylinders filled with boron trifluoride should be stored in a warehouse with a shed and away from heat sources. The ambient temperature should always be kept below 60°C. Gas cylinders in use should be placed in a room with forced ventilation.
6.8 The factory products must be accompanied by a quality analysis result report and a product certificate. The certificate should include: a.
Manufacturer name;
Product name and grade;
c. Gas cylinder number;
Filling quantity (kg), pressure (MPa); d.
This standard code.
7 Safety requirements
7.1 Boron trifluoride is a colorless gas that emits white smoke in humid air. It decomposes with water and has a pungent smell. It is non-flammable, highly toxic, and the wet gas is highly corrosive. When using it, you should wear leather gloves, protective glasses and face protection to prevent contact with boron trifluoride. 7.2 Positive pressure respirators or face respirators with air pipelines should be available near the workplace. 7.3 It is not allowed to transfer gas from one cylinder to another at will, and the cylinders cannot be pressurized at will. 7.4 The maximum allowable content of boron trifluoride in the air of the workplace is 3mg/m2. When discharging boron trifluoride, alkaline aqueous solutions such as caustic potash must be used for absorption and neutralization, and the absorbent and neutralizer must be effective and reliable. Additional notes:
This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Southwest Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Guangming Chemical Research Institute of the Ministry of Chemical Industry. The main drafter of this standard is Li Jingxing.7 Calculation of results
The amount of silicon is obtained from the standard curve by the measured absorbance of the sample solution, and the content of silicon tetrafluoride is calculated according to formula (3). Vim
2 = 2 414 Vm
Wherein: 31
The content of SiF in the sample gas, 10-' (mol/mol), the total volume of the absorption solution, mL;
The mass of silicon obtained from the standard curve, mg; V2—the sampling volume of the sample solution during colorimetry, mL; m-
2 414—
-The mass of the sample in the absorption solution, g,
Conversion coefficient.
The arithmetic mean of two parallel measurements is taken as the determination result. 4.4 Determination of sulfate content
4.4.1 Method and principle
The sulfate content is determined by turbidimetry. In an acidic solution, in the presence of a stabilizer, sulfate and barium ions form a uniform barium sulfate suspension, the turbidity of which is proportional to the sulfate ion concentration, and this is used to determine trace amounts of sulfate. 4.4.2 Instruments
Same as 4.3.2.
4.4.3 Reagents
4.4.3.1 Sodium chloride (GB1266);
4.4.3.2 Potassium sulfate (HG3-920);
4.4.3.3 Chloride (GB652);
4.4.3.4 Hydrochloric acid (GB622);
4.4.3.5 Anhydrous ethanol (GB678);
4.4.3.6 Propylene glycol (GB 687);
4.4.3.7 Deionized water.
4.4.4 Solution
GB/T 14603—93
4.4.4.1 Stabilizing solution: Take 15g sodium chloride, add 60mL deionized water, 6mL hydrochloric acid, 10mL propylene glycol, 20mL ethanol, and mix well;
4.4.4.2 Sulfate standard solution: Accurately weigh 0.08710g potassium sulfate, dissolve it in a 1L volumetric flask with deionized water and dilute to the scale. The sulfate concentration of this solution is 5×10-4mol/L; 4.4.4.3 Barium chloride solution: Dissolve 40g barium chloride in deionized water and dilute to 100mL. The concentration of barium chloride in this solution is 400g/1.
4.4.5 Drawing the standard curve
Add 0.00, 1.00, 2.00, 3.00, 4.00, 5.00, 6.00mL of sulfate standard solution to a series of 25mL volumetric flasks, add 2.5mL of stabilizing solution and 5mL of barium chloride solution and dilute to the scale, shake for 1min, and let stand for 5min. Use an absorption cell with a wavelength of 420nm and a thickness of 2cm to measure the absorbance of the series of standard solutions. Use the absorbance as the ordinate and the amount of sulfate (mol) as the abscissa to draw the standard curve. 4.4.6 Sampling
Same as 4.3.5.2.
