This standard specifies the technical requirements, test methods, inspection rules, and packaging, labeling, storage, and transportation requirements for liquid and powdered caramel colors made by the ammonium sulfite method, ammonia method, and common method. This standard applies to liquid and powdered caramel colors made by the ammonium sulfite method, ammonia method, and common method using sucrose, starch syrup, xylose mother liquor, etc. as raw materials, and used as colorants in foods. GB 8817-2001 Food Additive Caramel Color (Ammonium Sulfite Method, Ammonia Method, Common Method) GB8817-2001 Standard Download Decompression Password: www.bzxz.net

GB8817—2001
This standard is mainly revised by adopting the US Food Chemical Code (FCCIV--1996) in a non-equivalent manner. The indicators of ammonia nitrogen and 4-methylimidazole are slightly better than foreign standards. The items and indicators are mainly based on the FCC IV-1996 standard. This standard is revised on the basis of GB8817-1988 "Food Additive Caramel Color" (Ammonia Method), QB1412-1991 "Food Additive Caramel Color (Ammonium Sulfite Method)" and QB2392--1998 (Food Additive Caramel Color (Ammonium Sulfite Method and Common Method)". In addition, the total nitrogen, total sulfur and mercury content indicators are added according to the requirements of FCCIV-1996 standard, making this standard more monitorable and practical. From the date of implementation, this standard will replace GB8817-1988, QB1412-1991 and QB2392-1998. This standard is proposed by the State Bureau of Light Industry.||t t||This standard is under the jurisdiction of the National Food Fermentation Standardization Center. The drafting units of this standard: Chongqing Tianfu Cola Yulong Food and Beverage Co., Ltd., China Food Fermentation Industry Research Institute, Shanghai Aipu Food Industry Co., Ltd., Jianjiang Ruian Kangwei Pharmaceutical Co., Ltd., Chongqing Dark Horse Food Additive Company, Dalian Hongyuan Food Co., Ltd. The main drafters of this standard: Peng Gang, Tan Jirong, Zheng Jiufang, Xiu Yan, Ge Yi, Zhang Yaqin, Ye Tianbao. 69
1 Scope
National Standard of the People's Republic of China
Caramel
Food additives
(Sulfite ammonia caramel, ammonia caramel, plain caramel)
GB 8817—2001
Replaces GB8817—1988
This standard specifies the technical requirements, test methods, inspection rules, and packaging, marking, storage, and transportation requirements for liquid and powdered caramel color made by the ammonium sulfite method, ammonia method, and common method. This standard is applicable to liquid and powdered caramel color made by the ammonium sulfite method, ammonia method, and common method using sucrose, starch syrup, xylose mother liquor, etc. as raw materials, and used as a colorant in food. 2 Referenced Standards
The provisions contained in the following standards constitute this standard through reference. The provisions of the standard. When this standard is published, the versions shown are valid. All standards are subject to revision. Parties using this standard should explore the possibility of using the latest versions of the following standards. GB/T602—1988 Preparation of standard solutions for determination of impurities in chemical reagents GB/T5009.5—1985 Determination of protein in food GB/T5009.17—1996 Determination of total mercury in food GB/T5009.34—1996 Determination of sulfite in food GB/T8449—1987 Determination of lead in food additives GB/T 8450—1987
Determination of lead in food additives
GB/T 8451—1987
Limit test method for heavy metals in food additives 3 Requirements
3.1 Sensory indicators
3.1.1 Color and appearance: dark brown, thick liquid or powdery. 3.1.2 Odor: Caramel flavor, no peculiar smell. 3.1.3 After dilution, the product should be clear, without turbidity and precipitation. 3.2 Physical and chemical indicators (see Table 1)
Absorbance, E (610nm)
Loss on drying.%,
Inspected by quality blood test tape Total weekly 203-06 Standard China
0. 05 ~~0. 6
2002-02-01 implementation
Ammonia (NH3),
Sulfur dioxide (SO4),%
4-Methylimidazole,%
Arsenic (As),mg/kg
Lead (Pb),mg/kg
Heavy metals (Ph),mg/kg
Total nitrogen* (N),%
Total mercury (Hg),mg/kg
Total sulfur (S),%
GB 8817-2001
Table 1 (end)
Note: The index value of the item with * is the index value when the absorbance is 0.10 absorption unit (when the chromaticity is not equal to 0.10, the relevant indexes shall be converted and then compared and judged with this table); ammonia nitrogen and 4-methylimidazole are not detected for caramel color produced by the common method. 4 Test method
Unless otherwise specified, the reagents and instruments used in the test are analytical reagents, distilled water or deionized water and common laboratory instruments.
4.1 Sensory test
4.1.1 Color and appearance
Suck or pour the sample (liquid or powder) into a colorless glass beaker and observe its color and appearance. 4.1.2 Odor
Dilute the sample into a 5g/L to 20g/L aqueous solution and smell its odor. 4.7.3 Clarity
Dilute the sample into a 2g/L4g/L aqueous solution and place it in a 50mL colorimetric tube. Observe from top to bottom in a bright place. 4.2 Determination of absorbance
Weigh 0.5g of sample (accurate to 0.002g). Make up to volume with water in a 500mL volumetric flask, use a 1cm colorimetric dish, and measure its absorbance at 610mm with a spectrophotometer.
4.3 Determination of loss on drying
4.3.1 Determination method
Use a weighing bottle that has been weighed to a constant weight to weigh 2g of sample (accurate to 0.0002g), dry at 105℃ for 2h, cool, and weigh. 4.3.2 Expression of analytical results
Wherein: X~
-Loss on drying: %
-Mass of weighing bottle and sample before drying, g; m. .
Mass of weighing bottle and sample after drying, g: mz
m—Mass of sample, g.
