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GB/T 46510-2025: Determination of free formaldehyde in water-based material of toys - High performance liquid chromatography
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GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 97.200.50 CCS Y 57 GB/T 46510-2025 Determination of free formaldehyde in water-based material of toys - High performance liquid chromatography Issued on: OCTOBER 05, 2025 Implemented on: OCTOBER 05, 2025 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... 4 4 Method summary... 4 5 Reagents and materials... 5 6 Instruments and equipment... 5 7 Sample extraction... 6 8 Determination... 6 9 Calculation of results... 7 10 Limit of quantitation... 7 11 Precision... 7 12 Test report... 7 Annex A (informative) Reference conditions for liquid chromatography of free formaldehyde... 8 Annex B (informative) Liquid chromatogram of formaldehyde derivatives... 9 Annex C (informative) Precision test results... 10 Determination of free formaldehyde in water-based material of toys - High performance liquid chromatography Warning -- Use of this document can involve hazardous materials, operations, and equipment. This document does not purport to address all safety problems associated with their use. It is the responsibility of the user of this document to take appropriate measures to ensure the safety and health of personnel prior to application of the document and to determine the applicability of any restrictions for this purpose.1 Scope
This document describes the high-performance liquid chromatography (HPLC) method for the determination of free formaldehyde in water-based materials of toys. This document applies to the determination of free formaldehyde in water-based materials of toys such as bubble solution, finger paint, ink, and water-based gels. Other materials of toys can also be tested using this method after validation. NOTE. Toys made of water-based gel materials, such as slime and artificial water.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 6682 Water for analytical laboratory use - Specification and test methods3 Terms and definitions
This document does not contain any terms or definitions that need to be defined.4 Method summary
Weigh an appropriate amount of sample and extract by vortexing with an aqueous phosphoric acid solution. Free formaldehyde in the extract is separated by high- performance liquid chromatography (HPLC), derivatized post-column, detected at a specific wavelength, and quantified using the external standard method. NOTE. Other validated methods (such as pre-column derivatization-HPLC) can also be used to determine free formaldehyde in the extract.5 Reagents and materials
Unless otherwise specified, use only analytical grade reagents. 5.1 Water, GB/T 6682, grade 1. 5.2 Formaldehyde. Standard solution, CAS No.. 50-00-0. 5.3 Phosphoric acid, 85 % by mass. 5.4 Ammonium acetate. 5.5 Glacial acetic acid. 5.6 Acetylacetone. 5.7 Aqueous phosphoric acid solution. Take 2 mL of phosphoric acid (5.3), slowly add it to 998 mL of water, mix well, and adjust the pH to 2.0 ± 0.1. 5.8 Post-column derivatization solution. Weigh 62.5 g of ammonium acetate (5.4), add 7.5 mL of glacial acetic acid (5.5), 5 mL of acetylacetone (5.6), add water to 1000 mL, and shake well. This solution is effective for 3 days. 5.9 Formaldehyde series standard solutions. Accurately transfer an appropriate amount of formaldehyde standard solution (5.2) into 10 mL volumetric flasks, and dilute with phosphoric acid aqueous solution (5.7) to prepare a series of standard solutions of 0.05 mg/L, 0.1 mg/L, 0.2 mg/L, 0.5 mg/L, 1.0 mg/L, 2.0 mg/L, 5.0 mg/L, and 10.0 mg/L. Prepare before use. The concentration range of the standard solutions can be adjusted according to the sample content level during actual testing. 5.10 Filter membrane. 0.45 μm, aqueous phase.6 Instruments and equipment
6.1 High-performance liquid chromatograph with diode array detector. 6.2 Post-column derivatization apparatus. 6.3 Vortex mixer. 6.4 Analytical balance. Accuracy 0.1 mg. 6.5 Stoppered colorimetric tubes. 6.6 Pipettes. Capacity 10 μL ~ 100 μL, capacity 100 μL ~ 1000 μL, and capacity 1 mL ~ 5 mL. 6.7 Volumetric flasks.7 Sample extraction
Weigh 0.2 g (accurate to 0.1 mg) of sample into a 10 mL stoppered colorimetric tube (6.5), shake well, add phosphoric acid aqueous solution (5.7) to the mark, and vortex for 1 min. If necessary, purify the extract using a suitable purification method. Filter the extract through a 0.45 μm microporous membrane; the filtrate is used as the test solution. The test solution shall be tested within 12 h.8 Determination
8.1 Instrumental determination conditions Since the test results depend on the instrument used, universal parameters for chromatographic analysis cannot be provided. The parameters set shall ensure effective separation of the analyte from other components during determination. See Annex A for specific examples. 8.2 Qualitative and quantitative analysis 8.2.1 Qualitative analysis Analyze the standard solution and sample solution according to the above analytical conditions (8.1). Qualitative analysis is performed using the retention time and spectrum of the chromatographic peaks. The chromatogram and retention time of formaldehyde derivatives are shown in Annex B. 8.2.2 Quantitative analysis Quantitative analysis is performed using the external standard method. A linear regression is performed with the concentration of the series of standard solutions as the abscissa and the peak area of the formaldehyde derivative as the ordinate to establish a standard curve and obtain the regression equation. The mass concentration of free formaldehyde in the test solution is obtained from the standard curve. The content of free formaldehyde in the sample is calculated according to Clause 9. If the measured free formaldehyde content exceeds the range of the standard curve, it shall be diluted with phosphoric acid aqueous solution (5.7) and reanalyzed. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
