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National Standard of the People's Republic of China
Food additive
DL-Tartaric acid
Food additive
DL-Tartaric acid
GB15358-94
This standard specifies the technical requirements, test methods, inspection rules, and marking, packaging, transportation, storage, etc. of food additive DL-tartaric acid.
This standard applies to DL-tartaric acid obtained by oxidation and hydrolysis of maleic anhydride and hydrogen peroxide. This product is mainly used as an acidity regulator and leavening agent for candies, biscuits, canned foods, etc. Molecular formula: C4H606·nH20 (crystalline product n=1, anhydrous product n=0)Chemical name: 2,3-dihydroxysuccinic acid
Relative molecular weight: crystalline product 168.11; anhydrous product 150.09 (according to the international relative atomic mass in 1989)Cited standards
GB/T601
GB/T602
GB/T603
GB/T613
GB/T617
GB/T6284
GB/T6678
GB/T8450
GB/T9728
3 Product classification
Chemical reagents Preparation of standard solutions for titration analysis (volume analysis) Preparation of standard solutions for determination of impurities in chemical reagents Preparation of preparations and products used in test methods of chemical reagents General method for determination of specific rotation of chemical reagents General method for determination of melting point range of chemical reagents General method for determination of water content in chemical products Gravimetric method General rules for sampling of chemical products
Determination of arsenic in food additives
Chemical reagents General method for determination of sulfate
This product has crystalline products (containing one crystal water) and anhydrous products, which are called DL-tartaric acid (crystalline product) and DL-tartaric acid (anhydrous product) respectively.
4 Technical requirements
4.1 Appearance
The crystalline product is colorless crystals or white crystalline powder; the anhydrous product is white granules or powder. 4.2 Food additive DL-tartaric acid shall meet the requirements of the following table. -
DL-Tartaric acid content (dry basis), %
Melting point range, ℃
Sulfate (SO4), %
Crystalline
200~206
Anhydrous
200206
Heavy metal (Pb), %
Arsenic (As), %
Oxidized substances
Heating loss, %
Ignition residue, %
Test method
The reagents and water used in this standard, unless otherwise specified, refer to analytical reagents and distilled water or water of corresponding purity.
Standard solutions, impurity standard solutions, preparations and products required in the test, unless otherwise specified, shall be prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603. 5.1 Identification test
5.1.1 Optical rotation test
Weigh 1g of sample, add 10mL of water to dissolve, and measure according to the provisions of GB/T613. There should be no optical rotation. 5.1.2 Acid-base test
Weigh 1g of the sample, add 10mL of water to dissolve it, and test it with blue litmus paper. It should turn red. 5.1.3 Reactivity test of tartrate
5.1.3.1 Reagents and solutions
b. Nitric acid;
c. Sulfuric acid;
Sodium hydroxide solution: 40g/L;
Silver nitrate solution; 20g/L;
Ammonia solution: 2→5
Acetic acid solution: 1→4;
Ferrous sulfate solution: 80g/L;
Hydrogen peroxide solution: 1→10;
i. Resorcinol solution: 20g/L;
j. Potassium bromide solution: 100g/L.
5.1.3.2 Analysis steps
Weigh 5g of the sample, add a small amount of water to dissolve it, then neutralize it with sodium hydroxide solution until it is neutral, add water to make it up to 100mL, as sample solution A. Then proceed as follows. a. Add silver nitrate solution to sample solution A to generate a white precipitate. When the precipitate is separated and nitric acid is added to one part, the precipitate will dissolve. Add ammonia solution to the other part and heat it, the precipitate will dissolve and a silver mirror should be slowly generated. b. Add 2 drops of acetic acid solution, 1 drop of ferrous sulfate solution, 23 drops of hydrogen peroxide solution and excess sodium hydroxide solution to sample solution A, and it will turn red-purple to purple. c. Add 2-3 drops of sample solution A to 5mL of sulfuric acid that has been pre-added with 2-3 drops of resorcinol solution and 2-3 drops of potassium bromide solution, heat it on a water bath for 5-10 minutes, the solution should turn dark blue, and when it is poured into excess water after cooling, it will turn red. 5.2 Determination of DL-tartaric acid content
5.2.1 Method summary
The aqueous solution of the sample (dried first). Titrate with a standard alkali solution of known concentration in the presence of phenol indicator solution to measure the total acidity of the sample (in terms of C4H606). 5.2.2 Reagents and solutions
a. Standard sodium hydroxide titration solution: c(NaOH)=0.1mol/L; b. Phenol indicator solution: 10g/L.
