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GB/T 33386-2016 PDF in English


GB/T 33386-2016 (GB/T33386-2016, GBT 33386-2016, GBT33386-2016)
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GB/T 33386-2016: PDF in English (GBT 33386-2016)

GB/T 33386-2016
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.080.20
G 17
2,3,3,3-Tetrafluoropropene (HFO-1234yf)
for Industrial Use
ISSUED ON: DECEMBER 30, 2016
IMPLEMENTED ON: JULY 01, 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 method ... 5 
5 Test rules ... 10 
6 Signs, packaging, transportation and storage ... 12 
7 Safety ... 13 
Appendix A (Normative) Typical preparation chromatograms and relative
retention values for the determination of 2,3,3,3-tetrafluoropropene for industrial
use ... 14 
Appendix B (Normative) Typical chromatograms and relative retention values
for the determination of non-condensable gases in the gas phase of 2,3,3,3-
tetrafluoropropene for industrial use ... 16 
Appendix C (Informative) Saturated vapor pressure at different temperatures of
2,3,3,3-tetrafluoropropene for industrial use ... 17 
2,3,3,3-Tetrafluoropropene (HFO-1234yf)
for Industrial Use
1 Scope
This Standard specifies the requirements, test methods, test rules, signs,
packaging, transportation, storage and safety of 2,3,3,3-tetrafluoropropene for
industrial use (HFO-1234yf, also referred to as: R1234yf).
This Standard applies to 2,3,3,3-tetrafluoropropene (HFO-1234yf), which is
refined from raw materials such as tetrachloropropene and pentafluoropropane,
applies gas-phase or liquid-phase methods, reacts with anhydrous hydrogen
fluoride under the action of catalyst, which mainly uses single or mixed working
medium to replace tetrafluoroethane (HFC-134a).
Molecular formula: CF3CF-CH2
Relative molecular mass: 114.05 (according to the international relative atomic
mass in 2013);
2 Normative references
The following documents are indispensable for the application of this document.
For dated references, only the dated version applies to this document. For
undated references, the latest edition (including all amendments) applies to this
document.
GB/T 191, Packaging. Pictorial marking for handling of goods
GB/T 601, Chemical reagent. Preparations of reference titration 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
indication, are identified as analytical reagents and grade-3 water which is
specified in GB/T 6682.
The standard solutions, preparations and products which are used in the test
method shall be prepared according to the provisions of GB/T 601 and GB/T
603 when no other requirements are specified.
4.1 Appearance
Place the liquid-phase sample in a 50 mL dry colorimetric tube. When the liquid-
phase volume of the sample is about 10 mL, use a dry cloth to dry the frost or
moisture that is attached to the outer wall of the colorimetric tube; observe the
color of the sample, whether it’s turbid or not and whether there is solid particle
or not, in a lateral perspective.
4.2 Determination of the content of 2,3,3-tetrafluoropropene
4.2.1 Method summary
Use gas chromatography; under the selected chromatographic conditions, the
sample passes through the column after vaporization, which separates the
components; use hydrogen flame ionization detector (FID) to detect; use
compensating area normalization method to calculate the content of 2,3,3,3-
tetrafluoropropene.
4.2.2 Reagents
4.2.2.1 Nitrogen: the volume fraction is greater than 99.995%.
4.2.2.2 Hydrogen: the volume fraction is greater than 99.995%.
4.2.2.3 Helium: the volume fraction is greater than 99.995%.
4.2.2.4 Air: it is dried and purified by silica gel or molecular sieve.
4.2.3 Instruments
4.2.3.1 Gas chromatograph: it is equipped with hydrogen flame ionization
detector (FID). Take benzene as the sample; the overall sensitivity requires the
detection-limit D ≤ 1 x 10-11 g/s; the stability shall meet the requirements of GB/T
9722; the linear range shall meet the analysis requirements.
4.2.3.2 Recorder: chromatographic workstation or chromatographic data
processor.
4.2.3.3 Sampling cylinder: double-valve small cylinder, of which the volume is
not less than 150 mL, and the working pressure shall be greater than the
pressure of the same product.
4.2.5.1.3 Preparation of the calibration standard sample
According to the pressure of gas of each impurity component, in the order from
low-pressure component to high-pressure component, use a quantitative tube
which has valves at both ends to gradually add gas of each impurity component
to the gas distribution bottle; use 2,3,3,3-tetrafluoropropene as the background
gas, so as to narrow the content of each impurity with the to-be-test sample.
Balance it for 20 min ~ 30 min. The calibration standard sample is valid for 3d
