GB 25971-2010Fire extinguishing agent hexafluoro propane (HFC236fa) (English PDF)

5.1 General provisions

The reagents and water used in this standard refer to the analytical reagents and the tertiary water specified in GB/T 6682 when no other requirements are specified.

The standard solution used in the test shall be prepared in accordance with the requirements of GB/T 601 and GB/T 603 when no other requirements are specified.

5.2 Sampling

5.2.1 Sampling cylinders

Sampling cylinders should meet the following requirements.

a) Material is made of stainless steel;

b) Design pressure should not be less than 1.5MPa.

5.2.2 Treatment of sampling cylinders

Sampling cylinders Before use for the first time, wash with water and a suitable solvent such as ethanol or acetone. After washing, at 105 ° C to 110 ° C

Electric blast drying oven baking 3h ~ 4h, while the vacuum cylinder to the absolute pressure is not higher than 1.3kPa, and in this pressure to maintain 1h ~

2h, then close the cylinder valve for sampling.

Prior to each subsequent sampling, the residual hexafluoropropane (HFC236fa) extinguishant sample in the cylinder should be vented at 1.3 kPa

Under the conditions of vacuum 1h, and then pour a small amount of hexafluoropropane (HFC236fa) extinguishing agent, continue to vacuum 1h to keep the sampling cylinder

Clean and dry.

5.2.3 Sampling method

With a dry stainless steel tube connected to the filling of hexafluoropropane (HFC236fa) fire extinguishing agent on the outlet valve, stainless steel tube to

As short as possible, slightly open the cylinder valve, release hexafluoropropane (HFC236fa) fire extinguishing agent, flush the valve and connecting pipe 1min, and then connect

The end of the tube is quickly connected to the sampling cylinder valve. The sampling cylinder on the platform scales (if necessary, the sampling cylinder can be immersed in the ice salt bath),

The hexafluoropropane (HFC236fa) extinguishant cylinder outlet valve open, open the sampling cylinder valve, so that hexafluoropropane (HFC236fa) fire

Poured into them. The quality of the poured sample is determined by the quality change indicated by the scale. After sampling, first close the sampling cylinder valve, then

And then close the filling of hexafluoropropane (HFC236fa) fire extinguishing agent cylinder valve, remove the connecting pipe. All tests should be liquid sampling.

5.3 Determination of purity

5.3.1 Measuring instruments

The instrument was equipped with a gas chromatograph equipped with a capillary column and a hydrogen flame detector (with hydrogen as the carrier gas, and the sensitivity of the benzene

Higher than 8000 mV · mL/mg).

5.3.2 Determination conditions

The measurement conditions are shown in Table 2.

Table 2 Purity measurement conditions

Project Conditions Project Conditions

Detector Hydrogen Flame Detector

Detector temperature/° C 300

Column flow rate/(mL/min) 20

Compensated gas flow rate (mL/min) 45

Inlet temperature /.200 ° C

Inlet

Split/splitless inlet,

Split ratio of 40. 1

Column temperature/° C.200

Column GasPro30m × 0.32mm

5.3.3 Measurement steps

5.3.3.1 Start the gas chromatograph, adjust the instrument according to the conditions specified in 5.3.2, so that the conditions of the instrument is stable and meet the requirements.

5.3.3.2 The hexafluoropropane (HFC236fa) extinguishing agent sampling cylinder connected to the sampling tube, down the cylinder (liquid phase gasification sample), open the cylinder valve

Door, so that hexafluoropropane (HFC236fa) extinguishant exhaust 1s ~ 3s, and then into the gas chromatograph for determination (chromatogram see attached

Recorded A).

5.3.3.3 Calculate the purity of hexafluoropropane (HFC236fa) extinguishing agent by using the area normalization method.

5.3.3.4 The arithmetic mean of the results of the three parallel measurements shall be the result of the determination. The absolute deviation of each measurement shall not be more than 0.05%.

5.4 Determination of acidity

5.4.1 Principles Overview

So that the sample gasification, bubbling into the laboratory three water, the absorption of acidic substances to bromocresol green as the indicator solution, titration with sodium hydroxide standard

Solution titration to obtain acidity (in terms of HCl).

5.4.2 Reagents and instruments

The reagents used, the instruments and their requirements are as follows.

a) sodium hydroxide standard titration solution. molar concentration of 0.01mol/L;

b) bromocresol green indicator. concentration of 1g/L;

c) electronic balance. sense of 1g;

d) micro burette. the smallest scale value of 0.01mL;

e) Porous gas bottle. volume 250mL;

f) Erlenmeyer flask. volume 250mL.

5.4.3 Determination steps

5.4.3.1 Add 100 mL of laboratory tertiary water to each of the three porous gas bottles, add a third

Bromocresol green indicator (2 ~ 3) drops in series with a catheter.

