GB 5009.137-2025 PDF EnglishUS$110.00 · In stock · Download in 9 seconds
GB 5009.137-2025: National food safety standard - Determination of antimony in foods Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid GB 5009.137: Historical versions
Similar standardsGB 5009.137-2025: National food safety standard - Determination of antimony in foods---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/GB5009.137-2025GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA National Food Safety Standard - Determination of Antimony in Foods Issued on: MARCH 16, 2025 Implemented on: SEPTEMBER 16, 2025 Issued by. National Health Commission of the People’s Republic of China; State Administration for Market Regulation. Table of ContentsForeword... 3 1 Scope... 4 Method I - Hydride Atomic Fluorescence Spectrometry... 4 2 Principle... 4 3 Reagents and Materials... 4 4 Instruments and Equipment... 6 5 Analytical Steps... 7 6 Expression of Analytical Results... 9 7 Precision... 10 8 Others... 10 Method II - Inductively Coupled Plasma Mass Spectrometry... 10 Appendix A Reference Conditions of Microwave Digestion Instrument... 11 National Food Safety Standard - Determination of Antimony in Foods1 ScopeThis Standard specifies the determination method of antimony in foods by hydride atomic fluorescence spectrometry and inductively coupled plasma mass spectrometry. This Standard is applicable to the determination of antimony in foods. Method I - Hydride Atomic Fluorescence Spectrometry2 PrincipleAfter the specimen is digested by acid heating, in an acidic medium, the antimony in the specimen reacts with sodium borohydride or potassium borohydride to generate volatile antimony hydride, which is carried into the atomizer by the carrier gas for atomization. Under the excitation of the antimony hollow cathode lamp, atomic fluorescence is generated, and its fluorescence intensity is proportional to the antimony content and is quantified by the external standard method.3 Reagents and MaterialsUnless otherwise specified, all reagents used in this Method are guaranteed reagents and the water is Grade-2 water specified in GB/T 6682. 3.1 Reagents 3.1.1 Nitric acid (HNO3). 3.1.2 Hydrochloric acid (HCl). 3.1.3 Perchloric acid (HClO4). 3.1.4 Thiourea [(NH2)2CS]. analytical grade. 3.1.5 Potassium iodide (KI). analytical grade. 3.1.6 Ascorbic acid (C6H8O6). analytical grade. 3.1.7 Potassium borohydride (KBH4) or sodium borohydride (NaBH4). 3.1.8 Potassium hydroxide (KOH) or sodium hydroxide (NaOH). 3.1.9 Tartaric acid (C4H6O6). purity 99.5%. 3.1.10 Argon (Ar). purity > 99.99%. 3.2 Preparation of Reagents 3.2.1 Nitric acid-perchloric acid mixture (10 + 1). measure-take 10 mL of perchloric acid and slowly add it into 100 mL of nitric acid and mix it well. 3.2.2 Hydrochloric acid solution (1 + 1). measure-take 50 mL of hydrochloric acid, add it to 50 mL of water and mix it well. 3.2.3 Thiourea-ascorbic acid solution. respectively weigh-take 10.0 g of thiourea and 10.0 g of ascorbic acid, dissolve in 100 mL of water, mix it well, and store it in a dark place. Prepare it immediately before use. 3.2.4 Thiourea-potassium iodide solution. respectively weigh-take 2.0 g of thiourea and 10.0 g of potassium iodide, dissolve in 100 mL of water, mix it well, and store it in a dark place. Prepare it immediately before use. 3.2.5 Potassium hydroxide solution (5.0 g/L). weigh-take 5.0 g of potassium hydroxide, use water to dissolve it and dilute to 1,000 mL, and mix it well. Prepare it immediately before use. The potassium hydroxide in the solution may also be replaced by sodium hydroxide. 3.2.6 Potassium borohydride solution (20 g/L). weigh-take 10.0 g of potassium borohydride, use potassium hydroxide solution (5.0 g/L) to dissolve it and dilute it to 500 mL, mix it well, and prepare it immediately before use. The potassium borohydride in the solution may also be replaced by 7.0 g of sodium borohydride. 3.2.7 Nitric acid solution (1 + 5). measure-take 100 mL of nitric acid, add it to 500 mL of water and mix it well. 3.2.8 Hydrochloric acid solution (5 + 95). measure-take 50 mL of hydrochloric acid, add it to 950 mL of water, and mix it well. 3.2.9 Nitric acid solution (1 + 1). measure-take 50 mL of nitric acid, add it to 50 mL of water, and mix it well. 3.2.10 Nitric acid solution (2.5 mol/L). measure-take 173 mL of nitric acid, use water to dissolve it and dilute it to 1,000 mL, and mix it well. 3.3 Standard Substance Metallic antimony (Sb, CAS No.. 7440-36-0). purity > 99.99%. 3.4 Preparation of Standard Solutions 3.4.1 Antimony standard stock solution (1,000 mg/L). weigh-take 0.50 g (accurate to 0.0001 g) of metallic antimony into a beaker, add 5.0 g of tartaric acid and 10.0 mL of nitric acid solution (1 + 1), after dissolution, transfer it to a 500 mL volumetric flask, use 2.5 mol/L nitric acid solution to reach a constant volume to the scale and mix it well. Place in a polyethylene plastic bottle, and store at room temperature away from light. The shelf life is 2 years. Or use antimony standard solution that has been certified by the state and awarded a standard substance certificate. 3.4.2 Antimony standard intermediate solution (100 mg/L). accurately pipette 1.00 mL of antimony standard stock solution (1,000 mg/L) into a 10 mL volumetric flask, add water to the scale and mix it well. Place it in a polyethylene plastic bottle, and store at 0 C ~ 5 C in a sealed container away from light. The shelf life is 6 months. 