4.4 Determination of ammonia nitrogen
4.4.1 Reagents and solutions
4. 4. 1. 1
Boric acid (GB/T628): 2% solution.
m,—m
（1）
GB 8817—2001
4.4.1.2 Methyl red-bromocresol green mixed indicator solution: Mix 5 parts of 0.2% bromocresol green ethanol solution with 1 part of 0.2% methyl red ethanol solution.
4.4.1.3 Magnesium oxide (HGB1294).
4.4.1.4 Hydrochloric acid (GB/T622) 0.1 mal/L solution, prepared and calibrated according to GB/T602. 4.4.2 Determination method
Weigh 5g of sample (accurate to 0.01g) and place it in a 500mL distillation flask, add 2g of magnesium oxide and 200mL of water, and distill it by direct fire. The distillate is absorbed in 5mL of 2% boric acid solution with 5 drops of mixed indicator liquid. When the distillate is about 100mL, stop distillation and titrate the distillate with 0.1mol/I. hydrochloric acid until it turns grayish red.
4.4.3 Expression of analysis results
Where: X,-
X - V×cX0.017 × 100 × 0.1/Anom
Ammonia nitrogen, in NH3:, %;
The volume of 0.1mol/L hydrochloric acid consumed, mL
The concentration of hydrochloric acid standard solution, mol/L;
0.017——The number of grams of ammonia equivalent to 1.00mL1.000mol/L hydrochloric acid solution, g; m
Weigh the mass of the sample,
The absorbance of the sample at 610nm;
Converted to the value when the color is 0.1.
0. 1/Aa10
4.5 Determination of sulfur dioxide
Determined in accordance with GB/T5009.34.
4.6 Determination of 4-methylimidazole (thin layer method) 4.6.1 Reagents and solutions
4.6.1.1 Chloroform-anhydrous ethanol mixed solution (82). 4.6.1.2 Sodium carbonate (HGB1293), 10% solution. 4.6.1.3 Sulfuric acid (GB/T625), 0.05 mol/L solution. 4.6.1.4 Silica gel (GF254) (for thin layer chromatography). 4.6.1.5 Sodium bicarbonate (GB/T640).
4.6.1.6 Sodium bicarbonate (GB/T640), 8% solution. 4.6.1.7 Developing agent [ether-trifluoromethane-methanol (822)] 4.6.1.8 Color developer
A: 0.5% p-aminobenzenesulfonic acid in 2% hydrochloric acid solution; B: 0.5% sodium nitrite solution.
Mix A and B in equal amounts before use.
4.6.1.9 4-Methylimidazole standard solution
++++++++o+++a+++++( 2)
Weigh the sample 4-methylimidazole (accurate to 0.1000g) and place it in a 100mL volumetric flask. Add 95% ethanol to the mark. Each 1mL of this solution is equivalent to 1.0mg 4-methylimidazole. Before use, dilute it with 95% ethanol to a 4-methylimidazole standard solution with each 1mL equivalent to 0.1mg. 4.6.2 Method and steps
4.6.2.1 Extraction
Weigh 5 g of sample (accurate to 0.01 g) and add 15 mL of water to dissolve it. Add 15 mL of 10% sodium carbonate. In a 250 mL separatory funnel, add 80 mL of chloroform-anhydrous ethanol mixed solution. Shake vigorously for 4 min to 5 min. After complete stratification, collect the chloroform-anhydrous ethanol extract in a 250 mL stoppered conical flask. Extract the water layer again with 70 mL of chloroform-anhydrous ethanol mixed solution and combine the extracts. Add 20 mL of 0.05 mol/1.5 mol sulfuric acid to the extract, shake vigorously for 60 times, separate the water layer, and concentrate the solution to 2 mL to 3 mL in a water bath at 60℃～70℃. Slowly add about 0.2 g of sodium bicarbonate powder until no bubbles are generated, and dissolve it in ethanol to 5 mL. 4.6.2.2 Plate making
Weigh 3 g of silica gel (GF254), add 1 mL of 80% sodium bicarbonate solution and 6 mL of steamed filling water, mix and apply on a 125 mm×85 mm thin plate, dry it naturally in the air, and then put it in an oven at 120C to dry for 2 minutes. After taking it out, put it in a desiccator for use. 4.6.2.3 Spotting
Spot 10uL, 20uL, 30uL of 4-methylimidazole standard solution and 100L of sample diluent on the thin plate. Develop the thin plate in the developing agent until the solvent front reaches 10 cm, take out the thin plate, blow dry and spray with a newly prepared color developer. Within 5min~10min, the yellow spot of 4-methylimidazole can reach the deepest depth and remain stable for several hours. Determine the content of 4-methylimidazole in the sample by comparing the spot size and color depth with the standard spot. 4.6.3 Expression of analysis results
× 1 000 × 1 000
Wherein: X-~4-methylimidazole content, %; C——the amount of sample spot equivalent to the standard spot, ug; m——sample mass + g;
V——spot volume, μL
V——total volume of sample solution, μL, Aso——absorbance of sample at 610nm; 0.1/A61c---converted to the content when the color is 0.1. 4.7 Determination of arsenic
Determined by wet digestion and stele method in accordance with GB/T8450---1987. 4.8 Determination of lead
Determined by wet digestion in accordance with GB/T8449--1987. 4.9 Determination of heavy metals
Determined by wet digestion in accordance with GB/T8451--1987. 4.10 Determination of total nitrogen
Determine in accordance with GB/T5009.5.
