Some standard content:
National Standard of the People's Republic of China
Gas for electronic industry
Phosphine
1 Subject content and scope of application
GB/T14851-93
This standard specifies the technical requirements, test methods, inspection rules, safety requirements, packaging, marking, transportation and storage of phosphine products. This standard applies to phosphine products obtained and refined by methods such as thermal decomposition of phosphorous acid, hydrolysis of phosphide, reaction of elemental phosphorus with water or alkali. It is mainly used for epitaxy, ion implantation and doping in the production of semiconductor devices and integrated circuits. Phosphine is a highly toxic, flammable, colorless gas with a rotten fish smell, which can spontaneously combust at high concentrations in the air. Molecular formula: PH3
Relative molecular mass: 33.9975 (according to the international atomic weight in 1989) 2 Reference standards
GB4845
GB5099
GB5274
Dangerous goods packaging mark
Nitrogen inspection method
Steel seamless gas cylinder
Preparation and weighing method of mixed gas for gas analysis calibration GB5832.1
GB7144
GB7445
GB8980
GB9721
3 Technical requirements
Determination of trace moisture in gas, electrolysis method Gas cylinder color marking
High purity nitrogen
General rules for chemical reagent molecular absorption spectrophotometry (ultraviolet and visible light part) The quality of phosphine shall meet the technical requirements of Table 1. Table 1 Technical requirements
Phosphine purity, 10-2
Arsenic content, 106
Carbon dioxide content, 10-6
Hydrogen content, 10~6
Nitrogen content, 10.
Oxygen content, 106
Total diameter content, 10s
Water content, 10
Approved by the State Administration of Technical Supervision on December 30, 1993 Electronic grade
Light-emitting diode grade
Implemented on October 1, 1994
GB/T 14851-
Note: ①This standard does not include the technical requirements for particles and heavy metals. ②Purity and content are both volume fractions.
③The shelf life of phosphine is one year.
4 Test method
4.1 Purity
Purity of phosphine () is expressed in volume fraction. Calculated according to formula (1): =100-(9++++++)×10-4
Wherein: 9
Arsine content, 10-6, V/V;
Carbon dioxide content, 10-6V/V;
Hydrogen content, 10-6, V/V;
Nitrogen content, 10-6, V/V;
Oxygen content, 10-6, V/V;
Total hydrocarbon content, 10-6, V/V;
Water content, 10-6, V/V.
4.2 Determination of Arsine Content
4.2.1 Method and Principle
(1)
Use potassium hypobromite solution to oxidize arsenic and phosphine in the sample into arsenic acid and phosphoric acid to eliminate the interference of phosphine. Excess potassium hypobromite is decomposed and removed by hydroxylamine hydrochloride. In an acidic solution, arsenic acid is reduced to As(I) by potassium iodide and stannous chloride. Zinc particles react with acid to produce new ecological hydrogen, which further reduces As(I) to arsenic. Arsenic gas is absorbed by silver diethyldithiocarbamate·trichloromethane solution to produce a purple-red product, which is determined by spectrophotometry. Triethanolamine is added to increase the color stability of the product. 4.2.2 Instruments and Devices
General laboratory instruments, such as balances, various volumetric devices, etc. Spectrophotometers should comply with the provisions of GB9721. The schematic diagram of the recommended arsine gas absorption device is shown in Figures A1 and A2 of Appendix A (reference). 4.2.3 Reagents, solutions and materials
4.2.3.1 Potassium hydroxide (GB2306): analytical grade; 4.2.3.2
Hydroxylamine hydrochloride (GB6685): analytical grade, c(H,NOH·HCl)=2mol/L solution; Stannous chloride (GB638): analytical grade;
Potassium iodide (GB1272): analytical grade, c(KI)=1mol/L solution; Sulfuric acid (GB625): analytical grade;
