Some standard content:
National Standard of the People's Republic of China
Food additive
Ethyl p-hydroxybenzoate
UDC 661.782.1
GB 8850-88
This standard applies to ethyl p-hydroxybenzoate made by esterification of p-hydroxybenzoic acid and ethanol with sulfuric acid as catalyst. This product is used as an anti-corrosion agent in food processing.
Molecular formula, C.HioO3
Structural formula:
Molecular weight: 166.18 (according to the international atomic weight in 1985) 1 Technical requirements
CO, CH2 CHa
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 (on SO.), %
Parahydroxybenzoic acid and salicylic acid
Loss on drying, %
Ignition residue, %
Arsenic (As), %
Heavy metal (on Pb), %
2 Test methods
115 ~118
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, 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. Implementation from 1988 to 11-01.
2.1 Identification
2.1.1 Reagents and solutions
GB 8850--88
2.1.1.1 Sodium hydroxide (GB62977): 40g/L solution2.1.1.2 Sulfuric acid (GB 625-77): 10% (m/V） s2.1.1.3 Barium chloride (GB 652-78): 25% (m/V） 2.1.1.4 Sodium hydroxide (GB629-77): 80g/L solution, 2.1.1.5 Sulfuric acid (GB625-77): 1+17 solution, 2.1.1.6 Iodine (GB 675-77): 12.7g/L solution. 2.1.2 Identification method
2.1.2.1 Take about 0.5g sample (accurate to 0.01g), add 10ml 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. According to GB617-77 "Melting Point Determination Method", the melting point is 213℃~217℃.
2.1.2.2 Take 0.5g of sample (accurate to 0.01g), add 5ml of sodium hydroxide solution (2.1.1.4), place in a boiling water bath and heat for 5min, add 6ml of sulfuric acid solution (2.1.1.5), cool, filter, add 5ml of sodium hydroxide (2.1.1.4) to the filtrate, warm to 50℃, then add 5ml of iodine solution (2.1.1.6), the odor of iodoform appears, and then a precipitate is formed. 2.2 Determination of ethyl p-hydroxybenzoate content 2.2.1 Reagents and solutions
2.2.1.1 Sodium hydroxide (GB629-77) * 40g/L solution, 2.2.1.2 Sulfuric acid (GB 625-77): c(H,SO)=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 (pH6.5): 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 with water to 100ml, then it can be used. 2.2.2 Determination method
Weigh 2g of sample (accurate to 0.0002g) that has been dried at 80℃ for 2h 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 and 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 content results
The percentage content (X) of CgHoO3 is calculated according to formula (1): XI = - 2 (V1-V2)X0. 1662 x
The volume of sulfuric acid standard solution consumed by the blank, m!, where: V
V, —The volume of sulfuric acid standard solution consumed by the sample, ml—The concentration of sulfuric acid standard solution, mol/L; C
The mass of the sample, g,
0.1662---The mass of each millimole of CgHloO3, g. Take the arithmetic mean as the reported result, and the difference between two parallel determination results shall not be greater than 0.2%. 2.3 Determination of melting point
Carry out in accordance with GB617--77 "Melting Point Determination Method". 2.4 Determination of acidity
2.4.1 Reagents and solutions
GB 8850--88
2.4.1.1 Methyl red (HG 3--958-76): 0.1% methyl red indicator solution; 2.4.1.2 Sodium hydroxide (GB629-77): c (NaOH) = 0.1mol/L standard solution. 2.4.2 Determination method
Weigh 0.75g sample (accurate to 0.01g), co-heat in 15ml of about 80℃ hot water for 1min, cool, filter, take 10ml filtrate, add 2 drops of methyl red indicator solution, and drip with sodium hydroxide standard solution (2.4.1.2) until it turns yellow. The consumption of sodium hydroxide solution shall not exceed 0.2ml.
