Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/T 2310—92
Published on May 17, 1992
Ministry of Chemical Industry of the People's Republic of China
Implemented on January 1, 1993
W Chemical Industry Standard of the People's Republic of China
Subject Content and Scope of Application
HG/T2310—92
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage of dodecanol. This standard applies to dodecanol obtained by esterification and high-pressure hydrogenation of natural oils and fats to make mixed alcohols and then distillation. Molecular formula: CH(CH2)CH,OH
Relative molecular mass: 186.34 (according to the international relative atomic mass in 1989) 2 Reference standards
GB1250
GB3143
GB6365
GB6678
GB8170
Preparation of standard solutions for titration analysis (volumetric analysis) of chemical reagents Preparation of preparations and products used in test methods of chemical reagents Methods of expressing and determining limit values Color determination method for liquid chemical products (Hazen unit - platinum-cobalt color number) Determination of free alkalinity or free acidity of surfactants Titration method General rules for sampling of chemical products
Rules for rounding off values
Octadecanol
ZBG17027
3 Technical requirements
3.1 Appearance: white solid or transparent liquid at room temperature. 3.2 The quality of dodecanol shall meet the requirements of the following table. Item
Color, Hazen
Acid value, mgKoH/g
Saponification value, mgKOH/g
Iodine value, gIz/100g
Hydroxy value, mgKoH/g
Purity, %
Alkanes, %
Superior product approved by the Ministry of Chemical Industry of the People's Republic of China on 1992-05-17
295~301| |tt||First-class products
294~304
Qualified products
285~315
1993-01-01 implementation
W.bzsoso:com4Test method
HG/T2310-92
The reagents and water used in this standard shall use analytical pure reagents and distilled water or water of equivalent purity unless otherwise specified. The standard solutions, preparations and products used in this standard shall comply with the provisions of GB601 and GB603 unless otherwise specified.
4.1 Determination of chromaticity
The determination shall be carried out in accordance with the provisions of GB3143.
4.2 Determination of acid value
The determination shall be carried out in accordance with the provisions of GB6365.
The endpoint is titration until the pink color does not fade for 30 seconds. 4.3 Determination of saponification value
4.3.1 Principle of the method
Excess alkali neutralizes the acid in the sample and reacts with the esters in the sample to saponify. After the reaction is completed, the remaining alkali is neutralized with acid. 4.3.2 Reagents and solutions
4.3.2.1 Neutral anhydrous ethanol: neutralize with alkali until it is neutral to phenolic acid. 4.3.2.2 Potassium hydroxide ethanol solution: 28g/L. Weigh 28g potassium hydroxide and dissolve it in 30mL distilled water, dilute it to 1000mL with aldehyde-free ethanol, let it stand for 24h, pour out the supernatant, discard the precipitate, store the solution in a brown bottle with a lid and plug it for use. Preparation of aldehyde-free ethanol: Reflux 5g aluminum sheet in 1000mL neutral anhydrous ethanol for 1h, then distill it immediately. 4.3.2.3 Standard titration solution of hydrochloric acid: c(HCI) = 0.5mol/L. 4.3.2.4 Phenol indicator solution: 10 g/L.
4.3.3 Instruments
4.3.3.1 Water bath or electric hot plate.
4.3.4 Analysis steps
Weigh 10 g of sample (accurate to 0.0002 g), place in a ground-mouth conical flask, use a pipette to transfer 50.0 mL of potassium hydroxide ethanol solution, install a reflux condenser, place in a water bath, the water bath temperature should not be lower than 95°C, heat and reflux for 1 h, rinse the condenser wall with 10 mL of neutral anhydrous ethanol solution, remove the conical flask, add 2 to 3 drops of phenolphthalein indicator solution, and titrate with hydrochloric acid standard titration solution until the red color disappears as the end point. At the same time, perform a blank test.
4.3.5 Calculation of analysis results
The saponification value Xi (mgKOH/g) is calculated according to formula (1): X, = . -V) : × 0. 0561 ×1 00..m
Where: V. Volume of standard hydrochloric acid solution consumed in blank test, mL; V1-volume of standard hydrochloric acid solution consumed in titration of sample, mL: ci-concentration of standard hydrochloric acid solution, mol/L; (1)
0.0561-mass of potassium hydroxide equivalent to 1.00mL standard hydrochloric acid solution c (HC1) = 1.000mol/L], expressed in grams;
m-mass of sample, g.
