Some standard content:
TC5 67. 040
National Standard of the People's Republic of China
GB/T 5009.15——2003
Generation of GB/5909.151S96
Determination of cadmium in food
foods2003-08-11 Issued
Ministry of Health of the People's Republic of China
Standardization Administration of the People's Republic of China
2004-01-01 Implementation
GB/T5009.15—2003
This standard replaces GB/T5009.15—2003.1.1996.3 This standard mainly changes as follows: The Chinese names of the standards are changed, but the Chinese names are changed to GB/T2K1.4:2:111.2.111.4.2. ... The first part of this standard was drafted by the Food Hygiene Inspection Institute of the Ministry of Health, the Institute of Nutrition and Food Hygiene of the Chinese Academy of Preventive Medicine, and the Food Hygiene Supervision Institute of the Ministry of Health. The first part of this standard was drafted by the Food Hygiene Inspection Institute of Shanghai, Shanxi Provincial Health Prevention Station, the Nutrition and Food Hygiene Institute of the Chinese Academy of Preventive Medicine, and the Food Hygiene Supervision and Inspection Institute of Jiangsu Province. The fourth part of this standard was drafted by the Guangxi Import and Export Commodity Inspection and Quarantine Institute, the Ministry of Health, the Sichuan Provincial Health Station, and the Beijing Municipal Health Inspection Station. This standard is the first edition of the standard. It was first revised in 1985 and revised for the first time in 1996. This is the second revision. 112
1 Scope
Determination of cadmium in food
This standard specifies the determination method of cadmium in various types of food: This standard is applicable to the determination of cadmium in all types of food. GB/T5009.15—2003
The detection limit of this method is: 0.1/100% by calcite atomization method: 5.0g/kg by flame atomization method: 5g/g by flame atomization method: 1.2rg/kg by calcite atomization method: The detection limit of the standard is 0-50g/mL. Method 1: Absorption spectroscopy
2 Principle
After the sample is treated with acid or hydrolysis, it is injected into the absorption spectrophotometer. After the sample is treated with hydrolysis or hydrolysis, it absorbs 225nm. At a certain concentration, its absorption value is calculated and compared with the standard column. 3 Reagents
3.1 Acid
3.2 Alkaline acid
3.3 Biochemical (30%)
3.4 Commercial acid
3.5 Nitrate: slowly add 30% nitric acid into 50mL water. 3.6: Nitric acid (3.m1/1.), take 3.2.mL nitric acid and add it into 50mL water, and then add 100mL of nitric acid. 3.7 Station (1 +). Take 5ml and slowly add it into 53mL water. 3.8 Ammonium phosphate solution 20F/1.): Weigh 2.0 ammonium phosphate and dilute to 10UmL with water. 3.9 Mixed acid, acid + chlorine (4-1), take 4 parts of nitric acid and 1 part of peroxychloric acid and mix: 3.10 Standard preparation: Weigh 1.0008 sodium sulfate (9%.99%) and add 20TmL of hydrochloric acid (1+1) solution in batches, add 2 drops of chlorine, transfer to 10mL volumetric flask, add water to the scale, mix well, and the change is 1mL containing 0.0mg chlorine. 3.11 Standard use: 10.0 ml of each absorption standard is stored in a 1cc ml volumetric bottle, nitric acid (0.5uL/L) is added to the mark, and diluted several times to make a total of 10w.U of each standard. 4 Apparatus
All new glassware must be diluted with nitric acid (11) and rinsed repeatedly with water. Finally, rinse with deionized water. 4.1 Original absorption spectrophotometer with egg furnace and hollow pole lamp 4.2 Muffle
4.3 Constant temperature + replacement box.
4.5 Hydrogen digester, small digester or positive hydrophobic bomb. 4.6 Adjustable electric heating plate with adjustable medium furnace.
5 Step test
5.1 Sample treatment
5.1.1 During the sample collection and preparation process, be sure to avoid rapid sample contamination. 113
GB/T 5009.15—2003
5.1.2 After removing impurities from roots and beans, grind them and store them in a bottle after 2 days. Keep them for future use. 5.1.3 For fresh fruits, blood, meat and eggs with high water content, use food processor or pulper to beat the skin and homogenize, add plastic cells, keep in reserve, 5.2 Sample digestion (any of the following methods can be used for digestion according to experimental conditions) 5.2.1 Digestion by force Digestion method: weigh 1.00g2.05g sample (10, high fat content test sample 1.0g), weigh the sample (20g fresh, 10g fresh, 20g fresh, 10g fat content test sample), press to digest, weigh the sample) 4. Soak overnight. Then add hydrogen peroxide [30%>2:sT.~31ml (the total volume should not exceed about one tenth of the chain volume!). Put it in a stainless steel jacket tightly and put it in a constant temperature drying oven at 12U℃~.1h~.4, cool it naturally to the actual temperature in the oven, use a sterile pipe to wash or filter the digestion (depending on the digestion conditions, the amount of starch can be determined by agreement 0ml-m, use a small amount of actual paint end, add sugar and set the scale, mix well and prepare Use; the company's example is to make sure the test space,
5.2.2 ten-method ash amine 1.935.0g root period code) station dry porcelain report. First, on a low fire in the inquiring electric protection until no increase in carbonization, transfer to the muffle furnace 56h ~ 81. Cool, if ~ other samples are not completely dead, then add 1m. Mix the acid on a low fire in the inquiring electric protection, and cool it several times until it is completely digested. Dissolve it with nitric acid (0.5m/m) Solution pipette will be sent to the sample digestion or flow (the digestion policy has no sedimentation surface) 10m25TL through the chapter plate. A small amount of water is used to wash the material and the flow is reduced and discarded. The frequency is determined and the rate is returned. Mix the material for use; the blank 5.2.3 needs to be tested later. Weigh 1.00g--5.09 sample in the porcelain end, add 2mL--4 waist and drag it over a low fire for 2.-3. After carbonization, the acid should be ground. Continue to digest until smoke stops. Transfer to muffle furnace, keep constant temperature at 590℃ and then raise to 0℃ for 20min. Cool, add 1mL acid (1mL/1mL). Pour the test and digestion solution into a volumetric flask, wash with small amount of water several times, and make up to 100% water. At the same time, make a reagent blank. 