5.2.3 Analysis steps
5.2.3.1 Sample treatment of crystallized product
Weigh about 5g of the sample, accurate to 0.0002g, and place it in a weighing bottle with a lid that has been weighed to a constant weight. Dry it in an oven at 105110℃ to a constant weight, which is the dried product B.
5.2.3.2 Determination
Crystalline product: weigh about 2g of the dried substance B in 5.2.3.1, accurate to 0.0002g; Anhydrous product: weigh about 2g of the dried substance C in 5.8, accurate to 0.0002g. Dissolve with water, transfer to a 250mL volumetric flask, dilute to the mark, transfer 25mL to a 250mL conical flask with a pipette, add 2-3 drops of phenol crisp indicator solution, and titrate with sodium hydroxide standard titration solution until it is slightly pink, and the end point is that it does not fade for 10 seconds. Perform a blank test at the same time. 5.2.4 Expression of analysis results
The content of DL-tartaric acid (in terms of C4H6O6) (X1) is expressed as mass percentage and calculated according to formula (1): (V1-V2)XCX0.07504
Wherein: V1—volume of sodium hydroxide standard titration solution consumed by the sample, mL; -volume of sodium hydroxide standard titration solution consumed by the blank test, mL: V2
cactual concentration of sodium hydroxide standard titration solution, mol/Lm1—mass of sample, g;
0.07504—mass of DL-tartaric acid in grams equivalent to 1.00mL sodium hydroxide standard titration solution (c(Na0H)=1.000mol/L)).
5.2.5 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.2%, and the arithmetic mean shall be taken as the determination result. 5.3 Determination of melting point range
5.3.1 The sample is the dried substance C in 5.8. The heating device is a round-bottom beaker. The heat transfer liquid is silicone oil. The rest is carried out in accordance with the provisions of GB/T617.
5.3.2 Allowable difference
The difference between the results of two parallel determinations. The initial melting point and the final melting point shall not exceed 0.4℃. The arithmetic mean is taken as the determination result.
5.4 Determination of sulfate (in terms of SO4)
Weigh 0.25g of the sample to an accuracy of 0.01g. Put it in a 50mL colorimetric tube and add about 20mL of water to dissolve it as the detection solution. Take 1.00mL of sulfate standard solution as the limit standard (each 1mL is equivalent to 0.1mgS04). The rest is carried out in accordance with the provisions of GB/T9728.
5.5 Determination of heavy metal limit (in terms of Pb)
5.5.1 Reagents and solutions
a. Nitric acid:
b. Hydrochloric acid solution: 1→4;
c. Glacial acetic acid solution: 1→20;
d. Ammonia solution: 1→4;
e. Sodium sulfide solution: weigh 5g of sodium sulfide and dissolve it in a mixture of 10mL of water and 30mL of glycerol. The solution is valid within three months;
f. Lead standard solution: 0.01mgPb/mL, take 10mL of the solution containing 0.1mgPb/mL and dilute it to the scale in a 100mL volumetric flask;
g. Phenol indicator solution: 10g/L.
5.5.2 Analysis steps
Take the residue D in 5.9, add 1mL of hydrochloric acid solution and 0.2mL of nitric acid, evaporate it on a water bath, add 1mL of hydrochloric acid solution and 20mL of water to dissolve it, filter it if necessary, add 1 drop of phenol indicator solution, add ammonia solution until the solution turns slightly red, add 0.5mL of glacial acetic acid solution,Transfer to a 50mL colorimetric tube, add water to 25mL, add 2 drops of sodium sulfide solution, shake well, and place in a dark place for 5min. The color should not be darker than the standard.
Take 2.00mL of lead standard solution for limit standard and treat it in the same way as the sample. 5.6 Determination of arsenic (as As)
5.6.1 Reagents and solutions
Arsenic standard solution: 0.001mgAs/mL, take 10mL of solution containing 0.1mgAs/mL in a 1000mL volumetric flask and dilute to the
mark.
5.6.2 Analysis steps
Weigh 1.0g of the sample, place it in a conical flask for arsenic spot method determination, dissolve it with 10mL of water, take 2.00mL of arsenic standard solution for limit standard, and proceed according to the provisions of arsenic spot method in GB/T8450. 5.7 Determination of easily oxidizable substances
5.7.1 Summary of the method
Under acidic conditions, the easily oxidizable substances in the sample react with potassium permanganate solution, causing the purple color of the potassium permanganate solution to fade, and the determination is carried out by visual timing method.
