GB 6051-1985 Trifluoromethane fire extinguishing agent (1301 fire extinguishing agent)
Some standard content:
National Standard of the People's Republic of China
Bromotrifluoromethane (1301 Fire Extinguishing Agent) Fire extinguishing agent of bromotrifluoromethane UDC 547.22
GB 6051-85
This standard is the specific requirements for the quality of halogenated hydrocarbon fire extinguishing agent bromotrifluoromethane products. This standard does not discuss the use conditions of this product in fire extinguishing equipment.
This standard refers to the part of bromotrifluoromethane fire extinguishing agent in the international standard ISO7201-1982 "Fire-extinguishing agent-halogenated hydrocarbon".
1 Symbols and codes
Molecular formula: CF, Br
Molecular weight: 148.93
If arranged in order according to the number of carbon, fluorine, chlorine and bromine atoms, bromotrifluoromethane can be abbreviated as 1301. Technical requirements
1301 fire extinguishing agent shall comply with the requirements of Table 1:
Purity, % (mol/mol)
Water, mg/kg
Acidity (in terms of HBr), mg/kg
Evaporation residue, % (m/m)
Halide ions
Permanent gas in the vapor phase of the original filling container (expressed as air), % (mol/mol)<Suspended matter or precipitation
3 Test method
3.1 Sampling
3.1.1 Sampling cylinder and treatment method
The sampling cylinder shall adopt the sampling cylinder in GB4065-83 "Difluoromonochloromonobromomethane fire extinguishing agent". 99.6
Test passed
Test passed
Before the first use of the sampling cylinder, check whether the inside is clean. If the inner surface is not clean, wash it with water and appropriate solvent (such as ethanol or acetone). After washing, bake it in an oven at 105~110℃ for 3~4h, evacuate the bottle while it is hot to an absolute pressure of no more than 10mmHg, and keep it at this pressure for 1~2h, close the cylinder valve, and prepare for sampling. Before each subsequent sampling, the 1301 sample remaining in the bottle must be emptied, and the vacuum is still drawn at 10mmHg for 1h, and then a small amount of 1301 is added, and the vacuum is continued for 1h to ensure the cleanliness and dryness of the sampling cylinder. Issued by the National Bureau of Standards on June 3, 1985
Implemented on March 1, 1986
3.1.2 Sampling method
GB6051-85
Connect a dry stainless steel capillary to the outlet valve of the 1301 cylinder (the stainless steel capillary should be as short as possible. The capillary and cylinder valve should be blown with high-purity nitrogen for 2 to 3 minutes), slightly open the cylinder valve, release 1301, and flush the valve and connecting pipe for 1 minute, then quickly connect the end of the connecting pipe to the sampling cylinder valve, immerse the sampling cylinder in an ice-salt bath, and place it on a bench scale, open all the outlet valves of the 1301 cylinder, and then open the sampling cylinder valve to fill it with 1301. Determine the amount of sample filled from the weight change indicated by the bench scale. After sampling, close the sampling cylinder valve first, and then close the 1301 cylinder valve. Disconnect the connecting pipes and put down the sampling cylinder. Www.bzxZ.net
Except for the determination of permanent gases in the gas phase (3.7), all tests should be sampled from the liquid phase. To ensure the liquid phase sample, the cylinder filled with 1301 should be placed upside down during the sampling process (if there is a siphon in the cylinder, it can be placed upright). 3.2 Determination of purity Gas chromatography
3.2.1 Instrument and determination conditions
3.2.1.1 Instrument
SP-2305 gas chromatograph, thermal conductivity detector or other chromatographs with the same sensitivity as SP-2305. 3.2.1.2 Determination conditions
Chromatographic column: 3m long stainless steel tube, inner diameter 4mm; a.
b. Stationary phase: GDX-104, 60-80 mesh. It needs to be activated before use. The activation conditions are nitrogen flow (30-50 ml/min) and 140℃ for no less than 6 hours.
c. Carrier gas: hydrogen, flow rate is 45 ml/min (measured by soap film flowmeter). d. Temperature control: column temperature is 115℃, vaporization temperature is 100℃, and detection chamber temperature is 100℃. e. Bridge current: 200mA.
f. Recorder: full scale range is 5mV, full scale length is 250mm, and paper speed is 10mm/min. g. Detector sensitivity control: To ensure the sensitivity of chromatographic analysis, under the specified operating conditions, with 1301 as the sample, the sensitivity S301 should not be less than 1500mV.ml/ml, as expressed by formula (1). 1.065×C,.C,F ·A·K>1500mV.ml/m. (1)Si301
Wherein: 1.065-
-peak area correction coefficient;
-1301 chromatographic peak area, mm2,
reciprocal of recording paper speed, min/mm;
recorder sensitivity, mV/mm;
-carrier gas flow, ml/min;
-1301 injection volume, ml,
K——detector attenuation multiple.