Sodium hydroxide (GB629): analytical grade, c(NaOH)-5mol/L solution; Bromine water (HG3-900): analytical grade;
Chloroform (GB682): analytical grade;
Lead acetate (HG 3-974): analytical grade, c[Pb(C,H,O,),)=1 mol/L solution; 4.2.3.9
4. 2. 3. 11
4. 2. 3. 14
4. 2. 3. 16
Arsenic trioxide (GB673): analytically pure; Arsenic-free zinc (GB2304): analytically pure;
Triethanolamine: analytically pure;
Silver diethyldithiocarbamate: analytically pure; High-purity nitrogen (GB8980): superior grade,
Hydrochloric acid (GB622): analytically pure;
Potassium permanganate: chemically pure, c(KMnO,)=0.1mol/L solution; GB/T14851--93
4.2.3.17 Distillation Water: should meet the specification of secondary water in GB6682; 4.2.3.18 Potassium hypobromite absorption solution: weigh 25g potassium hydroxide and dissolve it in 100mL water, then add 10mL bromine, stir evenly, and seal for storage;
4.2.3.19 Stannous chloride solution: weigh 40g stannous chloride (SnCl2·2H20) and dissolve it in 100mL concentrated hydrochloric acid; 4.2.3.20 DDC silver solution: weigh 0.25g silver diethyl dithiocarbamate, mix it into a paste with a little chloroform, add 2mL triethanolamine, and then dilute it to 100mL with chloroform, shake it vigorously to dissolve it as much as possible, let it stand for 24 hours, and filter it with slow filter paper into a brown bottle. This is the DDC silver solution. Place in the refrigerator, valid for one week; 4.2.3.21 Arsenic standard solution: weigh 0.1270g of arsenic trioxide dried to constant weight in a sulfuric acid dryer, dissolve in 2.0mL of sodium hydroxide solution c(NaOH) = 2mol/L, add 10mL of sulfuric acid c(÷H,SO,) = 2mol/L, dilute with water to 100mL. This solution is equivalent to 1mg/ml. Arsenic. Dilute with water to 10μg/mL when used; 4.2.3.22 Lead acetate cotton ball: soak the absorbent cotton in lead acetate c[Pb(C2H,O,)) = 1 mol/L solution, take out after 1h, dry and set aside.
4.2.4 Drawing of standard curve of hydrogen iodide
Into 6 250mL conical flasks, add 3mL of potassium hypobromite absorption solution and 0, 0.10, 0.20, 0.30, 0.40 and 0.50mL of arsenic standard solution in sequence according to the quantities in Table 2, let it stand for 1h, add 7mL of phosphoric acid c(一H,PO,)=3mol/L, add water to make up to 80mL, add 0.5mL of hydroxylamine hydrochloride c(H,NOH·HCl)=2mol/L solution, let it stand for 10min to make the yellow color of bromine fade, then add 7mL of (1+1) sulfuric acid and 2mL of potassium iodide c(KI)=1 mol/L solution, let it stand for 10min, and then add 0.5mL of hydroxylamine hydrochloride c(H,NOH·HCl)=2mol/L solution. mL of stannous chloride c(SnCl,·2H,O)=2mol/1 solution, let stand for 10 minutes, then add 5g of each zinc granule, immediately install the airway with lead acetate cotton ball as shown in Appendix A (reference) Figure A1, and quickly insert the other end of the airway into a small measuring cylinder containing 5.00mL of DDC silver solution. After about 40 minutes of reaction, remove the small measuring cylinder, add chloroform to 5.00mL, mix well and pour into a 1cm absorption cell. Put the absorption cell into the spectrophotometer, at a wavelength of 520nm, use the reagent blank (i.e., absorption cell No. 0) as a reference, and measure the absorbance values of the light-absorbing compounds with different amounts of arsenic hydrogen standard solution added. Table 2 Parameters for drawing the standard curve of arsenic
Potassium hypobromite absorption solution, mL
10μg/mL arsenic standard solution, ml
Absorption cell number
c(一HaPO,)=3 mol/L Phosphoric acid, mL
Water, ml
c(H,N(OH ·HCI)=2 mol/L Hydroxylamine hydrochloride, ml1+1 Sulfuric acid, mL
c(KI)=1 mol /L Potassium iodide, mL
c(SnClz - 2H,O) = 2 mol/L stannous chloride, mL arsenic-free zinc particles, g
equivalent amount of arsenic hydrogen, ug