Take the arithmetic mean of two parallel determinations as the result. 4.3.6 Allowable difference
The difference between two parallel determinations should not be greater than 0.4mgKOH/g. 4.4 Determination of iodine value
4.4.1 Principle of the method
W.bzsoso.coIHG/T2310—92
Under specified conditions, how many grams of iodine are consumed by 100g of sample, which is used to measure the unsaturation of the substance. 4.4.2 Reagents and solutions
4.4.2.1 Carbon tetrachloride or chloroform;
4.4.2.2 Glacial acetic acid;
4.4.2.3 Potassium iodide solution: 150g/L;
4.4.2.4 Glacial acetic acid solution of iodine chloride (Wei's solution): 16.2g/L. Dissolve 16.2g of iodine chloride in 1L of glacial acetic acid. Or weigh 13g of iodine and dissolve it in 1L of glacial acetic acid, and pass dry chlorine gas until the solution changes from brown to orange-red. Calibrate according to blank determination before and after passing chlorine gas. The volume consumed by the sodium thiosulfate standard titration solution (4.4.2.5) should be twice that of the former, otherwise it needs to be adjusted. 4.4.2.5 Sodium thiosulfate standard titration solution: c (Na2S2Os) = 0.1 mol/L, 4.4.2.6 Starch indicator solution: 10 g/L.
4.4.3 Analysis steps
Weigh 5 g (accurate to 0.0002 g) of the sample into an iodine volumetric flask, add 25 mL of carbon tetrachloride or chloroform to dissolve, accurately transfer 25.0 mL of Wei's solution, cover the bottle with a stopper, seal the bottle mouth with potassium iodide solution, shake it slowly, and place it in a dark place at room temperature for 1 hour. After taking it out, add 25 mL of potassium iodide solution and 50 mL of water, and titrate with sodium thiosulfate standard titration solution until it turns light yellow, then add about 1 mL of starch indicator solution, and continue to titrate until the blue disappears as the end point. At the same time, do a blank test.
4.4.4 Calculation of analysis results
The iodine value X2 (gI2/100g) is calculated according to formula (2): (V.-V).cX0.1269
2×100
Wherein: V. — Volume of sodium thiosulfate standard titration solution consumed for blank, mL; V. — Volume of sodium thiosulfate standard titration solution consumed for titration of sample, mL; c2 — Concentration of sodium thiosulfate standard titration solution, mol/L(2)
0.1269 — Mass of iodine in grams equivalent to 1.00mL sodium thiosulfate standard titration solution c (NazS20s) = 1.000mol/L];
— Mass of sample, g.
The arithmetic mean of two parallel determinations is taken as the result. 4.4.5 Allowable difference
The difference between two parallel determinations shall not be greater than 0.2gI2/100g. 4.5 Determination of hydroxyl value
4.5.1 Principle of the method
Alcohol reacts with excess acetylating agent. After the reaction is completed, water is added to hydrolyze the remaining acetic anhydride, and then the generated acetic acid is neutralized with alkali.
4.5.2 Reagents and solutions
4.5.2.1 Neutral anhydrous ethanol: neutralize with alkali until it is neutral to phenolic acid; 4.5.2.2 Acetylation agent: pyridine: acetic anhydride = 4 + 1; 4.5.2.3 Potassium hydroxide ethanol standard titration solution: c (KOH) = 0.5mol/L. Weigh 28g potassium hydroxide and dissolve it in 30mL distilled water, dilute to 1000mL with aldehyde-free ethanol, leave for 24h, pour out the supernatant, discard the precipitate, store the solution in a brown bottle with a lid and seal it for later use.
Preparation of aldehyde-free ethanol: Reflux 5g aluminum flakes in 1000mL neutral anhydrous ethanol for 1h, then distill immediately. 4.5.2.4 Phenolphthalein indicator solution: 10g/L.
4.5.3 Analysis steps
ww.bzsoso：comHG/T2310—92
Weigh 0.5~1.0g of sample (accurate to 0.0002g) into an iodine volumetric flask, accurately transfer 3mL of freshly prepared acetylation reagent, place a small funnel on the bottle mouth, put it into a constant temperature glycerol bath maintained at 96℃~99℃, immerse the bottom of the iodine volumetric flask about 1cm deep, and heat to reflux for 1h. Take it out and cool to room temperature, add 2mL of water from the small funnel mouth, shake the hook, and then put it into a glycerol bath at 96℃~99℃ and heat to hydrolyze for 5min. Take it out and cool to room temperature, rinse the inner and outer walls of the funnel and the inner wall of the bottle with 50mL of neutral anhydrous ethanol. Add 3 drops of phenolphthalein indicator solution, and titrate with potassium hydroxide ethanol standard titration solution until the reddish color lasts for 30s as the end point. At the same time, do a blank test.