4.4.7 Determination
Accurately pipette 10.00mL of sample solution into a 25mL volumetric flask, add 2.5mL of stabilizing solution and 5mL of barium chloride solution and dilute to the scale. Shake for 1min and let stand for 5min. The absorbance was measured with a wavelength of 420 nm and a 2 cm thick absorption cell. 4.4.8 Calculation of results
According to the measured absorbance of the sample solution, the amount of sulfate was obtained from the standard curve, and the content of sulfate was calculated according to formula (4). x = 67.805 V.m2
?×10%
Wherein: r.—the content of sulfate in the sample gas, 10-6 (mol/mol); V3
the total volume of the absorption solution, ml,
n-—the amount of sulfate obtained from the standard curve, mol; V,—the sampling volume of the sample solution during turbidimetric determination, mL; m2-the mass of the sample in the absorption solution, g;
67.805-the molar mass of boron trifluoride [M(BF,)], g/mol. The arithmetic mean of two parallel measurements was taken as the measurement result. 5 Inspection rules
5.1 The products shall be inspected by the quality supervision department of the manufacturer to ensure that they meet the requirements of this standard. 5.2 Boron trifluoride shall be inspected bottle by bottle. If one of the indicators in the inspection result does not meet the requirements of this standard, the bottle shall be unqualified. s
*（4)
5.3 Users have the right to accept in accordance with the provisions of this standard. GB/T14603-93
5.4 When the supply and demand parties have objections to the quality of the product, they may jointly accept or apply for arbitration. 6 Marking, packaging, transportation and storage
6.1 The use, transportation and storage of gas cylinders shall comply with the relevant provisions of the "Gas Cylinder Safety Supervision Regulations" and the "Dangerous Goods Transportation Regulations". 6.2 The packaging marking shall comply with the provisions of GB1906.3 Gas cylinders filled with boron trifluoride shall comply with the provisions of GB11640. The color marking of gas cylinders shall comply with the provisions of GB7144. 6.4 The valve and bottle neck threaded connection of the gas cylinder filled with boron trifluoride shall not leak. Safety helmets must be worn. 6.5 Gas cylinders (including return gas cylinders) should be heated and evacuated before filling. 6.6 The filling amount of boron trifluoride in the gas cylinder is measured by actual weight, and the filling pressure is 12.0 ± 0.5 MPa at 20°C. 6.7 Gas cylinders filled with boron trifluoride should be stored in a warehouse with a shed and away from heat sources. The ambient temperature should always be kept below 60°C. Gas cylinders in use should be placed in a room with forced ventilation.
6.8 The factory products must be accompanied by a quality analysis result report and a product certificate. The certificate should include: a.
Manufacturer name;
Product name and grade;
c. Gas cylinder number;
Filling quantity (kg), pressure (MPa); d.
This standard code.
7 Safety requirements
7.1 Boron trifluoride is a colorless gas that emits white smoke in humid air. It decomposes with water and has a pungent smell. It is non-flammable, highly toxic, and the wet gas is highly corrosive. When using it, you should wear leather gloves, protective glasses and face protection to prevent contact with boron trifluoride. 7.2 Positive pressure respirators or face respirators with air pipelines should be available near the workplace. 7.3 It is not allowed to transfer gas from one cylinder to another at will, and the cylinders cannot be pressurized at will. 7.4 The maximum allowable content of boron trifluoride in the air of the workplace is 3mg/m2. When discharging boron trifluoride, alkaline aqueous solutions such as caustic potash must be used for absorption and neutralization, and the absorbent and neutralizer must be effective and reliable. Additional notes:
This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Southwest Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Guangming Chemical Research Institute of the Ministry of Chemical Industry. The main drafter of this standard is Li Jingxing.3.5.2.
4.4.7 Determination
Accurately pipette 10.00mL of sample solution into a 25mL volumetric flask, add 2.5mL of stabilizing solution and 5mL of barium chloride solution and dilute to the mark. Shake for 1min and let stand for 5min. Measure the absorbance with a wavelength of 420nm and a 2cm thick absorption cell. 4.4.8 Calculation of resultsWww.bzxZ.net
According to the measured absorbance of the sample solution, the amount of sulfate is obtained from the standard curve and the content of sulfate is calculated according to formula (4). x = 67. 805 V.m2
?×10%
Wherein: r.—Sulfate content in sample gas, 10-6 (mol/mol); V3
Total volume of absorption solution, ml,
n-—Amount of sulfate found from the standard curve, mol; V,—Sampling volume of sample solution during turbidimetric determination, mL; m2-Mass of sample in absorption solution, g;
67.805-Molar mass of boron trifluoride [M(BF,)], g/mol. The arithmetic mean of two parallel determinations is the determination result. 5 Inspection rules
5.1 Ex-factory products shall be inspected by the quality supervision department of the manufacturer to ensure that the ex-factory products meet the requirements of this standard. 5.2 Boron trifluoride shall be inspected bottle by bottle. If one of the indicators in the inspection result does not meet the requirements of this standard, the bottle of product shall be unqualified. s
*（4)
5.3 The user has the right to inspect and accept in accordance with the provisions of this standard. GB/T14603-93
5.4 When the supply and demand parties have objections to the product quality, they may jointly inspect and accept, or apply for arbitration. 6 Marking, packaging, transportation and storage
6.1 The use, transportation and storage of gas cylinders shall comply with the relevant provisions of the "Gas Cylinder Safety Supervision Regulations" and the "Dangerous Goods Transportation Regulations". 6.2 The packaging markings shall comply with the provisions of GB1906.3 Gas cylinders filled with boron trifluoride shall comply with the provisions of GB11640. The color markings of gas cylinders shall comply with the provisions of GB7144. 6.4 The valve and bottleneck threaded connection of gas cylinders filled with boron trifluoride shall not leak. Safety helmets must be worn6.5 Gas cylinders (including return gas cylinders) should be heated and evacuated before filling. 6.6 The filling amount of boron trifluoride in the gas cylinder is measured by actual weight. When the filling pressure is 20℃, it is 12.0±0.5MPa. 6.7 Gas cylinders containing boron trifluoride should be stored in a warehouse with a shed and away from heat sources. The ambient temperature should always be kept below 60℃. Gas cylinders in use should be placed in a room with forced ventilation.
