GB/T 14190-2017 PDF English
US$455.00 · In stock · Download in 9 secondsGB/T 14190-2017: Testing methods of fiber grade polyester (PET) chip Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedureStatus: Valid GB/T 14190: Evolution and historical versions
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
| GB/T 14190-2017 | English | 455 |
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Testing methods of fiber grade polyester (PET) chip
| Valid |
| GB/T 14190-2008 | English | 959 |
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Test methods of fiber grade polyester chip
| Obsolete |
| GB/T 14190-1993 | English | 639 |
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Analysis methods for fiber grade polyester chip
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GB/T 14190-2017: Testing methods of fiber grade polyester (PET) chip---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT14190-2017
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
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
GB/T 6682 Water for analytical laboratory use - Specification and test
methods
GB/T 8170 Rules of rounding off for numerical values & expression and
judgement of limiting values
ISO 3105 Glass capillary kinematic viscometers - Specifications and
operating instructions
3 Terms and definitions
For the purpose of this document, the terms and definitions defined in GB/T 4146 (all parts) and the following apply.
3.1bright polyester (PET) chip
Polyester (PET) chips that are not matted.
3.2 semi-dull polyester (PET) chip
Polyester (PET) chips of which the titanium dioxide content is greater than 0.20 %
and less than or equal to 0.50 % (mass fraction).
3.3 full dull polyester (PET) chip
Polyester (PET) chips of which the titanium dioxide content is greater than or
equal to 1.50 % (mass fraction).
3.4 agglomerate particle
Particles, in PET chips, that are determined to be greater than or equal to 10 μm.
3.5 irregular chip
Polyester chip (PET) of which the length is greater than or equal to 4 times that
of the normal chip; the thickness, width or diameter is greater than or equal to
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.
5.1.1.3 Solvents
5.1.1.3.4 Selection of solvents
The calculation method for the intrinsic viscosity of PET chips is related to the
solvent used. Two different solvents are available. 5.1.1.3.1, 5.1.1.3.2.
5.1.1.3.5 Solvent stability test
The elution time of the solvent used is measured periodically. If the elution time
of the solvent exceeds 1 % of the initial value (the initial value is the solvent
elution time measured after solvent preparation), the solvent shall be discarded,
and a new solvent shall be prepared.
5.1.1.4 Sample
5.1.1.4.1 WEIGH (0.125 ± 0.005) g of sample to the nearest 0.1 mg, and
PLACE it in an Erlenmeyer flask with stopper. If the water content of the sample
is more than 0.5 %, the sample shall be placed in a vacuum drying oven at a
5.1.1.6 Test procedure
5.1.1.6.1 FILTER the solution through a filter and ADD it to the Ubbelohde
viscometer so that the liquid level is between the liquid filling lines.
5.1.1.7 Calculation of results
5.1.1.7.1 For tests using phenol/1,1,2,2-tetrachloroethane (mass ratio 50.50)
as solvent, calculate the relative viscosity (ηr), the specific viscosity (ηsp) and
the intrinsic viscosity ([η]) according to formula (3) ~ formula (5).
5.1.1.8 Expression of results
The calculation result of the intrinsic viscosity is expressed as the average value
of the test values of the two parallel samples, and rounded off to the third
decimal place according to GB/T 8170.
5.1.1.9 Precision
5.1.1.9.1 Repeatability
For the determined values of 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 %.
5.1.1.9.2 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 %.
5.1.2 Method B (relative viscometer method)
5.1.2.1 Method summary
The PET sample is dissolved in the mixed solvent of phenol and
tetrachloroethane, and then the solution and the blank solvent containing no
sample flow in the two capillaries of the viscometer. The viscometer monitors
the pressure drop p1 of the first solvent reference capillary and the pressure
drop p2 of the second sample capillary. The relative viscosity is obtained from
the ratio of p2 and p1, and the intrinsic viscosity of the sample is obtained by a
mathematical model. The schematic diagram is shown in Figure 2.
5.1.2.2 Solvents
Same as 5.1.1.3.
5.1.2.3 Instruments and equipment
5.1.2.6 Precision
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.
5.2.1.2 Instruments and equipment
5.4.2.7 Expression of results
The calculation result is expressed as the average value of the two test-values,
and is rounded off to one decimal place according to GB/T 8170.
5.4.2.8 Precision
5.4.2.8.1 Repeatability
For the determined values of the two independent test results obtained under
repeatability conditions, when the terminal carboxyl group is 15.0 mol/t ~ 35.0
mol/t, the absolute difference between the two tests does not exceed the
repeatability limit (2.0 mol/t), and the case where it exceeds the repeatability
limit (2.0 mol/t) does not exceed 5 %.