4.5.4 Calculation of analysis results
Hydroxy value X: (mgKOH/g) is calculated according to formula (3): (V.-Vs).csX 0. 0561
Wherein: V. is the volume of the standard potassium hydroxide ethanol titration solution consumed in the blank test, mL; V: is the volume of the standard potassium hydroxide ethanol titration solution consumed in the titration of the sample, mL; Cs is the concentration of the standard potassium hydroxide ethanol titration solution, mol/L; (3)
0.0561 is the mass of potassium hydroxide expressed in grams equivalent to 1.00mL of the standard potassium hydroxide ethanol titration solution [c(K0H)=1.000mol/L);
m is the mass of the sample, g.
The arithmetic mean of two parallel determinations is taken as the result. 4.5.5 Allowable difference
The difference between the two parallel determinations shall not be greater than 3mgKOH/g. 4.6 Determination of Purity
4.6.1 Reagents and Materials
4.6.1.1 Carrier Gas and Auxiliary Gas
Carrier Gas: Nitrogen or Ammonia, purity greater than 99.9%; a.
Combustion Gas: Hydrogen, purity greater than 99.7%;
Combustion Auxiliary Gas: Secondary Purified Air.
4.6.1.2 Reagents and Materials Used in Preparing Chromatographic Columns a.
Fixed Liquid: SE-30+Decaethylene Glycol-20M; Carrier: 101 White Silylated Carrier. Particle Size 0.180.25mm (80~60 Mesh); b.
c. Solvent: Chloroform.
4.6.2 Instruments
4.6.2.1 Gas Chromatograph
Detector: Hydrogen Flame Ionization Detector. 4.6.2.2 Chromatographic column
a. Column tube: stainless steel tube or glass tube with an inner diameter of 3.5~4.0mm and a length of 2m. b. Filling material:
Ratio: carrier: stationary phase = 100:5 (polyethylene glycol-20M is 0.05%) (mass ratio) Method of coating stationary phase: weigh 1.25g methyl silicone SE-30 and 12.5mg polyethylene glycol-20M in a beaker, add 100mL chloroform to dissolve, add 25g of carrier, stir slightly, dry under infrared lamp or dry naturally. c. Filling method:
Plug the outlet end of the chromatographic column (the end connected to the detector) with a little glass wool, evacuate the outlet end, and load about 20g of stationary phase under gentle vibration, fill evenly and tightly, and then plug it with glass wool. d. Aging of chromatographic column
HG/T2310—92
Install the filled chromatographic column into the chromatographic column box, check the airtightness, pass nitrogen, gradually raise the temperature to 210℃, and age at 210℃ for more than 8 hours until the baseline is stable.
4.6.2.3 Sample injector: micro glass syringe. 4.6.2.4 Chromatographic data processor: recorder or integrator. 4.6.3 Analysis steps
4.6.3.1 Adjust the instrument
Adjust the instrument according to the following reference conditions:
Vaporization chamber temperature: 250℃;
Detection chamber temperature: 250℃;
Column box temperature: 170℃;
Nitrogen flow rate: 25~30ml/min;
Hydrogen flow rate: 25~30ml/min;
f. Air flow rate: 500ml/min;
gInjection volume: 0.02~0.1μl.
4.6.3.2 Calibration method: Corrected area normalization method. 4.6.3.3 Test: Adjust the instrument according to the above provisions. After the baseline is stable, use a micro glass syringe to inject the sample and use the chromatograph recorder or integrator to process and calculate the data according to the corrected area normalization method. 4.6.4 Calculation of analysis results
4.6.4.1 For each component X1, expressed as mass percentage, calculate according to formula (4): A,f
wherein, X, one-to-one corresponds to the content of component i, when X, is Xc12 alcohol represents purity, %; A corresponds to the chromatographic peak area of component i;
corresponds to the quantitative correction factor of the chromatographic peak of the component. The arithmetic mean of two parallel determinations is taken as the result. 4.6.4.2 Correction factor is calculated according to formula (5): fw
wherein: f—mass correction factor;
f's(w)
A, W, As, W. One is the peak area and mass of the analyte and the known chromatographic pure standard, respectively. 4.6.5 Allowable difference
The difference between two parallel determinations shall not be greater than 0.5%. 4.6.6 Detection limit
The minimum detection concentration is 0.05%.
