Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2303-92
Industrial Acetanilide
Published on May 17, 1992
Ministry of Chemical Industry of the People's Republic of China
Implemented on January 1, 1993www.bzxz.net
W Chemical Industry Standard of the People's Republic of China
Subject Content and Scope of Application
Acetanilide
HG2303-92
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage of industrial acetanilide. This standard applies to acetanilide obtained by acylation and distillation of aniline and glacial acetic acid. This product is mainly used as a raw material for the production of medicines, dyes and other organic products.
Molecular formula: CHNO
Structural formula:
Relative molecular mass: 135.166 (according to the international relative atomic mass in 1989) 2 Reference standards
GB1250
GB6283
GB6678
Packaging, storage and transportation pictorial symbols
Chemical reagents Titration analysis (volume analysis) Preparation of standard solutions for chemical reagents Melting point range determination General method Methods for expressing and determining limit values Determination of moisture content in chemical products Karl Fischer method (general method) General rules for sampling of chemical products
GB6679
General rules for sampling of solid chemical products
ZBC10005
5 Method for determining the content of impurities in raw materials
Color inspection method of solution
3 Technical requirements
3.1 Appearance: small pieces of beige to light brown, with a small amount of powder allowed. 3.2 Industrial acetanilide should meet the requirements of Table 1. Table 1
Solution color (orange-yellow), No.
Acetanilide content, %
Melting point range, ℃
Approved by the Ministry of Chemical Industry of the People's Republic of China on May 17, 1992Superior product
113~116
First-class product
Qualified product
112~116
Implemented on January 1, 1993||tt ||W. Aniline content, %
Water, %
Ash, %
4 Test method
HG2303-92
Continued Table 1
Superior quality
First-class quality
Qualified quality
The reagents used in this standard test should be analytical reagents that meet the current national standards or industry standards, and the test water should be distilled water or water of equivalent purity. The standard solution for titration is prepared according to the requirements of GB601. If the instrument is not specified, it is a general laboratory instrument. 4.1 Determination of solution color
4.1.1 Reagents and solutions
4.1.1.1 Potassium dichromate solution: 800 mg/L, prepared according to the requirements of ZBc10005;4.1.1.2 Cobalt chloride solution: 59.5 g/L, prepared according to the requirements of ZBC10005;4.1.1.3 Copper sulfate solution: 62.4 g/L, prepared according to the requirements of ZBC10005;4.1.1.4
95% ethanol;
Colorimetric stock solution: prepared according to Table 2, storage period of three months. Table 2
Cobalt chloride solution
Potassium dichromate solution
4.1.1.6 Standard colorimetric solution: prepared according to the following method, use period of one week. Copper sulfate solution
Use a pipette to draw 1mL of the colorimetric reserve solution into a 25mL colorimetric tube, dilute to 10.0mL with water, and obtain the orange-yellow No. 2 standard colorimetric solution.
4.1.2 Analysis steps
Weigh 0.10g of the finely ground sample into a 25mL colorimetric tube, dissolve it with ethanol and dilute to 10.0mL, and shake well. With white paper as the background, observe axially, and its color should not be darker than the standard colorimetric solution. 4.2 Determination of acetanilide content
4.2.1 Principle of the method
Heat acetanilide in an acidic solution to hydrolyze aniline. Aniline reacts quantitatively with sodium nitrite to form a diazonium salt. A slightly excess of sodium nitrite solution depolarizes the electrode, and current flows through the solution. The ammeter pointer suddenly deflects and no longer returns to indicate the titration end point, or a slightly excess of titrant reacts with the starch potassium iodide external indicator to produce a blue color to indicate the titration end point. Calculate the acetanilide content based on the consumption of sodium nitrite standard titration solution.
Reaction equation:
-NHCOCII+HO-
-NH,+NaNO,+2 HCI-→
4.2.2 Reagents and solutions
-NH, + CH,COOH
N=N·CI+NaCI+2H20
.bzsoso:com4.2.2.1 Potassium bromide;
4.2.2.2 Hydrochloric acid solution: (1+3);
HG2303—92
4.2.2.3 Sodium nitrite standard titration solution: c(NaNO2)=0.1mol/L;4.2.2.4 Starch potassium iodide indicator solution: Weigh 2g of soluble starch and add 5mL of water to make a paste. Take another 0.5g potassium iodide and 1g zinc chloride and dissolve them in 45mL water and boil. Pour the starch paste into the potassium iodide solution, boil for 2min while stirring, and store in a brown reagent bottle after cooling. The shelf life is one week.