4.11 Determination of total sulfur
4.11.1 Reagents and solutions
4.11.1.1 Magnesium oxide (HGB1294).
4.11.1.2 Magnesium nitrate [Mg(NO,)*6H2O] (HG 3—1077). 4.11.1.3 Sucrose (HG 3—1001).
4.11.1.4 Nitric acid (GB/T626).
4.11.1.5 Hydrochloric acid (1:1) (GB/T622). 4.11.1.6 10% barium chloride (GB/T652). X 100 X 0.1/A610
4.11.2 Determination method
Select the largest porcelain crucible that matches the muffle furnace (to prevent splashing), add 1g~3g magnesium oxide (MgO) or equivalent magnesium nitrate [Mg(NO:)；·6H,0] 6.4g~19.2g, 1g sucrose powder, slowly add 50mL nitric acid, weigh 5g of sample (accurate to (.01g) (weigh 5g for total sulfur content ≤2.5%, weigh 1g for total sulfur content>2.5%). Steam in a steam bath Make it into a paste, then carbonize it on an electric furnace until it is smokeless, then put it in a muffle furnace, heat it to 525℃, keep the temperature for 4h~5h, and cool it. Dissolve the sample in 100mL of water, neutralize it with hydrochloric acid to pH=7 (using precision test paper), add 2mL of hydrochloric acid, filter the solution into a beaker, heat it to boiling, and slowly add 20mL of 10% chloride (BaCl2) to the hot solution while stirring, boil it for 5min, and leave it overnight. Filter it with ash-free filter paper, transfer all the precipitates to the filter paper, 173
GB 8817-2001
Wash the filter paper and precipitate thoroughly with hot water. Then put the filter paper and precipitate into a constant weight oven, keep it at 105°C for 1 hour, and take it out. Heat it with an electric furnace and slowly carbonize it until it disappears. Finally, ash it at 800°C in a muffle furnace for 1 hour, cool it, and weigh it. Perform a blank test in the same way. 4.11.3 Expression of analysis results
X, = (W- W:)/S × 0. 137 × 100 × 0.1/A610 Where: X
Total sulfur content, %;
Residue after burning of barium sulfate, B:
Wn——Mass of blank test, g;
S—Mass of sample, g;bZxz.net
0.137—Coefficient of conversion of barium sulfate into sulfur; A6l0
Absorbance of sample at 610nm:
0.1/ArlConverted into total sulfur content when the color is 0.1. 4.12 Determination of total mercury
Determined in accordance with GB/T5009.17.
5 Inspection rules
5.1 Products of the same variety with intact packaging produced by the same equipment and the same shift are considered a batch. (4)
5.2 In each batch of production Randomly select samples from the products. For liquid, select small samples of 5% of the number of pieces or barrels of each product (at least 3 pieces or 3 barrels). Each piece (or barrel) should be sampled for no less than 500ml. For powder, 2 bags should be used. The sample taken from each bag should not be less than 250g. Mix the bundled samples quickly and evenly, and put them in two clean and dry large-mouth bottles respectively. Label them with the manufacturer's name, batch and sampling date. One copy is sent to the laboratory for testing and the other copy is kept for future reference. 5.3 Loss on drying (solid) and absorbance are mandatory inspection items. Arsenic, lead, heavy metals, ammonia nitrogen, sulfur dioxide, 4-methylimidazole, total nitrogen and total sulfur are type inspection items.
5.4 If one of the indicators does not meet this indicator during the inspection, double the number of products from the same batch should be re-sampled for re-inspection. If the re-inspection results still do not meet this standard, the batch of products will be judged as unqualified. 5.5 If the supply and demand parties have any objection to the product quality, the two parties may negotiate and select the relevant statutory arbitration department to proceed in accordance with the relevant provisions of this standard.
6 Marking, packaging, transportation, storage
6.1 Marking
The product packaging should firmly indicate the product name, manufacturer name, factory address, trademark, model, standard number, production date, net content, storage period, production license, batch number, etc. And indicate the words "food additives". 6.2 Packaging
Plastic packaging made of packaging materials that meet food hygiene standards should be used. The liquid specifications are 2, 10.20.30kg, and the powder specifications are 0.5, 1, 2.5, 10kg, or packaged according to the specifications required by the demander. The sealing requirements are strict, and the liquid and powder are all packaged with corrugated paper. 6.3 Storage
The product should be stacked in a ventilated, clean and dry place, and must not be mixed with toxic, harmful, corrosive and other substances. 6.4 Transportation
Avoid transporting the product together with harmful, toxic and polluting substances. Prevent heavy pressure, collision, rain, exposure to the sun, etc. 6.5 Shelf Life
From the date of production, if the above packaging, storage and transportation conditions are met and the original packaging is intact, the shelf life is 12 months. 7101g) add 15mL water to dissolve, add 15mL of 10% sodium carbonate, add 80mL of chloroform-anhydrous ethanol mixed solution to a 250mL separatory funnel, shake vigorously for 4min~5min, after complete separation, collect the chloroform-anhydrous ethanol extract in a 250mL stoppered conical flask, extract the water layer again with 70mL of chloroform-anhydrous ethanol mixed solution, and combine the extracts. Add 20mL of 0.05mol/1. sulfuric acid to the extract, shake vigorously for 60 times, separate the water layer, and concentrate the solution to 2mL~3mL on a 60℃~70℃ water bath, slowly add about 0.2g of sodium bicarbonate fine powder until no bubbles are generated, and dissolve it to 5mL with ethanol. 4.6.2.2 Plate preparation
Weigh 3g of silica gel (GF254), add 1mL of 80% sodium bicarbonate solution and 6mL of steamed filling water, mix and apply on a 125mm×85mm thin plate, dry naturally in the air, and then put it in an oven at 120C for 2min, take it out and put it in a desiccator for use. 4.6.2.3 Spotting
Spot 10uL, 20uL, 30uL of 4-methylimidazole standard solution and 100L of sample diluent on the thin plate respectively. Develop the thin plate in the developing agent until the solvent front reaches 10 cm, take out the thin plate, blow dry it, and spray it with a newly prepared color developer. Within 5min~~10min, the yellow spot of 4-methylimidazole can reach the deepest depth and remain stable for several hours. According to the size and color depth of the spot compared with the standard spot, determine the content of 4-methylimidazole in the sample. 4.6.3 Expression of analysis results
× 1 000 × 1 000
Wherein: X-~4-methylimidazole content, %; C——the amount of sample spot equivalent to the standard spot, ug; m——sample mass + g;
V——spot volume, μL
V——total volume of sample solution, μL, Aso——absorbance of sample at 610nm; 0.1/A61c---converted to the content when the color is 0.1. 4.7 Determination of arsenic
Determined by wet digestion and stele method in accordance with GB/T8450---1987. 4.8 Determination of lead
Determined by wet digestion in accordance with GB/T8449--1987. 4.9 Determination of heavy metals
Determined by wet digestion in accordance with GB/T8451--1987. 4.10 Determination of total nitrogen
Determine in accordance with GB/T5009.5.