5.2.4 Mixed digestion method: weigh 1.00~5.33g of sample into a 13- or 14-ounce beaker, put a few glass beads, add 13 ml, and let it sit overnight. Digest on a stove with a small bucket until it turns brown-black. Add more water until the digestion solution is colorless and transparent or with a yellow tint. Pour the sample digestion solution into a 25-mL volumetric flask or filter (depending on the salt content of the sample after digestion), and rinse with a small amount of water. 5.3 Determination 5.3.1 Instrument conditions: Adjust to the best state according to the performance of each instrument: Reference conditions are wavelength 228.2 [m: fast chain 0, = m ~ 10m, lamp current KmA-mmAT drying temperature 120 ℃ 2% s ashing system 35015s ~ 2 ℃ 3 atomic 5.3.2 Standard preparation: Pipette three prepared standard working solutions 0.0, 1.0, 2.0, 3.0, 5.0, 7.0, 10.0 mL into a 10 mL volumetric flask, and dilute until full, equivalent to 0.01, 1.0, 3.0, 0.0, 7.0, 10.0 mL, and pipette 10 ± 1 mL each into a furnace. , and obtain the value and the linear relationship between the absorbance value and the surface value. 5.3.3 Sample determination, absorb 10L of each of the column and the test agent, and measure the absorption of the sample: Substitute the standard series: the linear equation is used to calculate the content of the sample. 5.3.4 Use of bulk modifier: For organic samples, add an appropriate amount of base modifier (20g/1.5L) to eliminate the worry. When you are testing the sample, you should also try your best to use the base modifier when measuring the sample. 6 Results
The content of the sample is calculated according to formula (1: x-(axx0
X——Sample content, unit is microgram per dry gram and gram per liter (ug/kg or g/.》A———the content of sample digestion liquid, in g/mL; A———the content of air in the digestion liquid, in g/mL; V—the total volume of sample digestion liquid, in mL; m———the mass of the sample, in g or mL; the calculation result shall be mathematically valid.
7 Precision
GH/T 5009.15—2003
The absolute difference between the results of two independent determinations under the conditions of standard deviation shall not exceed 2% of the average of the paired methods. Second method atomic absorption spectrometry
(I) Potassium 4-methyl 2-nitropropene-2-yl method
8 Principle
After treatment, the iodine ions and iodine ions form a complex in acidic ionization, and then are separated by 1-methylpentyl ketone-2-yl ionization. After atomization, it absorbs the 228.82m resonance line. The total absorption is proportional to the absorption amount. It is quantitatively compared with the standard series. User reagents
9, 14-methylbenzene-2-yl (MBK, meaning different in name!). 9.2 Phosphorus (1+10),
9.3 Magnesium (+ 11): Base: 3mT. Salt monohydrate is diluted to 12ml in appropriate amount of water.9.4 Potassium acid (17): 52% magnetite is added to appropriate amount of water and then diluted to 120ml. 9.5 Acid catalysis: acetic acid and ionized acid are catalyzed by H1. 9.5 Vegetable acid (1+).
9.7 Potassium hydroxide solution (250g 71.)
9.3 Standard acid: weigh 1.000C (92.99X), add 2 drops of nitric acid, add 10ml of water, dilute to 10ml, mix, and put in a polyol bottle. This solution is equivalent to 1 ml of 9.9 standard solution, absorb Take 100 ml of the standard solution and add it to 100 ml of the sample. Add 1+11% ethanol to the sample and mix until the sample is equivalent to 5.20 % rust per ml. Collect it with a spectrophotometer. 11 Analysis steps 11.1 Sample preparation 11.1.1 Cereals: remove pollutants and dust: remove all foreign matter when necessary. , screen, sieve, about 400-500g/mL, incubate at low heat for about 8 hours without smoke, remove from heat, add a small amount of water after cooling, heat over low heat. Do not heat, add a little water when necessary, mix, and process in this way until there is no acid in the white powder, cool, add 1J acid (1+1!) and transfer to 50mL container The bottle can be repeatedly swelled with hydrochloric acid (1+11), washed with water, diluted to the scale, and the sample can be collected in the same way or mixed with 1+11) and the reagent test can be carried out according to the same operation method. 11.1.2 Collect fruits and vegetables, clean the edible parts, chop them into a mixture, weigh 10.0Ug~20.0Ug of the mixture and add 115
GB/T 5009. 15-2003
Add mL of acid (1→). Carbonize over low heat, and then proceed as per 1).1. until smokeless, place in muffle furnace.\ proceed as per the following procedure:
11.1.3, for aquatic products and Chinese products, take the Sichuan food part and mix thoroughly: weigh 0.00g~10.00g and place in porcelain, carbonize over low heat, and then proceed as per 11.1.1 until smokeless, place in muffle furnace.…\ proceed to achieve operation. After the milk is mixed, take 5mL, add 1uL of the solution to the porcelain block (110). Dry it in a water bath, then char it over low heat, and continue with 1]. 1. From \ until there is no more, proceed with 11.2 according to the law. Take 25L (or the whole amount) of the above prepared liquid and reagent solution, add 10m sulfuric acid (+1) to 125mL of each, and then add 10mT water. You can: absorb 00.25, 0.50.1.50.2.50.5.50.5.00rl standard use (when the battery is C2.05 0.1, 0.3, 0.5, 9, 7, 1.0 (%). Add 1 μL of acid to 35 mL in 25 mL buckets, add 10 μL of sulfuric acid (1 μL) and 1 μL of water, mix, add 10 ml of potassium iodide solution 250 g/L to the sample filtrate, reagent solution and standard solution, add 10 ml of MIBK to each bucket, control for 2 min, and stratify by static volume to about 0.55-25%; discard the lower layer, use a little absorbent cotton to separate the lower part, pour the MIBK layer into a 10 mL tight tube through degreased cotton for later use. 11.3 Determination of
The determination is carried out in a flame atomizer in a cabinet. The determination conditions are: lamp battery 6mA~7A, wavelength 228.82m, acquisition wavelength C.15nm--n2nm, air flow rate 5L/min. (It depends on the instrument model and is adjusted to the optimum conditions. The absorbance of the content against the concentration is used to make a standard curve to calculate the correlation coefficient. The sample received value is compared with the curve or the result is used to calculate the content. The content of
in the sample is calculated according to formula (2). YAX
mx(V,/V,)xi000
Wherein:
the amount of reagent in the sample, the unit is gram or gram per liter (g/g or /I); x
A: the mass of the sample in the measuring box, the unit is microgram (μg); A: the mass of the sample completely eliminated from the reagent solution, the unit is g or liter (g or mL); V: the total volume of the reagent treatment solution, the unit is liter (m2); The results of the screening test shall retain two valid mathematical values.