4.2.3 Instruments and Devices
4.2.3.1 Magnetic stirrer,
4.2.3.2 Permanent stop titrator or a device made according to Figure 1. K
Figure 1 Schematic diagram of measuring instrument installation
R-resistance (its resistance is similar to the critical damping resistance of the galvanometer); R
Rr-resistance (60~70Ω, so that the voltage applied to the two electrodes is about 50mV); R2-resistance (2000Ω); B-1.5V dry battery, K-switch, G-galvanometer (sensitivity is 10-A/grid), P-platinum electrode When using a permanent stop titrator, select a polarization voltage of 50mV, a sensitivity of 10-A/grid, and a threshold value of 60 grids. Before use or after passivation, the platinum-platinum electrode should be soaked in a washing solution for 4060s, or soaked in a boiling nitric acid solution containing a small amount of ferric chloride for 30s, and then washed with distilled water to activate it. 4.2.4 Analysis steps
Weigh 0.3g (accurate to 0.0002g) of sample and place it in a 250mL conical flask with a ground mouth, add 30mL of hydrochloric acid solution, connect a spherical condenser, heat and reflux for 30min, and rinse the inner wall of the condenser with a small amount of water after cooling. Transfer all the solution to a 250mL beaker, add 70mL of hydrochloric acid solution and 5g of potassium bromide, dilute to 150mL with water, and stir on a magnetic stirrer to dissolve the potassium bromide. a. Permanent stop method to indicate the reaction end point (arbitration method) Place a platinum-platinum electrode in the above reaction solution, insert the tip of the burette about 2/3 below the liquid surface, and titrate rapidly with sodium nitrite standard titration solution at 10-25℃ under stirring. When it is close to the end point, lift the tip of the burette out of the liquid surface, rinse with a small amount of water, and then titrate slowly until the ammeter pointer suddenly deflects and stays for 1min without returning to the end point. At the same time, perform a blank test. b. External indicator method to indicate the end point of the reaction
Insert the tip of the burette 2/3 below the liquid surface, and titrate rapidly to the near end point at 10-25°C with sodium nitrite standard titration solution under stirring. Lift the tip of the burette out of the liquid surface, rinse with a small amount of water, and continue to titrate slowly under strong stirring until a small amount of solution is dipped into a glass rod, and the starch potassium iodide indicator solution immediately turns blue. If it still turns blue after stirring for 13 minutes, it is the end point. Perform a blank test at the same time. 4.2.5 Expression and calculation of results
The mass percentage of industrial acetanilide X is calculated according to formula (1): X, = (V1) × 0.135 2 × 1001. 451 4Xm
Wherein: c——actual concentration of sodium nitrite standard titration solution, mol/L; V1——volume of sodium nitrite standard titration solution consumed by the titration sample, mL; V. —volume of sodium nitrite standard titration solution consumed by the blank test, mL; —mass of the sample, g;
0.1352 —mass of acetanilide equivalent to 1.00mL sodium nitrite standard titration solution [c (NaNO2) = 1.000mol/L], expressed in grams;
X2 —aniline content determined according to the provisions of Article 4.4 of this standard, %; 1.4514 —coefficient for converting aniline to acetanilide. The arithmetic mean is taken as the test result.
4.2.6 Allowable difference
The difference between two parallel determination results shall not exceed 0.2%. 4.3 Determination of melting point range
Perform in accordance with the provisions of GB617.
