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1 Translated English of Chinese Standard: YC/T ICS X 85 Record Number: Tobacco Industry Standard of the People s Republic of China YC Determination of volatile organic compounds in cigarette carton and packet packaging papers - Headspace-gas chromatography 卷烟条与盒包装纸中挥发性有机化合物的测定顶空 - 气相色谱法 Issued on: October 13, 2006 Implemented on: October 13, 2006 Issued by: State Tobacco Monopoly Administration Page 1 of 16
2 Table of Contents Foreword Scope Principle Reagents and materials Instruments and conditions Warning Sampling Procedure Calculation Precision and accuracy Test report Annex A Annex B Annex C Page 2 of 16
3 Foreword The Annex A, Annex B, and Annex C of this Standard are informative. This Standard was proposed by the State Tobacco Monopoly Administration. This Standard shall be under the jurisdiction of the National Standardization Technical Committee on Tobacco (TC 144). Drafting organizations of this Standard: Shanghai Tobacco (Group) Corporation, Zhengzhou Tobacco Research Institute, China Tobacco Standardization Research Center, Guangdong Cigarette Factory, and China National Tobacco Quality Supervision and Inspection Center. Main drafters of this Standard: Zhang Longgen, Sun Wenliang, Liu Huimin, Han Yunhui, Shen Guanglin, Xie Yan, Chen Zaigen, Li Qingchang, Kong Haohui, and Lu Yifeng. Page 3 of 16
4 Determination of volatile organic compounds in cigarette carton and packet packaging papers - Headspace-gas chromatography 1 Scope This Standard specifies the determination method [headspace-gas chromatography (HS-GC)] of volatile organic compounds [benzene, toluene, ethylbenzene, xylene (o-, m-, p-), ethanol, isopropanol, n-butanol, acetone, 4-methyl-2-pentanone, butanone, cyclohexanone, ethyl acetate, n-propyl, N-butyl acetate ester, Isopropyl acetate, and Propylene glycol methyl ether (1-methoxy-2-propanol, 2-methoxy-1-propanol)] in cigarette carton and packet packaging papers. This Standard applies to cigarette carton and packet packaging papers. Other printed or coated papers can also refer to this Standard. 2 Principle In a closed container and under certain temperature, there exists a distribution equilibrium between the gas phase (headspace) and the matrix (liquid- or solid-phase) of the volatile components in the sample. When the equilibrium is reached, ACCESS the gas-phase portion INTO gas chromatograph for separation. After the matrix is corrected, it can determine the content of each volatile component in the sample. 3 Reagents and materials The following reagents shall be analytically pure. 3.1 Standard samples Benzene (C 5 H 6 ) Toluene (C 7 H 8 ) Ethylbenzene (C 8 H 10 ) Xylene (C 8 H 10 ) Ethanol (C 2 H 6 O). Page 4 of 16
5 3.3.5 ADD 50.00mL of 4th-level standard solution (3.3.4) into a 250mL volumetric flask. DILUTE with glyceryl triacetate (3.2) to constant volume as the 5th-level standard solution The standard solutions should be placed in the refrigerator (-18 C) for storage, valid for six months. When it is used, PLACE them at room temperature. They can be used after it reaches the room temperature. 4 Instruments and conditions 4.1 Headspace instruments Static headspace instrument (HS) Headspace vial: 20mL~25mL Sample loop: 3.0mL Sample equilibrium temperature: 80 C Sample-loop temperature: 100 C Transmission line temperature: 120 C Sample equilibrium time: 45.0min Pressure applied on sample vial: 138kPa Pressurization time: 0.20min Inflation time: 0.20min Equilibrium time of sample-loop: 0.05min Injection time: 1.0min. 4.2 Gas chromatography VOC capillary column (VOCOL column or an equivalent column), 60m 0.32mm (inner diameter) 1.8μm (thickness) Carrier gas: helium (He) Inlet temperature: 150 C Constant-current mode, column flow of 3.8mL/min, split ratio of 10: Programmed temperature-rise: 40 C. MAINTAIN for 2min. Then RAISE the Page 6 of 16
6 6.2 Sample preparation Sample preparation is carried out under room temperature and normal pressure. Sample preparation shall be quick and accurate, and ensure that the sample is not contaminated. For each sample, it shall prepare 2 parallel samples Hard packet packaging paper: TAKE a piece of hard packet packaging papers. With reference to the printing indentations, CUT the main package surface accurately (see Annex A). The area is 22.0cm 5.5cm. ROLL the cut sample INTO cylinder shape with the printed surface face-inward. PUT it into headspace vial (4.1.2) immediately. ADD 1000μL of glyceryl triacetate (3.2), SEAL for test Soft packet packaging paper: TAKE a sheet of soft packet packaging papers (see Annex B). The area is 15.5cm 10.0cm. FOLD the cut sample INTO cylinder shape with the printed surface face-outward. PUT it into headspace vial (4.1.2) immediately. ADD 1000μL of glyceryl triacetate (3.2), SEAL for test Carton packaging paper: TAKE a sheet of carton packaging paper. Accurately CUT a sample of 22.0cm 5.5cm in front of and central region of the package (see Annex C). ROLL the cut sample INTO cylinder shape with the printed surface face-inward. PUT it into headspace vial (4.1.2) immediately. ADD 1000μL of glyceryl triacetate (3.2), SEAL for test. 7 Procedure 7.1 Qualitative analysis TAKE one standard sample for headspace-gas chromatograph analysis. DETERMINE its retention time. DETERMINE all standard samples (3.1) respectively. And DETERMINE the retention time of standard samples. The chromatogram of mixed standard samples is shown in Figure 1. Page 8 of 16
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