GB 33372-2020 PDF English
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| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
| GB 33372-2020 | English | 165 |
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Limit of volatile organic compounds content in adhesive
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| GB/T 33372-2016 | English | 879 |
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Limit of volatile organic compound content in adhesives
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GB 33372-2020: Limit of volatile organic compounds content in adhesive---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/GB33372-2020
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 83.180
G 39
Replacing GB/T 33372-2016
Limit of volatile organic compounds content in
adhesive
Issued on: MARCH 04, 2020
Implemented on: DECEMBER 01, 2020
Issued by. State Administration for Market Regulation;
Standardization Administration of the People’s Republic of
China.
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative references... 4
3 Terms and definitions... 5
4 Classification... 5
5 Limit of VOC content... 5
6 Test method... 8
7 Inspection rules... 8
8 Labels for packages... 9
Appendix A (Normative) Determination of VOC content in solvent-based
adhesive... 10
Appendix B (Normative) Determination of water content in adhesive... 12
Appendix C (Normative) Determination of acetone, methyl acetate and dimethyl
carbonate... 17
Appendix D (Normative) Determination of VOC content in water-based
adhesive... 21
Appendix E (Normative) Determination of VOC content in bulk adhesive... 26
1 Scope
This Standard specifies the limit requirements, test methods, inspection rules
and packaging marks of volatile organic compounds (hereinafter referred to as
VOC) content in adhesive under specified conditions.
This Standard applies to the limitation of volatile organic compounds content in
solvent-based, water-based and bulk adhesives.
This Standard does not apply to.
-- adhesives that are used as intermediates or as raw materials for
production without entering the circulation field;
-- adhesives for testing or evaluation in any research and development,
quality assurance or analytical laboratory;
-- urea formaldehyde, phenolic formaldehyde, melamine formaldehyde
adhesives;
-- special functional surface treatment agent that is applied when materials
are bonded.
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 2793, The method for determination of nonvolatile content of adhesives
GB/T 2943, Terms of adhesive
GB/T 6682, Water for analytical laboratory use - Specification and test
methods
GB/T 13354, Test method for density of adhesives in fluid form - Method of
weight cup
GB 19340, Adhesives for footwear and case and bag
GB/T 20740, Adhesive - Sampling
GB 30982, Limit of hazardous substances in construction adhesive
GB 37822, Standard for fugitive emission of volatile organic compounds
HG/T 2492-2018, Ethyl α-cyanoacrylate instantaneous adhesives
3 Terms and definitions
Terms and definitions determined by GB/T 2943, GB 37822 and the following
ones are applicable to this document.
3.1 Volatile organic compounds content
VOC content
The measured mass of the volatile organic compounds per unit volume or mass
of the adhesive under the specified conditions.
3.2 Solvent-based adhesive
Adhesive that uses volatile organic solvent as the main dispersion medium.
3.3 Water-based adhesive
Adhesive that uses water as the main dispersion medium.
3.4 Bulk adhesive
Adhesive whose dispersion medium content is less than 5% of the total.
4 Classification
According to different dispersion media and contents in adhesive products, it is
divided into three types. solvent-based, water-based, and bulk.
Note. in general, water-based adhesive and bulk adhesive are low-VOC
adhesives.
5 Limit of VOC content
5.1 Basic requirements
5.1.1 The content of single volatile organic compounds, such as benzene series
(benzene, toluene and xylene), halogenated hydrocarbons (dichloromethane,
1,2-dichloroethane, 1,1,1-trichloroethane, 1,1,2-trichloroethane), toluene
diisocyanate, free formaldehyde, in adhesive products shall meet the
requirements of GB 30982 or GB 19340.
5.1.2 For adhesive products which are expressly used for a variety of purposes,
take the lowest limit of each requirement.
5.2 Limit of VOC content in solvent-based adhesive
The limit of the VOC content in solvent-based adhesive shall meet the
requirements of Table 1.
6 Test method
6.1 Sampling
Adhesive product sampling shall be carried out in accordance with GB/T 20740.
6.2 Determination of VOC content
6.2.1 The determination of VOC content in solvent-based adhesive shall be
performed according to Appendix A.
6.2.2 The VOC content in water-based adhesive shall be determined in
accordance with the provisions of Appendix D.
6.2.3 The VOC content in bulk adhesive shall be determined in accordance with
the provisions of Appendix E.
7 Inspection rules
7.1 Inspection items
7.1.1 All requirements that are listed in this Standard are type inspection items.
7.1.2 Under normal production conditions, type inspection shall be carried out
at least once a year.
7.1.3 Type inspection shall be carried out in any of the following cases.
-- when a new product is initially finalized;
-- when the product is produced off-site;
-- when there are major changes in production formulas, processes, and key
raw material sources;
-- when production is resumed after 3 months of suspension.