4.11 Determination of total sulfur
4.11.1 Reagents and solutions
4.11.1.1 Magnesium oxide (HGB1294).
4.11.1.2 Magnesium nitrate [Mg(NO,)*6H2O] (HG 3—1077). 4.11.1.3 Sucrose (HG 3—1001).
4.11.1.4 Nitric acid (GB/T626).
4.11.1.5 Hydrochloric acid (1:1) (GB/T622). 4.11.1.6 10% barium chloride (GB/T652). X 100 X 0.1/A610
4.11.2 Determination method
Select the largest porcelain crucible that matches the muffle furnace (to prevent splashing), add 1g~3g magnesium oxide (MgO) or equivalent magnesium nitrate [Mg(NO:)；·6H,0] 6.4g~19.2g, 1g sucrose powder, slowly add 50mL nitric acid, weigh 5g of sample (accurate to (.01g) (weigh 5g for total sulfur content ≤2.5%, weigh 1g for total sulfur content>2.5%). Steam in a steam bath Make it into a paste, then carbonize it on an electric furnace until it is smokeless, then put it in a muffle furnace, heat it to 525℃, keep the temperature for 4h~5h, and cool it. Dissolve the sample in 100mL of water, neutralize it with hydrochloric acid to pH=7 (using precision test paper), add 2mL of hydrochloric acid, filter the solution into a beaker, heat it to boiling, and slowly add 20mL of 10% chloride (BaCl2) to the hot solution while stirring, boil it for 5min, and leave it overnight. Filter it with ash-free filter paper, transfer all the precipitates to the filter paper, 173
GB 8817-2001
Wash the filter paper and precipitate thoroughly with hot water. Then put the filter paper and precipitate into a constant weight oven, keep it at 105°C for 1 hour, and take it out. Heat it with an electric furnace and slowly carbonize it until it disappears. Finally, ash it at 800°C in a muffle furnace for 1 hour, cool it, and weigh it. Perform a blank test in the same way. 4.11.3 Expression of analysis results
X, = (W- W:)/S × 0. 137 × 100 × 0.1/A610 Where: X
Total sulfur content, %;
Residue after burning of barium sulfate, B:
Wn——Mass of blank test, g;
S—Mass of sample, g;
0.137—Coefficient of conversion of barium sulfate into sulfur; A6l0
Absorbance of sample at 610nm:
0.1/ArlConverted into total sulfur content when the color is 0.1. 4.12 Determination of total mercury
Determined in accordance with GB/T5009.17.
5 Inspection rules
5.1 Products of the same variety with intact packaging produced by the same equipment and the same shift are considered a batch. (4)
5.2 In each batch of production Randomly select samples from the products. For liquid, select small samples of 5% of the number of pieces or barrels of each product (at least 3 pieces or 3 barrels). Each piece (or barrel) should be sampled for no less than 500ml. For powder, 2 bags should be used. The sample taken from each bag should not be less than 250g. Mix the bundled samples quickly and evenly, and put them in two clean and dry large-mouth bottles respectively. Label them with the manufacturer's name, batch and sampling date. One copy is sent to the laboratory for testing and the other copy is kept for future reference. 5.3 Loss on drying (solid) and absorbance are mandatory inspection items. Arsenic, lead, heavy metals, ammonia nitrogen, sulfur dioxide, 4-methylimidazole, total nitrogen and total sulfur are type inspection items.
5.4 If one of the indicators does not meet this indicator during the inspection, double the number of products from the same batch should be re-sampled for re-inspection. If the re-inspection results still do not meet this standard, the batch of products will be judged as unqualified. 5.5 If the supply and demand parties have any objection to the product quality, the two parties may negotiate and select the relevant statutory arbitration department to proceed in accordance with the relevant provisions of this standard.
