GB 30982-2014 PDF in English
GB 30982-2014 (GB30982-2014) PDF English
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Limit of hazardous substances in construction adhesive
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GB 30982-2014: PDF in English GB 30982-2014
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 83.180
G 38
Limit of hazardous substances in construction
adhesive
ISSUED ON: JULY 24, 2014
IMPLEMENTED ON: MAY 01, 2015
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 Terms and definitions ... 4
4 Requirements ... 5
5 Test methods ... 6
6 Inspection rules ... 7
7 Packaging marks ... 8
Annex A (normative) Determination of free formaldehyde content in water-
based construction adhesive ... 9
Annex B (normative) Determination of benzene, toluene and xylene content 17
Annex C (normative) Determination of halogenated hydrocarbon content ... 21
Annex D (normative) Determination of toluene diisocyanate content ... 25
Annex E (normative) Determination of phthalate compound ... 28
Limit of hazardous substances in construction
adhesive
1 Scope
This Standard specifies terms and definitions, requirements for the allowable
limits of hazardous substances to the human body and the environment, test
methods, inspection rules, packaging marks of construction adhesive.
This Standard is applicable to construction adhesive for bonding or sealing.
This Standard is applicable to solvent-based construction adhesive, water-
based construction adhesive and bulk construction adhesive.
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 601-2002, Chemical Reagent - Preparations of Standard Volumetric
Solutions
GB/T 2943, Terms of adhesive
GB/T 6682-2008, Water for analytical laboratory use - Specification and test
methods
GB 18583-2008, Indoor decorating and refurbishing materials - Limit of
harmful substances of adhesives
3 Terms and definitions
For the purposes of this document, the terms and definitions defined in GB/T
2943 as well as the followings apply.
3.1 construction adhesive
adhesive that is used in the construction industry and related fields to bond
adherends together through adhesion
3.2 solvent-based construction adhesive
5.2 Benzene, toluene, xylene
The determination of benzene, toluene and xylene content shall be carried out
in accordance with the provisions of Annex B.
5.3 Halogenated hydrocarbon
The determination of halogenated hydrocarbon content is carried out in
accordance with the provisions of Annex C.
5.4 Toluene diisocyanate
The determination of toluene diisocyanate content is carried out in accordance
with the provisions of Annex D.
5.5 Phthalate compound
The determination of the content of phthalate compound shall be carried out in
accordance with the provisions of Annex E.
The type and content of phthalate compound can also be confirmed and
calculated according to the actual production formula.
5.6 Total volatile organic compound
The total volatile organic compound content is determined in accordance with
the provisions of Annex F of GB 18583-2008.
6 Inspection rules
6.1 Type inspection
All technical requirements listed in this standard are type inspection items.
Under normal production conditions, type inspection shall be carried out at least
once a year. Type inspection shall be carried out when the production formula,
process and raw materials have major changes or when production resumes
after 3 months of suspension.
6.2 Sampling method
Randomly take 3 samples from the same batch of products. Each sample is not
less than 0.5kg.
6.3 Determination of inspection result
Among the 3 samples taken, take 1 sample for determination according to the
provisions of this Standard. If the inspection results of all items meet the
Annex A
(normative)
Determination of free formaldehyde content in water-based construction
adhesive
A.1 Acetylacetone spectrophotometry
A.1.1 Overview
This method specifies the determination of free formaldehyde content in water-
based construction adhesive.
This method is suitable for water-based construction adhesive with free
formaldehyde content greater than 0.05g/kg.
A.1.2 Principle
Use water to dissolve the water-based construction adhesive. Distill free
formaldehyde dissolved in water with water. In acetic acid-ammonium acetate
buffer solution with pH=6, formaldehyde interacts with acetylacetone in distillate.
Quickly generate stable yellow compounds under boiling water bath conditions.
Measure the absorbance at 415nm after cooling. According to the standard
curve, calculate the free formaldehyde content in the sample.
A.1.3 Reagents
Unless otherwise specified, in the analysis, only the confirmed analytically-pure
reagents and distilled water or deionized water or equivalent purity water are
used.
A.1.3.1 Ammonium acetate.
A.1.3.2 Glacial acetic acid: ρ=1.055g/mL.
A.1.3.3 Acetylacetone: ρ=0.975g/mL. Acetylacetone solution: 0.25% (volume
fraction). Weigh 25g of ammonium acetate (A.1.3.1). Add a small amount of
water to dissolve. Add 3mL of glacial acetic acid (A.1.3.2) and 0.25mL of
acetylacetone (A.1.3.3). After mixing, add water to 100mL. Adjust pH=6.0. This
solution is stored at 2°C~5°C and can be stable for one month.