7.2 Product sampling
Randomly select three samples from the same batch of products, each of which
is not less than 0.5 kg.
8 Labels for packages
Adhesive products that pass the inspection according to this Standard shall be
clearly indicated that the product meets this Standard on the packaging or the
product documentation.
Appendix A
(Normative)
Determination of VOC content in solvent-based adhesive
A.1 Overview
Place an appropriate amount of the adhesive in a blast drying oven at a
constant temperature; measure the amount of the volatiles in the adhesive
within a prescribed time. Use the gas chromatography to determine the content
of low photochemical reaction compounds; use Karl Fischer method or gas
chromatography to determine the water content in the adhesive; subtract the
water content and the acetone, methyl acetate and dimethyl carbonate amount
from the amount of the volatiles in the adhesive, to obtain the VOC content in
the adhesive.
A.2 Test steps
A.2.1 General
Perform two parallel determinations for all tests.
A.2.2 Density
Prepare the mixed sample according to the matching requirements that are
expressed by the adhesive product; after stirring well, measure the density of
the sample according to the method that is specified in GB/T 13354, at a test
temperature of (23 ± 2) °C.
A.2.3 Volatile content of the sample
A.2.3.1 One-component sample
Determine the non-volatile content of the sample according to the method that
is specified in GB/T 2793.
A.2.3.2 Multi-component sample
According to the matching requirements that is expressed by the adhesive
product, take about 2 g of the mixed sample; stir it well quickly; then, measure
the non-volatile content of the sample within 5 minutes according to the method
that is specified in GB/T 2793.
A.2.3.3 Volatile content of the sample
Calculate the volatile content of the sample according to Formula (A.1).
Where.
A.2.4 Water content
Perform the determination in accordance with Appendix B.
A.2.5 Acetone, methyl acetate and dimethyl carbonate content
Perform the determination in accordance with Appendix C.
A.2.6 VOC content
Perform the calculation of VOC content in solvent-based adhesive according to
Formula (A.2).
Appendix B
(Normative)
Determination of water content in adhesive
B.1 Overview
For the water content in the adhesive, use the gas chromatography or the Karl
Fischer method to determine; the gas chromatography is the arbitration method.
B.2 Gas chromatography
B.2.1 Reagents and materials
B.2.1.1 Distilled water. in accordance with the requirements of grade-3 water in
GB/T 6682.
B.2.1.2 Dilution solvent. anhydrous N, N-dimethylformamide (DMF), analytical
reagent.
B.2.1.3 Internal standard. anhydrous isopropanol, analytical reagent.
B.2.1.4 Carrier gas. hydrogen, helium or nitrogen, the purity is not less than
99.995%.
B.2.2 Apparatus
B.2.2.1 Gas chromatograph. equipped with a thermal conductivity detector and
a programmed heating controller.
B.2.2.2 Chromatographic column. a stainless-steel column whose length is 1 m
and outer diameter is 3.2 mm; it is filled with polymer porous microspheres of
177 μm ~ 250 μm. (For programmed heating, the initial temperature of the
column is 80 °C; the holding time is 5 min; the heating rate is 30 °C/min; the
termination temperature is 170 °C; the holding time is 5 min. For the constant
temperature, the column temperature is 140 °C; after the isopropanol peak is
completed, adjust the column temperature to 170 °C, to wait for the completion
of DMF peak. If the test is continued, lower the column temperature to 140 °C
again.)
B.2.2.3 Recorder.
B.2.2.4 Injector. micro-syringe, 10 μL.
B.2.2.5 Stoppered glass bottle. 10 mL.
B.2.2.6 Balance. accuracy of 0.1 mg.
B.2.3 Test steps
B.2.3.1 Determination of response factor R of water
In the same stoppered glass bottle, weigh about 0.2 g of distilled water and
about 0.2 g of isopropanol (accurate to 0.1 mg); add 2 mL of N, N-
dimethylformamide; mix well. Use a micro-syringe to take 1 μL of the standard
mixture; inject it into the chromatograph; record its chromatogram.
Calculate the response factor R of water according to Formula (B.1).
B.2.3.2 Determination of water content
Weigh 0.6 g of the stirred-well sample and 0.2 g of isopropanol (accurate to 0.1
mg); add to a stoppered glass bottle; then, add 2 mL of N, N-dimethylformamide;
cover the stopper; at the same time, prepare isopropanol without sample AND
N, N-dimethylformamide as the blank sample. Shake the bottle that contains
the sample vigorously; let it stand for 15 minutes to precipitate; or use a low-
speed centrifuge to make it precipitate. Draw 1 μL of supernatant from the
sample bottle; inject it into the chromatograph; record its chromatogram.
