GB/T 5009.16-2003 Determination of tin in food

This standard specifies the determination method of tin in food. This standard is applicable to the determination of tin in various foods. The detection limit of this method: 2mg/kg for phenanthene colorimetry; 0.23ng/mL for hydride atomic fluorescence spectrometry, linear range of standard curve: 0ng/mL～20ng/mL. GB/T 5009.16-2003 Determination of tin in food GB/T5009.16-2003 Standard download decompression password: www.bzxz.net

[CS 67.040
National Standard of the People's Republic of China
GB/T5009.16—2003
GBT5009.16193%
Determination of tin in food
2003-0-11 issued
Ministry of Health and Family Planning of the People's Republic of China
Standardization Administration of China
2004-01-01 implementation
This standard replaces G/Tb039.1-109 Determination of the content of carbon in foods Method 3: Compared with CB/T501>9.5-199, this standard has the following changes: The Chinese name of the standard has been modified and changed to Determination of the content of carbon in foods; (R/T5009.16-2003
Continued from (13/T20001.4202: Standard abbreviations Part 4: Chemical analysis The original method of the standard was revised by Liu Yu; the atomic fluorescence spectrophotometry of the chemical compound was used as the first method, and the colorimetric method was used as the second method: This standard is proposed and standardized by the Ministry of Health of the People's Republic of China. The first method of the standard was drafted by Beijing Municipal Epidemic Prevention Station, Ministry of Health and Family Planning, Food Industry Supervision and Inspection Quality Supervision Institute, and Beijing Export Food Supervision and Inspection Institute. The second method of the standard was drafted by the Food Hygiene Supervision Institute of the Ministry of Health. The main drafters of the first standard were Mao Hong, Chang Shi Jian, Zhao Ge, Ge Ping, and Shi Zhudian. The fifth standard was first issued in 18R5 and was revised for the 11th time. This is the 12.1
CE/T 5009.16—2003
Tin is one of the essential trace elements for human body. Excessive intake of tin may cause the occurrence of tin poisoning. In 2009, the FAO/WHD and JECFA experts meeting revised the recommended daily intake of tin to 24tg/(sg/week). my country has formulated the standard for food safety. The current standard method is the relative sensitivity method, which is not sensitive enough to meet the requirements of the determination of samples. This time, the nitride atomic fluorescence amplification method is proposed to replace the current standard method. The method is simple, fast, and has a small number of batches. It uses domestic instruments and is suitable for the determination of tin in food within the scope of 1. This standard stipulates that the determination method of tin in food shall be used as the standard method. This standard Applicable to the determination of various types of real products. CB/5009.16—2003
This method is published, the colorimetric limit is 2/k; the detection limit of the oxidation bed carbon optical latent method is: 2/mT standard curve fullness, 3rg/ml.~-200nR/L, 2 Normative documents
The following documents become the terms of this standard through the reference of this standard. For the referenced documents with a date, the subsequent revisions (excluding the contents of the referenced documents) are not applicable to this standard. However, the parties who have reached an agreement based on this standard are encouraged to study whether the latest versions of these documents can be used. For the referenced documents without a date, the latest version applies to this standard. G3T59, 1—2003 Determination of total tin and inorganic substances in food Method 1 Hydride atomic fluorescence method
3 Principle
The sample is digested by aldehyde heat, tin is oxidized to tetravalent tin, and is converted into micro hydride under the action of oxidizing agent, and is carried into an atomizer by gas for sequential ionization. Under the irradiation of a special tin-converting cathode lamp, when the tin atoms are excited to a high energy state, they emit light at a characteristic wavelength when they are deactivated to the ground state. The fluorescence intensity is proportional to the content and is comparable to that of standard 4 Reagents
4.1 Sulfuric acid (superior grade).
4.2 Magnesium hydroxide + calcium hydroxide solution mixed to 1+1>.
4.3 Sulfur sulfide (119), take 100ml sodium borohydride and add 000ml sodium hydroxide to water and mix well. 4.4 Sulfur sulfide (159g/L) + ascorbic acid (152g/L): weigh 15g sodium borohydride and 10.5g sodium borohydride respectively and add to water, and add to 109l<, and store in a color bottle.
4.5 Borohydride bath solution (7/1): weigh 7g sodium borohydride, add to sodium hydroxide solution (5R4), and make up to 1000ml. 4.6 Tin standard application: accurately pipette 10ug/l. Tin national standard box wave (standard signal BW3035) 1.0mL in 100mL volume, and use environmental acid solution (1!9) to make up the volume. The concentration of this dense liquid is 1ug/m.5 Instrument
5.1 Double cat original one Fischer photometer,
5.2 Electric heating plate,
6 Analysis steps
6.1 Sample preparation
Grain, remove large impurities and dust, carbon crush through 40F, wash and dry fruits, vegetables, meat, and aquatic products, take the good part to make pulp,
GB/T 5009.16—2003
6.2 Sample digestion
6.2.1 Take the test sample 1.-501 and add 1.m1. concentrated acid, 10.mT. nitric acid (-1), 3 tablets of sodium chlorate, and place overnight. Heat and digest on the next day. If the sample is small, add appropriate amount of acid and continue digestion until white smoke appears. When the liquid volume is close to 1ml, remove the sample and cool it down. Transfer the digestion sample into a 5:ml container or bottle with water, add water to the volume to 5:1, shake well, and do a blank test at the same time.
6.2.2 Take 10mL of the sample after the volume is fixed and mix it in 15mL colorimetric medium (150g/L) with acid (/), shake well.