6 Marking, packaging, transportation, storage
6.1 Marking
The product packaging should firmly indicate the product name, manufacturer name, factory address, trademark, model, standard number, production date, net content, storage period, production license, batch number, etc. And indicate the words "food additives". 6.2 Packaging
Plastic packaging made of packaging materials that meet food hygiene standards should be used. The liquid specifications are 2, 10.20.30kg, and the powder specifications are 0.5, 1, 2.5, 10kg, or packaged according to the specifications required by the demander. The sealing requirements are strict, and the liquid and powder are all packaged with corrugated paper. 6.3 Storage
The product should be stacked in a ventilated, clean and dry place, and must not be mixed with toxic, harmful, corrosive and other substances. 6.4 Transportation
Avoid transporting the product together with harmful, toxic and polluting substances. Prevent heavy pressure, collision, rain, exposure to the sun, etc. 6.5 Shelf Life
From the date of production, if the above packaging, storage and transportation conditions are met and the original packaging is intact, the shelf life is 12 months. 7101g) add 15mL water to dissolve, add 15mL of 10% sodium carbonate, add 80mL of chloroform-anhydrous ethanol mixed solution to a 250mL separatory funnel, shake vigorously for 4min~5min, after complete separation, collect the chloroform-anhydrous ethanol extract in a 250mL stoppered conical flask, extract the water layer again with 70mL of chloroform-anhydrous ethanol mixed solution, and combine the extracts. Add 20mL of 0.05mol/1. sulfuric acid to the extract, shake vigorously for 60 times, separate the water layer, and concentrate the solution to 2mL~3mL on a 60℃~70℃ water bath, slowly add about 0.2g of sodium bicarbonate fine powder until no bubbles are generated, and dissolve it to 5mL with ethanol. 4.6.2.2 Plate preparation
Weigh 3g of silica gel (GF254), add 1mL of 80% sodium bicarbonate solution and 6mL of steamed filling water, mix and apply on a 125mm×85mm thin plate, dry naturally in the air, and then put it in an oven at 120C for 2min, take it out and put it in a desiccator for use. 4.6.2.3 Spotting
Spot 10uL, 20uL, 30uL of 4-methylimidazole standard solution and 100L of sample diluent on the thin plate respectively. Develop the thin plate in the developing agent until the solvent front reaches 10 cm, take out the thin plate, blow dry it, and spray it with a newly prepared color developer. Within 5min~~10min, the yellow spot of 4-methylimidazole can reach the deepest depth and remain stable for several hours. According to the size and color depth of the spot compared with the standard spot, determine the content of 4-methylimidazole in the sample. 4.6.3 Expression of analysis results
× 1 000 × 1 000
Wherein: X-~4-methylimidazole content, %; C——the amount of sample spot equivalent to the standard spot, ug; m——sample mass + g;
V——spot volume, μL
V——total volume of sample solution, μL, Aso——absorbance of sample at 610nm; 0.1/A61c---converted to the content when the color is 0.1. 4.7 Determination of arsenic
Determined by wet digestion and stele method in accordance with GB/T8450---1987. 4.8 Determination of lead
Determined by wet digestion in accordance with GB/T8449--1987. 4.9 Determination of heavy metals
Determined by wet digestion in accordance with GB/T8451--1987. 4.10 Determination of total nitrogen
Determine in accordance with GB/T5009.5.
4.11 Determination of total sulfur
4.11.1 Reagents and solutions
4.11.1.1 Magnesium oxide (HGB1294).
4.11.1.2 Magnesium nitrate [Mg(NO,)*6H2O] (HG 3—1077). 4.11.1.3 Sucrose (HG 3—1001).
4.11.1.4 Nitric acid (GB/T626).
4.11.1.5 Hydrochloric acid (1:1) (GB/T622). 4.11.1.6 10% barium chloride (GB/T652). X 100 X 0.1/A610
4.11.2 Determination method
Select the largest porcelain crucible that matches the muffle furnace (to prevent splashing), add 1g~3g magnesium oxide (MgO) or equivalent magnesium nitrate [Mg(NO:)；·6H,0] 6.4g~19.2g, 1g sucrose powder, slowly add 50mL nitric acid, weigh 5g of sample (accurate to (.01g) (weigh 5g for total sulfur content ≤2.5%, weigh 1g for total sulfur content>2.5%). Steam in a steam bath Make it into a paste, then carbonize it on an electric furnace until it is smokeless, then put it in a muffle furnace, heat it to 525℃, keep the temperature for 4h~5h, and cool it. Dissolve the sample in 100mL of water, neutralize it with hydrochloric acid to pH=7 (using precision test paper), add 2mL of hydrochloric acid, filter the solution into a beaker, heat it to boiling, and slowly add 20mL of 10% chloride (BaCl2) to the hot solution while stirring, boil it for 5min, and leave it overnight. Filter it with ash-free filter paper, transfer all the precipitates to the filter paper, 173
GB 8817-2001
Wash the filter paper and precipitate thoroughly with hot water. Then put the filter paper and precipitate into a constant weight oven, keep it at 105°C for 1 hour, and take it out. Heat it with an electric furnace and slowly carbonize it until it disappears. Finally, ash it at 800°C in a muffle furnace for 1 hour, cool it, and weigh it. Perform a blank test in the same way. 4.11.3 Expression of analysis results
X, = (W- W:)/S × 0. 137 × 100 × 0.1/A610 Where: X
Total sulfur content, %;
Residue after burning of barium sulfate, B:
Wn——Mass of blank test, g;
S—Mass of sample, g;
0.137—Coefficient of conversion of barium sulfate into sulfur; A6l0
Absorbance of sample at 610nm:
0.1/ArlConverted into total sulfur content when the color is 0.1. 4.12 Determination of total mercury
Determined in accordance with GB/T5009.17.
5 Inspection rules
5.1 Products of the same variety with intact packaging produced by the same equipment and the same shift are considered a batch. (4)
5.2 In each batch of production Randomly select samples from the products. For liquid, select small samples of 5% of the number of pieces or barrels of each product (at least 3 pieces or 3 barrels). Each piece (or barrel) should be sampled for no less than 500ml. For powder, 2 bags should be used. The sample taken from each bag should not be less than 250g. Mix the bundled samples quickly and evenly, and put them in two clean and dry large-mouth bottles respectively. Label them with the manufacturer's name, batch and sampling date. One copy is sent to the laboratory for testing and the other copy is kept for future reference. 5.3 Loss on drying (solid) and absorbance are mandatory inspection items. Arsenic, lead, heavy metals, ammonia nitrogen, sulfur dioxide, 4-methylimidazole, total nitrogen and total sulfur are type inspection items.
5.4 If one of the indicators does not meet this indicator during the inspection, double the number of products from the same batch should be re-sampled for re-inspection. If the re-inspection results still do not meet this standard, the batch of products will be judged as unqualified. 5.5 If the supply and demand parties have any objection to the product quality, the two parties may negotiate and select the relevant statutory arbitration department to proceed in accordance with the relevant provisions of this standard.
