GB/T 33387-2016 PDF English
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Trans-1,3,3,3-tetrafluoropropene [HFO-1234ze(E)] for Industrial Use
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GB/T 33387-2016: PDF in English (GBT 33387-2016) GB/T 33387-2016
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.080.20
G 17
Trans-1,3,3,3-tetrafluoropropene [HFO-1234ze(E)] for
Industrial Use
[HFO-1234ze(E)]
ISSUED ON: DECEMBER 30, 2016
IMPLEMENTED ON: JULY 1, 2017
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of the People’s Republic of
China.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative References ... 4
3 Requirements ... 5
4 Test Methods ... 6
5 Inspection Rules ... 11
6 Marking, Packaging, Transportation and Storage ... 12
7 Safety ... 14
Appendix A (normative) Typical Preparation Chromatogram and Relative
Retention Value of the Content Determination of Trans-1,3,3,3-
tetrafluoropropene for Industrial Use ... 15
Appendix B (normative) Typical Chromatogram and Relative Retention Value
of the Content Determination of Non-condensable Gas in the Gas Phase of
Trans-1,3,3,3-tetrafluoropropene for Industrial Use ... 18
Appendix C (informative) Saturated Vapor Pressure of Trans-1,3,3,3-
tetrafluoropropene for Industrial Use at Different Temperatures ... 20
Trans-1,3,3,3-tetrafluoropropene [HFO-1234ze(E)] for
Industrial Use
1 Scope
This Standard stipulates the requirements, test methods, inspection rules, marking,
packaging, transportation, storage and safety for trans-1,3,3,3-tetrafluoropropene
[HFO-1234ze(E), which may also be referred to as: R1234ze(E)].
This Standard is applicable to trans-1,3,3,3-tetrafluoropropene [HFO-1234ze(E)],
which is refined through tetrachloropropene and pentafluoropropane as the raw
materials, through gas phase method or liquid phase method, and through the reaction
with anhydrous hydrogen fluoride under the effect of catalyst. It mainly replaces
tetrafluoroethane (HFC-234a) through single working medium or mixing working
medium.
Molecular formula: CF3CH=CFH
Relative molecular mass: 114.05 (in accordance with the international relative atomic
mass in 2013)
2 Normative References
The following documents are indispensable to the application of this document. In
terms of references with a specific date, only versions with a specific date are
applicable to this document. In terms of references without a specific date, the latest
versions (including all the modification lists) are applicable to this document.
GB/T 191 Packaging - Pictorial Marking for Handling of Goods
GB/T 601 Chemical Reagent - Preparations of Standard Volumetric Solutions
GB/T 603 Chemical Reagent - Preparations of Reagent Solutions for Use in Test
Methods
GB/T 6681-2003 General Rules for Sampling Gaseous Chemical Products
GB/T 6682 Water for Analytical Laboratory Use - Specification and Test Methods
GB/T 7376-2008 Determination of Micro-amounts of Water in Industrial Fluorinated
Alkane
GB/T 7778 Number Designation and Safety Classification of Refrigerants
4 Test Methods
Warning---some test processes stipulated in this Standard might lead to
dangerous situations, users shall adopt appropriate safety and health protection
measures.
When no other requirements are indicated regarding the reagents and water used in
the test methods, they shall all refer to reagents which are confirmed as analytically
pure, and Grade-3 water stipulated in GB/T 6682.
When no other requirements are indicated regarding the standard solutions, prepared
solutions and products used in the test methods, they shall all be prepared in
accordance with the stipulations in GB/T 601 and GB/T 603.
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
4.2.2.1 Nitrogen: volume fraction is more than 99.995%.
4.2.2.2 Hydrogen: volume fraction is more than 99.995%.
4.2.2.3 Helium: volume fraction is more than 99.995%.
4.2.2.4 Air: dried and purified through silica gel or molecular sieve.
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 Inspection Rules
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.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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