5.3 Preparation of standard series
Standard curve: Pipette the marked 0.0, U., 0.5, 1.0.=.5.2.C. into 15L colorimetric tube, add the acid solution +) 2.1.-21..U.5.0.m. with water to 1U, add 2mL. Sulfur source 15/T.)-anti-blood test (150L mixed resources,
5.4 Determination
.4.1 Instrument model: negative pressure xuV single 75mA original 7 temperature seat, 800, furnace height, 10mm group curve gas, : 200mTmia flow rate r5c5aL/min measurement: standard curve method reading method: drop and! Delay time: 1 time, 13% addition time, 8* Injection volume: 2mL6.4.2 Completion: According to the test conditions, you can choose the following method. 6.4.2.: Liquid concentration measurement method: Set the instrument performance conditions. After the required source rate is determined, start observing the plate and inject samples continuously until the number is stable. After the number is determined, transfer to the standard measurement source and draw the standard line. After the sample is transferred to the test, measure the test group air and test rod digestion solution respectively. Before each test, remember to disinfect and wash the instrument. The test result is calculated according to the following formula.
8.4.2.2 Automatic calculation method: Set the instrument to the most appropriate condition. Enter the following data on the detailed data screen: sample mass (or rlL), dilution volume (rml.), and select the concentration unit price of the result. Raise the furnace temperature to the specified temperature, measure after setting, continue to use the standard sample, set the speed, switch to the standard series measurement, make a standard curve, and before switching to the sample measurement, you can enter the measurement state, inject the test blank digestion solution, and take the average value as the subtraction compensation, and then you can set the test rods in turn. After the measurement, click "Scan Report" to print the subtraction result automatically. 7 Calculation of results
Sample content () Enter the formula and
X=GGzYx:000
x1300:1c
In the formula:
—Sample content in grams/or/
—Sample digestion to the specified degree, the unit is nanograms per unit area/meter): Sample blank digestion solution liquid concentration , in grams per liter? /m) or sample digestion liquid total bed, in liters (ml.): m sample mass volume, in grams (R or mJ. The sieve result retains two significant figures.
White precision
The absolute difference of the results obtained under the conditions of bean refolding shall not exceed the arithmetic mean value. Second method: phenoxyacetone colorimetric method
9 Principle bZxz.net
After digestion, the tetravalent phenoxyacetic acid forms a red complex with the surrounding in a weakly reactive solution and is compared with the standard series batch in the presence of a protective colloid.
10 Reagents
101 Tartaric acid solution 1001)
10.2 Cyclic acid (m acid <1 mL/L), prepare when used. 10.3 Animal gelatin solution: 5/1.>, mix before use, 10.4 Indicative solution (10g), take 10g, use 7% decomposition rate 135L 10.5 Hydrogenated water 11,
GR/T 50O9.16—2003
10.6 Please measure 100ml of acid and mix it in 100ml of water. 10.7 Liquor 1), 1/1.1 weigh, 0.10g of it (1.17-Hydroxy-9-phenylbenzene (total 17-hydroxy-9-phenylenediol). Add a small amount of ethanol and sulfuric acid [-) to dissolve and dilute with methanol to [0mL
10.8 standard volume, fill with 0.10C0 gold (.%, stomach in a beaker, add 1?mT. sulfuric acid, increase the temperature, heat until the pot is completely separated, the surface is positive, heat the case to cool, slowly add 50mT. water, pour into a 100mL bottle, wash with acid ([-9] several times, add the washing liquid into the volumetric bottle, and dilute to Scale, mud spoon. This stock solution is equivalent to 1. UK pot
10.9 Stock standard solution: Pipette 10. (mL of steel standard solution into 100ml. Rate of application, dilute with acid <1 + 9) to 1.50. The next dilution is until each milliliter is equivalent to 10.0R tin. 11 Instrument
Spectrophotometer.
12 Analysis steps
12. Sample preparation
12.1. Sample digestion
Same as G3/T s9. :1 3003 12.1.
12.1.2 Sample pretreatment and standard curve preparation Pipette 1.93mL--5.92ml sample digestion solution and the same amount of reagent solution, and place them in 25mL colorimetric tubes: Pipette 0.5.20, 0.40, 0.901.001. Standard solution equivalent to 0.2.0, 4.0.6.0.8.C.10.C, and place them in 2L colorimetric tubes respectively.
12.2 Sample measurement||tt || Test digestion formula: add 0.5m tartaric acid solution (1/1.3) and 1m phenol indicator solution to the standard solution (111), add 1m flux (1+9), 5g gelatin (5g/1.3) and 2m sodium pyrophosphate (10/1.3), mix until 35m, add 2m sodium pyrophosphate (0.1/1.3), mix for 1h, measure the absorbance in a 2cm colorimetric cup with water, and measure the absorbance at 490nm. Subtract the absorbance value of the zero tube from the upper point, calculate the range of the straight line or the range of the standard, compare the absorbance value of the sample with the curve or substitute it to find out the content, and calculate the content of the sample according to the formula (2. (mm) × = 000
: X (V7VX100
Where:
2 The content of the sample in the pot, the single empty is per gram or nanogram per gram (m% or mg) The mass obtained in the digestibility of the sample is determined, and these digits are grams R), 2) | |tt||GB/I5009.16—203
formula: the total volume of the blank solution measured in grams [product quality, unit is gram R,
formula details: the total volume of the digestion solution measured in liters (mL): the volume of the sample digestion solution measured in liters (mI.) Calculation results: retain the effective efficacy of the
precision spot
under any other conditions, the difference between the two independent results shall not exceed 1% of the arithmetic mean, 1
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.