4.4 Determination of aniline content
4.4.1 Principle of the method
Aniline and sodium nitrite react quantitatively under acidic conditions to undergo diazotization reaction, and the aniline content is calculated based on the amount of sodium nitrite consumed. 4.4.2 Reagents and solutions
4.4.2.1 Potassium bromide;
4.4.2.2 Hydrochloric acid solution: 1+3);
4.4.2.3 Ethanol;
4.4.2.4 Standard titration solution of sodium nitrite: c(NaNO2)=0.05mol/L;4.4.2.5 Starch potassium iodide indicator (same as 4.2.2.4). 4.4.3 Analysis steps
Weigh 1.5g (accurate to 0.0002g) of the sample, place it in a 400mL beaker, add 10mL of ethanol to dissolve, add 250mL of water to dilute, add 10mL of hydrochloric acid solution and 0.5g of potassium bromide, and place it on a magnetic stirrer to dissolve. Insert the tip of the burette to about 2/3 below the liquid surface, and titrate rapidly with sodium nitrite standard titration solution at 10-25℃ under stirring to the near end point. Lift the tip of the burette out of the liquid surface and rinse with a small amount of water. Continue to titrate slowly under strong stirring until a small amount of solution is dipped into a glass rod and the starch potassium iodide indicator immediately turns blue. Stir for 1 minute and then try again. If it still turns blue, it is the end point. Perform a blank test at the same time. 4.4.4 Expression and calculation of results
The mass percentage of aniline X2 in industrial acetanilide is calculated according to formula (2): Xz=X (V:-Vo)×0. 093 12)
Where: ci——actual concentration of sodium nitrite standard titration solution, mol/L; V2—volume of sodium nitrite standard titration solution consumed by the titration sample, mL; V. —Volume of sodium nitrite standard titration solution consumed in blank test, mL; m—mass of sample, g;
....(2)
HG2303-92
0.09312——Mass of aniline in grams equivalent to 1.00mL sodium nitrite standard titration solution [c (NaNO2) 1.000mol/L];
The arithmetic mean is taken as the test result.
4.4.5 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.03%. 4.5 Determination of water content (Karl Fischer method) 4.5.1 Analysis steps
Weigh 1g sample (accurate to 0.002g), add 5mL of anhydrous methanol to dissolve, and perform the following operations according to GB6285. Visually observe the titration end point.
4.5.2 Allowable difference
The difference between two parallel determination results shall not exceed 0.02%, and the arithmetic mean shall be taken as the test result. 4.6 Determination of ash
4.6.1 Analysis steps
Weigh 4g of sample (accurate to 0.002g), place in a constant volume of 50mL porcelain, heat in a closed electric furnace or on an electric hot plate in a fume hood until acetanilide is completely sublimated, then move into a high-temperature furnace, burn at 650±25℃ for 30min, move into a dryer to cool to room temperature, and weigh.
4.6.2 Expression and calculation of results
The mass percentage of ash Xs in industrial acetanilide is calculated according to formula (3): Xg=ml=m2×100
Where: m1—ash content and crucible mass after burning, g; m2——crushed crucible mass, g;
m——sample mass, g.
The arithmetic mean is taken as the test result.
4.6.3 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.001%. 5 Inspection rules
5.1 Industrial acetanilide shall be sampled and inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that each batch of products shipped out of the factory meets the requirements of this standard. Each batch of products shipped out of the factory shall be accompanied by a quality certificate in a certain format, including the product name, manufacturer name, product grade, production date or batch number, and this standard number.
5.2 The user unit has the right to accept the received product according to the requirements of this standard. 5.3 All technical indicators listed in this standard are type inspection items. Under normal production conditions, ash content is inspected once every half month, and other items are factory inspection items.
5.4 The batch size of industrial acetanilide shall not exceed 5t. 5.5 Sampling method
5.5.1 The number of sampling units shall be selected in accordance with the provisions of GB6678. 5.5.2 Sampling Procedures
Use a stainless steel sampler to insert along the center line of the package to 2/3 of its depth to take a sample, each of which is not less than 100g, and place it in a clean and dry sugar porcelain plate. After mixing and evenly hooking, use the quartering method to reduce it to 500g, and evenly pack it in two clean and dry brown ground-mouth reagent bottles. Paste labels on the bottles, indicating the sample name, manufacturer name, production date or batch number, sampling date and sampler name. One bottle is sent to the quality inspection department for inspection, and the other bottle is kept for three months for future reference. 5
W.bzsoso.cOmHG2303—92
5.6 If one of the indicators does not meet the requirements of this standard, re-sampling and inspection should be carried out from twice the amount of packages. Even if only one indicator of the re-inspection result does not meet the requirements of this standard, the entire batch of products cannot be accepted. 5.7 When the supply and demand parties have a dispute over product quality, the national arbitration institution agreed by both parties shall conduct arbitration in accordance with the provisions of this standard. 5.8 The rounded value comparison method is used to determine whether the test data meets the standard requirements. The rounded value comparison method is used. 6 Marking, packaging, transportation, storage
6.1 The inner packaging of industrial acetanilide is a polyethylene blown film bag with a thickness of not less than 0.05mm. The outer packaging is a B-type plastic woven bag. The net weight of each bag is 25kg or 50kg.