draw a standard curve with arsenic hydrogen content versus absorbance value. 4.2.5 Sample determination
connect a 500mL (volume is based on the calibration value) fixed volume sampling tube to the phosphine sample gas cylinder, evacuate with a vacuum pump until the vacuum reaches -0.1MPa, open the gas cylinder, pass the sample gas into the sampling tube at a flow rate of 100mL/min for about 5min, and connect the outlet to an absorption bottle filled with potassium permanganate solution. After sampling, close the inlet first and then the outlet. As shown in Figure A2 of Appendix A (reference), connect the sampling tube 4 in series with the absorption tubes 6 and 7 each containing 40 ml of potassium hypobromite absorption solution and the tail gas absorption bottle 8 containing potassium permanganate solution. Use high-purity nitrogen to purge for 2 hours at a flow rate of 50 ml/min, then increase the nitrogen flow rate to 100 ml/min and purge for another 10 minutes to blow all the sample gas into the absorption tube. Combine the two-stage absorption liquid and transfer it to a 250 ml conical flask and leave it for 1 hour. Except for not adding arsine hydrogen standard solution, phosphoric acid and water, the remaining steps are carried out according to 4.2.4 to measure the absorbance. 4.2.6 Calculation of results
According to the measured absorbance value, the amount of arsenic is found from the arsenic standard curve, and the content of arsenic in the phosphine to be measured is calculated according to formula (2):
￥ 22. 4
9 = × . 95
In the formula, 9--the content of arsenic in phosphine, 106, w--the amount of arsenic found from the standard curve, ug; V--the volume of the phosphine sample taken, mL.
77.95--the molar mass of arsenic, g/mol. The arithmetic mean of the results of two parallel determinations is taken as the final determination result. The relative deviation of parallel determinations is not more than 20%. 4.3 Determination of carbon dioxide and total hydrocarbon content
4.3.1 Principle of the method
The carbon dioxide and total hydrocarbon contents are determined by gas chromatography. The main component phosphine is pre-cut and separated, and carbon dioxide and total hydrocarbons are separated by chromatographic columns. The carbon dioxide flowing out of the chromatographic column is converted into methane by a methanogenization furnace and detected by hydrogen flame ionization detector gas chromatography. 4.3.2 Instruments
A hydrogen flame ionization detector gas chromatograph with a minimum detection concentration of methane not greater than 0.4×10- is used. The gas flow of the chromatograph is shown in Figure A3 of Appendix A (reference). The installation and commissioning of the chromatograph shall be carried out according to the instrument manual. 4.3.3 Determination reference conditions
Detector: hydrogen flame ionization detector; Carrier gas: high-purity hydrogen with a purity not less than 99.999%, which shall meet the requirements of GB7445; Carrier gas flow rate: about 60mL/min;
Chromatographic column: stainless steel column with a length of about 8m and an inner diameter of 3mm, filled with porapakQ, particle size 0.3~0.45mm, column temperature 60℃; Converter temperature: about 360~～380℃;
High-purity nitrogen flow rate: about 40mL/min;
g. Air flow rate: about 400mL/min;
Injection volume: about 0.15mL.
4.3.4 Determination steps [see Appendix A (reference) Figure A3] Start the instrument according to the gas chromatograph instruction manual, turn on the carrier gas, air, and nitrogen, adjust them to the required values after ignition, and stabilize the instrument. After the sampling system (including the quantitative tube) is fully replaced with high-purity nitrogen, it is fully replaced with sample gas of more than 20 times the volume of the pipeline to make the sample representative.