5.4.3.2 Wipe dry sampling cylinders and valves, weighing, accurate to 1g, the sampling cylinder valve outlet with the first porous gas bottle connection,

Slowly open the cylinder valve to make the liquid sample gasification through the three porous gas bottle, about 100g after the sample into the cylinder valve closed,

Remove the sample cylinder, dry, weigh, accurate to 1g.

5.4.3.3 If the indicator liquid in the third porous gas bottle does not change color, continue with the following steps, otherwise re-test.

5.4.3.4 The water of the first and second porous gas bottles was combined, transferred to a conical flask, added with bromocresol green indicator solution (2 to 3)

Sodium hydroxide standard solution titrated to the end.

5.4.4 Calculation

The mass fraction x (%) of the acidity (in HCl) of hexafluoropropane (HFC236fa) extinguishing agent is calculated according to equation (1)

x = CNaOH × V × 0.0365m1 - m2 ×

100% (1)

Where.

V --- consumption of sodium hydroxide standard titration solution in milliliters (mL);

CNaOH - the actual concentration of sodium hydroxide standard titrant in moles per liter (mol/L);

m1 --- the quality of the sample before the sample is absorbed, in grams (g);

m2 --- the quality of the sample after absorption of the sample, in grams (g);

0.0365 --- equivalent to 1.00mL sodium hydroxide standard titrant in grams of hydrogen chloride quality.

The arithmetic mean of the results of two parallel measurements is taken as the result of the measurement. The difference between the two parallel measurements is not more than 0.0001%.

5.5 Moisture determination

Determination of moisture according to the provisions of GB/T 7376.

5.6 Determination of evaporation residue

Principle of 5.6.1

The sample was evaporated and the mass of the high boiling residue was weighed to determine the evaporation residue content.

5.6.2 Reagents and instruments

The reagents used, the instruments and their requirements are as follows.

a) Washing solution. dichloromethane (analytical grade);

b) Evaporator. composed of evaporation tube and weighing tube, as shown in Figure 1;

c) constant temperature water tank;

d) electric blast oven. adjustable temperature to 105 °C ± 2 °C.

Figure 1 evaporator

5.6.3 Determination steps

5.6.3.1 The weighing tube is dried in an electric blast oven at 105 ° C ± 2 ° C for about 30 minutes and then cooled in a desiccator.

0.1 mg, connected to the evaporation tube.

5.6.3.2 Weigh the sample to the non-boiling sample about 800g in the evaporator, part of the weighing tube immersed in the constant temperature of the tank, so that the sample steamed

hair. The temperature of the constant temperature water tank is adjusted to the sample which can be evaporated at 1.5h ~ 2.0h.

5.6.3.3 After the gasification of the sample, add 10 mL of the cleaning solution to the evaporator and place the weighing tube in a constant temperature water tank of about 90 ° C.

After the liquid gas is vaporized and the gasification is completed, the weighing tube is dried in an electric blast oven at 105 ° C ± 2 ° C for about 30 minutes. After drying in a dryer

Cooling, called quasi-0.1mg so far.

5.6.4 Calculation

Evaporation residue Y (%) Calculated according to formula (2).

Y = m1 - m2m 100%

(2)

Where.

m1 --- the quality of the weighing tube, in grams (g);

m2 --- the quality of the weighing tube after gasification of the sample, in grams (g);

m --- the quality of the sample, in grams (g).

5.7 Determination of suspended solids or precipitates

10 mL of the non-boiling cooling sample was placed in a tube of about 15 mL in diameter, and the frost or moisture attached to the outer wall of the test tube was dried,

Phenomenon to observe whether there is turbidity or sediment.

5.8 Determination of fire extinguishing concentration (cup burner method)

The determination of the extinguishing concentration (cup burner method) is in accordance with the requirements of A.1 to A.4 and A.6 in Appendix A of GB/T 20702-2006.

Line, the fuel is n-heptane.

5.9 Toxicity determination

5.9.1 Test device

5.9.1.1 Device overview

The test device consists of an extinguishing agent and an air supply system, a mouse motion recording system, a mouse basket, and an exposure tank.

As shown.

5.9.1.2 Mouse cage

The mouse cage was made of aluminum, as shown in Figure 3, the cage quality (60 ± 10) g; mouse cage in the bracket should be able to flexible rotation, no fixed

Standing point.

The unit is in millimeters

Figure 3 mouse basket

5.9.1.3 Exposure box

The exposed container is made of a colorless, transparent plexiglass material with an effective space of about 9.2 L and can hold 10 mice for exposure

test.

5.9.1.4 Extinguishant and air supply systems

The extinguishant and air supply system consists of an air source (bottled compressed air or air compressor to extract clean ambient air) and an adjustable

2.5 gas flow meter and gas pipeline composition.

