Some standard content:
National Standard of the People's Republic of China
Food additive
Propyl p-hydroxybenzoate
UdC 661.782.1
GB 8851-88
This standard applies to propyl p-hydroxybenzoate made by esterification of p-hydroxybenzoic acid and propanol with sulfuric acid as catalyst. The product is used as a protective agent in food processing.
Molecular formula: C1oH12O3
Structural formula:
Molecular weight: 180.21 (according to the international atomic weight in 1985) 1 Technical requirements
CO+ CH2 CH, CH,
1.1 Appearance: white crystalline powder, odorless or with a slight special aroma, slightly bitter and burning. 1.2 Items and indicators
Content (on dry basis), %
Melting point, ℃
Sulfate (as SO4), %
Parahydroxybenzoic acid and salicylic acid
Loss on drying, %
Ignition residue, %bZxz.net
Arsenic (As), %
Heavy metal (as Pb), %
Test method
The standard solutions, impurity standard solutions, preparations and products used in this standard are prepared in accordance with the provisions of GB601-77 "Preparation Method of Chemical Reagent Standard Solutions", GB602-77 "Preparation Method of Chemical Reagent Impurity Standard Solutions" and GB603-77 "Preparation Method of Chemical Reagent Preparations and Products" (the concentration of standard solutions should be expressed in terms of molar concentration). The reagents used are all analytically pure reagents, the water used is distilled water or water of corresponding purity, and the instruments used are general laboratory instruments. Approved by the Ministry of Chemical Industry of the People's Republic of China on February 4, 1988 368
Implementation on November 1, 1988
2.1 Identification
GB 8851--88
2.1.1 Reagents and solutions
2.1.1.1 Sodium hydroxide (GB 629-77): 40g/L solution; 2.1.1.2 Sulfuric acid (GB 625-77): 10% (m/V) 2.1.1.3 Barium chloride (GB 652-78): 25% (m/V). 2.1.2 Identification method
2.1.2.1 Take about 0.5g of sample (accurate to 0.01g), add 10ml of sodium hydroxide solution (2.1.1.1) and boil for 30min, evaporate to about 5ml, cool, add sulfuric acid solution (2.1.1.2) to make it acidic, filter, wash the precipitate with water until the filtrate is not turbid when tested with barium chloride solution (2.1.1.3), then dry the precipitate at 105±2℃ for 1h, and determine the melting point according to GB617--77 "Melting Point Determination Method" to be 213~217℃.
2.2 Determination of propyl paraben content 2.2.1 Reagents and solutions
2.2.1.1 Sodium hydroxide (GB629-77): 40g/L solution; 2.2.1.2 Acid (GB 625-77): c(H,SO4)=0.5mol/L standard solution; 2.2.1.3 Bromothymol blue (HG3-1222-79): 0.1% ethanol solution, 2.2.1.4 Sodium hydroxide (GB629-77): 4g/L solution, 2.2.1.5 Phosphate buffer solution (pH 6.5): weigh 0.68g anhydrous potassium dihydrogen phosphate (GB1274-77) (accurate to 0.001g), add 13.9ml sodium hydroxide solution (2.2.1.4) and dilute to 100ml with water, then it can be used. 2.2.2 Determination method
Weigh 2g of the sample (accurate to 0.0002g) that has been dried in a desiccator containing silica gel for 5h and place it in a conical flask. Use a 50ml burette to add 40ml of sodium hydroxide solution (2.2.1.1), slowly heat to boiling, reflux for 1h, cool to room temperature, add 5 drops of bromothymol blue indicator solution (2.2.1.3), and titrate with sulfuric acid standard solution (2.2.1.2). Take another 40ml phosphate buffer solution (2.2.1.5) and add 5 drops of bromothymol blue indicator solution as the end point color control solution. Perform a blank test at the same time.
2.2.3 Expression and calculation of results
The percentage content X, of propyl paraben is calculated according to formula (1): Xi = 20 (VV,) × 0.1802
Wherein: V,-
the volume of sulfuric acid standard solution consumed by blank, ml., the volume of sulfuric acid standard solution consumed by a sample, ml, the concentration of sulfuric acid standard solution, mol / LC
the mass of a sample, g
0.1802—
-the mass of each millimole of CioH12O3, g.