13 Precision
The absolute difference of the results obtained under repeated conditions shall not exceed 1 of the arithmetic mean. (II) Diisobutyl ester method
14 Principle
The test Y is treated with 2115 ions. The halogen forms a complex with the diisobutyl ester and is separated by acetic acid. The halogen is introduced into the atomic absorption. After atomization, it absorbs 22,2m of energy. Its absorption value is quantitatively compared with the standard series. 15 Reagents
15.7 Water:
15.2 Aldehyde: Same as 3.!
15.3 citric acid mixed solution (m.o1/L>, weigh 226.3g sodium iodide and 48.46 citric acid water tank solution, add He when necessary
GB/T 5009.15—2003
Melt, cool and dilute to 0L in water: treat with dichloromethane-butyl acetate solution (1 mL) to reduce the air temperature before use. 15.4 Amine-butyl acetate (1 g/L): weigh 0.16 mL, add 10 mL of chloroform to dissolve, then add butyl acetate to dilute to 100% before use.
15.5 Standard fast liquid, same as! 9.
Dry and store the photometric juice,
17 Analysis steps
17.1 Sample treatment
17.1.1 All: remove foreign matter 17.1.2 Wash and cool the edible parts of fruits and vegetables, mince and mix thoroughly. 17.1.3 Meat products: 17.1.4 Sample digestion: weigh the above sample, place it in a 25ml high-type beaker, add 15ml of mixed acid, and heat it on a hot plate or sand. Digestion should be carried out according to the requirements. If necessary, the amount of water can be adjusted to facilitate the digestion. Filter until the sample is colorless and slightly yellow. After cooling, filter until the residual acid is completely removed. Repeat this process twice. Refrigerate for 25 minutes. mL water in the test cup, add the contents to 125mL of the test solution. Take the same amount of mixed solution as the test sample and perform the reagent blank test in the same way. 17.2 Extraction and separation
Take 0, C.2%, 0.50, .50, 2.50, 3.50, 5.0ml of standard working solution (equivalent to C.0, 0.5, C.1, 0.3, 0.5.0, 7, 1%). Place them in a 125mL separatory funnel respectively, and add salt (1+=1) to 25mL: D sample treatment solution, test blank solution and saw standard shrinkage to each separatory funnel 5ml. Sodium citrate was washed with water (1g/1.0), and the pH was adjusted to 5-6.4 with ammonia water. Then, water was added to 50 mL each and mixed. 5.0 mL of methyl ethyl thioacetate (1g/1.0) was added to each, and the pH was adjusted to 5-6.4 with water. Then, 50 mL of methyl thioacetate was added to each, and mixed. Then, 5.0 mL of diisocyanate (1g/L, 2 mmol) was added to each, and the layers were separated. The lower aqueous phase was discarded, and the organic layer was placed in a test tube for later use. 17.3 Determination of the results of the determination of the amount of the sample in the test tube was calculated by formula 5. X = (A, -A,)×1 000
mX1000
Wherein:
X—the content of dapoxies in the sample, in grams per gram (nR/ke); A
is the mass of the reagent solution, in micrograms (μg); 2: the mass of the sample, in g (g).
The statistical results shall retain two valid digits.
19 Density
The absolute difference of the error in the repeated determinations shall not exceed 15% of the arithmetic mean.
GR/T 5009.15—2003
20 Principle
The third method is colorimetric method
After digestion, the ions react with aldehyde nitrogen in the liquid to form a red complex, which is dissolved in trioxane and determined by series comparison.
21. 1 Trichloroethane.
21.2 Triamides. 21.3 Aldehyde: nitric acid-isochlorous acid (A-1), 21.4 Potassium arsenate (400/L): 21.5 Sodium hydroxide (200 g) 21.6 Sodium citrate (250 g/L): 21.7 Reagents: Weigh 4 mg of 6-hydroxybenzoic acid and dissolve in 50 mL of dichloromethane, add to brown solution. 21.8 Standard solution: same as 9. 21.9 Standard solution: same as 9., but dilute to 1.6 g per liter. 22 Only spectrophotometer is required. 23 Analytical steps 23.1 Sample digestion: Take 5.00 ~ 10.00 In two 150 mL bottles, add 15 r[.~-20 1mL of strong aldehyde (if the test is done overnight at room temperature, the next day is the day of digestion), heat on low heat, and after the foam disappears, slowly increase the heat, and add a small amount of nitric acid if necessary, until the solution is colorless or slightly yellow, and cool to room temperature. Take a mixed acid equivalent to the sample, and perform the test with the same operation method as the sample. 23.2
Wash the new sample and the test blank with 20mL of water several times into a 25T separatory funnel to check the oxidation reaction (20)g/H,
Pipette 6, 3.5, 1.0, 3.0.5.0.7.0, 10.3ml of standard use (equivalent to 9, 0.5, 1.0, 3.0.5.0, 7..10.0ml) and place them in 12 minutes, then add 200/1 sodium chloride solution to make it equal to 2 Adjust the sample digestion solution, add 3ml sodium citrate (ESV/L) 4mL alcohol (4g/L) and potassium hydroxide (2g), mix. Then add 5ml trichloromethane and 2ml trichloromethane, shake immediately, let stand for stratification, pass the trichloromethane layer through debonded cotton, adjust the absorption point with monoxide, and record the absorbance at wavelength 565 in a cm colorimetric cup. After subtracting six blank values from each standard point, prepare a standard curve, or calculate the return value between the standard points, compare the content with the surface line or substitute it to find out the result. Calculate the same as in the 18th competition. 25 Sugar density 26 Principle 4th method Atomic fluorescence method GD/T 5009.152003
After wet digestion or drying or oxidization, the food sample is added with potassium hydride to generate volatile substances in the reaction with the oxidizing agent, and then vaporized in a quartz atomizer. Under the excitation of the emission of a special chamber cathode lamp, atomic fluorescence is generated. The fluorescence noise is proportional to the substance being measured under the same conditions and is comparable to the standard series. 27 Test Conditions