Turn valve 8 to inject the sample, enter the chromatographic column 6 for separation, and the outflowing carbon dioxide and hydrocarbon impurities enter the methanogen 12 after passing through valve 5, valve 8 and resistance column 11. After the carbon dioxide and hydrocarbon impurities are converted into methane, they enter the hydrogen flame detector 13 for detection. When methane, carbon dioxide, ethylene, acetylene and ethane flow out of the chromatographic column 6 in succession, turn valve 5, use back-blowing gas to take phosphine out through valve 8, resistance column 10 and flowmeter 9 to vent, and record the retention time of phosphine by thermal conductivity; when phosphine completely flows out of the chromatographic column 6, propane passes through valve 8, resistance column 11 and converter 12 and enters the detector 13 for detection. The peak area A of carbon dioxide and hydrocarbon impurities is measured from the chromatogram;. 4.3.5 Calibration
Use the weighing method (see GB5274) or the exponential dilution method (see GB4845) to prepare standard gas with high-purity hydrogen as the base gas. The content of carbon dioxide and hydrocarbons in the prepared standard gas is about 50% to 200% of the content of carbon dioxide and hydrocarbons in the sample gas. Directly inject the standard gas and measure the peak area A of carbon dioxide and hydrocarbons. .
4.3.6 Result calculation
4.3.6.1 The content of carbon dioxide and hydrocarbons in phosphine is calculated according to formula (3): A
Where: 9----The content of the measured component in the sample gas, 10-6, V/V; 9-The content of the measured component in the standard gas, 10-s, V/V; A,——-The peak area of the measured component in the sample gas, mm2; A-The peak area of the measured component in the standard gas, mm. 4.3.6.2 The total content of hydrocarbons in phosphine is calculated according to formula (4): Total hydrocarbons
Where: 9.--The content of different hydrocarbons in the sample gas, calculated according to formula (3). 4.3.6.3 The arithmetic mean of two parallel determinations is taken as the determination result. The relative deviation of parallel determinations shall not exceed 10%. 4.4 Determination of hydrogen content
4.4.1 Principle of the method
·(3)
(4)
Gas chromatography using dual gas paths, dual chromatographic columns, cutting backflush process, high-purity nitrogen as carrier gas, direct injection through a six-way valve, and detection by a thermal conductivity detector.
4.4.2 Instrument
A thermal conductivity detector gas chromatograph with a minimum detection concentration of hydrogen not higher than 2×10-6 is used. The gas path flow of the chromatograph is shown in Figure A4 in Appendix A (reference).
4.4.3 Determination reference conditions
Detector: thermal conductivity cell, cold resistance value 1200; a.
Bridge current: about 120mA;
Carrier gas, backblowing gas: high-purity nitrogen with a purity not less than 99.9996%, which should comply with the provisions of GB8980; c.
Carrier gas, backblowing gas flow rate: about 30ml/mind each.
Chromatographic column: the front column is about 80cm long, with an inner diameter of 4mm, filled with porapakQ, particle size 0.15~0.2mm, and the column temperature is room temperature; the rear column is about 2m long, with an inner diameter of 4mm, filled with 5A molecular sieve, particle size 0.3~0.45mm, and the column temperature is room temperature; both are stainless steel columns; chromatographic column treatment: the front column is passed through high-purity nitrogen at 250℃ for about 4h, and the rear column is evacuated at 350℃ for about 4h; f.
Injection volume: about 4mL.
4.4.4 Determination steps [see Appendix A (reference) Figure A4) Start the instrument according to the chromatograph instruction manual, turn on the carrier gas, adjust the flow rate to the selected value, connect the thermal conductivity cell power supply, adjust all parts of the instrument to meet the determination conditions, and wait for the instrument to work stably. First use high-purity nitrogen, then use sample gas, and fully replace the injection pipeline, quantitative tube and valve body through valve 14 to make the sample taken representative. The sample gas used for replacement must be detoxified and then vented. After replacement, rotate valve 14 to inject the sample, record the retention time of hydrogen, and after hydrogen flows out of column 20, synchronously rotate valves 18 and 19 to cut the gas in column 20, backflush with nitrogen, and vent the nitrogen phosphide in the chromatographic column 20. The hydrogen flowing out of column 20 is carried to detector 11 by carrier gas through column 21 for detection.