2.5 Determination of sulfate
2.5.1 Reagents and solutions
2.5.1.1 Hydrochloric acid (GB622--77): 1+3 solution, 2.5.1.2 Chloride ((GB 652-78): 25% (m/V) 2.5.1.3 Sulfate impurity standard solution: Prepare according to GB602-77 and dilute 10 times (1ml=10MgSO,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 (GB 64078): 1% (m/V) solution; 2.6.1.3 Sulfuric acid (GB625-77): take 5.7ml of sulfuric acid and dilute to 100ml, 2.6.1.4 Ferric oxide (HG3-1085-77): 0.18% (m/V) test solution (prepare when needed). 2.6.2 Determination method
Weigh 0.5g sample (accurate to 0.001g) and place it in a separatory funnel and dissolve it in 30ml ether (2.6.1.1). Add 20ml sodium bicarbonate solution (2.6.1.2) and shake to mix. Take the water layer and wash it 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 an evaporating dish, evaporate the ether on a water bath, and then dry in a desiccator (sulfuric acid) to constant weight. The mass of the residue should not exceed 5 mg. Dissolve the residue in 25 ml of water, heat and filter at about 70 ° C, take 5 ml of the filtrate, add 2 to 3 drops of freshly 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 2g of sample (accurate to 0.0002g) into a Φ50～80mm weighing bottle with constant weight, place it in a constant temperature box at 80±2℃, dry for 2h, take it out and weigh it.
2.7.2 Expression and calculation of results
1-Loss on drying content X2 is calculated according to formula (2), X, =
mi --m2
total mass of weighing bottle and sample before drying, g; where. m-
total mass of weighing bottle and sample after drying, g; m3-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).
GB 8850--88
2.8.2 Determination method
Weigh 2g of sample (accurate to 0.0002g) in a constant-weight porcelain or quartz crucible, add 0.5ml of sulfuric acid (2.8.1.1) to moisten it, then slowly ignite 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, and then ignite it in a high-temperature furnace at 450-550℃ for 3h and weigh it.
2.8.3 Result expression and calculation
The percentage content X3 of the ignition residue is calculated according to formula (3): X =
Wherein: m4
Mass of the ignition residue, 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)
× 100
2.9.1.2 Sulfuric acid (GB625--77): 1:1 Sulfuric acid solution (V/V) 2.9.1.3 30% hydrogen peroxide (HG3-1083-77) 2.9.1.4 Arsenic impurity standard solution: Prepare according to GB602-77 and dilute 100 times (1ml=1gAs). 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 (2.9.1.3) 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 proceed according to 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 proceed according to the "arsenic spot method" of GB610. 2.10 Determination of heavy metals
2.10.1 Reagents and solutions
2.10.1.1 Saturated hydrogen sulfide water: prepared according to GB603772.10.1.2 Glacial acetic acid (GB676-78): 25% (V/V) solution2.10.1.3 Lead impurity standard solution: prepared according to GB602-77 and diluted 10 times (1ml=10ugPb)2.10.1.4 Acetone (GB 686-78).
2.10.2 Determination method
Weigh 2g 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, and place in a dark place for 10min. The color should not be darker than the standard.
The standard is to absorb 2ml lead (Pb) impurity standard solution (2.10.1.3) and treat it in the same way as the sample. 3 Inspection rules
3.1 The product shall be inspected by the production and quality inspection department before leaving the factory. The manufacturer shall ensure that the products leaving the factory meet the requirements of this standard and attach a quality manual in a certain format.
3.2 The receiving unit has the right to accept all received products in accordance with the requirements of this standard. 3.3 Inspection by batch, with the output of each shift of production as a batch. Select samples from 10% of the number of bags in each batch, and the small batch shall not be less than 8 bags. Take out no less than 50g of samples from the selected bags, and the total mass of the total samples of each batch shall not be less than 250g. Mix the taken samples thoroughly, reduce them to 100g by quartering method, and put them in clean and dry sample bottles. Label the bottles with the following instructions: manufacturer's name, product name, batch number, and production date. 3.4 If the sampling fails, re-sample from twice the packaging for re-inspection. If qualified, the goods should be accepted. If even one of the indicators in the re-inspection result fails, the entire batch of products will be unqualified. 4 Marking, packaging, transportation, storage
4.1 The following marks should be printed on plastic bags and cartons: manufacturer's name, address, product name, trademark, batch number, net weight, production date, and packaging mark with the words "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 stored in a carton. The large package cartons are sealed with sealing glue.