6 Marking, packaging, transportation, storage
6.1 Marking
The product packaging should firmly indicate the product name, manufacturer name, factory address, trademark, model, standard number, production date, net content, storage period, production license, batch number, etc. And indicate the words "food additives". 6.2 Packaging
Plastic packaging made of packaging materials that meet food hygiene standards should be used. The liquid specifications are 2, 10.20.30kg, and the powder specifications are 0.5, 1, 2.5, 10kg, or packaged according to the specifications required by the demander. The sealing requirements are strict, and the liquid and powder are all packaged with corrugated paper. 6.3 Storage
The product should be stacked in a ventilated, clean and dry place, and must not be mixed with toxic, harmful, corrosive and other substances. 6.4 Transportation
Avoid transporting with harmful, toxic and polluting substances. Prevent heavy pressure, collision, rain, exposure, etc. 6.5 Shelf Life
From the date of production, if the above packaging, storage and transportation conditions are met and the original packaging is intact, the shelf life is 12 months. 713 Expression of analysis results
× 1 000 × 1 000
Wherein: X-~4-methylimidazole content, %; C——sample spot equivalent to the amount of standard push spot, ug; m——sample mass + g;
V——spot volume, μL
V——total volume of sample solution, μL, Aso——absorbance of sample at 610nm; 0.1/A61c---converted to the content when the color is 0.1. 4.7 Determination of arsenic
Determined by wet digestion and stele method in accordance with GB/T8450---1987. 4.8 Determination of lead
Determined by wet digestion in accordance with GB/T8449--1987. 4.9 Determination of heavy metals
Determined by wet digestion in accordance with GB/T8451--1987. 4.10 Determination of total nitrogen
Determine in accordance with GB/T5009.5.
4.11 Determination of total sulfur
4.11.1 Reagents and solutions
4.11.1.1 Magnesium oxide (HGB1294).
4.11.1.2 Magnesium nitrate [Mg(NO,)*6H2O] (HG 3—1077). 4.11.1.3 Sucrose (HG 3—1001).
4.11.1.4 Nitric acid (GB/T626).
4.11.1.5 Hydrochloric acid (1:1) (GB/T622). 4.11.1.6 10% barium chloride (GB/T652). X 100 X 0.1/A610
4.11.2 Determination method
Select the largest porcelain crucible that matches the muffle furnace (to prevent splashing), add 1g~3g magnesium oxide (MgO) or equivalent magnesium nitrate [Mg(NO:)；·6H,0] 6.4g~19.2g, 1g sucrose powder, slowly add 50mL nitric acid, weigh 5g of sample (accurate to (.01g) (weigh 5g for total sulfur content ≤2.5%, weigh 1g for total sulfur content>2.5%). Steam in a steam bath Make it into a paste, then carbonize it on an electric furnace until it is smokeless, then put it in a muffle furnace, heat it to 525℃, keep the temperature for 4h~5h, and cool it. Dissolve the sample in 100mL of water, neutralize it with hydrochloric acid to pH=7 (using precision test paper), add 2mL of hydrochloric acid, filter the solution into a beaker, heat it to boiling, and slowly add 20mL of 10% chloride (BaCl2) to the hot solution while stirring, boil it for 5min, and leave it overnight. Filter it with ash-free filter paper, transfer all the precipitates to the filter paper, 173
GB 8817-2001
Wash the filter paper and precipitate thoroughly with hot water. Then put the filter paper and precipitate into a constant weight oven, keep it at 105°C for 1 hour, and take it out. Heat it with an electric furnace and slowly carbonize it until it disappears. Finally, ash it at 800°C in a muffle furnace for 1 hour, cool it, and weigh it. Perform a blank test in the same way. 4.11.3 Expression of analysis results
X, = (W- W:)/S × 0. 137 × 100 × 0.1/A610 Where: X
Total sulfur content, %;
Residue after burning of barium sulfate, B:
Wn——Mass of blank test, g;
S—Mass of sample, g;
0.137—Coefficient of conversion of barium sulfate into sulfur; A6l0
Absorbance of sample at 610nm:
0.1/ArlConverted into total sulfur content when the color is 0.1. 4.12 Determination of total mercury
Determined in accordance with GB/T5009.17.
5 Inspection rules
5.1 Products of the same variety with intact packaging produced by the same equipment and the same shift are considered a batch. (4)
5.2 In each batch of production Randomly select samples from the products. For liquid, select small samples of 5% of the number of pieces or barrels of each product (at least 3 pieces or 3 barrels). Each piece (or barrel) should be sampled for no less than 500ml. For powder, 2 bags should be used. The sample taken from each bag should not be less than 250g. Mix the bundled samples quickly and evenly, and put them in two clean and dry large-mouth bottles respectively. Label them with the manufacturer's name, batch and sampling date. One copy is sent to the laboratory for testing and the other copy is kept for future reference. 5.3 Loss on drying (solid) and absorbance are mandatory inspection items. Arsenic, lead, heavy metals, ammonia nitrogen, sulfur dioxide, 4-methylimidazole, total nitrogen and total sulfur are type inspection items.
5.4 If one of the indicators does not meet this indicator during the inspection, double the number of products from the same batch should be re-sampled for re-inspection. If the re-inspection results still do not meet this standard, the batch of products will be judged as unqualified. 5.5 If the supply and demand parties have any objection to the product quality, the two parties may negotiate and select the relevant statutory arbitration department to proceed in accordance with the relevant provisions of this standard.
