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SN/T 5217-2019 PDF English

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SN/T 5217-2019: (Determination of Brominated Vegetable Oil in Exported Food)
Status: Valid

Std ID	Contents [version]	USD	STEP2	[PDF] delivered in	Standard Title (Description)	Status
SN/T 5217-2019	English	189	Add to Cart	3 days [Need to translate]	(Determination of Brominated Vegetable Oil in Exported Food)	Valid

Standard similar to SN/T 5217-2019

GB 5413.12 | GB 5413.10 | SN/T 1888.4 | SN/T 5216 | SN/T 5219 | SN/T 5218 |

Basic data

Standard ID	SN/T 5217-2019 (SN/T5217-2019)
Description (Translated English)	(Determination of Brominated Vegetable Oil in Exported Food)
Sector / Industry	Commodity Inspection Standard (Recommended)
Classification of Chinese Standard	C53
Classification of International Standard	67.050
Word Count Estimation	8,887
Date of Issue	2019
Date of Implementation	2020-07-01
Issuing agency(ies)	General Administration of Customs

SN/T 5217-2019: (Determination of Brominated Vegetable Oil in Exported Food)

---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Determination of brominated vegetable oils in food for export The People's Republic of China Entry-Exit Inspection and Quarantine Industry Standards 2019-12-27 release 2020-07-01 Implementation Issued by the General Administration of Customs of the People's Republic of China

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009. This standard was proposed and managed by the General Administration of Customs of the People's Republic of China. Drafting organization of this standard. Gongbei Customs of the People's Republic of China. The main drafters of this standard. Feng Jiawang, Qian Zhenjie, Chen Jing, Pan Liang, Tang Shiming, Zeng Junjie. Determination of Brominated Vegetable Oil Content in Imported and Exported Food

1 Scope

This standard specifies the method for determination of brominated vegetable oil content in imported and exported food. This standard applies to the determination of brominated vegetable oil content in beverages and fruit juices.

2 Method summary

After the sample is extracted and concentrated, it reacts with zinc powder under acidic conditions. After the reaction solution is diluted and purified, it is leached with potassium hydroxide solution Wash liquid, anion exchange column separation, conductivity detector detection. Qualitatively by retention time and quantified by external standard method.

3 Reagents and materials

Unless otherwise specified, the reagents used in this standard are of analytical grade, and the experimental water is ultrapure water with a conductivity of 18.2 MΩ·cm. 3.1 Ether. 3.2 Petroleum ether. boiling range 30 ℃ ~ 60 ℃. 3.3 Glacial acetic acid. 3.4 Diethyl ether-petroleum ether mixed extract. Take 500 mL of diethyl ether and 500 mL of petroleum ether and mix it evenly, and seal it for later use. 3.5 Anhydrous sodium sulfate (Na2SO4). Burn at 650°C for 4 hours, cool to room temperature in a desiccator, and store in a sealed bottle for later use. 3.6 Potassium hydroxide. pure superior grade. 3.7 Zinc powder. 3.8 Potassium bromide (KBr) standard product (CAS number. 7758-02-3). purity ≥ 99%. 3.9 Bromide ion standard stock solution (1 g/L). accurately weigh 0.148 9 g of potassium bromide, dissolve it in water, dilute to 100 mL, and store at 4 ℃. 3.10 Bromide ion standard working solution (50 mg/L). accurately pipette 5.00 mL bromide ion standard stock solution (3.9), dilute and dilute to 100 mL, store at 4°C. 3.11 Acetic acid solution (1 to 9, volume ratio). Take 10 mL of glacial acetic acid, add 90 mL of water, mix well, and bottle it for later use. 3.12 Potassium hydroxide stock solution (1 mol/L). Weigh 5.61 g of potassium hydroxide, dissolve it in 100 mL of water, shake it well, and pour it into a polyethylene container. In the container, keep it tightly closed until the solution is clear. 3.13 Potassium hydroxide eluent (15 mmol/L). Take 15 mL of the supernatant of potassium hydroxide stock solution (3.12) and dilute to 1 L with water. It can be used after vacuum degassing and filtering, or it can use equipment that can automatically generate eluent to produce a solution of the same concentration online. 3.14 Strong acid cation exchange column (1 mL). H-type polystyrene-based strong acid resin packing with an average particle size of 40 μm, used before use Wash with 20 mL of water. 3.15 C18 solid phase extraction column (250 mg). C18 packing with an average particle size of 40 μm, activated with 5 mL methanol before use Wash with 20 mL of water. 3.16 0.45 μm water filter membrane.

4 Apparatus and equipment

4.1 Ion chromatograph, electrical conductivity detector. 4.2 Analytical balance. Sensitivity is 0.1 g, 0.0001 g. 4.3 Separation funnel, 500 mL. 4.4 Rotary evaporator. 4.5 Boiling water bath (or dry thermostat). 4.6 Ultra-pure water machine.