3.2.2 Determination steps and calculation method
Adjust the chromatograph according to the conditions specified in 3.2.1.2. After the instrument is stable, measure the sensitivity of the thermal conductivity detector to 1301 (it is not necessary to do this measurement every time). After meeting the requirements, the purity of 1301 can be measured. When sampling, first connect the 1301 sampling cylinder to the sampling tube, put the cylinder down (take liquid gasification sample), open the cylinder valve, exhaust the 1301 for 0.5 to 1 minute, use a glass syringe to draw 2 to 3 ml of 1301 sample, inject it into the chromatograph, and use the peak area normalization method (or peak height quantification method) to calculate the 1301 purity according to formula (2): 1301 purity (%) three
In the formula: A01-
-1301 chromatographic peak area, mm2;
Detector attenuation multiple;
A1301·K
A, — the sum of the areas of all chromatographic peaks except the air peak, mm2. 3.2.3 Determination results and allowable deviations
: (2)
The arithmetic mean of the results of three parallel determinations is taken as the determination result. The absolute deviation of each determination should be less than 0.1. 328
3.3 Determination of water content Karl Fischer method
3.3.1 Reagent treatment and preparation
GB 6051—85
3.3.1.1 Anhydrous methanol: Take 5g magnesium and 0.5g iodine, place them in a round-bottom flask, add 70ml methanol, reflux until all the magnesium turns into grayish white flocculent magnesium methoxide, then add about 900ml methanol, continue to reflux for 30min, and then conduct fractional distillation. Collect anhydrous methanol at 64-65℃. 3.3.1.2 Anhydrous pyridine: Add an appropriate amount of sodium hydroxide to the reagent pyridine, reflux for 4 hours, and then fractionate to collect anhydrous pyridine at 114-116°C.
3.3.1.3 Iodine: Dry the sublimated iodine in a sulfuric acid dryer for more than 48 hours. 3.3.1.4 Sulfur dioxide-pyridine solution: Absorb the dried sulfur dioxide with 100ml of anhydrous pyridine (cooled with ice on the outside) until the total volume increases to 200ml. Weigh the weight of sulfur dioxide before and after. This solution is stored in a brown ground-mouth bottle, placed in a thermos bottle and stored with ice. This solution contains about 0.7g of sulfur dioxide per milliliter. 3.3.1.5 Karl Fischer reagent: Place 9g of iodine and 500ml of anhydrous methanol in a 1000ml round-bottom flask with a ground-mouth stopper, and stir thoroughly to dissolve the iodine. Add 27ml of anhydrous pyridine and 13ml of sulfur dioxide-pyridine solution to this solution, shake well, then add 460ml of anhydrous methanol, shake well and place in a desiccator. Place for at least 24 hours before use. The titer of this reagent for water is about 0.4mg/ml. 3.3.1.6 Methanol-water standard solution: Add 50ml of anhydrous methanol to a very dry 100ml volumetric flask, add 2 drops of distilled water (weigh with a dropper, and weigh the weight of 2 drops of water by reduction method), then add anhydrous methanol to the scale line of the volumetric flask, and shake well. 3.3.2 Instruments
3.3.2.1 Automatic microburette: The volume of the burette is 3ml, the minimum graduation is 0.01ml, and the liquid storage bottle is a 1000ml brown bottle. 3.3.2.2 Titration cell: Volume is about 250ml, connected to the automatic microburette containing Karl Fischer reagent by means of a ground glass interface. The other three ground interfaces on the titration cell, one is installed with a platinum electrode, another is installed with a gas injection tube or a liquid injection head, and the third interface is installed with a silica gel drying tube as a discharge port for the gas passing into the titration cell. There is a ground stopcock at the lower end of the titration cell for discharging liquid. 3.3.2.3 Electromagnetic stirrer
3.3.2.4 End point detection device
Dry battery: 1.5V;
b. Electric key
Variable resistor: 10k2;
Microammeter: 150uA.