Record the chromatographic elution curve of hydrogen and measure its peak area A. 4.4.5 Calibration
Prepare hydrogen standard gas by weighing method or exponential dilution method. The base gas is high-purity nitrogen, and the hydrogen content in the standard gas is about 50% to 200% of the hydrogen content in the sample gas. Inject the standard gas directly and measure the chromatographic peak area A of hydrogen. 593
4.4.6 Result calculation
The hydrogen content in phosphine is calculated according to formula (3). GB/T14851-93
The arithmetic mean of two parallel determinations is taken as the determination result. The relative deviation of parallel determinations shall not exceed 5%. 4.5 Determination of nitrogen content
4.5.1 Principle of the method
Same as 4.4.1. The carrier gas is 99.999% high-purity hydrogen. It shall comply with the provisions of GB7445. 4.5.2 Instrument
A gas chromatograph with a thermal conductivity detector whose minimum detection concentration of nitrogen is not higher than 3×10-6 is used. The chromatographic flow chart is shown in Appendix A (reference) Figure A4.
4.5.3 Reference conditions for determination
a Detector: thermal conductivity cell, cold resistance value 1202; b. Bridge current: about 230mA;
Purity of carrier gas and back-blowing gas: not less than 99.999% high purity hydrogen; c
d. Carrier gas and backflush gas flow rate: about 50mL/min each; e
Chromatographic column: the front column is about 80cm long, with an inner diameter of 4mm, filled with porapakQ, with a particle size of 0.150.2mm, and a column temperature of 50℃; the rear column is about 2m long, with an inner diameter of 4mm, filled with 13X molecular sieve, with a particle size of 0.3~~0.45mm, and a column temperature of room temperature, both of which are stainless steel columns; f. Injection volume: about 4mL.
4.5.4 Determination steps [see Appendix A (reference) Figure A4] 4.5.4.1 Start the instrument according to the instrument manual. The carrier gas is high purity hydrogen, with a flow rate of about 50mL/min. 4.5.4.2 Blank test: Use high-purity hydrogen to fully replace the sample injection line and quantitative tube, rotate valve 14 to inject, and after passing through valve 18, column 20, valve 19 and column 21, enter detector 11 for detection, check the sealing of the injection system, and it is normal if there is no chromatographic peak on the recorder. 4.5.4.3 Determination: Use hydrogen first, then use sample gas, and fully replace the sample injection line, quantitative tube and valve body through valve 14 to make the sample representative. The sample gas used for replacement must be detoxified in the detoxification tank 24 filled with potassium permanganate solution and then vented. After replacement, rotate valve 14 to inject, record the retention time of oxygen and nitrogen, and after oxygen and nitrogen flow out of column 20, synchronously rotate valves 18 and 19 to cut the gas in column 20, backflush with hydrogen, and vent the phosphine. The oxygen and nitrogen flowing out of column 20 are separated by chromatographic column 21, and the nitrogen is brought into detector 11 for detection by carrier gas.
Record the chromatographic elution curve of nitrogen and measure its peak area As. 4.5.5 Calibration
The base gas is high-purity hydrogen. The nitrogen content in the standard gas is about 50% to 200% of the nitrogen content in the sample gas. Directly inject the standard gas and measure the chromatographic peak area A of nitrogen. .
4.5.6 Result calculation
The nitrogen content in phosphine is calculated according to formula (3). The arithmetic mean of two parallel determinations is the determination result. The relative deviation of parallel determinations is not more than 5%. 4.6 Determination of oxygen content
4.6.1 Principle of the method
Use a gas chromatography method with dual gas paths, dual chromatographic columns, cutting backflush process, high-purity nitrogen as carrier gas, direct injection of six-way valve, and electron capture detector detection.
4.6.2 Instrument
Use a gas chromatograph with an electron capture detector with a minimum detection concentration of oxygen not higher than 1×10-. See Appendix A (reference) Figure A4 for the chromatographic process.
4.6.3 Reference conditions for determination
a Detector: Electron capture detector: Pulse period 150μssb. Carrier gas, purge gas: High-purity nitrogen with a purity not less than 99.9996%, and then treated with water removal and deoxygenation, 59.4
GB/T 14851-93
c. Carrier gas, purge gas flow rate: about 50mL/min each; d. Chromatographic column: The front column is about 80cm long, with an inner diameter of 4mm, filled with porapakQ, with a particle size of 0.15~0.2mm, and the column temperature is room temperature; the rear column is about 2m long, with an inner diameter of 4mm, filled with 5A molecular sieve, with a particle size of 0.3~～0.45mm, and the column temperature is room temperature; both are stainless steel columns; e. Injection volume: about 4ml.