（5）
W.bzsoso.coI4
4.7 Determination of alkane content
HG/T2310-92
C12 alcohol chromatogram
1—C1o alcohol; 2—C14 alkane; 3—C12 alcohol; 4—C16 alkane The sum of the contents of each carbon chain alkane component in the sample is the alkane content. Follow the provisions of 4.6.1 to 4.6.4.2 in the purity determination method. 4.7.1 Allowable difference
The difference between two parallel determination values shall not be greater than 0.3%. 5 Inspection rules
5.1 Dodecanol shall be inspected by the quality inspection department of the manufacturer, and the manufacturer shall ensure that each batch of dodecanol shipped from the factory meets the requirements of this standard.
5.2 The user has the right to inspect and accept dodecanol in accordance with the provisions of this standard. 5.3 Each batch of products leaving the factory shall be accompanied by a quality certificate, which includes: manufacturer name, product name, grade, production date, batch number, net weight, proof that the product quality complies with this standard and the number of this standard. 5.4 Sampling shall be carried out in accordance with the provisions of GB6678, and the total amount of samples shall not be less than 500g. 5.5 Melt and mix the samples taken; put equal amounts into two clean and dry bottles with ground stoppers, and paste labels on the bottles, indicating the manufacturer name, product name, grade, batch number and sampling date. One bottle is for inspection and the other bottle is kept for two months for future reference. 5.6 If one of the indicators in the test results does not meet the requirements of this standard, dodecanol should be taken from twice the amount of packaging containers for re-testing. Even if only one indicator in the re-test results 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 objections to the product quality, they can negotiate to resolve the issue, or conduct arbitration in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection".
6 Marking, packaging, transportation and purchase and storage
6.1 Marking: The packaging container of dodecanol should have obvious and firm markings, including: manufacturer name, product name, trademark, production date, grade, batch number, net weight, and this standard number. 6.2 Packaging: Dodecanol should be packed in firm, dry, clean galvanized barrels or aluminum barrels, with a net weight of 160kg per barrel. 6.3 Transportation: The barrel cover must be tightly sealed during transportation to avoid leakage. 6.4 Storage: Dodecanol should be stored in a dry and ventilated warehouse. The storage period is 1 year from the date of leaving the factory. 6
Additional instructions:
HG/T2310-92
This standard was 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 technical jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Wuxi Chemical Industry Group Corporation. The main drafters of this standard are Gong Fuying, Feng Jing, Tan Xiangzhen, Zhang Hongguang and Cheng Xiaoming.0561
Wherein: V. -- Volume of potassium hydroxide ethanol standard titration solution consumed in blank test, mL; V: -- Volume of potassium hydroxide ethanol standard titration solution consumed in titration of sample, mL; Cs -- Concentration of potassium hydroxide ethanol standard titration solution, mol/L; (3)
0.0561 -- Mass of potassium hydroxide expressed in grams equivalent to 1.00mL potassium hydroxide ethanol standard titration solution [c(K0H)=1.000mol/L);
m -- Mass of sample, g.
Take the arithmetic mean of two parallel determinations as the result. 4.5.5 Allowable difference
The difference between two parallel determinations shall not exceed 3mgKOH/g. 4.6 Determination of Purity
4.6.1 Reagents and Materials
4.6.1.1 Carrier Gas and Auxiliary Gas
Carrier Gas: Nitrogen or Ammonia, purity greater than 99.9%; a.
Combustion Gas: Hydrogen, purity greater than 99.7%;
Combustion Auxiliary Gas: Secondary Purified Air.
4.6.1.2 Reagents and Materials Used in Preparing Chromatographic Columns a.
Fixed Liquid: SE-30+Decaethylene Glycol-20M; Carrier: 101 White Silylated Carrier. Particle Size 0.180.25mm (80~60 Mesh); b.
c. Solvent: Chloroform.
4.6.2 Instruments
4.6.2.1 Gas Chromatograph
Detector: Hydrogen Flame Ionization Detector. 4.6.2.2 Chromatographic column
a. Column tube: stainless steel tube or glass tube with an inner diameter of 3.5~4.0mm and a length of 2m. b. Filling material:
Ratio: carrier: stationary phase = 100:5 (polyethylene glycol-20M is 0.05%) (mass ratio) Method of coating stationary phase: weigh 1.25g methyl silicone SE-30 and 12.5mg polyethylene glycol-20M in a beaker, add 100mL chloroform to dissolve, add 25g of carrier, stir slightly, dry under infrared lamp or dry naturally. c. Filling method:
Plug the outlet end of the chromatographic column (the end connected to the detector) with a little glass wool, evacuate the outlet end, and load about 20g of stationary phase under gentle vibration, fill evenly and tightly, and then plug it with glass wool. d. Aging of chromatographic column
HG/T2310—92
Install the filled chromatographic column into the chromatographic column box, check the airtightness, pass nitrogen, gradually raise the temperature to 210℃, and age at 210℃ for more than 8 hours until the baseline is stable.