5.5 Test methods for chromaticity
5.5.1 Method A (dry pulverization method)
5.5.1.1 Method summary
After the sample is dried and pulverized, the chromaticity of the sample is tested
with an automatic color difference meter, and the results are expressed in
HunterLab color systems L, a, and b.
NOTE. The color value test can only be compared if the materials are the same, the chip dicing,
size and appearance are basically the same, the instrument geometry is the same and the
viewing hole surface is close.
5.5.1.2 Instruments and equipment
5.5.1.2.1 Color difference meter. D65 light source, 10° angle of view, 0°/45° or
45°/0° light path geometry, HunterLab color system, it is recommended to use
45 mm ~ 52 mm viewing hole surface.
5.5.1.2.2 Sample cup. quartz glass.
5.5.1.2.3 Air drying oven.
5.5.1.2.4 Sample sieve. 833 μm and 350 μm.
5.5.1.3 Test procedure
5.5.1.3.1 PLACE the sample in the air dying oven, HEAT the bright PET chip at
(140 ± 5) °C for 60 min; HEAT the semi-dull PET chip and full dull PET chip at
(135 ± 5) °C for 30 min. After taking out the cooling, it was pulverized and sieved
to obtain particles of 350 μm to 833 μm.
NOTE. Chips that are not crystallized or have a very slow rate of crystallization can also be
measured directly.
5.5.1.3.2 PLACE the sieved sample particles in the sample cup, make the
sample tightly packed; PLACE it on the measuring hole, determine the
chromaticity (L value, a value and b value) of the sample. The measurement is
carried out every about 120° of rotation, and a total of three points are
measured.
5.6 Test method for aggregated particles
5.6.1 Method summary
The aggregated particles in the sample are observed under a microscope, the
size is measured, and the number is counted.
5.6.2 Instruments and equipment
5.6.2.1 Microscope (magnification 200 times to 400 times) and microscope
illumination.
5.6.2.2 Slicer. the division value is 1 μm.
5.6.2.3 Balance. the minimum division value is 0.1 mg.
5.6.2.4 Cover slip. the thickness is 0.17 mm.
5.6.2.5 Medical tweezer and scissor.
5.6.2.6 Micrometer. the division value is 0.01 mm.
5.6.2.7 Slide. the thickness is 1 mm.
5.6.3 Reagents
Oil or wetting agent of which the refractive index is close to nD20 = 1.51.
5.6.4 Test procedure
5.6.4.1 Randomly TAKE five PET chips from the sample, and CUT each chip
into 5 to 8 pieces of slices with a thickness of 20 μm with the slicer, so that the
total mass of the sliced slices reaches 3 mg ~ 5 mg, to the nearest 0.1 mg.
PLACE the slices on a clean glass slide, WET them well with reagents (or other
physical means), PRESS the cover slip tightly against the sample to form a flat
surface.
5.6.4.2 PLACE the slide containing the slices on the microscope stage,
ADJUST the focal length of the microscope, and OBSERVE the aggregated
particles larger than or equal to 10 μm (or the required size) with transmitted
light. Round particles are measured and counted by their diameter, and
particles of other shapes are measured and counted by the longest part.
5.6.5 Calculation of results
The aggregated particle is calculated according to formula (10).
5.11.5 Test procedure
5.11.5.1 ADD 5 mL of hydrochloric acid solution to the residue after ashing,
HEAT to dissolve, COOL and FILTER into a 100 mL beaker with filter paper,
and WASH the filter paper with approximately 40 mL of distilled water to the
beaker.
5.11.5.2 MEASURE the absorbance of the sample solution according to the
procedure of 5.11.1.2, 5.11.4.3.
5.11.6 Calculation of results
The iron content is calculated according to formula (18).
5.11.7 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 one decimal place according to GB/T 8170.
5.11.8 Precision
5.11.8.1 Repeatability
For the determined values of the two independent test results obtained under
repeatability conditions, when the iron content is 0.5 mg/kg ~ 4.0 mg/kg, the
absolute difference between the two tests does not exceed the repeatability
limit (0.5 mg/kg), and the case where it exceeds the repeatability limit (00.5
mg/kg) does not exceed 5 %.
5.11.8.2 Reproducibility
The absolute difference between the two independent test results obtained
under reproducibility conditions, when the iron content is 0.5 mg/kg ~ 4.0 mg/kg,
is not greater than the reproducibility limit (1.0 mg/kg), and the case where it
exceeds the reproducibility limit (1.0 mg/kg) does not exceed 5 %.
5.12 Test report
The test report shall include.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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