27.1 Sulfur (super pure).
27.2 Magnetic Acid (super pure).
27.3 Magnesium Chloride (super pure).
27.4 Selenium Oxide (39%).
27.5 Disulfur dioxide·tetrachloride solution (0.=/L): Weigh C.25R disulfide and dissolve it in carbon tetrachloride in a 100mL volumetric flask and dilute to 100mL.
27.E sulfuric acid solution (C.25ra0./L>: Carefully add 11ml of sulfuric acid into 00mL of water, cool and dilute to 1CCumL, accurate). 27./Air drop micro <0%/1.) agent Take 13R mirror dolphin with sulfuric acid (0.2001/1.> melt and dilute to 2 (0m1. Hook 27.8 containing transfer liquid: weigh 0.4038g cobalt oxide hexahydrate (a, +6H0), or 0.220 sodium chloride (CC,), add water to 100ml. salt bottle, dilute to 100ml, this solution concentration is equivalent to 1mg of cobalt per liter, when applied, the concentration of cobalt ions is 0g: ml.
27.9 Hydroxide gas melt (: R/T) : Weigh 1% potassium hydride. Dissolve in water until the viscosity reaches 200 mL. Mix well. 27.10 Potassium hydride solution (30 mL): Take H3PO4 and dissolve in 1% potassium hydride. And determine the concentration of 1% to 1% of the solution. 27.11 Standard solution <1.00 mg/L: 102 mL/L. 12 Standard solution: Accurately pipette the standard solution and dilute to 50 mL/mL with a saturation (0.2 mL/L). 28 Standard solution 25.1 Dual-phase laser spectrometer with coded polarization lamp, can be a type of intermittent flow sample inlet or a mouse or optical instrument. 28.2 Temperature-controlled digester: The test site's glass sieve and digester must be soaked with nitric acid (1-0) for 24 hours, and then rinsed with deionized water before use.
29 Analysis steps
29.1 Sample digestion
Weigh 0.1% of the sample that has been sieved by the powder (sieve) and place it in the digester. Samples with high moisture content should be first Dry the sample in a refrigerator and add nitric acid-perchloric acid (10% hydrogen peroxide) or place overnight. Heat digest the next day, filter out the digestion liquid if it is yellow or colorless, remove all the nitric acid. Use about 25ml of 0.20mul/L of acid to digest the sample and transfer it to a 50mT volume plate. Add 20% carbon tetrachloride (0.1mol/L) and 1mT containing solution. Reduce to 53mL of sulfuric acid (0.23mol/L), mix and test, and do the reagent test at the same time. 29.2 Preparation of standard series
Pipette 5ug/mL standard sample to obtain 0.450.90, 1.63.3.60.5.40ml.5UmL volumetric bottle, add 0.2u/L>about 2rT. Add S.0mL of dichloromethane (J.5/1.), incubate bacteria for 2min. Add 101r:1. sparse agent <50)g/) and 1nL of solution containing 101r:1. sparse agent (U.2)ml/1. adjust to 0ml. (the concentration of each phase is about 0.501.00, 2.C04.20.5.2)r8/m.), and make a standard blank at the same time. The number of standard blank grain batch test samples should be increased by at least 113
G/T 5009.15—2003
Based on the performance of each instrument model and the working conditions of the reference instrument, the instrument should be in a stable state. In the sample test form, enter the following parameters: sample mass (g or ml), sieve volume (45Tm).), select the concentration unit of the result, gradually increase the furnace temperature to the required temperature, and measure after stabilization. Continuous standard blank injection: After the reading is stable, switch to the standard series measurement, and before switching to the detailed test, enter the blank automatic measurement state, monthly sample blank automatic sampling: let the receiver take the average value as the research value, and then measure the test values in turn. After the determination is completed, select the "print" report to automatically print the test results. 30 Auxiliary results calculation
The content in the sample is calculated by formula (1)
K-3 Aldehyde: nitric acid-isochlorous acid (A-1), 21.4 Potassium hydroxide solution (400/L): 21.5 Sodium hydroxide (200 g) 21.6 Sodium citrate (250 g/L): 21.7 Reagents: Weigh 4 mg of 6-hydroxybenzoic acid and dissolve in 50 mL of dichloromethane, add to brown solution. 21.8 Standard solution: same as 9. 21.9 Standard solution: same as 9., but dilute to 1.6 g per liter. 22 Only spectrophotometer is required. 23 Analytical steps 23.1 Sample digestion: Take 5.00 ~ 10.00 In two 150 mL bottles, add 15 r[.~-20 1mL of strong aldehyde (if the test is done overnight at room temperature, the next day is the day of digestion), heat on low heat, and after the foam disappears, slowly increase the heat, and add a small amount of nitric acid if necessary, until the solution is colorless or slightly yellow, and cool to room temperature. Take a mixed acid equivalent to the sample, and perform the test with the same operation method as the sample. 23.2
Wash the new sample and the test blank with 20mL of water several times into a 25T separatory funnel to check the oxidation reaction (20)g/H,
Pipette 6, 3.5, 1.0, 3.0.5.0.7.0, 10.3ml of standard use (equivalent to 9, 0.5, 1.0, 3.0.5.0, 7..10.0ml) and place them in 12 minutes, then add 200/1 sodium chloride solution to make it equal to 2 Adjust the sample digestion solution, add 3ml sodium citrate (ESV/L) 4mL alcohol (4g/L) and potassium hydroxide (2g), mix. Then add 5ml trichloromethane and 2ml trichloromethane, shake immediately, let stand for stratification, pass the trichloromethane layer through debonded cotton, adjust the absorption point with monoxide, and record the absorbance at wavelength 565 in a cm colorimetric cup. After subtracting six blank values from each standard point, prepare a standard curve, or calculate the return value between the standard points, compare the content with the surface line or substitute it to find out the result. Calculate the same as in the 18th competition. 25 Sugar density 26 Principle 4th method Atomic fluorescence method GD/T 5009.152003
After wet digestion or drying or oxidization, the food sample is added with potassium hydride to generate volatile substances in the reaction with the oxidizing agent, and then vaporized in a quartz atomizer. Under the excitation of the emission of a special chamber cathode lamp, atomic fluorescence is generated. The fluorescence noise is proportional to the substance being measured under the same conditions and is comparable to the standard series. 27 Test Conditions