3.3.2.5 Balance (or platform scale): weighing 5kg, sensitivity below 0.1g. The assembly of the instrument and the end point detection circuit diagram are shown in Figures 1 and 2. 329
GB 605185
Karl Fischer method for water content determination
2-micro burette: 3-titration cell; 4-electromagnetic stirring; 5-end point control 1-Fischer reagent storage bottle,
Figure 2 End point control circuit diagram
3.3.3 Determination steps
3.3.3.1 Calibration of Karl Fischer reagent
GB 6051—85
Add 50m3 of anhydrous methanol to the titration cell, start the electromagnetic stirrer, adjust the variable resistor so that the pointer of the microammeter indicates 5uA, and titrate with the Karl Fischer reagent to be calibrated to anhydrous state (the pointer of the microammeter deflects to 70uA and can remain without reversing for more than half a minute).
Use a syringe that has been dried in advance to inject 0.5ml of anhydrous methanol into the titration cell, and titrate with the Karl Fischer reagent to be calibrated until the anhydrous state (the microammeter indicates 70uA), record the volume of the reagent used (V), add 0.5ml of methanol-water standard solution in the same way, and titrate with the Karl Fischer reagent to be calibrated until the microammeter pointer reaches the same value (70uA) and can maintain it for at least half a minute without reversing. Record the volume of the reagent used (V,), and the titration degree of Karl Fischer reagent against water is calculated according to formula (3): T
Where: T-
-The titration degree of Karl Fischer reagent against water, mg/ml; - The water content in 0.5ml of methanol-water standard solution, mg; w
V,-The volume of Karl Fischer reagent used to titrate 0.5ml of methanol-water standard solution, ml; V,-The volume of Karl Fischer reagent used to titrate 0.5ml of anhydrous methanol, ml. 3.3.3.2 Determination of water content in the sample
Start the stirrer and titrate the methanol solution in the titration cell with the calibrated Karl Fischer reagent until it is anhydrous. Invert the sampling cylinder, open the needle valve on the flat bottle, and introduce the 1301 sample into the methanol solution in the titration cell. Expel air for 2 to 3 minutes to remove the water in the pipeline, and then use Karl Fischer reagent to drip the methanol solution in the bottle until it is anhydrous. After weighing the sampling cylinder (accurate to 0.1g), pass the 1301 sample into the titration cell at a flow rate of about 1.5g/min (after calibration, the float flowmeter can be used to adjust the air intake speed), so that the total amount is about 10g (the sampling amount can be appropriately increased or decreased depending on the water content of the sample, and the total water content in the sample is controlled to be about 0.1mg). After passing, close the cylinder valve and titrate with Karl Fischer reagent until it is anhydrous, that is, the pointer of the microammeter deflects to the same scale as before adding the sample, and can be maintained for more than half a minute. Record the volume of Karl Fischer reagent used, and then weigh the sampling cylinder. The difference between the weight of the cylinder before and after sampling is the weight of the sample.
The moisture content is calculated according to formula (4):
Where: X-
-moisture content, mg/kg;
The titer of Karl Fischer reagent for water, mg/ml; The volume of Karl Fischer reagent consumed when titrating the sample, mi, and the weight of the sample, g.
3.3.4 Determination results and allowable deviations
The arithmetic mean of the results of three parallel determinations is taken as the determination result. The absolute deviation of each determination should be less than 1. 3.4 Determination of acidity
3.4.1 Reagents and instruments
3.4.1.1 Methyl red (HG3-958--76): 0.1% ethanol solution; 3.4.1.2 Hydrochloric acid (GB622-77): analytical grade, 0.0100N standard solution; 3.4.1.3 Scale: weighing 2kg, sensitivity below 1g, 3.4.1.4 Graduated pipette: 0.1ml (minimum graduation is 0.005ml). (4)
3.4.2 Determination steps
In 300ml of distilled water, add 10 drops of 0.1% methyl red indicator, and adjust the solution to light orange with 0.01N hydrochloric acid. This is the blank solution.
In a 250ml conical flask, add 0.185ml 0.0100N hydrochloric acid standard solution and 100ml blank solution (this solution is pink). 331
This solution is used as the standard solution containing 3mg/kg HBr. GB 6051-85
In another 250ml gas washing bottle, add 100ml blank solution and pass 50g 1301 into it (bubble and absorb for about 1h, and weigh the sample weight by reduction method). After the ventilation is completed, shake the solution in the bottle, wash the upper bottle of the liquid surface thoroughly, then observe the color of the solution and compare it with the standard solution. The pink color of the sample solution should be lighter than that of the standard solution (or the sample solution is yellow or orange) to be qualified.
3.5 Determination of evaporation residue
3.5.1 Instrument
Conical flask: 100ml.
Bench scale: weighing 2kg, sensitivity below 1g.