6 Marking, packaging, transportation, storage
6.1 Marking
The product packaging should firmly indicate the product name, manufacturer name, factory address, trademark, model, standard number, production date, net content, storage period, production license, batch number, etc. And indicate the words "food additives". 6.2 Packaging
Plastic packaging made of packaging materials that meet food hygiene standards should be used. The liquid specifications are 2, 10.20.30kg, and the powder specifications are 0.5, 1, 2.5, 10kg, or packaged according to the specifications required by the demander. The sealing requirements are strict, and the liquid and powder are all packaged with corrugated paper. 6.3 Storage
The product should be stacked in a ventilated, clean and dry place, and must not be mixed with toxic, harmful, corrosive and other substances. 6.4 Transportation
Avoid transporting the product together with harmful, toxic and polluting substances. Prevent heavy pressure, collision, rain, exposure to the sun, etc. 6.5 Shelf Life
From the date of production, if the above packaging, storage and transportation conditions are met and the original packaging is intact, the shelf life is 12 months. 713 Expression of analysis results
× 1 000 × 1 000
Wherein: X-~4-methylimidazole content, %; C——sample spot equivalent to the amount of standard push spot, ug; m——sample mass + g;
V——spot volume, μL
V——total volume of sample solution, μL, Aso——absorbance of sample at 610nm; 0.1/A61c---converted to the content when the color is 0.1. 4.7 Determination of arsenic
Determined by wet digestion and stele method in accordance with GB/T8450---1987. 4.8 Determination of lead
Determined by wet digestion in accordance with GB/T8449--1987. 4.9 Determination of heavy metals
Determined by wet digestion in accordance with GB/T8451--1987. 4.10 Determination of total nitrogen
Determine in accordance with GB/T5009.5.
4.11 Determination of total sulfur
4.11.1 Reagents and solutions
4.11.1.1 Magnesium oxide (HGB1294).
4.11.1.2 Magnesium nitrate [Mg(NO,)*6H2O] (HG 3—1077). 4.11.1.3 Sucrose (HG 3—1001).
4.11.1.4 Nitric acid (GB/T626).
4.11.1.5 Hydrochloric acid (1:1) (GB/T622). 4.11.1.6 10% barium chloride (GB/T652). X 100 X 0.1/A610
4.11.2 Determination method
Select the largest porcelain crucible that matches the muffle furnace (to prevent splashing), add 1g~3g magnesium oxide (MgO) or equivalent magnesium nitrate [Mg(NO:)；·6H,0] 6.4g~19.2g, 1g sucrose powder, slowly add 50mL nitric acid, weigh 5g of sample (accurate to (.01g) (weigh 5g for total sulfur content ≤2.5%, weigh 1g for total sulfur content>2.5%). Steam in a steam bath Make it into a paste, then carbonize it on an electric furnace until it is smokeless, then put it in a muffle furnace, heat it to 525℃, keep the temperature for 4h~5h, and cool it. Dissolve the sample in 100mL of water, neutralize it with hydrochloric acid to pH=7 (using precision test paper), add 2mL of hydrochloric acid, filter the solution into a beaker, heat it to boiling, and slowly add 20mL of 10% chloride (BaCl2) to the hot solution while stirring, boil it for 5min, and leave it overnight. Filter it with ash-free filter paper, transfer all the precipitates to the filter paper, 173
GB 8817-2001
Wash the filter paper and precipitate thoroughly with hot water. Then put the filter paper and precipitate into a constant weight oven, keep it at 105°C for 1 hour, and take it out. Heat it with an electric furnace and slowly carbonize it until it disappears. Finally, ash it at 800°C in a muffle furnace for 1 hour, cool it, and weigh it. Perform a blank test in the same way. 4.11.3 Expression of analysis results
X, = (W- W:)/S × 0. 137 × 100 × 0.1/A610 Where: X
Total sulfur content, %;
Residue after burning of barium sulfate, B:
Wn——Mass of blank test, g;
S—Mass of sample, g;
0.137—Coefficient of conversion of barium sulfate into sulfur; A6l0
Absorbance of sample at 610nm:
0.1/ArlConverted into total sulfur content when the color is 0.1. 4.12 Determination of total mercury
Determined in accordance with GB/T5009.17.
5 Inspection rules
5.1 Products of the same variety with intact packaging produced by the same equipment and the same shift are considered a batch. (4)
5.2 In each batch of production Randomly select samples from the products. For liquid, select small samples of 5% of the number of pieces or barrels of each product (at least 3 pieces or 3 barrels). Each piece (or barrel) should be sampled for no less than 500ml. For powder, 2 bags should be used. The sample taken from each bag should not be less than 250g. Mix the bundled samples quickly and evenly, and put them in two clean and dry large-mouth bottles respectively. Label them with the manufacturer's name, batch and sampling date. One copy is sent to the laboratory for testing and the other copy is kept for future reference. 5.3 Loss on drying (solid) and absorbance are mandatory inspection items. Arsenic, lead, heavy metals, ammonia nitrogen, sulfur dioxide, 4-methylimidazole, total nitrogen and total sulfur are type inspection items.
5.4 If one of the indicators does not meet this indicator during the inspection, double the number of products from the same batch should be re-sampled for re-inspection. If the re-inspection results still do not meet this standard, the batch of products will be judged as unqualified. 5.5 If the supply and demand parties have any objection to the product quality, the two parties may negotiate and select the relevant statutory arbitration department to proceed in accordance with the relevant provisions of this standard.