~ 4d.
The mass mi of the gas of the impurity component i, which is expressed in
grams (g), is calculated according to Formula (1):
Where:
Vi -- the volume of the gas of the added impurity component i, in milliliters (mL);
Mi -- the molar mass of the added impurity component i, in grams per mole
(g/mol);
24 450 -- the value of the volume of 1 mol of gas at 25°C and 101.325 kPa (1
atm), in milliliters (mL).
4.2.5.1.4 Calculation of the content of each impurity component in the
calibration standard sample
The mass fraction wi of the impurity component i in the calibration standard
sample is calculated according to Formula (2):
Where:
mi -- the mass of the impurity component i in the calibration standard sample,
in grams (g);
m -- the mass of the background sample in the calibration standard sample, in
grams (g);
4.2.5.1.5 Determination of relative mass correction factor
Take a certain amount of calibration standard sample; measure according to
fHFO-1234yf -- the correction factor of the peak area of 2,3,3,3-tetrafluoropropene;
Ai -- the peak area of the component i;
fi -- relative mass correction factor of the component i.
The arithmetic mean of the results of two parallel determinations is taken as the
report result. The absolute difference between the results of two parallel
measurements shall not be greater than 0.10%.
4.3 Determination of moisture
It shall be performed according to the provisions of Karl Fischer Coulometry of
5.3, or Electrolysis of 5.4 in GB/T 7376-2008. Karl Fischer Coulometry shall be
taken as the arbitration law.
4.4 Determination of acidity
It shall be performed according to provisions of GB/T 33065.
4.5 Determination of evaporation residue
It shall be performed according to provisions of GB/T 33066.
4.6 Determination of non-condensable gas in the gas phase
It shall be performed according to provisions of GB/T 33063. The external
standard method shall be taken as the arbitration law. Typical chromatograms
and relative retention values for the determination of non-condensable gases
in the gas phase of 2,3,3,3-tetrafluoropropene for industrial use are given in
Appendix B. The values of saturated vapor pressure at 25°C are given in
Appendix C.
4.7 Determination of chloride (Cl-)
It shall be performed according to provisions of GB/T 33064.
5 Test rules
5.1 Type inspection
All items which are specified in this Standard are type inspection items. Under
normal production conditions, type inspections shall be conducted at least once
a month. In any of the following cases, type inspection shall also be carried out:
a) when a key production process is updated;
b) when there are changes in the main raw materials;
c) date of manufacture or batch number;
d) product quality inspection results or inspection conclusions;
e) Code of this Standard.
6.2.3 When the cylinder is filled, it shall meet the requirements of GB 14193;
the filling factor of 2,3,3,3-tetrafluoropropene is not more than 0.91 kg/L;
besides, it shall be posted with signs as required.
6.2.4 For the cylinder which is used for the first time, it shall ensure that the
cylinder is dry and clean. For re-used cylinders, a positive pressure shall be
maintained in the cylinder after use.
6.3 Transportation
Since steel cylinders and tank cars which contain 2,3,3,3-tetrafluoropropene for
industrial use are pressurized containers, during loading and unloading and
transportation, they shall be lightly loaded and unloaded; the containers shall
be fastened with helmets; and it is strictly prohibited to hit, drag, drop and direct
sun exposure. The transportation shall comply with the relevant provisions of
the People's Republic of China on the transportation of dangerous goods by
railways and highways, and shall be accompanied by the “Chemical Safety
Technical Data Sheet” and the “Chemical Safety Label”.
6.4 Storage
2,3,3,3-tetrafluoropropene for industrial use shall be stored in a ventilated, cool
and dry place; it cannot be placed near heat sources; and it is strictly prohibited
to be exposed to sunlight, rain and corrosive substances.
7 Safety
7.1 2,3,3,3-tetrafluoropropene for industrial use shall comply with the
requirements of GB 13690.
7.2 The safety of 2,3,3,3-tetrafluoropropene for industrial use, according to the
provisions of GB/T 7778, belongs to A2L.
7.3 When 2,3,3,3-tetrafluoropropene in high concentrations is inhaled, there will
be mild central nervous system depression and arrhythmia (arhythmia). When
its liquids (or rapidly diffusing gases) is contacted, it will cause irritation and
frostbite. Field personnel shall take necessary protective measures and wear
protective equipment.
......
 
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.