GB/T 37999-20191,1,1,3,3-Pentafluoropropane(HFC-245fa) for industrial use (English PDF)

4.1 General

The reagents and water used in the test method refer to the reagents confirmed to be analytically pure, and grade three water specified in GB/T 6682 when no other requirements are indicated.

4.2 Determination of appearance

Pour about 10mL of liquid specimen from the outlet of the sampling cylinder into a 50mL dry colorimetric tube. Wipe off the frost or moisture attached to the outer wall of the test tube with a dry cloth. Observe the color of the specimen and the presence or absence of visible solid particles in a lateral perspective.

4.3 Determination of 1,1,1,3,3-pentafluoropropane content

4.3.5.1.4 Use background sample 1,1,1,3,3-pentafluoropropane to repeatedly replace the air in the gas cylinder. Vacuum again. Introduce the background sample in the liquid phase to the gas cylinder. Slightly over exceed. Balance to normal pressure after complete vaporization. Use a syringe to add a certain volume of each impurity component gas one by one. Quantitatively add the liquid in the 4.3.5.1.3 sample bottle to the gas bottle. Make the amount of each impurity close to the composition of the test sample. Equilibrate for 20min~30min to completely vaporize each component. After being evenly mixed, it is the sample for calibration. Take a certain amount of calibration sample. Determine according to the chromatographic operating conditions given in Table 2.

4.3.5.1.5 The mass fraction wLi of each impurity component i in the liquid mixed sample is calculated according to formula (1):

4.3.5.1.6 The mass mi of the impurity component i in the liquid mixed sample added to the calibration sample, in grams, is calculated according to formula (2):

A1 - The peak area of 1,1,1,3,3-pentafluoropropane; fi - The relative mass correction factor for component i; Ai - The peak area of component i.

Take the arithmetic average of two parallel determination results as the report result. The absolute difference between the two parallel determination results of 1,1,1,3,3-pentafluoropropane is not more than 0.01%.

4.3.1 Method summary

Use gas chromatography. Under selected chromatographic conditions, the specimen is vaporized and passed through the chromatographic column to separate the components. Use a hydrogen flame ionization detector to detect.

The content of 1,1,1,3,3-pentafluoropropane is calculated by the corrected area normalization method.

4.3.2 Reagents or materials

4.3.2.1 Nitrogen: The volume fraction is greater than 99.995%

4.3.2.3 Air: Dried and purified by silica gel or molecular sieve.

4.3.2.2 Hydrogen: The volume fraction is greater than 99.995%

4.3.3 Instruments and equipment

4.3.3.1 Gas chromatograph: Equipped with a flame ionization detector (FID) for capillary column analysis. The sensitivity of the whole machine shall meet the requirements of GB/T 9722. The linear range meets the analysis requirements.

4.3.3.2 Recorder: Chromatography workstation or processor.

4.3.3.3 Injector: 1mL gas-tight syringe or automatic injection valve.

4.3.3.4 Sampling cylinder: Double-valve type stainless-steel small cylinder. The. […]

4.3.5.1.3 Take a screw-top sample bottle with septum. Insert the injection

needle into the septum to release the pressure in the bottle. In the order of boiling point from high to low, use a syringe to sequentially add the exact mass of impurity components to the sample bottle. After adding, shake well. Put on a label. Store in a refrigerator below 10°C for future use. This sample is a liquid mixed sample.

NOTE: The impurity component refers to the component in the specimen whose boiling point is higher than that of 1,1,1,3,3-pentafluoropropane.

Where, mLi - The mass of each impurity component liquid added to the screw-top sample bottle, in grams (g).

Where, m0 - The mass of the liquid mixed sample added to the calibration sample, in grams (g); wLi - The mass fraction of each impurity component i in the liquid mixed sample. Where, f1 - The relative mass correction factor of 1,1,1,3,3-pentafluoropropane;

4.4 Determination of moisture

Determine according to the provisions of GB/T 7376-2008 5.3.

Take the arithmetic average of the two parallel determination results as the report result. When the moisture content is <=0.0005%, the absolute difference between the two parallel determination results is not more than 0.0002%. When 0.0005%< moisture content<=0.0020%, the absolute difference between the two parallel determination results is not more than 0.0003%. When the moisture is greater than 0.0020%, the absolute difference between the two parallel determination results is not greater than 10% of the arithmetic mean of the two determination values.

4.5 Determination of acidity (as HCl)

Carry out according to the method specified in 5.4.2 of GB/T 33065-2016.

4.6 Determination of evaporation residue

Carry out according to the method specified in 5.4.2 of GB/T 33066-2016.

4.7 Chloride (Cl-) test

According to the regulations in GB/T 31401. The specimen size is about 33g±1g.

4.8 Determination of non-condensable gases in the gas phase

According to the regulations in GB/T 31400.

5.1 Type inspection

All items specified in the requirements of this Standard are type inspection items.

Under normal production conditions, type inspection shall be carried out at least once a month. Type inspection shall also be carried out in one of the following situations:

a) When updating the key production process, and the main raw materials have changed;

b) When production is stopped and resumed;

c) When a major quality accident occurs;

d) When there is a big difference between the exit-factory inspection result and the last type inspection;

e) When the quality supervision agency requests it in accordance with the law.

5.2 Exit-factory inspection

The appearance, 1,1,1,3,3-pentafluoropropane, and moisture in the requirements of this Standard are exit-factory inspection items.

5.3 Batching

1,1,1,3,3-pentafluoropropane for industrial use takes the products of uniform mass as a batch. One batch of steel bottled products shall be no more than 50t, or one batch of products is in one storage tank and one tank car.

5.4 Sampling

5.4.1 The sampling of 1,1,1,3,3-pentafluoropropane for industrial use shall be carried out in accordance with the provisions of 7.10 in GB/T 6681-2003. The total amount of sampling shall meet the needs of inspection.

5.4.2 The sampling cylinder and sampling tube shall be vacuum dried. The sample shall enter the sampling cylinder in the liquid phase. Use the drain valve of the sampling cylinder tube to adjust the sample volume. The sampling volume shall not exceed the allowable filling volume of the cylinder.

5.4.3 Label the sampling cylinder, indicating the product name, batch number, sampling date and the name of the sampler for inspection.

5.4.4 The number of sampling units of steel bottle packaging products shall meet the requirements of Table 3. and shall comply with TSG R4002.

a) Name of the manufacturer;

b) Product name and model;

6.3 Transportation

Steel cylinders and tank trucks containing 1,1,1,3,3-pentafluoropropane are pressure vessels. In the process of loading and unloading transportation, it shall be lightly loaded and unloaded. Shock, drag, drop and direct exposure are strictly prohibited. Safety helmets should be worn for repetitive steel cylinders.

The transportation process shall comply with the relevant regulations of the People's Republic of China on the transportation of dangerous goods by railways and highways. It shall be accompanied by a "chemical safety technical specification" and a "chemical safety label".

6.4 Storage

1,1,1,3,3-pentafluoropropane for industrial use shall be stored in a cool, dry place, away from heat sources, and strictly prohibited from sunlight and rain. […]