4.6.4 Determination steps [See Appendix A (reference) Figure A4] 4.6.4.1 Start the instrument according to the chromatograph instruction manual, fully replace the gas system with high-purity nitrogen, adjust the flow of carrier gas and purge gas to the selected value, turn on the detector power, adjust all parts of the instrument to achieve the determination conditions, and wait for the instrument to work stably. : 4.6.4.2 Blank test:
a. Dilution bottle blank test: High-purity nitrogen is discharged from the 4th route through the exponential dilution bottle, the quantitative tube of valve 14 and valve 15. Turn valve 14 to bring the gas in the quantitative tube to valves 18, valve 19, column 20 and column 21, and go to the detector through the three-way. It is normal if there is no chromatographic peak on the recorder. b Cutting blank test: The second nitrogen gas is discharged after passing through valve 19, regulating valve 17, resistance column 16 and valve 18, and valves 18 and 19 are rotated synchronously to pass through the third carrier gas, which passes through valve 14, valve 18, resistance column 16, regulating valve 17, valve 19, column 21 and tee 22 and enters the detector. It is normal if no chromatographic peak appears on the recorder.
4.6.4.3 Determination of retention time: The sample gas in the sample gas cylinder 30 is discharged after passing through the detoxification tank through valve 15, and the sample gas is discharged after passing through valve 15, valve 14 and detoxification tank. Turn valve 14, the sample enters the quantitative tube, and the third carrier gas brings the sample gas to the four-way valve and chromatographic column, and then passes through the three-way valve through the thermal conductivity cell to measure the retention time of oxygen, nitrogen and phosphine. .4.6.4.4 Determination: During replacement, high-purity nitrogen is used first, followed by sample gas, which is processed through valve 15, valve 14, flow meter 25 and detoxification tank 24 and then discharged. Turn valve 14 to inject the sample, and the carrier gas brings the sample gas in the quantitative tube into column 20 through valve 18, and records the retention time of oxygen. After the oxygen flows out of column 20, turn valves 18 and 19 synchronously to cut the gas in column 20, and backflush with nitrogen to blow out the gas in the column. Oxygen passes through chromatographic column 21 and is brought into detector 23 by carrier gas for detection.
Record the chromatographic elution curve of oxygen and measure its peak area As. 4.6.5 Calibration
Calibrate with standard gas prepared by weighing method or exponential dilution method. The base gas is high-purity nitrogen, and the oxygen content in the standard gas is about 50% to 200% of the oxygen content in the sample gas. Inject the standard gas directly and measure the chromatographic peak area A of oxygen. 4.6.6 Calculation of results
The oxygen content in phosphine is calculated according to formula (3). The arithmetic mean of two parallel determinations is the determination result. The relative deviation of parallel determinations shall not exceed 10%. 4.7 Determination of water content
Perform according to GB5832.1.
5 Inspection rules
5.1 Phosphine is inspected by the quality supervision department of the manufacturer, and the manufacturer guarantees that its product quality meets the requirements of this standard. 5.2 The quality of phosphine is inspected bottle by bottle and item by item. 5.3 When one of the indicators in the inspection result does not meet the requirements of this standard, the bottle product is unqualified. 5.4 The user shall also inspect in accordance with the provisions of this standard. 5.5 When the user and the manufacturer have differences of opinion on product quality, both parties shall conduct joint inspection or apply for arbitration. 6 Packaging, marking, transportation and storage
6.1 The packaging and transportation of phosphine gas cylinders shall comply with the "Regulations on Gas Cylinder Safety Supervision" and relevant regulations of the transportation department. 6.2 The packaging mark shall comply with the provisions of GB190. 6.3 The color marking of phosphine gas cylinders shall comply with the provisions of GB7144. The gas cylinders shall be painted white and marked with the word "phosphine" in bright red.
