Some standard content:
National Standard of the People's Republic of China
Food additive
Cacao pigment
UDC 647. 97 : 664
GB8818-88
This standard applies to brown powder obtained by extraction, concentration, refining and spray drying with cocoa shell as raw material and water as solvent, which is used as a colorant in the food industry.
Technical requirements
1.1 Appearance: This pigment is brown powder. It is easily soluble in water and 0.1% aqueous solution is clear. 1.2 Items and indicators
Water insoluble matter, %
Weight loss on drying, %
Ignition residue, %
Absorbance e: 400nm±5
Heavy metals (in terms of Pb), %
Arsenic (As), %
Lead (Pb), %
2 Test methods
2.1 Identification
2.1.1 Physical properties
This product is a brown powder, which is susceptible to moisture.
0.1% aqueous solution is brown and transparent, 0.1% 6mol1/L sodium hydroxide solution, the color deepens and becomes reddish brown, 0.1% 6mol1/L hydrochloric acid solution, the color fades and becomes yellowish brown.
2.1.2 Maximum absorption peak
0.01% aqueous solution has two absorption peaks under visible-ultraviolet spectrophotometer, one maximum absorption peak at 195nm and one smaller absorption peak at 275nm.
2.2 pH determination
The sample is prepared into 1% aqueous solution with distilled water and measured with an acidometer. 2.3 Determination of water-insoluble matter
2.3.1 Determination procedure
Weigh about 0.5g of sample (accurate to 0.0002g) into a 500mL beaker, add 200mL of distilled water, cover with blood, heat to boil (Approved by the Ministry of Commerce of the People's Republic of China on February 12, 1988 and implemented on July 1, 1988)
GB8818-88bzxz.net
【h), stir frequently while hot. Use G that has been dried and weighed to a constant weight, filter under reduced pressure on a sintered funnel, wash the filter thoroughly with hot distilled water, and dry at 105℃ to a constant weight.
2.3.2 Calculation and result expression
X =M=M×100
Where: X,---water insoluble matter, %
Mass of vertical melting funnel and insoluble matter, B;
Mass of vertical melting funnel, 8
Mass of sample, name.
2.4 Determination of loss on drying
2.4.1 Apparatus
Aluminum box, diameter 45~50mm, height 25mm.
2.4.2 Determination procedure
Weigh 2g of sample (accurate to 0.0002g) in an aluminum box that has been dried and weighed to a constant weight. The thickness of the sample is about 5mm. Spread evenly, open the cover and dry in a drying oven at 105℃ for 4h and weigh to a constant weight. 2.4.3 Calculation and result expression
Where: X,
Loss on drying, %;
-Mass of aluminum box and sample before drying, B;
Mass of aluminum box and sample after drying, g;
M.Mass of sample. B.
2.5 Determination of ignition residue
2.5.1 Determination procedure
· (2)
Weigh 3g of sample (accurate to 0.002g) and place it in a porcelain crucible that has been kept constant at 700-800℃, first carbonize at low temperature (about 300℃), then at the highest temperature (about 500℃), transfer it to a Muffle furnace, and ignite it at 800℃ to constant weight. 2.5.2 Calculation and result expression
Where: X,—
Residue on ignition, %:
M. Add the mass of the residue to the crucible + g;
-the mass of the crucible, more:
M,-the mass of the sample, B.
2.6 Determination of absorbance
2.6.1 Instrument: spectrophotometer, with 1cm colorimetric blood. 2.6.2 Determination procedure
M. -M,
Put the sample in a desiccator and dry-burn it at room temperature for 24 hours. Weigh 1B (accurate to 0.0002g) and dissolve it in distilled water and make it up to 100mL. Mix and filter. Take 2mL of the filtrate with a pipette and dilute it with distilled water. Make it up to 100mL (i.e., 0.02% aqueous solution). Use a spectrophotometer and distilled water as the reference solution to measure its absorbance at a wavelength of 400nm±5 in 1cm colorimetric blood. 2.6.3 Calculation and result expression
1××50
(4)
Wherein; E: --- absorbance of the sample measured: M, --- mass of the sample accurately weighed, B; 50 -- dilution multiple.
2.7 Determination of heavy metals
2.7.1 Reagents
GB8818-88
2.7.1.1 Phenol butter (HGB3080-50) indicator solution: 1% ethanol solution. 2.7.1.2 Nitric acid (GB626-78): analytical grade. 2.7.1.3 Sodium hydroxide (GB629-77): analytical grade, 10% solution. 2.7.1.4 Glacial acetic acid (GB676-78), analytical grade, 30% solution. 2.7.1.5 Saturated hydrogen sulfide water: pass hydrogen sulfide gas into water without carbon dioxide until saturated (this solution is prepared before use).
