GB/T 33387-2016Trans-1,3,3,3-tetrafluoropropene[HFO-1234ze(E)] for industrial use (English PDF)

4.1 Appearance

Place liquid sample in a 50 mL dry colorimetric tube. When the sample liquid volume reaches around 10 mL, use dry cloth to wipe-dry frost or moisture attached to the external wall of the colorimetric tube. Through horizontal perspective, observe the sample's color; determine whether there is any turbidity or solid particle.

4.2 Determination of Trans-1,3,3,3-tetrafluoropropene Content

4.2.1 Method summary

Use gas chromatography; under the selected chromatographic conditions, through gasification, sample passes the chromatographic column, which separates its various components. Use hydrogen flame ionization detector (FID) for detection. Use corrected area normalization method to calculate the content of trans-1,3,3,3-tetrafluoropropene.

4.2.2 Reagents

4.2.2.2 Hydrogen: volume fraction is more than 99.995%

4.2.2.1 Nitrogen: volume fraction is more than 99.995%

4.2.2.4 Air: dried and purified through silica gel or molecular sieve.

4.2.2.3 Helium: volume fraction is more than 99.995%

4.2.3 Instruments

4.2.3.1 Gas chromatograph: equipped with hydrogen flame ionization detector (FID).

Take benzene as the sample; the overall sensitivity requirement detection limit is. Stability shall comply with the stipulations in GB/T 9722. Linear

4.2.5 Analytical procedures

4.2.5.1 Determination of relative mass correction factor

4.2.5.1.1 The content of various standard substances used in the tests shall be accurately determined in advance. In the preparation of standard samples for calibration, multiply the mass of the standard substances being taken by the actual content for correction.

4.2.5.1.2 When trans-1,3,3,3-tetrafluoropropene is used as the background sample to prepare the standard samples for calibration, inspect beforehand under the test conditions stipulated in this Standard. In the component to be tested, no impurity peak shall emerge, otherwise, it shall be corrected.

4.2.5.1.3 Preparation of standard samples for calibration

In accordance with the pressure of various impurity component gases, arrange the sequence from low-pressure component to high-pressure component. Use a quantitative tube, which is equipped with valve on both ends, to respectively add the various impurity component gases to the gas cylinder. Take trans-1,3,3,3-tetrafluoropropene as the background gas, so that the content of the various impurities could approach the composition of the sample to be tested. Maintain the balance for 20 min ~ 30 min. The standard sample for calibration may remain valid for 3 d ~ 4 d.

Mass mi of gas of impurity component i, expressed in (g), shall be calculated in accordance with Formula (1):

Where, Vi---volume of gas of impurity component i being added, expressed in (mL);

Mi---molar mass of impurity component i being added, expressed in (g/moL);

24,450---numerical value of volume of 1 mol of gas at 25 °C, 101.325 kPa (1 atm), expressed in (mL).

4.2.5.1.4 The calculation of the content of various impurity components in the standard samples for calibration Mass fraction wi of impurity component i in the standard samples for calibration shall be calculated in accordance with Formula (2): […]

5.1 Type Inspection

All the items stipulated in this Standard are type inspection items. Under normal production, type inspection shall be conducted at least once every month. Under one of the following circumstances, type inspection shall also be conducted:

a) When pivotal production process is updated;

b) When there are changes in the main raw materials;

c) When production is resumed after suspension;

d) When there are relatively significant differences between the exit-factory inspection result and the previous type inspection;

e) When it is stipulated in the contract.

5.2 Exit-factory Inspection

Appearance, trans-1,3,3,3-tetrafluoropropene, moisture and non-condensable gas in the gas phase, which are stipulated in Chapter 3, are exit-factory inspection items.

5.3 Group Batch

Each batch of trans-1,3,3,3-tetrafluoropropene cylinder products for industrial use shall be not more than 50 t; or, a storage tank or a tank truck of products shall constitute a batch.

5.4 Sampling

5.4.1 Comply with the stipulations in 7.10 in GB/T 6681-2003. The total sampling size shall guarantee the demand of inspections.

5.4.2 Sampling steel cylinder and sampling tube shall be vacuum dried. Sample shall be injected into the sampling steel cylinder in liquid phase (except from the determination of non-condensable gas in the gas phase). The sampling size shall not exceed the allowable filling volume of the cylinder.

5.4.3 In terms of non-condensable gas in the gas phase, inject gas phase sample in the packaging container into the sampling steel cylinder. After reaching a pressure balance, it should maintain for 120 s.

5.4.4 Stick a label onto the sampling steel cylinder; indicate the name (indicate gas phase sample and liquid phase sample), model number and batch number of the product; sampling date and the name of the sampler for inspection.

d) The marking of "avoid exposure to the sun" stipulated in GB/T 191.

6.2 Packaging

6.2.1 Trans-1,3,3,3-tetrafluoropropene for industrial use shall be packed in exclusive steel cylinders. Repetitively-used steel cylinder shall be coated with aluminum white paint, with steel seal number and tare of the steel cylinder in red font. Non-repetitively used steel cylinder shall be coated with yellowish green paint.

6.2.2 Product package of each batch of exit-factory trans-1,3,3,3-tetrafluoropropene for industrial use shall be attached with a quality certificate in a certain format, which includes the following content:

a) Manufacturer's name;

b) Product's name and grade;

c) Date of production, or batch No.;

d) Product quality inspection result, or inspection conclusion;

e) Serial number of this Standard.

6.2.3 The filling of steel cylinder shall comply with the stipulations in GB 14193. The filling coefficient of trans-1,3,3,3-tetrafluoropropene shall be not more than 1.20 kg/L.

In addition, the marking of filling shall be pasted in accordance with the requirements.

6.2.4 In terms of steel cylinders which are put into use for the first time, the dryness and cleanliness inside the steel cylinders shall be guaranteed. In terms of repetitively-used steel cylinders, after the usage of the products, positive pressure shall be maintained in the steel cylinders.

6.3 Transportation

Steel cylinders and tank trucks which are filled with trans-1,3,3,3-tetrafluoropropene for industrial use are pressure-containing containers. During the loading, unloading and transportation, they shall be lightly loaded and unloaded. A safety helmet shall be fastened to the containers. Collision, dragging, falling and direct exposure to the sun are strictly prohibited. The transportation shall comply with stipulations of the People's Republic of China on railway and highway regarding the transportation of dangerous goods. In addition, it shall also be attached with "Material Safety Data Sheet (MSDS)" and "Chemical Safety Label".

6.4 Storage

Trans-1,3,3,3-tetrafluoropropene for industrial use shall be stored in a well-ventilated, shady, cool and dry place. It shall not be near any heat sources. Exposure to the sun, the raindrops and corrosive substances is strictly prohibited. […]