6.2 Each package should be accompanied by a quality certificate as specified in Article 5.1. 6.3 The outer packaging should be painted with a firm mark, indicating the manufacturer's name, product name, product grade, production date or batch number, net weight and the "Hand Hook Prohibited" mark in Figure 2 of GB191. 6.4 Industrial acetanilide can be transported by various means of transportation. It should be protected from sunlight and rain during transportation and storage. It should be moisture-proof during storage and should not be close to fire sources.
Additional instructions:
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 technically managed by the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Sichuan Changshou Chemical General Plant, and Jilin Pharmaceutical Factory participated in the drafting. The main drafters of this standard are Dang Chengyu, Su Zuyu, Ye Qiong, and Wu Tingrong. This standard adopts Japanese Industrial Standard JISK4111-85 "Acetanilide" with reference. From the date of implementation of this standard, the former Ministry of Chemical Industry Standard HG2-388-66 will be invalid.2 Allowable difference
The difference between two parallel determination results shall not exceed 0.02%, and the arithmetic mean shall be taken as the test result. 4.6 Determination of ash
4.6.1 Analysis steps
Weigh 4g of sample (accurate to 0.002g), place in a constant volume of 50mL porcelain, heat in a closed electric furnace or on an electric hot plate in a fume hood until acetanilide is completely sublimated, then move into a high-temperature furnace, burn at 650±25℃ for 30min, move into a dryer and cool to room temperature, and weigh.
4.6.2 Expression and calculation of results
The mass percentage Xs of ash in industrial acetanilide is calculated according to formula (3): Xg=ml=m2×100
Where: m1—ash content and crucible mass after burning, g; m2——crushed crucible mass, g;
m——sample mass, g.
The arithmetic mean is taken as the test result.
4.6.3 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.001%. 5 Inspection rules
5.1 Industrial acetanilide shall be sampled and inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that each batch of products shipped out of the factory meets the requirements of this standard. Each batch of products shipped out of the factory shall be accompanied by a quality certificate in a certain format, including the product name, manufacturer name, product grade, production date or batch number, and this standard number.
5.2 The user unit has the right to accept the received product according to the requirements of this standard. 5.3 All technical indicators listed in this standard are type inspection items. Under normal production conditions, ash content is inspected once every half month, and other items are factory inspection items.
5.4 The batch size of industrial acetanilide shall not exceed 5t. 5.5 Sampling method
5.5.1 The number of sampling units shall be selected in accordance with the provisions of GB6678. 5.5.2 Sampling Procedures
Use a stainless steel sampler to insert along the center line of the package to 2/3 of its depth to take a sample, each of which is not less than 100g, and place it in a clean and dry sugar porcelain plate. After mixing and evenly hooking, use the quartering method to reduce it to 500g, and evenly pack it in two clean and dry brown ground-mouth reagent bottles. Paste labels on the bottles, indicating the sample name, manufacturer name, production date or batch number, sampling date and sampler name. One bottle is sent to the quality inspection department for inspection, and the other bottle is kept for three months for future reference. 5
W.bzsoso.cOmHG2303—92
5.6 If one of the indicators does not meet the requirements of this standard, re-sampling and inspection should be carried out from twice the amount of packages. Even if only one indicator of the re-inspection result does not meet the requirements of this standard, the entire batch of products cannot be accepted. 5.7 When the supply and demand parties have a dispute over product quality, the national arbitration institution agreed by both parties shall conduct arbitration in accordance with the provisions of this standard. 5.8 The rounded value comparison method is used to determine whether the test data meets the standard requirements. The rounded value comparison method is used. 6 Marking, packaging, transportation, storage
6.1 The inner packaging of industrial acetanilide is a polyethylene blown film bag with a thickness of not less than 0.05mm. The outer packaging is a B-type plastic woven bag. The net weight of each bag is 25kg or 50kg.
6.2 Each package should be accompanied by a quality certificate as specified in Article 5.1. 6.3 The outer packaging should be painted with a firm mark, indicating the manufacturer's name, product name, product grade, production date or batch number, net weight and the "Hand Hook Prohibited" mark in Figure 2 of GB191. 6.4 Industrial acetanilide can be transported by various means of transportation. It should be protected from sunlight and rain during transportation and storage. It should be moisture-proof during storage and should not be close to fire sources.