27.1 Sulfur (super pure).
27.2 Magnetic Acid (super pure).
27.3 Magnesium Chloride (super pure).
27.4 Selenium Oxide (39%).
27.5 Disulfur dioxide·tetrachloride solution (0.=/L): Weigh C.25R disulfide and dissolve it in carbon tetrachloride in a 100mL volumetric flask and dilute to 100mL.
27.E sulfuric acid solution (C.25ra0./L>: Carefully add 11ml of sulfuric acid into 00mL of water, cool and dilute to 1CCumL, accurate). 27./Air drop micro <0%/1.) agent Take 13R mirror dolphin with sulfuric acid (0.2001/1.> melt and dilute to 2 (0m1. Hook 27.8 containing transfer liquid: weigh 0.4038g cobalt oxide hexahydrate (a, +6H0), or 0.220 sodium chloride (CC,), add water to 100ml. salt bottle, dilute to 100ml, this solution concentration is equivalent to 1mg of cobalt per liter, when applied, the concentration of cobalt ions is 0g: ml.
27.9 Hydroxide gas melt (: R/T) : Weigh 1% potassium hydride. Dissolve in water until the viscosity reaches 200 mL. Mix well. 27.10 Potassium hydride solution (30 mL): Take H3PO4 and dissolve in 1% potassium hydride. And determine the concentration of 1% to 1% of the solution. 27.11 Standard solution <1.00 mg/L: 102 mL/L. 12 Standard solution: Accurately pipette the standard solution and dilute to 50 mL/mL with a saturation (0.2 mL/L). 28 Standard solution 25.1 Dual-phase laser spectrometer with coded polarization lamp, can be a type of intermittent flow sample inlet or a mouse or optical instrument. 28.2 Temperature-controlled digester: The test site's glass sieve and digester must be soaked with nitric acid (1-0) for 24 hours, and then rinsed with deionized water before use.
29 Analysis steps
29.1 Sample digestion
Weigh 0.1% of the sample that has been sieved by the powder (sieve) and place it in the digester. Samples with high moisture content should be first Dry the sample in a refrigerator and add nitric acid-perchloric acid (10% hydrogen peroxide) or place overnight. Heat digest the next day, filter out the digestion liquid if it is yellow or colorless, remove all the nitric acid. Use about 25ml of 0.20mul/L of acid to digest the sample and transfer it to a 50mT volume plate. Add 20% carbon tetrachloride (0.1mol/L) and 1mT containing solution. Reduce to 53mL of sulfuric acid (0.23mol/L), mix and test, and do the reagent test at the same time. 29.2 Preparation of standard series
Pipette 5ug/mL standard sample to obtain 0.450.90, 1.63.3.60.5.40ml.5UmL volumetric bottle, add 0.2u/L>about 2rT. Add S.0mL of dichloromethane (J.5/1.), incubate bacteria for 2min. Add 101r:1. sparse agent <50)g/) and 1nL of solution containing 101r:1. sparse agent (U.2)ml/1. adjust to 0ml. (the concentration of each phase is about 0.501.00, 2.C04.20.5.2)r8/m.), and make a standard blank at the same time. The number of standard blank grain batch test samples should be increased by at least 113
G/T 5009.15—2003
Based on the performance of each instrument model and the working conditions of the reference instrument, the instrument should be in a stable state. In the sample test form, enter the following parameters: sample mass (g or ml), sieve volume (45Tm).), select the concentration unit of the result, gradually increase the furnace temperature to the required temperature, and measure after stabilization. Continuous standard blank injection: After the reading is stable, switch to the standard series measurement, and before switching to the detailed test, enter the blank automatic measurement state, monthly sample blank automatic sampling: let the receiver take the average value as the research value, and then measure the test values in turn. After the determination is completed, select the "print" report to automatically print the test results. 30 Auxiliary results calculation
The content in the sample is calculated by formula (1)
K-3 Aldehyde: nitric acid-isochlorous acid (A-1), 21.4 Potassium hydroxide solution (400/L): 21.5 Sodium hydroxide (200 g) 21.6 Sodium citrate (250 g/L): 21.7 Reagents: Weigh 4 mg of 6-hydroxybenzoic acid and dissolve in 50 mL of dichloromethane, add to brown solution. 21.8 Standard solution: same as 9. 21.9 Standard solution: same as 9., but dilute to 1.6 g per liter. 22 Only spectrophotometer is required. 23 Analytical steps 23.1 Sample digestion: Take 5.00 ~ 10.00 In two 150 mL bottles, add 15 r[.~-20 1mL of strong aldehyde (if the test is done overnight at room temperature, the next day is the day of digestion), heat on low heat, and after the foam disappears, slowly increase the heat, and add a small amount of nitric acid if necessary, until the solution is colorless or slightly yellow, and cool to room temperature. Take a mixed acid equivalent to the sample, and perform the test with the same operation method as the sample. 23.2
Wash the new sample and the test blank with 20mL of water several times into a 25T separatory funnel to check the oxidation reaction (20)g/H,