5 Analysis steps

5.1 Sample preparation 5.1.1 Take a representative part of about 1 kg of the sample, shake it well, divide it into two parts, put them into clean containers as samples, and seal them. And mark. Store the sample at 4°C and avoid light to prevent contamination of the sample. 5.1.2 Beverages containing carbon dioxide gas should be fully stirred with a stirrer or ultrasonically removed to remove carbon dioxide before testing. 5.1.3 Beverages containing pulp or other insoluble solids should be processed with a homogenizer before testing. 5.2 Pre-treatment 5.2.1 Extract Accurately pipette.200 g (accurate to 0.1 g) of the mixed sample into a 500 mL separatory funnel (4.3), and add 100 mL to mix Shake the extraction solution (3.4) gently, cover the bottle stopper after exhausting, and shake at room temperature for about 10 minutes. After fully standing for stratification, the lower water phase Transfer to another 500 mL separatory funnel (4.3), repeat the above process once, combine the ether layers, and wash the ether layer once with 50 mL water. The ether solution is filtered and dehydrated by anhydrous sodium sulfate (3.5), and the filtrate is put into a 500 mL round-bottomed flask and placed on a rotary evaporator (4.4). 40 ℃ ± 2 ℃ under nitrogen filling conditions to steam to nearly dry (should not evaporate to dryness). 5.2.2 Conversion Use about 10 mL of ether (3.1) to transfer the extraction residue to a 100 mL colorimetric tube, add about 30 mg of zinc powder (3.7) and 5.0 mL of acetic acid solution (3.11), mix well, and place it in a boiling water bath (4.5) to heat for 5 min. After the reaction is over, take it out and let it cool. Dilute with water and dilute to 100 mL. Note. Ether is a flammable liquid, and its vapor forms an explosive mixture with air. It is very easy to burn and explode when exposed to open flames and high heat. Open flame should not be used during heating reaction The electric stove should be placed in a fume hood. 5.2.3 Purification 5.2.3.1 Removal of cations in the reaction solution Pass the cation exchange column before injection, and pass the constant volume reaction solution through the pre-activated cation exchange column. The sample flow rate should be < 2 mL/min, the first 10 mL that flows out is discarded, and the subsequent effluent is collected and passed through a 0.45 μm filter membrane for analysis. 5.2.3.2 Remove the pigment in the extract For some colored sample extracts, C18 column can be used to decolorize, the constant volume of the reaction solution is slowly passed through the pre-activated C18 column, The sample flow rate should be less than 2 mL/min, the first 10 mL that flows out is discarded, and the subsequent effluent is collected and passed through a 0.45 μm filter membrane for analysis. 5.3 Determination 5.3.1 Chromatographic reference conditions 5.3.1.1 Anion guard column. Ion Pac AG11-HC (50 mm × 4 mm) or equivalent column. 5.3.1.2 Anion analysis column. Ion Pac AS11-HC (250 mm × 4 mm) or equivalent chromatographic column. 5.3.1.3 Injection volume. 25 μL. 5.3.1.4 Potassium hydroxide eluent concentration. 15 mmol/L, isocratic elution for 20 min. 5.3.1.5 Flow rate of eluent. 1.0 mL/min. 5.3.1.6 Column temperature. 30°C. 5.3.1.7 Anion suppressor. ASRS-ULTRA Ⅱ type suppressor or equivalent suppressor. 5.3.1.8 Suppressor current. 38 mA. 5.3.1.9 Detector. conductivity detector, the temperature of the detection cell is 35 ℃. 5.3.2 Drawing the standard curve Accurately draw the bromide ion standard working solution (3.10) 0.00 mL, 0.10 mL, 0.50 mL, 1.00 mL, 5.00 mL, 10.00 mL, 15.00 mL in a 50 mL volumetric flask, dilute to the mark, and mix well. The bromide ion concentration of the above standard working solution is 0.0 mg/L, 0.1 mg/L, 0.5 mg/L, 1.0 mg/L, 5.0 mg/L, 10 mg/L, 15 mg/L. Sequential injection from low concentration to high concentration, with standard working solution concentration As the abscissa and the peak area as the ordinate, draw a standard working curve, and use the standard working curve to quantify the sample. Conditions in this method Below, the reference retention time of bromide ion is 10.8 min, and the standard chromatogram is shown in Figure A.1 in Appendix A. 5.3.3 Sample determination The response value of bromide ion in the sample solution to be tested should be within the linear response range of the instrument. If the bromide ion content in the sample is too high, it can be used as required Increase the dilution factor. 5.3.4 Blank test Except that no sample is added, all are carried out according to the above-mentioned measurement steps.

6 Expression of analysis results

The content of brominated vegetable oil in the sample is calculated according to formula (1). It is expressed as the arithmetic mean of two independent determination results obtained under repeatability conditions, and the test results are kept to one decimal place.

7 The lower limit of precision determination and the recovery rate

7.1 Low limit of determination The lower limit of this method is 0.5 mg/kg. 7.2 Add concentration range and recovery rate The experimental data of the added concentration and recovery rate of the orange-flavored beverage are shown in Table 1.