A.1.3.4 Hydrochloric acid solution: 1+5(V+V).
A.1.3.5 Sodium hydroxide solution: 30g/100mL.
based construction adhesive.
This method is suitable for water-based construction adhesive with free
formaldehyde content greater than 0.01g/kg.
A.2.2 Principle
Use water to dilute and extract free formaldehyde in the sample. After
derivatization with 2,4-dinitrophenylhydrazine to form formaldehyde hydrazine,
use high performance liquid chromatograph to determine. Use external
standard method to quantitatively determine.
A.2.3 Reagents and standard solutions
Except for special requirements, all reagents used are analytically-pure. The
water shall meet the requirements of grade one water in GB/T 6682-2008.
A.2.3.1 Reagents
A.2.3.1.1 Acetonitrile (chromatographically pure).
A.2.3.1.2 Phosphoric acid (chromatographically pure, mass fraction is 85%).
A.2.3.1.3 2,4-Dinitrophenylhydrazine (purity is greater than 97%).
A.2.3.1.4 Derivatization reagent: Weigh 0.1g of 2,4-dinitrophenylhydrazine
(A.2.3.1.3) into a 1000mL brown volumetric flask. Add 6mL of phosphoric acid
(A.2.3.1.2), acetonitrile (A.2.3.1.1) to set volume.
A.2.3.1.5 Formaldehyde-2,4-dinitrophenylhydrazone (standard product,
concentration is 1.0mg/mL, molecular formula: C7H6N4O4, relative molecular
weight: 210.15).
A.2.3.2 Standard solution
Use a pipette to accurately pipette 0.5mL of 1.0mg/mL formaldehyde-2,4-
dinitrophenylhydrazone (A.2.3.1.5) into a 50mL volumetric flask. Use
acetonitrile (A.2.3.1.1) to set volume. Set it as the first level standard solution.
Take 20.00mL of the first level standard solution and add it to a 50mL volumetric
flask. Use acetonitrile (A.2.3.1.1) to set volume. Set it as the second level
standard solution.
Take 20.00mL of the second level standard solution and add it to a 50mL
volumetric flask. Use acetonitrile (A.2.3.1.1) to set volume. Set it as the third
level standard solution.
Take 20.00mL of the third level standard solution and add it to a 50mL
volumetric flask. Use acetonitrile (A.2.3.1.1) to set volume. Set it as the fourth
Annex B
(normative)
Determination of benzene, toluene and xylene content
B.1 Principle
The adhesive sample is diluted and injected directly into the gas chromatograph.
After separation by chromatographic column, use hydrogen flame ionization
detector to detect. Use internal standard method to quantitatively determine.
B.2 Reagents and materials
B.2.1 Carrier gas: Nitrogen, purity ≥99.995%.
B.2.2 Fuel gas: Hydrogen, purity ≥99.995%.
B.2.3 Combustion gas: Air.
B.2.4 Auxiliary gas (septum purge and makeup gas): Nitrogen with the same
properties as the carrier gas.
B.2.5 Internal standard substance: The compound is not present in the sample,
and this compound can be completely separated from other components on the
chromatogram. The purity is at least 99% (mass fraction) or the purity is known.
For example: n-undecane, n-tetradecane.
B.2.6 Calibration compound: Benzene, toluene, xylene, with a purity of at least
99% (mass fraction) or the purity is known.
B.2.7 Dilution solvent: Organic solvent used to dilute the sample. It does not
contain any substances that interfere with the test. The purity is at least 99%
(mass fraction) or the purity is known. For example: ethyl acetate.
B.3 Instruments and equipment
B.3.1 Gas chromatograph. The configuration is as follows:
a) Injection port of splitter device, and the lining of the vaporization chamber
can be replaced;
b) Program temperature controller;
c) Detector: Flame ionization detector (FID);
d) Chromatographic column: It shall be able to separate the tested substance
shown in B.2.6 into the chromatograph. Record the retention time of each test
compound.
B.5.2.3 Qualitative analysis
Weigh 0.2g of product sample. Use appropriate amount of diluent (B.2.7) to
dilute the sample. Use the sample injector (B.3.2) to take 1.0μL of the mixed
sample and inject it into the chromatograph. Record the chromatogram.
Compare it with the retention time of the standard test compound determined
by B.5.2.2 to determine whether there is a tested compound.
