GB/T 14190-2017 English PDF (GBT14190-2017)

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GB/T 14190-2017: Testing methods of fiber grade polyester (PET) chip
GB/T 14190-2017
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 59.060.20
W 50
Replacing GB/T 14190-2008
Testing methods of fiber grade polyester (PET) chip
ISSUED ON. DECEMBER 29, 2017
IMPLEMENTED ON. JULY 01, 2018
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine of the People's Republic of China;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3
1 Scope ... 6
2 Normative references ... 6
3 Terms and definitions ... 7
4 General rules of test ... 8
4.1 Sampling ... 8
4.2 General specifications ... 8
5 Test methods ... 8
5.1 Test methods for intrinsic viscosity ... 8
5.2 Test methods for diethylene glycol ... 15
5.3 Test methods for melting point ... 22
5.4 Test methods for terminal carboxyl groups ... 25
5.5 Test methods for chromaticity ... 29
5.6 Test method for aggregated particles ... 31
5.7 Test methods for moisture ... 32
5.8 Test methods for powder and irregular chip ... 34
5.9 Test methods for titanium dioxide content ... 37
5.10 Test method for ash content ... 42
5.11 Test method for iron content ... 44
5.12 Test report ... 46
Annex A (informative) Numerical relationship between test methods for the
intrinsic viscosity of solvents of two different ratios ... 48
Annex B (informative) Recommended specification for diethylene glycol test
reaction tube ... 49
Testing methods of fiber grade polyester (PET) chip
Warning - Solvents such as phenol, tetrachloroethane, o-cresol, and
methanol used in the test methods are toxic, it shall avoid contact with
skin and inhalation of steam. Reagents such as sulfuric acid,
hydrochloric acid, and hydrogen peroxide are highly corrosive, it shall
avoid contact with the skin. The operator shall take appropriate safety and
health protection measures. When operating the gas chromatograph, if
the detector does not ignite, it is forbidden to open the hydrogen needle
valve to prevent the hydrogen from leaking into the space and causing an
explosion.
1 Scope
This Standard specifies the test methods for each analysis item of fiber grade
polyester (PET) chips.
This Standard applies to fiber grade polyester (PET) chips produced from
terephthalic acid and ethylene glycol. Other differential and functional
polyesters may also refer to this Standard.
2 Normative references
The following referenced documents are indispensable for the application of
this document. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any
amendments) applies.
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 4146 (all parts) Textiles - Man-made fibers
GB/T 6283 Chemical products - Determination of water Karl. Fischer method
(general method)
GB/T 6678 General principles for sampling chemical products
2 times that of the normal chip; less than 1/4 of the conventional particle (or
prescribed size); and of irregular shape.
4 General rules of test
4.1 Sampling
The laboratory samples in batch samples are in accordance with GB/T 6678,
and the sample volume is not less than 0.5 kg.
4.2 General specifications
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 titration solutions, preparations and products used in this
Standard are prepared in accordance with GB/T 601 and GB/T 603 when no
other requirements are specified.
5 Test methods
5.1 Test methods for intrinsic viscosity
5.1.1 Method A (capillary viscometer method)
5.1.1.1 Method summary
DETERMINE the elution time of the solvent at 25 °C and the PET solution at a
concentration of 0.005 g/mL, and CALCULATE the intrinsic viscosity according
to the determined elution time and the solution concentration of the sample.
The capillary viscometer uses 1B to meet the requirements that the kinetic
energy correction term of the viscometer is not considered.
5.1.1.2 Instruments and equipment
5.1.1.2.1 Constant temperature bath. temperature control (25.00 ± 0.05) °C.
5.1.1.2.2 Ubbelohde viscometer. a gas-liquid column Ubbelohde viscometer
(see Figure 1) in accordance with ISO 3105, model number 1B. Other types of
viscometers listed in ISO 3105 can also be used, and the measurement results
shall be guaranteed to be equal to the Ubbelohde viscometer specified above.
In case of dispute, an Ubbelohde viscometer shall be used.
5.1.1.2.3 Erlenmeyer flask with stopper. 100 mL.
WEIGH 0.125 g ~ 0.128 g of sample, accurate to 0.1 mg; PUT it into the sample
dissolution bottle, ADD a certain amount of solvent, to PREPARE the sample
with a concentration of (0.5000 ± 0.0070) g/100 mL; DISSOLVE it on the
heating device. After the sample is dissolved, COOL it to room temperature,
and MEASURE the filtrate with a relative viscometer. If the water content in the
sample is higher than 0.5 %, the treatment method is the same as 5.1.1.4.1; if
the sample contains inorganic materials or other additives, and their mass
fraction exceeds 0.5 %, the mass fraction shall be entered as an impurity into
the instrument parameter setting table.
According to the selected solvent and the corresponding mathematical model,
the instrument automatically calculates the intrinsic viscosity of the sample.
5.1.2.5 Expression of results
The calculation result is expressed as the average value of the test values of
the two parallel samples, and is rounded off to the third decimal place according
to GB/T 8170.
5.1.2.6 Precision
5.1.2.6.1 Repeatability
For the determined values of the two independent test results obtained under
repeatability conditions, when the intrinsic viscosity is 0.630 dL/g ~ 0.720 dL/g,
the absolute difference between the two tests does not exceed the repeatability
limit (0.006 dL/g), and the case where it exceeds the repeatability limit (0.006
dL/g) does not exceed 5 %.
5.1.2.6.2 Reproducibility
The absolute difference between the two independent test results obtained
under reproducibility conditions, when the intrinsic viscosity is 0.630 dL/g ~
0.720 dL/g, is not greater than the reproducibility limit (0.010 dL/g), and the
case where it exceeds the reproducibility limit (0.010 dL/g) does not exceed
5 %.
5.2 Test methods for diethylene glycol
5.2.1 Method A (methanol transesterification method)
5.2.1.1 Method summary
The sample is subjected to a transesterification reaction at high temperature
and in the presence of methanol, diethylene glycol is released, and then the
diethylene glycol content in the filtrate is measured by gas chromatography.
5.2.1.10.2 Reproducibility
The absolute difference between the two independent test results obtained
under reproducibility conditions, when the given diethylene glycol is 0.80 % ~
1.60 %, is not greater than the reproducibility limit (0.08 %), and the case where
it exceeds the reproducibility limit (0.08 %) does not exceed 5 %.
5.2.2 Method B (ethanolamine degradation method)
5.2.2.1 Method summary
The sample is degraded at high temperature and in the presence of
ethanolamine, diethylene glycol is released, and then the diethylene glycol
content in the filtrate is measured by gas chromatography....