3.5.2 Determination steps
First weigh the weight of the steel cylinder with 1301 sample on the bench scale (accurate to 1g), turn the steel cylinder upside down, slowly open the valve, and fill 1301 into a 100ml conical flask that has been dried to constant weight at 110±2℃ in advance. When the 1301 sample filled is 80-100g, close the cylinder valve and weigh the sample cylinder again (accurate to 1g). After the 1301 in the conical flask evaporates, dry it in an oven at 110±2℃ for 30min, move the conical flask into a dryer and place it for 20min, and weigh it (accurate to 0.0001g). Calculate the evaporation residue according to formula (5): Evaporation residue (%)
W——1301 sample weight, g.
3.6 Test for halide ions
3.6.1 Reagents and instruments
3.6.1.1 Methanol (GB683-79): analytical grade 3.6.1.2 Silver nitrate (GB670--77): analytical grade 3.6.1.3 Scale: weighing 2kg, sensitivity below 1g 3.6.1.4 Colorimetric tube: 25ml, with ground stopper. 3.6.2 Test steps
(5)
Add 5 ml of methanol and a few drops of saturated silver nitrate methanol solution to a dry colorimetric tube, pass 5 g of 1301 sample into the solution, shake it slightly (can be done in an ice bath if necessary), and if there is no turbidity or precipitation of silver halide, it is qualified. 3.7 The determination of permanent gas in the vapor phase of the original filling container is carried out by gas chromatography, and the instrument and determination conditions are the same as 3.2.1. 3.7.1 Determination steps
Use a sampling cylinder to sample the gas phase in the original filling cylinder, and the sampling method is in accordance with the provisions of 3.1.2. During the determination, connect the sampling cylinder and the six-way injection valve on the chromatograph with a metal capillary or a polytetrafluoroethylene capillary, open the cylinder valve, exhaust for 0.5 to 1 minute, and then use the six-way valve to inject the sample. If conditions permit, it is best to directly sample from the original filling cylinder. 3.7.2 Calculation method
Use the peak area normalization (or peak height quantification) method to calculate the percentage of permanent gas in the vapor phase of the original filling container (mol/mol) (expressed as air content) according to formula (6): Where: A#
Permanent gas (%) =
A#×100…
Air chromatographic peak area, mm2;
The sum of the areas of all chromatographic peaks including the air peak, mm2. 3.8 Determination of suspended matter or sediment
The liquid phase of the sample shall be inspected visually, and no suspended matter or sediment shall be found to be acceptable. 332
Inspection rules
GB 6051-85
4.11301 Fire extinguishing agents shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that the 1301 extinguishing agent leaving the factory meets the requirements of this standard.
4.2 The user has the right to accept the 1301 extinguishing agent received in accordance with the provisions of this standard. 4.3 When inspecting a whole batch of 1301, random sampling inspection shall be carried out in accordance with the proportion specified in Table 2. The sampling method shall be in accordance with Article 3.1. The so-called quantity in each batch refers to the number of cylinders packaged in each can of the manufacturer. Table 2
Number of bottles in each batch
Number of sampling bottles
50 or less
51~100
101~500
501~1000
4.4 If one indicator does not meet this standard during the inspection, new samples of the same number shall be drawn from other bottles in the batch for re-inspection. As a result of the re-test, even if only one indicator does not meet the requirements of this standard, the entire batch of 1301 fire extinguishing agent will be deemed unqualified and cannot be shipped or accepted.
4.5 When the supply and demand parties have objections to the product quality, they should resample from the original filled cylinder and send it to the designated inspection unit for inspection according to the test method specified in this standard, and the inspection results of the inspection unit shall prevail. 5 Marking, packaging, transportation, storage
5.1 The inside of the cylinder containing 1301 fire extinguishing agent should be very dry and clean, and the outside of the cylinder should be marked with "1301 fire extinguishing agent". Each bottle should be accompanied by a product quality certificate, which should indicate the manufacturer's name, product name, batch number, net weight, this standard number and production date. 5.2 The safety requirements for cylinders filled with 1301 fire extinguishing agent, transportation and storage of 1301 fire extinguishing agent shall be implemented in accordance with the relevant provisions of the "Regulations on Gas Cylinder Safety Supervision" issued by the State Administration of Labor. Additional notes:
This standard was proposed by the Ministry of Public Security of the People's Republic of China and is under the jurisdiction of the Tianjin Fire Science Research Institute of the Ministry of Public Security. This standard was drafted by the Tianjin Fire Science Research Institute of the Ministry of Public Security. The main drafters of this standard are Peng Chengxin and Chen Yuqian. 333
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