2.7.1.6 Lead standard solution: Prepare according to the preparation method of chemical reagent impurity standard solution GB602-77, dilute 10 times before use, and contain 0.01 mg lead per milliliter.
2.7.2 Determination procedures
Weigh 2g of sample (accurate to 0.0002g), place in porcelain evaporating blood, add 1.5mL sulfuric acid, wet and carbonize the sample, then move it into a muffle furnace, ash it at 500℃ to off-white, add 5mL nitric acid after cooling, evaporate to dryness on the aqueous solution, cool and dissolve in distilled water. Add 1 drop of phenol anhydride indicator solution, adjust with 10% sodium hydroxide solution until the red color just fades, filter into a 50mL Gang's colorimetric tube, wash the residue with distilled water for several times, and dilute to 25mL, add 0.5mL 30% acetic acid solution, dilute to 50mL with distilled water, which is tube A. Take another 50mL Gang's colorimetric tube, add 2.0mL lead standard solution and 0.5mL 30% acetic acid solution, dilute to 50mL with distilled water, which is tube B.
Add 10mL saturated hydrogen sulfide water to each tube A and B, spread evenly, place in the dark for 10min for colorimetric comparison, and the color of tube A shall not be darker than that of tube B.
2.8 Determination of arsenic
Take 5g of sample (accurate to 0.01g) and digest it by wet method, dilute to 50mL with water, take 10mL of dilution, and perform the arsenic determination according to GB5009.11-85 "Determination of total arsenic in food" method. 2.9 Determination of lead
Take 10mL of the wet digestion dilution under 2.8 and perform the test according to the dithiothrene colorimetric method in GB5009.12-85 "Determination of lead in food".
3 Acceptance rules
3.1 This product shall be inspected by the technical inspection department of the manufacturer. The manufacturer shall ensure that all products shipped meet the requirements of this standard. Each batch of products shipped shall be accompanied by a quality certificate. 3.2 Users may use the inspection rules and test methods specified in this standard. Acceptance inspection of the received products. 3.3 Sampling method: Samples should be selected from 10% of the number of packages in each batch. The number of small batches should not be less than 3 packages. Samples should be taken evenly from the selected packages, and no less than 100g of samples should be taken. The total weight of each batch of samples should not be less than 1k. The selected samples should be mixed and divided into 500g by quartering method. They should be placed in clean and dry wide-mouth bottles, labeled with the manufacturer name, product name, batch number and sampling date, and sent to the laboratory for analysis. 3.4 If any of the indicators in the inspection do not meet the requirements, When the standard is met, samples should be selected from twice the amount of packaging for verification. If the result of the re-inspection of the product does not meet the requirements of this standard even if only one indicator does not meet the requirements of this standard, the entire batch cannot be accepted. 3.5 When the supply and demand parties have disputes over product quality, an arbitration unit agreed upon by both parties may conduct verification. 4 Marking, packaging, transportation, storage
4.1 This pigment should be stored in clean and dry polyethylene bottles lined with polypropylene film bags (bottles and bags should meet the requirements of food hygiene packaging), and the seals must be tight. The net weight of each bottle is 500g, and 20 bottles are packed in one box. The carton must be firm, and the net weight of each box is 10kg. 477
GB881888
4.2 The box (bag) should be firmly marked with the manufacturer's name, product name, batch number, production date, net weight, and the words "food additive". 4.3 Each batch of pigments shipped out of the factory should be accompanied by a quality certificate, including: manufacturer's name, product name, batch number, production date and inspection date, number of pieces, weight and product quality, etc. 4.4. This pigment must not be mixed with harmful substances during storage and transportation, and should be kept dry and clean, away from sunlight, rain and heat. When stored, it should be placed at least 100mm above the ground to avoid moisture. 4.5 Storage period: Under the required storage conditions, the quality should remain stable within 12 months. Additional remarks:
This standard was proposed and coordinated by the Science and Technology Department of the Ministry of Commerce and the Food Hygiene Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by the Zhejiang Shaoxing Oil and Fragrance Factory and the Zhejiang Food Hygiene Supervision and Inspection Institute. The main drafters of this standard are Fu Xichun, Shao Fangde and Lu Desheng. 178
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