Pipette 6, 3.5, 1.0, 3.0.5.0.7.0, 10.3ml of standard use (equivalent to 9, 0.5, 1.0, 3.0.5.0, 7..10.0ml) and place them in 12 minutes, then add 200/1 sodium chloride solution to make it equal to 2 Adjust the sample digestion solution, add 3ml sodium citrate (ESV/L) 4mL alcohol (4g/L) and potassium hydroxide (2g), mix. Then add 5ml trichloromethane and 2ml trichloromethane, shake immediately, let stand for stratification, pass the trichloromethane layer through debonded cotton, adjust the absorption point with monoxide, and record the absorbance at wavelength 565 in a cm colorimetric cup. After subtracting six blank values from each standard point, prepare a standard curve, or calculate the return value between the standard points, compare the content with the surface line or substitute it to find out the result. Calculate the same as in the 18th competition. 25 Sugar density 26 Principle 4th method Atomic fluorescence method GD/T 5009.152003
After wet digestion or drying or oxidization, the food sample is added with potassium hydride to generate volatile substances in the reaction with the oxidizing agent, and then vaporized in a quartz atomizer. Under the excitation of the emission of a special chamber cathode lamp, atomic fluorescence is generated. The fluorescence noise is proportional to the substance being measured under the same conditions and is comparable to the standard series. 27 Test Conditions
27.1 Sulfur (super pure).Www.bzxZ.net
27.2 Magnetic Acid (super pure).
27.3 Magnesium Chloride (super pure).
27.4 Selenium Oxide (39%).
27.5 Disulfur dioxide·tetrachloride solution (0.=/L): Weigh C.25R disulfide and dissolve it in carbon tetrachloride in a 100mL volumetric flask and dilute to 100mL.
27.E sulfuric acid solution (C.25ra0./L>: Carefully add 11ml of sulfuric acid into 00mL of water, cool and dilute to 1CCumL, accurate). 27./Air drop micro <0%/1.) agent Take 13R mirror dolphin with sulfuric acid (0.2001/1.> melt and dilute to 2 (0m1. Hook 27.8 containing transfer liquid: weigh 0.4038g cobalt oxide hexahydrate (a, +6H0), or 0.220 sodium chloride (CC,), add water to 100ml. salt bottle, dilute to 100ml, this solution concentration is equivalent to 1mg of cobalt per liter, when applied, the concentration of cobalt ions is 0g: ml.
27.9 Hydroxide gas melt (: R/T) : Weigh 1% potassium hydride. Dissolve in water until the viscosity reaches 200 mL. Mix well. 27.10 Potassium hydride solution (30 mL): Take H3PO4 and dissolve in 1% potassium hydride. And determine the concentration of 1% to 1% of the solution. 27.11 Standard solution <1.00 mg/L: 102 mL/L. 12 Standard solution: Accurately pipette the standard solution and dilute to 50 mL/mL with a saturation (0.2 mL/L). 28 Standard solution 25.1 Dual-phase laser spectrometer with coded polarization lamp, can be a type of intermittent flow sample inlet or a mouse or optical instrument. 28.2 Temperature-controlled digester: The test site's glass sieve and digester must be soaked with nitric acid (1-0) for 24 hours, and then rinsed with deionized water before use.
29 Analysis steps
29.1 Sample digestion
Weigh 0.1% of the sample that has been sieved by the powder (sieve) and place it in the digester. Samples with high moisture content should be first Dry the sample in a refrigerator and add nitric acid-perchloric acid (10% hydrogen peroxide) or place overnight. Heat digest the next day, filter out the digestion liquid if it is yellow or colorless, remove all the nitric acid. Use about 25ml of 0.20mul/L of acid to digest the sample and transfer it to a 50mT volume plate. Add 20% carbon tetrachloride (0.1mol/L) and 1mT containing solution. Reduce to 53mL of sulfuric acid (0.23mol/L), mix and test, and do the reagent test at the same time. 29.2 Preparation of standard series
Pipette 5ug/mL standard sample to obtain 0.450.90, 1.63.3.60.5.40ml.5UmL volumetric bottle, add 0.2u/L>about 2rT. Add S.0mL of dichloromethane (J.5/1.), incubate bacteria for 2min. Add 101r:1. sparse agent <50)g/) and 1nL of solution containing 101r:1. sparse agent (U.2)ml/1. adjust to 0ml. (the concentration of each phase is about 0.501.00, 2.C04.20.5.2)r8/m.), and make a standard blank at the same time. The number of standard blank grain batch test samples should be increased by at least 113
G/T 5009.15—2003
Based on the performance of each instrument model and the working conditions of the reference instrument, the instrument should be in a stable state. In the sample test form, enter the following parameters: sample mass (g or ml), sieve volume (45Tm).), select the concentration unit of the result, gradually increase the furnace temperature to the required temperature, and measure after stabilization. Continuous standard blank injection: After the reading is stable, switch to the standard series measurement, and before switching to the detailed test, enter the blank automatic measurement state, monthly sample blank automatic sampling: let the receiver take the average value as the research value, and then measure the test values in turn. After the determination is completed, select the "print" report to automatically print the test results. 30 Auxiliary results calculation
The content in the sample is calculated by formula (1)
K-Add the reagent, shake it immediately and let it stand for stratification. Then, pass the chloroform layer through a debonded cotton and adjust the absorbance with monoxide. Measure the absorbance at a wavelength of 565 in a cm colorimetric cup. After subtracting the blank value from each standard point, prepare a standard curve or calculate the return value between the curves. Compare the content with the surface line or substitute it to find the result. Calculate the same as in the 18th chapter. 25 Sugar syrup
Same as in the 13th chapter.