5.7.2 Reagents and solutions
a. Sulfuric acid solution: 1→20;www.bzxz.net
b Standard potassium permanganate titration solution: c(1/5KMnO4)=0.1mol/L. 5.7.3 Analysis steps
Weigh 1.0g of the sample, add 25mL of water and 25mL of sulfuric acid solution to dissolve, and add 4.0mL of standard potassium permanganate titration solution while maintaining 20±1℃. The purple color of the test solution should not disappear within 3min under static conditions. 5.8 Determination of loss on heating
5.8.1 Summary of method
The sample is dried in an oven to lose surface water, crystal water and volatile substances, and the loss is calculated by weighing. 5.8.2 Analysis steps
The sample size of the crystalline product is 1g, accurate to 0.0002g; the sample size of the anhydrous product is 6g, accurate to 0.0002g. Others are carried out in accordance with the provisions of GB/T6284. The dried matter C of the crystalline product is reserved for the determination of the melting point range, and the dried matter C of the anhydrous product is reserved for the determination of the content and melting point range.
5.8.3 Allowable difference
The difference between the results of two parallel determinations is not greater than 0.05%, and the arithmetic mean is taken as the determination result. 5.9 Provisions for ignition residue
5.9.1 Reagents
Sulfuric acid.
5.9.2 Instruments
a. Porcelain: 25ml;
b. High temperature electric furnace;
c. Silica gel dryer.
5.9.3 Analysis steps
Weigh 2g of the sample, accurate to 0.0002g, and place it in a 25mL pot. Add a few drops of sulfuric acid to wet it, and heat it slowly to make it completely ash at low temperature. Cool it to room temperature, add 1mL of sulfuric acid, and slowly heat it until the white smoke disappears. Burn it in a high temperature furnace at 500±50℃ for 3h, cool it to room temperature in a silica gel dryer, and weigh it accurately to 0.0001g. The mass of the residue at this time should be less than 0.10% of the mass of the sample. Otherwise, the residue should be burned to constant weight. The residue D after burning is reserved for the determination of heavy metals.
5.9.4 Expression of analysis results
The ignition residue (X2) is expressed as mass percentage and calculated according to formula (2): M2
—-×100
X2=—
Wherein: m2—mass of ignition residue, g; m3—mass of sample, g.
5.9.5 Permissible difference
The difference between the results of two parallel determinations shall not exceed 0.005%, and the arithmetic mean shall be taken as the result. 6 Inspection rules
6.1. Food additive DL-tartaric acid shall be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer shall ensure that all products leaving the factory meet the requirements of this standard and shall be accompanied by a quality certificate, including: manufacturer name, factory address, product name, production license number, trademark, specification, standard number, batch number, production date. 6.2 The user unit has the right to inspect the received products in accordance with the provisions of this standard. 6.3 If the supplier and the buyer have any objection to the product quality, the supplier and the buyer shall negotiate to resolve the dispute, or the national arbitration institution agreed by both parties shall conduct arbitration in accordance with the provisions of this standard. 6.4 Each batch of products shall not exceed 1t.
6.5 Sampling method
6.5.1 The number of samples collected shall be in accordance with the provisions of Article 6.6 and Chapter 10 of GB/T6678. 6.5.2 Sampling steps
Open the packaging bag, take a number of samples from the top, middle and bottom, and each batch of samples shall not be less than 0.5kg. Grind the samples, mix them carefully, take part of them and divide them into two portions, each about 50-100g, put them into a sealed container, and affix a label indicating the manufacturer name, product name, specification, batch number, sampling date and name of the sampler. One copy is sent to the inspection department for inspection. The other copy is kept for three months for reference.
6.6 If one of the indicators in the test results does not meet the requirements of this standard, a sample should be taken from twice the amount of packaging for re-testing. If the re-test results still show that one of the indicators does not meet the requirements of this standard, the entire batch of products shall be unqualified. 7 Marking, packaging, transportation and storage
7.1 Marking
The packaging container should be firmly painted with the words "food additives" and marked with the manufacturer's name, product name, product specifications, trademark, production date, shelf life, batch number, net weight and this standard number. 7.2 Packaging
This product is packed in polyethylene bags for food and double-layer kraft paper bags, with a woven bag as the outer cover. The net weight of each bag is 25kg. It can also be packed according to user requirements.