Additional instructions:
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 technically managed by the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Sichuan Changshou Chemical General Plant, and Jilin Pharmaceutical Factory participated in the drafting. The main drafters of this standard are Dang Chengyu, Su Zuyu, Ye Qiong, and Wu Tingrong. This standard adopts Japanese Industrial Standard JISK4111-85 "Acetanilide" with reference. From the date of implementation of this standard, the former Ministry of Chemical Industry Standard HG2-388-66 will be invalid.2 Allowable difference
The difference between two parallel determination results shall not exceed 0.02%, and the arithmetic mean shall be taken as the test result. 4.6 Determination of ash
4.6.1 Analysis steps
Weigh 4g of sample (accurate to 0.002g), place in a constant volume of 50mL porcelain, heat in a closed electric furnace or on an electric hot plate in a fume hood until acetanilide is completely sublimated, then move into a high-temperature furnace, burn at 650±25℃ for 30min, move into a dryer to cool to room temperature, and weigh.
4.6.2 Expression and calculation of results
The mass percentage Xs of ash in industrial acetanilide is calculated according to formula (3): Xg=ml=m2×100
Where: m1—ash content and crucible mass after burning, g; m2——crushed crucible mass, g;
m——sample mass, g.
The arithmetic mean is taken as the test result.
4.6.3 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.001%. 5 Inspection rules
5.1 Industrial acetanilide shall be sampled and inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that each batch of products shipped out of the factory meets the requirements of this standard. Each batch of products shipped out of the factory shall be accompanied by a quality certificate in a certain format, including the product name, manufacturer name, product grade, production date or batch number, and this standard number.
5.2 The user unit has the right to accept the received product according to the requirements of this standard. 5.3 All technical indicators listed in this standard are type inspection items. Under normal production conditions, ash content is inspected once every half month, and other items are factory inspection items.
5.4 The batch size of industrial acetanilide shall not exceed 5t. 5.5 Sampling method
5.5.1 The number of sampling units shall be selected in accordance with the provisions of GB6678. 5.5.2 Sampling Procedures
Use a stainless steel sampler to insert along the center line of the package to 2/3 of its depth to take a sample, each sample of not less than 100g, and place it in a clean and dry sugar porcelain plate. After mixing and evenly hooking, use the quartering method to reduce it to 500g, and evenly pack it in two clean and dry brown ground-mouth reagent bottles. Paste labels on the bottles, indicating the sample name, manufacturer name, production date or batch number, sampling date and sampler name. One bottle is sent to the quality inspection department for inspection, and the other bottle is kept for three months for future reference. 5
W.bzsoso.cOmHG2303—92
5.6 If one of the indicators does not meet the requirements of this standard, re-sampling and inspection should be carried out from twice the amount of packages. Even if only one indicator of the re-inspection result does not meet the requirements of this standard, the entire batch of products cannot be accepted. 5.7 When the supply and demand parties have a dispute over product quality, the national arbitration institution agreed by both parties shall conduct arbitration in accordance with the provisions of this standard. 5.8 The rounded value comparison method is used to determine whether the test data meets the standard requirements. The rounded value comparison method is used. 6 Marking, packaging, transportation, storage
6.1 The inner packaging of industrial acetanilide is a polyethylene blown film bag with a thickness of not less than 0.05mm. The outer packaging is a type B plastic woven bag. The net weight of each bag is 25kg or 50kg.
6.2 Each package should be accompanied by a quality certificate as specified in Article 5.1. 6.3 The outer packaging should be painted with a firm mark, indicating the manufacturer's name, product name, product grade, production date or batch number, net weight and the "hand hook prohibited" mark in Figure 2 of GB191. 6.4 Industrial acetanilide can be transported by various means of transportation. It should be protected from sunlight and rain during transportation and storage. It should be moisture-proof during storage and should not be close to fire sources.
Additional instructions:
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 technically managed by the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Sichuan Changshou Chemical General Plant, and Jilin Pharmaceutical Factory participated in the drafting. The main drafters of this standard are Dang Chengyu, Su Zuyu, Ye Qiong, and Wu Tingrong. This standard adopts Japanese Industrial Standard JISK4111-85 "Acetanilide" with reference. From the date of implementation of this standard, the former Ministry of Chemical Industry Standard HG2-388-66 will be invalid.
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