5.9.1.5 mouse motion recording system

Mice were recorded with infrared or magnetic signals to monitor the rotation of the mice, and the time-motion profile of each mouse should be qualitatively

Reflect the angular speed of the cage every time.

5.9.2 Test animal requirements

5.9.2.1 Test animals shall be clean test mice in accordance with GB 14922.1 and GB 14922.2.

5.9.2.2 The test mice shall be obtained from the units that obtained the test animal production license and the genetic classification shall be in accordance with the inland line of GB 14923

Or closed group requirements.

5.9.2.3 Test mice obtained from production units should be subjected to environmental adaptive feeding. 2 days before the test, the weight of the test mice should be increased.

The age should be (5 ~ 8) weeks, the quality should be (21 ± 3) g.

5.9.2.4 8 or 10 mice in each test group. Male and female half, random group.

5.9.2.5 test drinking water should meet the requirements of GB 5749; feed should meet the requirements of GB 14924.3; environment and facilities should be

GB 14925 requirements.

5.9.3 Test procedure

5.9.3.1 5 min before the test, the mice should be numbered by weight, cage, and placed on the stent of the exposure test chamber, cover the exposed lid.

5.9.3.2 Open the fire extinguishing agent and air supply system and adjust the flow rate respectively so that the concentration of the extinguishant in the mixed gas of the fire extinguishing agent and the air reaches

5.8 test fire concentration of 1.3 times.

5.9.3.3 through the three-way cock will be the initial 10min mixture directly discharged, and then rotate the three-way cock, so that the mixture into the exposure

Box, test start.

5.9.3.4 The test was performed for 30 min, during which the behavioral changes were observed and recorded.

5.9.3.5 30min test end, quickly open the exposure box, remove the mice.

5.9.4 Observation of the test phenomenon

5.9.4.1 30min observation of mice during exercise. breathing changes, coma, spasm, jumping, struggling, can not stand up, want to run can not

And other symptoms; mouse eye changes. eyes closed, tears, swelling, loss of vision and so on. Record the time of the above phenomenon and the time of death.

5.9.4.2 The behavior of mice should be observed and recorded within 1 hour after the end of exposure and after exposure.

5.9.4.3 within 3 days after exposure, should observe the changes in various symptoms of mice, daily records of various phenomena and death.

5.9.5 Determination of Toxicity

5.9.5.1 When the following symptoms and characteristics occur in experimental mice, the toxicity is determined as "anesthesia".

a) in the exposure period, the mice have coma, jumping, spasm, loss of balance, supine, want to run can not wait for symptoms;

b) The mouse & apos; s motion profile showed that the mice had a longer time to stop the movement or no longer exercise at a time

The characteristic map of the ability;

c) mice died within 30 min of exposure or within 1 h.

5.9.5.2 When the following symptoms and characteristics occur in experimental mice, the toxicity is determined as "irritation".

a) during the exposure of mice seeking to avoid, there are obvious eye and respiratory behavior abnormalities, nose and mouth mucus increased; mild stimulation showed closed eyes,

Tears, breathing faster; moderate and severe stimulation of the performance of the cornea white, swelling, or even loss of vision, gas tightening and cough;

b) The mouse movement map showed that the mice were almost running;

c) mice within 3 days after exposure to slow, weak anorexia or death.

6.1 Inspection category and project

6.1.1 Factory inspection

Purity, acidity and moisture for the factory inspection project.

6.1.2 Type inspection

All items specified in Table 1 in Chapter 4 are type test items.

The product type test shall be carried out in any of the following cases.

a) new product identification or old products to plant production;

b) after the formal production, such as raw materials, processes have a greater change;

c) regular inspection every two years at the time of formal production;

d) When the production is resumed for more than one year;

e) When the State Quality Supervision Agency proposes to carry out the type inspection requirements.

Group 6.2, batch

Batch. one-time feeding in the processing equipment prepared by the uniform material.

Group. Products produced under the same environmental conditions, using the same raw materials and processes, including one or more batches.

6.3 Sampling

6.3.1 Type inspection samples shall be taken from products which are qualified for inspection by the factory.

6.3.2 According to "group", "batch" sampling, should be randomly selected not less than 2kg samples.

6.4 Determination of test results

6.4.1 Determination of factory inspection results

Factory test items, purity, acidity and water any one failed, then determine the factory inspection failed.

6.4.2 type test results to determine

Type test results meet one of the following conditions, that is, to determine the batch of qualified products, or sentenced to the batch of products failed.

a) the indicators are in compliance with the requirements of Chapter 4;

b) that only one Class B is unqualified and that other items meet the requirements of Chapter 4.