4.8 The product should be unloaded gently during transportation, and should not be pressed heavily or exposed to the sun or rain. 4.4 The product should be stored in a dry, ventilated and clean warehouse. 4.5 Under the above storage and transportation conditions and if the packaging is intact, 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 and Inspection Institute and Guangzhou Donghu Chemical Plant. The main drafters of this standard are Guan Huiyan, Li Renji and Chen Yunping. 3673 Lead impurity standard solution: Prepare according to GB602-77 and dilute 10 times (1ml=10ugPb) 2.10.1.4 Acetone (GB 686-78).
2.10.2 Determination method
Weigh 2g 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) and 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 absorb 2ml lead (Pb) impurity standard solution (2.10.1.3) and treat it in the same way as the sample. 3 Inspection rules wwW.bzxz.Net
3.1 Before the product leaves the factory, it shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that the products leave the factory meet the requirements of this standard and shall be accompanied by a quality manual in a certain format.
3.2 The receiving unit has the right to inspect and accept all received products in accordance with the requirements of this standard. 3.3 Inspection shall be carried out by batches, with the output of each shift of the production line as a batch. Samples shall be selected from 10% of the number of bags in each batch, and the small batch shall not be less than 8 bags. Take out no less than 50g of samples from the selected bags, and the total mass of the total samples of each batch shall not be less than 250g. Mix the taken samples thoroughly, reduce them to 100g by quartering method, and put them in clean and dry sample bottles. Label the bottles with the following instructions: manufacturer name, product name, batch number, and production date. 3.4 If the sampling fails, re-sample from twice the packaging for re-inspection. If it passes, the goods shall be accepted. If even one of the indicators in the re-inspection result is unqualified, the whole batch of products shall be unqualified. 4 Marking, packaging, transportation, storage
4.1 The following marks shall be printed on the plastic bags and cartons: manufacturer name, factory address, product name, trademark, batch number, net weight, production date, and the packaging mark of "food additive". 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 cartons are sealed with sealing glue.
4.8 The product should be unloaded gently during transportation, and should not be pressed heavily or 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 if the packaging is 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 the Food Hygiene Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by Guangdong Food Hygiene Supervision and Inspection Institute and Guangzhou Donghu Chemical Factory. The main drafters of this standard are Guan Huiyan, Li Renji and Chen Yunping.3 Lead impurity standard solution: Prepare according to GB602-77 and dilute 10 times (1ml=10ugPb) 2.10.1.4 Acetone (GB 686-78).
2.10.2 Determination method
Weigh 2g 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) and 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 absorb 2ml 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 leaves the factory, it shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that the products leave the factory meet the requirements of this standard and shall be accompanied by a quality manual in a certain format.
3.2 The receiving unit has the right to inspect and accept all received products in accordance with the requirements of this standard. 3.3 Inspection shall be carried out by batches, with the output of each shift of the production line as a batch. Samples shall be selected from 10% of the number of bags in each batch, and the small batch shall not be less than 8 bags. Take out no less than 50g of samples from the selected bags, and the total mass of the total samples of each batch shall not be less than 250g. Mix the taken samples thoroughly, reduce them to 100g by quartering method, and put them in clean and dry sample bottles. Label the bottles with the following instructions: manufacturer name, product name, batch number, and production date. 3.4 If the sampling fails, re-sample from twice the packaging for re-inspection. If it passes, the goods shall be accepted. If even one of the indicators in the re-inspection result is unqualified, the whole batch of products shall be unqualified. 4 Marking, packaging, transportation, storage
4.1 The following marks shall be printed on the plastic bags and cartons: manufacturer name, factory address, product name, trademark, batch number, net weight, production date, and the packaging mark of "food additive". 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 cartons are sealed with sealing glue.
4.8 The product should be unloaded gently during transportation, and should not be pressed heavily or 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 if the packaging is 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 the Food Hygiene Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by Guangdong Food Hygiene Supervision and 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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