Chemical Industry Standard of the People's Republic of ChinawwW.bzxz.Net HG2307—92 Industrial Ethyl Acetoacetate Published on May 17, 1992 Ministry of Chemical Industry of the People's Republic of China Implemented on January 1, 1993 Chemical Industry Standard of the People's Republic of China Industrial Ethyl Acetoacetate Subject Content and Scope of Application HG2307-—92 This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage of ethyl acetoacetate. This standard applies to industrial ethyl acetoacetate obtained by direct synthesis of diketene and ethanol. This product is mainly used as raw material for the manufacture of medicines, dyes and fragrances. Molecular formula: CH:COCH, COOC, He Relative molecular mass: 130.14 (according to the international relative atomic mass in 1989) 2 Reference standards GB1250 GB4472 GB6283 GB6678 GB8170 3 Technical requirements Chemical reagents Preparation of standard solutions for titration analysis (volumetric analysis) Preparation of preparations and products used in chemical reagent test methods General method for boiling range determination Chemical trial production Expression and determination method of limit values General rules for determination of density and relative density of chemical products Determination of water content in chemical products Karl Fischer method (general method) General rules for sampling of chemical products Rules for rounding off values 3.1 Appearance: colorless and transparent or slightly yellowish. Industrial ethyl acetoacetate shall meet the requirements of the following table: 3.2 Boiling range (175~185C), %(V/V) Water content, % Ethyl acetate solution test Acid content (calculated as acetic acid), % Density p20g/cm Approved by the Ministry of Chemical Industry of the People's Republic of China on 1992-05-17 Qualified products 1.020~1.030 Implemented on 1993-01-01 4 Test method HG2307-92 For the reagents and water used in this standard, analytical pure reagents and distilled water or water of equivalent purity shall be used unless other special requirements are specified. 4.1 Appearance Use visual method 4.2 Determination of boiling range Perform according to GB615. 4.3 Determination of water content Perform according to GB6283, and take 5.0mL of sample. 4.3.1 Allowable difference The difference between the results of two parallel determinations shall not exceed 0.03%. 4.4 Ethyl acetate solution test Add 5mL of sample to a 50mL graduated test tube, and then add 15mL of ethyl acetate. If there is no turbidity, it is qualified. 4.5 Determination of acidity 4.5.1 Reagents 4.5.1.1 Standard sodium hydroxide titration solution: c (NaOH) = 0.1 mol/L, preparation and calibration shall be in accordance with GB601; 4.5.1.2 Standard hydrochloric acid titration solution: c (HC1) = 0.1 mol/L, preparation and calibration shall be in accordance with GB601; 4.5.1.3 Phenol red indicator solution: 0.4 g/L. 4.5.2 Analysis steps Take 100 mL of water without carbon dioxide, add 5 drops of phenol red indicator solution, neutralize with standard hydrochloric acid titration solution, make the solution light red, keep it for at least 30 seconds, add 10.0 mL of sample, and titrate with standard sodium hydroxide solution until it turns light red, keep it for at least 30 seconds, which is the end point. 4.5.3 Expression of results The acid content (in acetic acid) X expressed as a mass percentage is calculated as follows: X = 9V: 0. 060 × 100 Wherein: c—actual concentration of sodium hydroxide standard titration solution, mol/L; a volume of sodium hydroxide standard solution used for titration, mL; p20——density of the sample (1.020 g/cm3); 0.060 —mass of acetic acid equivalent to 1.00 mL sodium hydroxide standard solution [c (Na0H) = 1.000 mol/L], expressed in grams. 4.5.4 Allowable difference The difference between the results of two parallel determinations shall not exceed 0.05%. 4.6 Determination of density Carry out according to the Weiss balance method in Article 2.3.2 of GB4472. 5 Inspection rules 5.1 Industrial ethyl acetoacetate shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that all products leaving the factory meet the requirements of this standard, and each batch of products leaving the factory shall have a quality certificate. The content includes the manufacturer name, product name, grade, batch number and the number of this standard. 5.2 Sampling HG2307-92 Each storage tank of ethyl acetoacetate is a batch number. Sampling in the packaging barrel shall be carried out in accordance with Article 6.6.2 of GB6678. On the basis of ensuring that the packaging barrel is dry and clean, the manufacturer can sample in the storage tank, but the sampling of the packaging barrel shall prevail in arbitration. 5.3 Mix the samples and divide them into two clean and dry ground glass bottles, seal and label them. And indicate the manufacturer name, product name, batch number, etc. One bottle is for inspection, and the other is kept for standby use, with a shelf life of three months. 5.4 The user has the right to inspect the quality of the ethyl acetoacetate received in accordance with the provisions of this standard. 5.5 The test results shall be determined according to the rounded value comparison method in GB1250. Rounding shall be carried out according to GB8170. 5.6 If one of the test results does not meet the standard requirements, the producer and user shall re-sample from the double amount of packaging for inspection. If only one item of the product re-inspection does not meet the requirements of this standard, the entire batch of products shall be unqualified. 5.7 When the supply and demand parties have a dispute over product quality and need arbitration, the arbitration institution shall be decided by both parties through consultation. The arbitration shall be carried out in accordance with the test methods specified in this standard. 6 Marking, packaging, transportation and storage 6.1 The name of the manufacturer, product name, grade batch number, registered trademark, net weight and this standard number shall be clearly marked on the packaging aluminum barrel. 6.2 Industrial ethyl acetoacetate shall be packaged in aluminum barrels. The barrel cover shall be sealed and leak-proof. The net weight of each barrel is 200kg, 100kg, etc. The packaging weight deviation is ±0.6%. 6.3 Industrial ethyl acetoacetate shall be stored in a cool and dry place. During transportation, it is necessary to prevent rain and sunlight exposure. Load and unload with care to prevent the aluminum drum from being damaged. Additional remarks: This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Shanghai Pengpu Chemical Plant. The main drafters of this standard are Chen Yong, Tang Yuanmao, and Chen Qiang. This standard refers to the Japanese Industrial Standard JIS K8031-1980 "Ethyl Acetoacetate (Reagent)". 3 Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.