6.8 The products leaving the factory must be accompanied by a quality analysis result report and a product certificate. The content of the certificate should include: a.
Manufacturer name;
Product name and grade;
c. Gas cylinder number;
Filling quantity (kg), pressure (MPa); d.
Code of this standard.
7 Safety requirements
7.1 Boron trifluoride is a colorless gas that emits white smoke in humid air. It decomposes with water and has a pungent smell. It is non-flammable, highly toxic, and the wet gas is highly corrosive. When using it, you should wear leather gloves, protective glasses and face protection to prevent contact with boron trifluoride. 7.2 Positive pressure respirators or face respirators with air pipelines should be available near the workplace. 7.3 It is not allowed to transfer gas from one cylinder to another at will, and the cylinders cannot be pressurized at will. 7.4 The maximum allowable content of boron trifluoride in the air of the workplace is 3mg/m2. When discharging boron trifluoride, alkaline aqueous solutions such as caustic potash must be used for absorption and neutralization, and the absorbent and neutralizer must be effective and reliable. Additional notes:
This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Southwest Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Guangming Chemical Research Institute of the Ministry of Chemical Industry. The main drafter of this standard is Li Jingxing.3.5.2.
4.4.7 Determination
Accurately pipette 10.00mL of sample solution into a 25mL volumetric flask, add 2.5mL of stabilizing solution and 5mL of barium chloride solution and dilute to the mark. Shake for 1min and let stand for 5min. Measure the absorbance with a wavelength of 420nm and a 2cm thick absorption cell. 4.4.8 Calculation of results
According to the measured absorbance of the sample solution, the amount of sulfate is obtained from the standard curve and the content of sulfate is calculated according to formula (4). x = 67. 805 V.m2
?×10%
Wherein: r.—Sulfate content in sample gas, 10-6 (mol/mol); V3
Total volume of absorption solution, ml,
n-—Amount of sulfate found from the standard curve, mol; V,—Sampling volume of sample solution during turbidimetric determination, mL; m2-Mass of sample in absorption solution, g;
67.805-Molar mass of boron trifluoride [M(BF,)], g/mol. The arithmetic mean of two parallel determinations is the determination result. 5 Inspection rules
5.1 Ex-factory products shall be inspected by the quality supervision department of the manufacturer to ensure that the ex-factory products meet the requirements of this standard. 5.2 Boron trifluoride shall be inspected bottle by bottle. If one of the indicators in the inspection result does not meet the requirements of this standard, the bottle of product shall be unqualified. s
*（4)
5.3 The user has the right to inspect and accept in accordance with the provisions of this standard. GB/T14603-93
5.4 When the supply and demand parties have objections to the product quality, they may jointly inspect and accept, or apply for arbitration. 6 Marking, packaging, transportation and storage
6.1 The use, transportation and storage of gas cylinders shall comply with the relevant provisions of the "Gas Cylinder Safety Supervision Regulations" and the "Dangerous Goods Transportation Regulations". 6.2 The packaging markings shall comply with the provisions of GB1906.3 Gas cylinders filled with boron trifluoride shall comply with the provisions of GB11640. The color markings of gas cylinders shall comply with the provisions of GB7144. 6.4 The valve and bottleneck threaded connection of gas cylinders filled with boron trifluoride shall not leak. Safety helmets must be worn6.5 Gas cylinders (including return gas cylinders) should be heated and evacuated before filling. 6.6 The filling amount of boron trifluoride in the gas cylinder is measured by actual weight. When the filling pressure is 20℃, it is 12.0±0.5MPa. 6.7 Gas cylinders containing boron trifluoride should be stored in a warehouse with a shed and away from heat sources. The ambient temperature should always be kept below 60℃. Gas cylinders in use should be placed in a room with forced ventilation.
6.8 The products leaving the factory must be accompanied by a quality analysis result report and a product certificate. The content of the certificate should include: a.
Manufacturer name;
Product name and grade;
c. Gas cylinder number;
Filling quantity (kg), pressure (MPa); d.
Code of this standard.
7 Safety requirements
7.1 Boron trifluoride is a colorless gas that emits white smoke in humid air. It decomposes with water and has a pungent smell. It is non-flammable, highly toxic, and the wet gas is highly corrosive. When using it, you should wear leather gloves, protective glasses and face protection to prevent contact with boron trifluoride. 7.2 Positive pressure respirators or face respirators with air pipelines should be available near the workplace. 7.3 It is not allowed to transfer gas from one cylinder to another at will, and the cylinders cannot be pressurized at will. 7.4 The maximum allowable content of boron trifluoride in the air of the workplace is 3mg/m2. When discharging boron trifluoride, alkaline aqueous solutions such as caustic potash must be used for absorption and neutralization, and the absorbent and neutralizer must be effective and reliable. Additional notes:
This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Southwest Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Guangming Chemical Research Institute of the Ministry of Chemical Industry. The main drafter of this standard is Li Jingxing.
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