6.4 The materials used for phosphine gas cylinders and their valves are carbon steel or stainless steel. 595
6.5 The valve of phosphine gas cylinders shall not be equipped with a safety valve. GB/T14851--93
6.6 Phosphine gas cylinders shall be stored at room temperature. Warning signs with the words "highly toxic" and "flammable" shall be set up at the entrances and exits of the storage area. 6.7 Open flames or the placement of flammable and combustible items are strictly prohibited within 10m of the storage area of phosphine gas cylinders, and effective and reliable fire-fighting equipment shall be available.
6.8 Applicable gas masks should always be available in the storage area. 6.9 The maximum filling quantity of bottled phosphine shall be calculated according to formula (5): GV.C
Wherein: G—mass of phosphine in the gas cylinder, kg; V—inner volume indicated on the gas cylinder, L;
C—filling coefficient of phosphine 0.2kg/L. The filling quantity of phosphine shall be calculated according to the actual weighed mass. (5)
6.10 Before leaving the factory, bottled phosphine shall be checked for leakage at the bottle mouth, bottle valve threaded connection and bottle valve stem, and the valve mouth shall be sealed and the bottle cap shall be installed.
Gas cylinders filled with phosphine (including returned gas cylinders) must be purged with inert gas, heated and evacuated before filling. 6.12
Phosphine should be accompanied by a product quality certificate when leaving the factory, and its contents should include: a.
Product name and specifications;
Manufacturer's name;
Production date, production batch number;
Gas cylinder number and volume;Www.bzxZ.net
The mass of phosphine (kg);
This standard code, etc.
7 Safety requirements
7.1 Phosphine is a highly toxic and flammable gas, and the allowable content in the air is 0.3mg/m2. Contact with phosphine can cause human poisoning, and the symptoms that appear quickly include nausea, vomiting, diarrhea, thirst, difficulty breathing, coughing with sputum, convulsions, paralysis and coma. Therefore, during the production, inspection and use process, phosphine should be prevented from leaking. Exhaust devices should be installed in the workplace. 7.2 The analysis system must be sealed. The phosphine tail gas from the sampling and replacement process must be detoxified before being discharged. 7.3 Phosphine gas cylinders should be stored away from heat sources and fire sources. Gas cylinders in use should be placed in the open air or in a forced ventilation room with shade. 7.4 Before passing phosphine, equipment and instruments should be flushed with dry inert gas, and pipelines should be leak tested. 7.5 Phosphine gas cylinders should be protected from impact and falling during transportation. 96
GB/T 14851-93
Appendix A
(reference)
Figure A1 Schematic diagram of arsenic analysis
1-10mL volumetric cylinder; 2-lead acetate cotton ball; 3-250mL conical flaskFigure A2 Schematic diagram of arsenic sample content processing flow 1-nitrogen cylinder; 2-pressure reducing valve; 3.5--glass piston 4-sampling tube; 6.7 absorption tube; 8-tail absorption bottle
, carrier gas H,
standard sample injection
Xiangpin injection
GB/T 14851—93
Figure A3 Schematic diagram of gas flow for analysis of THC and CO in phosphine 1, 9—flow meter; 2, 3—six-way valve: 4—exponential dilution bottle: 5, 8—four-way valve 6—chromatographic column 7—thermal conductivity cell: 10, 11 resistance column; 12—methanation furnace; 13—hydrogen flame detector; 14—fixed volume stopcock to amplifier
GB/T 14851 -- 93
Figure A4 Schematic flow chart of gas path for analysis of nitrogen, oxygen and hydrogen in phosphine29
1, 3, 6, 9—fine-tuning valve: 4, 7, 12, 27—pressure gauge; 2, 5, 8, 13, 25—flow meter, 10—exponential dilution bottle; 11—thermal conductivity cell; 14, 15 six-way valve, 16-resistance column; 17, 29-regulating valve; 18, 19—four-way valve; 20, 21—chromatographic column; 22—three-way valve; 23—electron capture detector; 24—detoxification tank: 26—stop valve; 28—vacuum pump; 30—sample gas cylinderAdditional instructions:
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 Lv Duojun.
This standard refers to the SEMI standard C3STD.6-88 "Electronic-grade phosphine in steel cylinders (tentative)" and C3STD.7-88 "Light-emitting diode-grade phosphine in steel cylinders (tentative)". 559
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