3.4.3 Antimony standard working solution (1.00 mg/L). accurately pipette 1.00 mL of antimony standard intermediate solution (100 mg/L) into a 100 mL volumetric flask, add water to the scale and mix it well. Place it in a polyethylene plastic bottle, and store at 0 C ~ 5 C in a sealed container away from light. The shelf life is 1 month. 3.4.4 Antimony standard series solutions. respectively and accurately pipette 0 mL, 0.100 mL, 0.200 mL, 0.400 mL, 0.600 mL, 0.800 mL, 1.00 mL and 2.00 mL of antimony standard working solution (1.00 mg/L) into 100 mL volumetric flasks, add a small amount of water to dilute them, then, add 10 mL of hydrochloric acid solution (1 + 1), 10 mL of thiourea-potassium iodide solution or thiourea-ascorbic acid solution, add water to reach a constant volume to the scale and mix them well. The mass concentration of the antimony standard series solutions is 0 g/L, 1.00 g/L, 2.00 g/L, 4.00 g/L, 6.00 g/L, 8.00 g/L, 10.0 g/L and 20.0 g/L. After leaving them for 1 hour, conduct the determination. Prepare them immediately before use. NOTE. the mass concentration range of antimony in the standard series solutions can be determined based on the sensitivity of the instrument, the actual antimony content in the sample and different instrument models.4 Instruments and EquipmentNOTE. all glassware and the polytetrafluoroethylene digestion inner tank and inner cover must be soaked in nitric acid solution (1 + 5) overnight, rinsed repeatedly with tap water, and finally rinsed with water. 4.1 Atomic fluorescence spectrometer. equipped with antimony hollow cathode lamp. 4.2 Balance. the division value is respectively 1 mg and 0.1 mg. 4.3 Adjustable electric heating plate. 4.4 Adjustable electric furnace. 4.5 Microwave digestion system. equipped with polytetrafluoroethylene digestion tank. solution is colorless, transparent or slightly yellow, continue heating to drive out the acid, until the volume reaches 0.5 mL ~ 1 mL. After cooling, transfer the solution to a 25 mL container and use a small amount of water to rinse the container several times. After all the solution has been transferred, add 2.5 mL of hydrochloric acid solution (1 + 1), add 2.5 mL of thiourea- potassium iodide solution or thiourea-ascorbic acid solution, use water to dilute it and reach a constant volume of 25 mL, shake it well, and after leaving it for 1 h, conduct the determination. Meanwhile, perform a blank test. 5.2.2 Microwave digestion Weigh-take 0.2 g ~ 0.8 g (accurate to 0.001 g; for the high-water content samples, the sampling amount can be appropriately increased to 1 g) of solid sample or pipette 1.00 mL ~ 3.00 mL of liquid specimen and place it in a microwave digestion tank. For samples containing ethanol or carbon dioxide, first, heat on an electric heating plate at low temperature to remove the ethanol or carbon dioxide, add 5 mL ~ 7 mL of nitric acid. In accordance with the operating procedures of microwave digestion (see Appendix A for the reference conditions of digestion), digest the specimen. After digestion is completed, wait for the digestion tank to cool down and then, open it, heat it at 140 C ~ 160 C to drive out the acid, until the volume reaches 0.5 mL ~ 1 mL, use a small amount of water to rinse the digestion tank several times, combine the washing liquid in a 25 mL container, add 2.5mL of hydrochloric acid solution (1 + 1); add 2.5 mL of thiourea- potassium iodide solution or thiourea-ascorbic acid solution, use water to dilute it and reach a constant volume of 25 mL, shake it well, and after leaving it for 1 h, conduct the determination. Meanwhile, perform a blank test. 5.2.3 Pressure tank digestion Weigh-take 0.2 g ~ 1 g of solid specimen (accurate to 0.001 g; for the high-water content samples, the sampling amount can be appropriately increased to 2 g) or pipette 1.00 mL ~ 5.00 mL of liquid specimen and place it in a polytetrafluoroethylene inner tank. For samples containing ethanol or carbon dioxide, first, heat on an electric heating plate at low temperature to remove the ethanol or carbon dioxide, and then, add 4 mL ~ 8 mL of nitric acid to soak overnight. Put on the inner cover, tighten the stainless-steel sheath, put it into the constant- temperature drying oven, and maintain it at 140 C ~ 160 C for 4 h ~ 5 h, in the oven, naturally cool to room temperature. Open the cover and take out the inner tank, heat at 140 C ~ 160 C to drive out the acid, until the volume reaches 0.5 mL ~ 1 mL. Use a small amount of water to rinse the digestion tank several times, combine the washing liquid in a 25 mL container, add 2.5 mL of hydrochloric acid solution (1 + 1), add 2.5 mL of thiourea-potassium iodide solution or thiourea-ascorbic acid solution, use water to dilute it and reach a constant volume of 25 mL, and shake it well. After leaving it for 1 h, conduct the determination. Meanwhile, perform a blank test. 5.3 Instrument Reference Conditions Instrument reference conditions. photomultiplier tube voltage is 270 V; hollow cathode lamp current is 40 mA; atomizer height is 8 mm; carrier gas is argon; carrier gas flow rate is 400 mL/min; shield gas flow rate is 800 mL/min; measurement mode is standard curve method; ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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