B.5.3 Calibration
B.5.3.1 Preparation of calibration sample: Weigh a certain amount (to the
nearest of 0.1mg) of various calibration compounds in B.2.6 into the sample
bottle (B.3.3). The weighed mass and the content of various compounds
contained in the sample to be tested shall be in the same order of magnitude.
Then weigh the internal standard substance (B.2.5) of the same order of
magnitude as the compound to be tested into the same sample preparation
bottle. Use an appropriate amount of diluent solvent (B.2.7) to dilute the mixture.
Seal the sample preparation bottle and shake it well.
B.5.3.2 Test of relative correction factor: Under the same chromatographic test
conditions as the test sample, optimize instrument parameters according to
B.5.1. Inject an appropriate amount of calibration mixture into the gas
chromatograph. Record the chromatogram. Respectively calculate the relative
correction factor of each compound according to formula (B.1):
Where,
Ri - Relative correction factor for compound I;
mi - Mass of compound i in calibration mixture, in grams (g);
mis - Mass of internal standard substance in calibration mixture, in grams (g);
Ais - Peak area of internal standard substance;
Ai - Peak area of compound i.
The determination result retains three significant digits.
B.5.4 Determination of sample
Annex C
(normative)
Determination of halogenated hydrocarbon content
C.1 Principle
The sample is directly injected into the gas chromatograph after dilution.
Dichloromethane, 1,2-dichloroethane, 1,1,1-trichloroethane, 1,1,2-
trichloroethane are completely separated from other components by capillary
chromatography column. Use electron capture detector to detect. Use internal
standard method to quantitatively determine.
C.2 Materials and reagents
C.2.1 Carrier gas: Nitrogen, purity ≥99.995%.
C.2.2 Auxiliary gas (septum purge and makeup gas): Nitrogen with the same
properties as the carrier gas.
C.2.3 Internal standard substance: The compound is not present in the sample,
and this compound can be completely separated from other components on the
chromatogram. The purity is at least 99% (mass fraction) or the purity is known.
For example: bromopropane.
C.2.4 Calibration compound: Dichloromethane, 1,2-dichloroethane, 1,1,1-
trichloroethane, 1,1,2-trichloroethane have a purity of at least 99% (mass
fraction) or the purity is known.
C.2.5 Dilution solvent: Organic solvent suitable for diluting samples. It does not
contain any substances that interfere with the test. The purity is at least 99%
(mass fraction) or the purity is known. For example: ethyl acetate, n-hexane.
C.3 Instruments and equipment
C.3.1 Gas chromatograph with the following configuration:
a) Injection port of splitter device. The vaporization chamber lining can be
replaced;
b) Program temperature controller;
c) Electron capture detector (ECD);
d) Chromatographic column: A chromatographic column that can completely
C.4.4 Qualitative analysis
Weigh about 0.2g of sample. Use appropriate amount of diluent to dilute the
sample. Use the sample injector to take 0.2μL of sample solution into the
chromatograph. Record the chromatogram. Compare with the retention time of
the standard test compound determined by C.4.3 to determine whether the
tested compound exists.
C.5 Calibration
C.5.1 Preparation of calibration sample
Respectively weigh a certain amount (to the nearest of 0.1mg) of the calibration
compound into a sample bottle. The weighed mass and the content of various
compounds contained in the sample to be tested shall be in the same order of
magnitude. Then weigh the internal standard of the same order of magnitude
as the test compound in the same sample bottle. Use diluent solvent to dilute
the mixture (the dilution concentration shall be within the linear range of the
instrument detector; if it exceeds the dilution factor, the dilution factor shall be
increased or multiple dilutions shall be made step by step). Seal the sample
bottle and shake well.
C.5.2 Determination of relative correction factor
Under the same chromatographic conditions as the test sample, optimize
instrument parameters according to C.4.2. Inject the appropriate amount of
calibration compound into the gas chromatograph. Record the chromatogram.
Respectively calculate the relative correction factor of each tested compound
according to (C.1):
Where,
Ri - Relative correction factor for compound I;
mi - Mass of compound i in calibration mixture, in grams (g);
mis - Mass of internal standard substance in calibration mixture, in grams (g);
Ais - Peak area of internal standard substance;
Ai - Peak area of compound i.
The determination result retains three significant digits.
Annex D
(normative)
Determination of toluene diisocyanate content
D.1 Principle
The sample is directly injected into the gas chromatograph after dilution. After
separation by chromatographic column, use hydrogen flame ionization detector
to detect. Use internal standard method to calculate the content of toluene
diisocyanate in the sample.
