GB 30982-2014Limit of hazardous substances in construction adhesive (English PDF)

1 Scope

GB 30982-2014 is the Chinese national standard on limit of hazardous substances in construction adhesive, in the field of rubber and plastic industries. It carries no /T suffix, which in the Chinese system means compliance is mandatory: a product or a practice within its scope has to meet it to be lawfully made, sold or carried out in China. It was issued on 24 July 2014 by the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China; Standardization Administration of China, and has been in force since 1 May 2015. Classification: ICS 83.180, CCS G38. This page is published from the official record of the standard held by the Chinese standards administration: the identification, the dates, the classification and the issuing body are taken from there. The clause text, the tables and the numeric limits are in the document itself, which is delivered complete in English translation.

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: rho=1.055g/mL. A.1.3.3 Acetylacetone: rho=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%;

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Notes and Explanations

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