7.3 Transportation
Strictly prevent rain during transportation, and should be handled and placed with care to prevent damage to the packaging. It cannot be mixed with toxic and harmful items. 7.4 Storage
This product should be stored in a cool and dry warehouse. It should not be piled in the open air and should not be stored together with toxic and hazardous items. 7.5 The shelf life of the food additive DL-tartaric acid is two years. If the sampling test results still meet the requirements of this standard after two years, it can continue to be used.
Additional instructions:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry and the Food Hygiene Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by Lin'an County Chemical Plant No. 2, Zhejiang Province. The main drafters of this standard are Tong Jian, Zhou Pengnian, Tao Hongjie, Hong Shulin, and Cai Mingzhu.
This standard refers to the "DL-Tartaric Acid Standard" of the fifth edition (1986) of the "Japanese Food Additive Code". Approved by the State Bureau of Technical Supervision on December 30, 1994 and implemented on October 1, 19959.3 Analysis steps
Weigh 2g of the sample, accurate to 0.0002g, and place it in a 25mL pot. Add a few drops of sulfuric acid to wet it, and slowly heat it to make it completely ash at low temperature. Cool it to room temperature, then add 1mL of sulfuric acid, and slowly heat it until the white smoke disappears. Burn it in a high-temperature furnace at 500±50℃ for 3h, cool it to room temperature in a silica gel dryer, and weigh it accurately to 0.0001g. The mass of the residue at this time should be less than 0.10% of the mass of the sample. Otherwise, the residue should be burned to constant weight. The residue D after burning is reserved for the determination of heavy metals.
5.9.4 Expression of analysis results
The ignition residue (X2) is expressed as mass percentage and calculated according to formula (2): M2
—-×100
X2=—
Wherein: m2—mass of ignition residue, g; m3—mass of sample, g.
5.9.5 Permissible difference
The difference between the results of two parallel determinations shall not exceed 0.005%, and the arithmetic mean shall be taken as the result. 6 Inspection rules
6.1. The food additive DL-tartaric acid shall be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer shall ensure that all products leaving the factory meet the requirements of this standard and shall be accompanied by a quality certificate, which shall include: manufacturer name, factory address, product name, production license number, trademark, specification, standard number, batch number, and production date. 6.2 The user unit has the right to inspect the received products in accordance with the provisions of this standard. 6.3 If the supplier and the buyer have any objection to the product quality, the supplier and the buyer shall negotiate to resolve the dispute, or the national arbitration institution agreed by both parties shall conduct arbitration in accordance with the provisions of this standard. 6.4 Each batch of products shall not exceed 1t.
6.5 Sampling method
6.5.1 The number of samples collected shall be in accordance with the provisions of Article 6.6 and Chapter 10 of GB/T6678. 6.5.2 Sampling steps
Open the packaging bag, take a number of samples from the top, middle and bottom, and each batch of samples shall not be less than 0.5kg. Grind the samples, mix them carefully, take part of them and divide them into two portions, each about 50-100g, put them into a sealed container, and affix a label indicating the manufacturer name, product name, specification, batch number, sampling date and name of the sampler. One copy is sent to the inspection department for inspection. The other copy is kept for three months for reference.
6.6 If one of the indicators in the test results does not meet the requirements of this standard, a sample should be taken from twice the amount of packaging for re-testing. If the re-test results still show that one of the indicators does not meet the requirements of this standard, the entire batch of products shall be unqualified. 7 Marking, packaging, transportation and storage
7.1 Marking
The packaging container should be firmly painted with the words "food additives" and marked with the manufacturer's name, product name, product specifications, trademark, production date, shelf life, batch number, net weight and this standard number. 7.2 Packaging
This product is packed in polyethylene bags for food and double-layer kraft paper bags, with a woven bag as the outer cover. The net weight of each bag is 25kg. It can also be packed according to user requirements.
7.3 Transportation
Strictly prevent rain during transportation, and should be handled and placed with care to prevent damage to the packaging. It cannot be mixed with toxic and harmful items. 7.4 Storage
This product should be stored in a cool and dry warehouse. It should not be piled in the open air and should not be stored together with toxic and hazardous items. 7.5 The shelf life of the food additive DL-tartaric acid is two years. If the sampling test results still meet the requirements of this standard after two years, it can continue to be used.