26 Principle
Method 4 Atomic Fluorescence Spectrometry
GD/T 5009.152003
After wet digestion or drying or purifying, the food sample is added with potassium hydride to generate volatile substances in the reaction with iodine and then vaporized in a quartz atomizer. Under the excitation of the emission of a special chamber cathode lamp, atomic fluorescence is generated. The fluorescence noise is proportional to the substance being measured under the same conditions and is comparable to the standard series. 27 Test Conditions
27.1 Sulfur (super pure).
27.2 Magnetic Acid (super pure).
27.3 Magnesium Chloride (super pure).
27.4 Selenium Oxide (39%).
27.5 Disulfur dioxide·tetrachloride solution (0.=/L): Weigh C.25R disulfide and dissolve it in carbon tetrachloride in a 100mL volumetric flask and dilute to 100mL.
27.E sulfuric acid solution (C.25ra0./L>: Carefully add 11ml of sulfuric acid into 00mL of water, cool and dilute to 1CCumL, accurate). 27./Air drop micro <0%/1.) agent Take 13R mirror dolphin with sulfuric acid (0.2001/1.> melt and dilute to 2 (0m1. Hook 27.8 containing transfer liquid: weigh 0.4038g cobalt oxide hexahydrate (a, +6H0), or 0.220 sodium chloride (CC,), add water to 100ml. salt bottle, dilute to 100ml, this solution concentration is equivalent to 1mg of cobalt per liter, when applied, the concentration of cobalt ions is 0g: ml.
27.9 Hydroxide gas melt (: R/T) : Weigh 1% potassium hydride. Dissolve in water until the viscosity reaches 200 mL. Mix well. 27.10 Potassium hydride solution (30 mL): Take H3PO4 and dissolve in 1% potassium hydride. And determine the concentration of 1% to 1% of the solution. 27.11 Standard solution <1.00 mg/L: 102 mL/L. 12 Standard solution: Accurately pipette the standard solution and dilute to 50 mL/mL with a saturation (0.2 mL/L). 28 Standard solution 25.1 Dual-phase laser spectrometer with coded polarization lamp, can be a type of intermittent flow sample inlet or a mouse or optical instrument. 28.2 Temperature-controlled digester: The test site's glass sieve and digester must be soaked with nitric acid (1-0) for 24 hours, and then rinsed with deionized water before use.
29 Analysis steps
29.1 Sample digestion
Weigh 0.1% of the sample that has been sieved by the powder (sieve) and place it in the digester. Samples with high moisture content should be first Dry the sample in a refrigerator and add nitric acid-perchloric acid (10% hydrogen peroxide) or place overnight. Heat digest the next day, filter out the digestion liquid if it is yellow or colorless, remove all the nitric acid. Use about 25ml of 0.20mul/L of acid to digest the sample and transfer it to a 50mT volume plate. Add 20% carbon tetrachloride (0.1mol/L) and 1mT containing solution. Reduce to 53mL of sulfuric acid (0.23mol/L), mix and test, and do the reagent test at the same time. 29.2 Preparation of standard series
Pipette 5ug/mL standard sample to obtain 0.450.90, 1.63.3.60.5.40ml.5UmL volumetric bottle, add 0.2u/L>about 2rT. Add S.0mL of dichloromethane (J.5/1.), incubate bacteria for 2min. Add 101r:1. sparse agent <50)g/) and 1nL of solution containing 101r:1. sparse agent (U.2)ml/1. adjust to 0ml. (the concentration of each phase is about 0.501.00, 2.C04.20.5.2)r8/m.), and make a standard blank at the same time. The number of standard blank grain batch test samples should be increased by at least 113
G/T 5009.15—2003
Based on the performance of each instrument model and the working conditions of the reference instrument, the instrument should be in a stable state. In the sample test form, enter the following parameters: sample mass (g or ml), sieve volume (45Tm).), select the concentration unit of the result, gradually increase the furnace temperature to the required temperature, and measure after stabilization. Continuous standard blank injection: After the reading is stable, switch to the standard series measurement, and before switching to the detailed test, enter the blank automatic measurement state, monthly sample blank automatic sampling: let the receiver take the average value as the research value, and then measure the test values in turn. After the determination is completed, select the "print" report to automatically print the test results. 30 Auxiliary results calculation
The content in the sample is calculated by formula (1)
K-Add the reagent, shake it immediately and let it stand for stratification. Then, pass the chloroform layer through a debonded cotton and adjust the absorbance with monoxide. Measure the absorbance at a wavelength of 565 in a cm colorimetric cup. After subtracting the blank value from each standard point, prepare a standard curve or calculate the return value between the curves. Compare the content with the surface line or substitute it to find the result. Calculate the same as in the 18th chapter. 25 Sugar syrup
Same as in the 13th chapter.
26 Principle
Method 4 Atomic Fluorescence Spectrometry
GD/T 5009.152003
After wet digestion or drying or purifying, the food sample is added with potassium hydride to generate volatile substances in the reaction with iodine and then vaporized in a quartz atomizer. Under the excitation of the emission of a special chamber cathode lamp, atomic fluorescence is generated. The fluorescence noise is proportional to the substance being measured under the same conditions and is comparable to the standard series. 27 Test Conditions
27.1 Sulfur (super pure).
27.2 Magnetic Acid (super pure).
27.3 Magnesium Chloride (super pure).
27.4 Selenium Oxide (39%).
27.5 Disulfur dioxide·tetrachloride solution (0.=/L): Weigh C.25R disulfide and dissolve it in carbon tetrachloride in a 100mL volumetric flask and dilute to 100mL.