D.2 Materials and reagents
D.2.1 Ethyl acetate: Anhydrous (use 0.5nm molecular sieve to dry), without
ethanol (ethanol content < 200×10-6).
D.2.2 N-tetradecane (chromatographically pure).
D.2.3 Toluene diisocyanate (a mixture of isomers).
D.2.4 Carrier gas: Nitrogen, purity ≥99.995%.
D.2.5 Fuel gas: Hydrogen, purity ≥99.995%.
D.2.6 Combustion gas: Air.
D.2.7 Auxiliary gas (septum purge and makeup gas): Nitrogen with the same
properties as the carrier gas.
D.3 Instruments and equipment
D.3.1 Gas chromatograph with the following configuration:
a) Injection port of splitter device. The gasification chamber lining can be
replaced;
b) Program temperature controller;
c) Detector: Flame ionization detector (FID);
d) Chromatographic column: It shall be able to separate the analyte
sufficiently, such as a polydimethylsiloxane capillary column.
D.3.2 Sample injector: The capacity shall be at least twice the injection volume.
d CAS No. 26761-40-0 is a mixture of isomers of diisodecyl phthalate (DIDP). This substance is suitable
for standard substance.
e CAS No. 68515-49-1 is a mixture of phthalates, containing three types of isomers: diisononyl
phthalate (DINP), diisodecyl phthalate (DIDP), and diisoundecyl phthalate (DIUP), of which the main
component is DIDP.
E.2.3 Standard stock solution: Respectively and accurately weigh an
appropriate amount of phthalate standard products. Use ethyl acetate to
prepare a mixed standard stock solution of which the concentration of dibutyl
phthalate (DBP), butyl benzyl phthalate (BBP), dihexyl phthalate (DNHP),
dioctyl phthalate (DOP) is 5g/L, the concentration of diisononyl phthalate
(DINP), diisodecyl phthalate (DIDP) is 50g/L.
NOTE: The standard stock solution shall be stored in a refrigerator at 0°C~4°C. The validity
period is 6 months.
E.2.4 Standard working solution: Use step-by-step dilution method to prepare
a mixed standard working solution of which the concentration of DBP, BBP,
DNHP, DOP is from 0.5mg/L to 10mg/L, and the concentration of DINP, DIDP
is from 5mg/L to 100mg/L.
NOTE: The standard stock solution shall be stored in the refrigerator at 0°C~4°C. The
validity period is 3 months.
E.2.5 Organic microporous membrane: Pore size is 0.45μm.
E.3 Instruments and equipment
Gas chromatography/mass spectrometry (GC-MS).
E.4 Determination
E.4.1 GC-MS working conditions
Since the test result depends on the instrument used, it is impossible to give
general parameters for chromatographic analysis. The set parameters shall
ensure that the measured component and other components can be effectively
separated during chromatographic determination. The following parameters are
available for reference:
a) Chromatographic column: Quartz capillary column;
b) Temperature program;
c) Carrier gas: Helium, purity ≥99.999%;
d) Sample injection mode: Split injection;
ion (see Table E.2) for peak area integration. DINP and DIDP shall be integrated
after leveling the baselines of the chromatographic peak groups of all their
isomers, respectively. Calculate the sum of their areas. Calculate the content of
each phthalate in the sample according to formula (E.1).
DINP and DIDP contain inseparable isomers. The peaks partially overlap. If
DOP exists at the same time, the DOP peaks will overlap with DINP peaks on
the chromatogram. Therefore, avoid mutual interference between DOP, DINP,
and DIDP when selecting quantitative ions. DOP selects m/z=293. DIDP selects
m/z=307. It may minimize mutual interference.
E.5 Result calculation
The content of each phthalate in the sample is calculated according to formula
(E.1):
Where,
wi - Content of phthalate i in the sample, in milligrams per kilogram (mg/kg);
ρis - Concentration of phthalate i in standard working solution, in milligrams per
liter (mg/L);
Ai - Peak area or sum of peak areas of phthalate i in test solution;
Aib - Peak area or sum of peak areas of phthalate i in blank;
V - Constant volume of test solution, in milliliters (mL);
Ais - Peak area or sum of peak areas of phthalate i in standard working solution;
ms - Mass of sample, in grams (g).
The calculation result is expressed to the single digit. Keep 3 effective digits.
E.6 Lower limit of detection and precision
E.6.1 Lower limit of detection
The lower limits of detection of this method for the content of 6 phthalate esters
are:
DBP, BBP, DNHP, DOP: 10mg/kg;
DINP, DIDP: 50mg/kg.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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