Take the arithmetic mean as the reported result, and the difference between two parallel determination results shall not exceed 0.2%. 2.3 Determination of melting point
Perform according to GB617-77 "Method for Melting Point Determination". 2.4 Determination of acidity
2.4.1 Reagents and solutions
2.4.1.1 Methyl red (HG 3~958-—76): 0.1% methyl red indicator solution; 2.4.1.2 Sodium hydroxide (GB 629-77): c (NaOH) = 0.1 mol / L standard solution. 2.4.2 Determination method Weigh 0.75g sample (accurate to 0.01g), heat in 15ml hot water at about 80℃ for 1min, cool, filter, take 10ml filtrate, add 2 drops of methyl red indicator (2.4.1.1), add sodium hydroxide standard solution (2.4.1.2) until it turns yellow, and the consumption of sodium hydroxide solution shall not exceed 0.2ml. 2.5 Determination of sulfate 2.5.1 Reagents and solutions GB 8851-88 2.5.1.1 Hydrochloric acid (GB622-77): 1+3 solution; 2.5.1.2 Barium chloride (GB 652-78) :25%(m/V)32.5.1.3 Sulfate impurity standard solution: Prepare according to GB602-77 and dilute 10 times (1ml=10μgSO,2-). 2.5.2 Determination method
Weigh 1g sample (accurate to 0.01g), add 100ml hot water, shake thoroughly and mix, heat for 5min, cool, add water to 100ml, filter, take 40ml filtrate in a 50ml colorimetric tube, add 5ml hydrochloric acid (2.5.1.1) and 3ml barium chloride solution (2.5.1.2), shake well, let stand for 10min, the turbidity should not be greater than the standard. Take 9.6ml sulfate impurity standard solution (2.5.1.3) in a 50ml colorimetric tube and treat it in the same way as the sample. 2.6 Determination of p-hydroxybenzoic acid and salicylic acid 2.6.1 Reagents and solutions
2.6.1.1 Ether (HG 3-1002-76)
2.6.1.2 Sodium bicarbonate (GB640-78): 1% (m/V) solution; 2.6.1.3 Sulfuric acid (GB625-77): take 5.7 ml of sulfuric acid and dilute it to 100 ml. 2.6.2 Determination method
Weigh 0.5g sample (accurate to 0.001g) and place it in a separatory funnel. Dissolve it with 30ml ether (2.6.1.1), add 20ml sodium bicarbonate solution (2.6.1.2) and shake to mix. Wash the water layer twice with ether, 20ml each time, then add 5ml sulfuric acid solution (2.6.1.3) and 30ml ether and shake again. Take out the ether layer, add 10ml water to the ether layer, shake gently to mix, remove the water layer, and filter. Wash the container and filter paper with a small amount of ether. Combine the washing liquid and the filtrate, place in evaporator III, evaporate the ether on a water bath, and then dry in a desiccator filled with sulfuric acid to constant weight. The mass of the residue should not exceed 5 mg. Dissolve these residues in 25 ml of water, heat and filter at about 70 ° C, take 5 ml of the filtrate, add 2 to 3 drops of newly prepared ferric chloride test solution (2.6.1.4), and the solution should not appear purple or reddish purple. 2.7 Determination of loss on drying
2.7.1 Determination method
Weigh 2 g of sample (accurate to 0.0002 g) in a Φ50~80 mm weighing bottle that has been constant weight, dry in a desiccator filled with silica gel for 5 hours, take out and weigh.
2.7.2 Expression and calculation of results
The percentage of loss on drying X2 is calculated according to formula (2): X2 =
Wherein: m,
tTotal mass of weighing bottle and sample before drying, g
TTotal mass of weighing bottle and sample after drying, g; Mass of sample before drying, g.
Take the arithmetic mean as the reported result.
2.8 Determination of ignition residue
2.8.1 Reagents
2.8.1.1 Sulfuric acid (GB 625-77).
(2)
2.8.2 Determination method
Weigh 2g of sample (accurate to 0.0002g) from a constant weight porcelain or quartz, add 0.5ml of sulfuric acid (2.8.1.1) to moisten it, then slowly burn it until it is completely carbonized, cool it, add 0.5ml of sulfuric acid, heat it at low temperature until the sulfuric acid vapor is completely removed, burn it in a high-temperature furnace at 450~550℃ for 3h, and weigh it.
2.8.3 Expression and calculation of results
The percentage content X3 of the ignition residue is calculated according to formula (3): 370
Where: m4-
Mass of the residue after ignition, g,
Mass of the sample, g.
Take the arithmetic mean as the reported result.
2.9 Determination of arsenic
2.9.1.1 Sulfuric acid (GB 625-77)
GB 8851-88
-×100
2.9.1.2 Sulfuric acid (GB 625--77) 1:1 sulfuric acid solution (V/V) 2.9.1.3 30% hydrogen peroxide (HG 3-1083-77) 2.9.1.4 Arsenic impurity standard solution: Prepare according to GB60277 and dilute 100 times (1 ml = 1 μg As). 2.9.2 Determination method
(3)
Weigh 1g sample (accurate to 0.01g) and place it in a conical flask, add 5ml sulfuric acid (2.9.1.1) and a few glass beads, heat on an adjustable electric furnace until carbonization begins, cool, slowly add 30% hydrogen peroxide until the digestion solution is clear and colorless, and then heat until white smoke is generated, cool, carefully add 10ml water, continue to heat until white smoke is generated, cool, carefully add water to wash the sample into the arsenic test bottle, and then follow the "arsenic spot method" of GB610-77 "Arsenic Determination Method". The standard is to take 1ml arsenic (As) impurity standard solution (2.9.1.4), add 6ml sulfuric acid solution (2.9.1.2), add 35ml water, and then follow the "arsenic spot method" of GB610-77. 2.10 Determination of heavy metals
2.10.1 Reagents and solutions
2.10.1.1 Saturated hydrogen sulfide water: prepared according to GB603-77. 2.10.1.2 Glacial acetic acid (GB 676-78): 25% (V/V) solution; 2.10.1.3 Lead impurity standard solution: prepared according to GB602--77 and diluted 10 times (1 ml = 10 μg Pb) 2.10.1.4 Acetone (GB 686-78).