27.E sulfuric acid solution (C.25ra0./L>: Carefully add 11ml of sulfuric acid into 00mL of water, cool and dilute to 1CCumL, accurate). 27./Air drop micro <0%/1.) agent Take 13R mirror dolphin with sulfuric acid (0.2001/1.> melt and dilute to 2 (0m1. Hook 27.8 containing transfer liquid: weigh 0.4038g cobalt oxide hexahydrate (a, +6H0), or 0.220 sodium chloride (CC,), add water to 100ml. salt bottle, dilute to 100ml, this solution concentration is equivalent to 1mg of cobalt per liter, when applied, the concentration of cobalt ions is 0g: ml.
27.9 Hydroxide gas melt (: R/T) : Weigh 1% potassium hydride. Dissolve in water until the viscosity reaches 200 mL. Mix well. 27.10 Potassium hydride solution (30 mL): Take H3PO4 and dissolve in 1% potassium hydride. And determine the concentration of 1% to 1% of the solution. 27.11 Standard solution <1.00 mg/L: 102 mL/L. 12 Standard solution: Accurately pipette the standard solution and dilute to 50 mL/mL with a saturation (0.2 mL/L). 28 Standard solution 25.1 Dual-phase laser spectrometer with coded polarization lamp, can be a type of intermittent flow sample inlet or a mouse or optical instrument. 28.2 Temperature-controlled digester: The test site's glass sieve and digester must be soaked with nitric acid (1-0) for 24 hours, and then rinsed with deionized water before use.
29 Analysis steps
29.1 Sample digestion
Weigh 0.1% of the sample that has been sieved by the powder (sieve) and place it in the digester. Samples with high moisture content should be first Dry the sample in a refrigerator and add nitric acid-perchloric acid (10% hydrogen peroxide) or place overnight. Heat digest the next day, filter out the digestion liquid if it is yellow or colorless, remove all the nitric acid. Use about 25ml of 0.20mul/L of acid to digest the sample and transfer it to a 50mT volume plate. Add 20% carbon tetrachloride (0.1mol/L) and 1mT containing solution. Reduce to 53mL of sulfuric acid (0.23mol/L), mix and test, and do the reagent test at the same time. 29.2 Preparation of standard series
Pipette 5ug/mL standard sample to obtain 0.450.90, 1.63.3.60.5.40ml.5UmL volumetric bottle, add 0.2u/L>about 2rT. Add S.0mL of dichloromethane (J.5/1.), incubate bacteria for 2min. Add 101r:1. sparse agent <50)g/) and 1nL of solution containing 101r:1. sparse agent (U.2)ml/1. adjust to 0ml. (the concentration of each phase is about 0.501.00, 2.C04.20.5.2)r8/m.), and make a standard blank at the same time. The number of standard blank grain batch test samples should be increased by at least 113
G/T 5009.15—2003
Based on the performance of each instrument model and the working conditions of the reference instrument, the instrument should be in a stable state. In the sample test form, enter the following parameters: sample mass (g or ml), sieve volume (45Tm).), select the concentration unit of the result, gradually increase the furnace temperature to the required temperature, and measure after stabilization. Continuous standard blank injection: After the reading is stable, switch to the standard series measurement, and before switching to the detailed test, enter the blank automatic measurement state, monthly sample blank automatic sampling: let the receiver take the average value as the research value, and then measure the test values in turn. After the determination is completed, select the "print" report to automatically print the test results. 30 Auxiliary results calculation
The content in the sample is calculated by formula (1)
K-In a 5UmL volumetric bottle, add sulfuric acid (0.2u/L> about 2rT.), add S.0mL of second-stream carbon tetrafluoride (J.5/1.), incubate the bacteria for 2min. Add 101r1.sparse origin (<50)g/) and 1nL of solution containing sulfuric acid (U.2)ml/1. adjust to 0ml. (the concentration of each phase is about 0.501.00, 2.C04.20.5.2)r8/m.), and make a standard blank at the same time. The number of standard blank grain batch test samples should be increased by at least 113
G/T 5009.15—2003
Based on the performance of each instrument model and the working conditions of the reference instrument, the instrument should be in a stable state. In the sample test form, enter the following parameters: sample mass (g or ml), sieve volume (45Tm).), select the concentration unit of the result, gradually increase the furnace temperature to the required temperature, and measure after stabilization. Continuous standard blank injection: After the reading is stable, switch to the standard series measurement, and before switching to the detailed test, enter the blank automatic measurement state, monthly sample blank automatic sampling: let the receiver take the average value as the research value, and then measure the test values in turn. After the determination is completed, select the "print" report to automatically print the test results. 30 Auxiliary results calculation
The content in the sample is calculated by formula (1)
K-In a 5UmL volumetric bottle, add sulfuric acid (0.2u/L> about 2rT.), add S.0mL of second-stream carbon tetrafluoride (J.5/1.), incubate the bacteria for 2min. Add 101r1.sparse origin (<50)g/) and 1nL of solution containing sulfuric acid (U.2)ml/1. adjust to 0ml. (the concentration of each phase is about 0.501.00, 2.C04.20.5.2)r8/m.), and make a standard blank at the same time. The number of standard blank grain batch test samples should be increased by at least 113
G/T 5009.15—2003
Based on the performance of each instrument model and the working conditions of the reference instrument, the instrument should be in a stable state. In the sample test form, enter the following parameters: sample mass (g or ml), sieve volume (45Tm).), select the concentration unit of the result, gradually increase the furnace temperature to the required temperature, and measure after stabilization. Continuous standard blank injection: After the reading is stable, switch to the standard series measurement, and before switching to the detailed test, enter the blank automatic measurement state, monthly sample blank automatic sampling: let the receiver take the average value as the research value, and then measure the test values in turn. After the determination is completed, select the "print" report to automatically print the test results. 30 Auxiliary results calculation
The content in the sample is calculated by formula (1)
K-
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