Calculate the mass fraction of water wH2O in the sample according to Formula
(B.3).
B.3 Karl Fischer method
B.3.1 Instruments and apparatuses
B.3.1.1 Karl Fischer moisture titrator.
B.3.1.2 Balance. accuracy of 0.1 mg.
B.3.1.3 Micro-syringe. 10 μL.
B.3.1.4 Dropping bottle. 30 mL.
B.3.1.5 Magnetic stirrer.
B.3.1.6 Beaker. 100 mL.
B.3.1.7 Petri dish.
B.3.2 Reagent
B.3.2.1 Distilled water. in accordance with the requirements of grade-3 water in
GB/T 6682.
B.3.2.2 Karl Fischer reagent. use appropriate reagents (for samples that do not
contain aldehyde and ketone compounds, the main components of the reagents
are iodine, sulfur dioxide, methanol, and organic bases. For samples that
contain aldehyde and ketone compounds, use special reagents for aldehyde
and ketone, whose main components are iodine, imidazole, sulfur dioxide, 2-
methoxyethanol, 2-chloroethanol and trichloromethane.
B.3.3 Test steps
B.3.3.1 Concentration calibration of Karl Fischer titrant
Add fresh Karl Fischer solvent into the titration cup of the titrator until the liquid
surface covers the electrode tip; use Karl Fischer titrant to titrate to the end
point (drift value < 10 μg/min). Use a micro-syringe to inject 10 μL of distilled
water into the titration cup; use the weight reduction method to obtain the mass
of the water (accurate to 0.1 mg); enter the mass into the titrator; use Karl
Fischer titrant to titrate to the end point; record the instrument displayed
calibration results.
Repeat the calibration until the difference between the two adjacent calibration
values is less than 0.01 mg/mL; find the average value of the two calibrations;
enter the calibration results into the titrator.
When the relative humidity of the test environment is less than 70%, it shall be
calibrated once a week; when the relative humidity is greater than 70%, it shall
be calibrated twice a week; if necessary, calibrate at any time.
Appendix C
(Normative)
Determination of acetone, methyl acetate and dimethyl carbonate
C.1 Principle
Directly inject the sample into the gas chromatograph after dilution; use
chromatographic column to separate it; then, use a hydrogen flame ionization
detector to detect; use the internal standard method to quantify.
C.2 Materials and reagents
C.2.1 Carrier gas. nitrogen, purity ≥ 99.995%.
C.2.2 Fuel gas. hydrogen, purity ≥ 99.995%.
C.2.3 Combustion-supporting gas. air.
C.2.4 Auxiliary gas (separate purge and makeup gas). nitrogen that has the
same properties as the carrier gas.
C.2.5 Internal standard. a compound that does not exist in the sample; the
compound can be completely separated from other components on the
chromatogram; the purity is at least 99% or known. Such as. n-heptane, n-
pentane and so on.
C.2.6 Calibration compounds. acetone, methyl acetate, dimethyl carbonate,
whose purity is at least 99% or known.
C.2.7 Dilution solvent. the organic solvent that is used to dilute the sample (it
does not contain any substance that interferes with the test); the purity is at
least 99% or known. Such as. ethyl acetate, n-hexane, etc.
C.3 Instruments and apparatuses
C.3.1 Gas chromatograph, which has the following configuration.
-- inlet of the split device; the lining of the vaporization chamber can be
replaced;
-- programmed heating controller;
-- detector, flame ionization detector;
-- chromatographic column, which shall be able to separate the analyte
sufficiently. Such as polydimethylsiloxane capillary columns, 6%
cyanopropylphenyl and 94% polydimethylsiloxane capillary columns,
polyethylene glycol capillary columns or equivalent models.
C.3.2 Injector. the capacity is at least twice the injection volume.
C.3.3 sample bottle. glass bottle of about 10 mL, with a sealable cap.
C.3.4 Balance. accuracy of 0.1 mg.
C.4 Gas chromatographic conditions
The gas chromatographic conditions are shown as below.
-- chromatographic column. polydimethylsiloxane capillary column, 30 m ×
0.32 mm × 1 μm;
-- temperature of the sample injector. 240 °C;
-- detector temperature. 280 °C;
-- column temperature. hold the initial temperature of 50 °C for 5 min; then,
rise the temperature to 280 °C at 10 °C/min; keep it for 5 min.
-- carrier gas flow velocity. 1.0 mL/min;
-- fuel gas flow velocity. 40 mL/min;
-- combustion-supporting gas flow velocity. 400 mL/min;
-- split ratio. 20.1;
-- injection volume. 1.0 μL.
Note. The best gas chromatography test conditions can also be selected
according to the performance of the used instrument and the actual
situation of the to-be-tested sample.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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