2.10.2 Determination method
Weigh 2g of sample (accurate to 0.001g) and place it in a 50ml colorimetric tube, add 23ml acetone (2.10.1.4) to dissolve, add 2ml glacial acetic acid solution (2.10.1.2), add water to 40ml, add 10ml saturated hydrogen sulfide water (2.10.1.1), shake well, place in a dark place for 10min, and the color should not be darker than the standard.
The standard is to take 2ml of lead (Pb) impurity standard solution (2.10.1.3), and treat it in the same way as the sample. 3 Inspection rules
3.1 Before the product is shipped, it shall be inspected by the production quality inspection department. The manufacturer shall ensure that the shipped products meet the requirements of this standard and shall be accompanied by a quality manual in a certain format.
3.2 The consignee has the right to inspect and accept all received products in accordance with the requirements of this standard. 3.3 Inspection by batch, with the production of the manufacturer\per shift as a batch, and samples shall be selected from 10% of the number of bags in each batch, and the small batch shall not be less than 3 bags. Take out no less than 50g of sample from the selected bag, and the total mass of the samples in each batch shall not be less than 250g. Mix the taken samples thoroughly, Use the quartering method to reduce to 100g, and put it in a clean and dry sample bottle. The bottle is labeled with the following instructions: manufacturer name, product name, batch number, and production date. 3.4 If a sampling fails, re-sample from two times the packaging for re-inspection. If even one indicator fails in the re-inspection result, the entire batch of products is unqualified.
4 Marking, packaging, transportation, and storage
4.1 The following marks should be printed on the plastic bag and the carton: manufacturer name, address, product name, trademark, batch number, net weight, production date, and the packaging mark of "food additives". 4.2 The product is packaged in food-grade polyethylene plastic bags, with a net weight of 0.5kg per bag. Every 20 bags form a large package, which is placed in a carton. The large package carton is sealed with sealing glue.
GB8851—88
4.3 The transportation should be unloaded lightly, not pressed heavily, and not exposed to the sun or rain. 4.4 This product should be stored in a dry, ventilated and clean warehouse. 4.5 Under the above storage and transportation conditions and with intact packaging, the storage period of this product is three years from the date of production. Additional remarks:
This standard is under the jurisdiction of Beijing Chemical Research Institute and Food Hygiene Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by Guangdong Food Hygiene Supervision Institute and Guangzhou Donghu Chemical Factory. The main drafters of this standard are Guan Huiyan, Li Renji and Chen Yunping. 3724 If a sampling fails once, re-sampling should be done from two times the packaging for re-testing. If even one index fails in the re-testing result, the whole batch of products shall be considered as unqualified products.
4 Marking, packaging, transportation, storage
4.1 The following marks shall be printed on the plastic bags and cartons: manufacturer name, address, product name, trademark, batch number, net weight, production date, and the packaging mark of "food additive". 4.2 The product shall be packaged in food-grade polyethylene plastic bags, with a net weight of 0.5kg per bag. Every 20 bags form a large package, which is placed in a carton. The large package cartons are sealed with sealing glue.
GB8851—88
4.3 The product shall be unloaded gently during transportation, and shall not be pressed heavily or exposed to the sun or rain. 4.4 The product shall be stored in a dry, ventilated and clean warehouse. 4.5 Under the above storage and transportation conditions and with the packaging intact, the storage period of this product is three years from the date of production. Additional Notes:
This standard is under the jurisdiction of Beijing Chemical Research Institute and Food Hygiene Inspection Institute of Ministry of Health. This standard was drafted by Guangdong Food Hygiene Inspection Institute and Guangzhou Donghu Chemical Factory. The main drafters of this standard are Guan Huiyan, Li Renji and Chen Yunping.4 If a sampling fails once, re-sampling should be done from two times the packaging for re-testing. If even one index fails in the re-testing result, the whole batch of products shall be considered as unqualified products.
4 Marking, packaging, transportation, storage
4.1 The following marks shall be printed on the plastic bags and cartons: manufacturer name, address, product name, trademark, batch number, net weight, production date, and the packaging mark of "food additive". 4.2 The product shall be packaged in food-grade polyethylene plastic bags, with a net weight of 0.5kg per bag. Every 20 bags form a large package, which is placed in a carton. The large package cartons are sealed with sealing glue.
GB8851—88
4.3 The product shall be unloaded gently during transportation, and shall not be pressed heavily or exposed to the sun or rain. 4.4 The product shall be stored in a dry, ventilated and clean warehouse. 4.5 Under the above storage and transportation conditions and with the packaging intact, the storage period of this product is three years from the date of production. Additional Notes:
This standard is under the jurisdiction of Beijing Chemical Research Institute and Food Hygiene Inspection Institute of Ministry of Health. This standard was drafted by Guangdong Food Hygiene Inspection Institute and Guangzhou Donghu Chemical Factory. The main drafters of this standard are Guan Huiyan, Li Renji and Chen Yunping.
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