Additional instructions:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry and the Food Hygiene Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by Lin'an County Chemical Plant No. 2, Zhejiang Province. The main drafters of this standard are Tong Jian, Zhou Pengnian, Tao Hongjie, Hong Shulin, and Cai Mingzhu.
This standard refers to the "DL-Tartaric Acid Standard" of the fifth edition (1986) of the "Japanese Food Additive Code". Approved by the State Bureau of Technical Supervision on December 30, 1994 and implemented on October 1, 19959.3 Analysis steps
Weigh 2g of the sample, accurate to 0.0002g, and place it in a 25mL pot. Add a few drops of sulfuric acid to wet it, and slowly heat it to make it completely ash at low temperature. Cool it to room temperature, then add 1mL of sulfuric acid, and slowly heat it until the white smoke disappears. Burn it in a high-temperature furnace at 500±50℃ for 3h, cool it to room temperature in a silica gel dryer, and weigh it accurately to 0.0001g. The mass of the residue at this time should be less than 0.10% of the mass of the sample. Otherwise, the residue should be burned to constant weight. The residue D after burning is reserved for the determination of heavy metals.
5.9.4 Expression of analysis results
The ignition residue (X2) is expressed as mass percentage and calculated according to formula (2): M2
—-×100
X2=—
Wherein: m2—mass of ignition residue, g; m3—mass of sample, g.
5.9.5 Permissible difference
The difference between the results of two parallel determinations shall not exceed 0.005%, and the arithmetic mean shall be taken as the result. 6 Inspection rules
6.1. Food additive DL-tartaric acid shall be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer shall ensure that all products leaving the factory meet the requirements of this standard and shall be accompanied by a quality certificate, including: manufacturer name, factory address, product name, production license number, trademark, specification, standard number, batch number, production date. 6.2 The user unit has the right to inspect the received products in accordance with the provisions of this standard. 6.3 If the supplier and the buyer have any objection to the product quality, the supplier and the buyer shall negotiate to resolve the dispute, or the national arbitration institution agreed by both parties shall conduct arbitration in accordance with the provisions of this standard. 6.4 Each batch of products shall not exceed 1t.
6.5 Sampling method
6.5.1 The number of samples collected shall be in accordance with the provisions of Article 6.6 and Chapter 10 of GB/T6678. 6.5.2 Sampling steps
Open the packaging bag, take a number of samples from the top, middle and bottom, and each batch of samples shall not be less than 0.5kg. Grind the samples, mix them carefully, take part of them and divide them into two portions, each about 50-100g, put them into a sealed container, and affix a label indicating the manufacturer name, product name, specification, batch number, sampling date and name of the sampler. One copy is sent to the inspection department for inspection. The other copy is kept for three months for reference.
6.6 If one of the indicators in the test results does not meet the requirements of this standard, a sample should be taken from twice the amount of packaging for re-testing. If the re-test results still show that one of the indicators does not meet the requirements of this standard, the entire batch of products shall be unqualified. 7 Marking, packaging, transportation and storage
7.1 Marking
The packaging container should be firmly painted with the words "food additives" and marked with the manufacturer's name, product name, product specifications, trademark, production date, shelf life, batch number, net weight and this standard number. 7.2 Packaging
This product is packed in polyethylene bags for food and double-layer kraft paper bags, with a woven bag as the outer cover. The net weight of each bag is 25kg. It can also be packed according to user requirements.
7.3 Transportation
Strictly prevent rain during transportation, and should be handled and placed with care to prevent damage to the packaging. It cannot be mixed with toxic and harmful items. 7.4 Storage
This product should be stored in a cool and dry warehouse. It should not be piled in the open air and should not be stored together with toxic and hazardous items. 7.5 The shelf life of the food additive DL-tartaric acid is two years. If the sampling test results still meet the requirements of this standard after two years, it can continue to be used.
Additional instructions:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry and the Food Hygiene Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by Lin'an County Chemical Plant No. 2, Zhejiang Province. The main drafters of this standard are Tong Jian, Zhou Pengnian, Tao Hongjie, Hong Shulin, and Cai Mingzhu.
This standard refers to the "DL-Tartaric Acid Standard" of the fifth edition (1986) of the "Japanese Food Additive Code". Approved by the State Bureau of Technical Supervision on December 30, 1994 and implemented on October 1, 1995
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