6 Marking, packaging, transportation, storage
6.1 Marking
The product packaging should firmly indicate the product name, manufacturer name, factory address, trademark, model, standard number, production date, net content, storage period, production license, batch number, etc. And indicate the words "food additives". 6.2 Packaging
Plastic packaging made of packaging materials that meet food hygiene standards should be used. The liquid specifications are 2, 10.20.30kg, and the powder specifications are 0.5, 1, 2.5, 10kg, or packaged according to the specifications required by the demander. The sealing requirements are strict, and the liquid and powder are all packaged with corrugated paper. 6.3 Storage
The product should be stacked in a ventilated, clean and dry place, and must not be mixed with toxic, harmful, corrosive and other substances. 6.4 Transportation
Avoid transporting the product together with harmful, toxic and polluting substances. Prevent heavy pressure, collision, rain, exposure to the sun, etc. 6.5 Shelf Life
From the date of production, if the above packaging, storage and transportation conditions are met and the original packaging is intact, the shelf life is 12 months. 71137 × 100 × 0.1/A610 Where: X
Total sulfur content, %;
Residue after burning of barium sulfate, B:
Wn——Mass of blank test, g;
S—Mass of sample, g;
0.137—Coefficient of conversion of barium sulfate into sulfur; A6l0
Absorbance of sample at 610nm:
0.1/ArlConverted into total sulfur content when the color is 0.1. 4.12 Determination of total mercury
Determined in accordance with GB/T5009.17.
5 Inspection rules
5.1 Products of the same variety with intact packaging produced by the same equipment and the same shift are considered a batch. (4)
5.2 Randomly select samples from each batch of products. For liquid, select 5% of the number of pieces or barrels of each product (at least 3 pieces or 3 barrels). Each piece (or barrel) should be sampled for no less than 500ml. For powder, 2 bags should be used. Each bag should be sampled for no less than 250g. Mix the bundled samples quickly and evenly. Put them in two clean and dry large-mouth bottles. Label them with the manufacturer's name, batch and sampling date. One copy should be sent to the laboratory for testing and the other copy should be kept for future reference. 5.3 Loss on drying (solid) and absorbance are mandatory inspection items. Arsenic, lead, heavy metals, ammonia nitrogen, sulfur dioxide, 4-methylimidazole, total nitrogen and total sulfur are type inspection items.
5.4 If one of the indicators does not meet this indicator during the inspection, double the number of products from the same batch should be re-sampled for re-inspection. If the re-inspection results still do not meet this standard, the batch of products will be judged as unqualified. 5.5 If the supply and demand parties have any objection to the product quality, the two parties may negotiate and select the relevant statutory arbitration department to proceed in accordance with the relevant provisions of this standard.
6 Marking, packaging, transportation, storage
6.1 Marking
The product packaging should firmly indicate the product name, manufacturer name, factory address, trademark, model, standard number, production date, net content, storage period, production license, batch number, etc. And indicate the words "food additives". 6.2 Packaging
Plastic packaging made of packaging materials that meet food hygiene standards should be used. The liquid specifications are 2, 10.20.30kg, and the powder specifications are 0.5, 1, 2.5, 10kg, or packaged according to the specifications required by the demander. The sealing requirements are strict, and the liquid and powder are all packaged with corrugated paper. 6.3 Storage
The product should be stacked in a ventilated, clean and dry place, and must not be mixed with toxic, harmful, corrosive and other substances. 6.4 Transportation
Avoid transporting the product together with harmful, toxic and polluting substances. Prevent heavy pressure, collision, rain, exposure to the sun, etc. 6.5 Shelf Life
From the date of production, if the above packaging, storage and transportation conditions are met and the original packaging is intact, the shelf life is 12 months. 71137 × 100 × 0.1/A610 Where: X
Total sulfur content, %;
Residue after burning of barium sulfate, B:
Wn——Mass of blank test, g;
S—Mass of sample, g;
0.137—Coefficient of conversion of barium sulfate into sulfur; A6l0
Absorbance of sample at 610nm:
0.1/ArlConverted into total sulfur content when the color is 0.1. 4.12 Determination of total mercury
Determined in accordance with GB/T5009.17.
5 Inspection rules
5.1 Products of the same variety with intact packaging produced by the same equipment and the same shift are considered a batch. (4)
5.2 Randomly select samples from each batch of products. For liquid, select 5% of the number of pieces or barrels of each product (at least 3 pieces or 3 barrels). Each piece (or barrel) should be sampled for no less than 500ml. For powder, 2 bags should be used. Each bag should be sampled for no less than 250g. Mix the bundled samples quickly and evenly. Put them in two clean and dry large-mouth bottles. Label them with the manufacturer's name, batch and sampling date. One copy should be sent to the laboratory for testing and the other copy should be kept for future reference. 5.3 Loss on drying (solid) and absorbance are mandatory inspection items. Arsenic, lead, heavy metals, ammonia nitrogen, sulfur dioxide, 4-methylimidazole, total nitrogen and total sulfur are type inspection items.
5.4 If one of the indicators does not meet this indicator during the inspection, double the number of products from the same batch should be re-sampled for re-inspection. If the re-inspection results still do not meet this standard, the batch of products will be judged as unqualified. 5.5 If the supply and demand parties have any objection to the product quality, the two parties may negotiate and select the relevant statutory arbitration department to proceed in accordance with the relevant provisions of this standard.
6 Marking, packaging, transportation, storage
6.1 Marking
The product packaging should firmly indicate the product name, manufacturer name, factory address, trademark, model, standard number, production date, net content, storage period, production license, batch number, etc. And indicate the words "food additives". 6.2 Packaging
Plastic packaging made of packaging materials that meet food hygiene standards should be used. The liquid specifications are 2, 10.20.30kg, and the powder specifications are 0.5, 1, 2.5, 10kg, or packaged according to the specifications required by the demander. The sealing requirements are strict, and the liquid and powder are all packaged with corrugated paper. 6.3 Storage
The product should be stacked in a ventilated, clean and dry place, and must not be mixed with toxic, harmful, corrosive and other substances. 6.4 Transportation
Avoid transporting the product together with harmful, toxic and polluting substances. Prevent heavy pressure, collision, rain, exposure to the sun, etc. 6.5 Shelf Life
From the date of production, if the above packaging, storage and transportation conditions are met and the original packaging is intact, the shelf life is 12 months. 71
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