4.6.2.3 Sample injector: micro glass syringe. 4.6.2.4 Chromatographic data processor: recorder or integrator. 4.6.3 Analysis steps
4.6.3.1 Adjust the instrument
Adjust the instrument according to the following reference conditions:
Vaporization chamber temperature: 250℃;
Detection chamber temperature: 250℃;
Column box temperature: 170℃;
Nitrogen flow rate: 25~30ml/min;
Hydrogen flow rate: 25~30ml/min;
f. Air flow rate: 500ml/min;
gInjection volume: 0.02~0.1μl.
4.6.3.2 Calibration method: Corrected area normalization method. 4.6.3.3 Test: Adjust the instrument according to the above provisions. After the baseline is stable, use a micro glass syringe to inject the sample and use the chromatograph recorder or integrator to process and calculate the data according to the corrected area normalization method. 4.6.4 Calculation of analysis results
4.6.4.1 For each component X1, expressed as mass percentage, calculate according to formula (4): A,f
wherein, X, one-to-one corresponds to the content of component i, when X, is Xc12 alcohol represents purity, %; A corresponds to the chromatographic peak area of component i;
corresponds to the quantitative correction factor of the chromatographic peak of the component. The arithmetic mean of two parallel determinations is taken as the result. 4.6.4.2 Correction factor is calculated according to formula (5): fw
wherein: f—mass correction factor;
f's(w)
A, W, As, W. One is the peak area and mass of the analyte and the known chromatographic pure standard, respectively. 4.6.5 Allowable difference
The difference between two parallel determinations shall not be greater than 0.5%. 4.6.6 Detection limit
The minimum detection concentration is 0.05%.
（5）
W.bzsoso.coI4
4.7 Determination of alkane content
HG/T2310-92
C12 alcohol chromatogram
1—C1o alcohol; 2—C14 alkane; 3—C12 alcohol; 4—C16 alkane The sum of the contents of each carbon chain alkane component in the sample is the alkane content. Follow the provisions of 4.6.1 to 4.6.4.2 in the purity determination method. 4.7.1 Allowable difference
The difference between two parallel determination values shall not be greater than 0.3%. 5 Inspection rules
5.1 Dodecanol shall be inspected by the quality inspection department of the manufacturer, and the manufacturer shall ensure that each batch of dodecanol shipped from the factory meets the requirements of this standard.
5.2 The user has the right to inspect and accept dodecanol in accordance with the provisions of this standard. 5.3 Each batch of products leaving the factory shall be accompanied by a quality certificate, which includes: manufacturer name, product name, grade, production date, batch number, net weight, proof that the product quality complies with this standard and the number of this standard. 5.4 Sampling shall be carried out in accordance with the provisions of GB6678, and the total amount of samples shall not be less than 500g. 5.5 Melt and mix the samples taken; put equal amounts into two clean and dry bottles with ground stoppers, and paste labels on the bottles, indicating the manufacturer name, product name, grade, batch number and sampling date. One bottle is for inspection and the other bottle is kept for two months for future reference. 5.6 If one of the indicators in the test results does not meet the requirements of this standard, dodecanol should be taken from twice the amount of packaging containers for re-testing. Even if only one indicator in the re-test results 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 objections to the product quality, they can negotiate to resolve the issue, or conduct arbitration in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection".
6 Marking, packaging, transportation and purchase and storage
6.1 Marking: The packaging container of dodecanol should have obvious and firm markings, including: manufacturer name, product name, trademark, production date, grade, batch number, net weight, and this standard number. 6.2 Packaging: Dodecanol should be packed in firm, dry, clean galvanized barrels or aluminum barrels, with a net weight of 160kg per barrel. 6.3 Transportation: The barrel cover must be tightly sealed during transportation to avoid leakage. 6.4 Storage: Dodecanol should be stored in a dry and ventilated warehouse. The storage period is 1 year from the date of leaving the factory. 6
Additional instructions:
HG/T2310-92
This standard was 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 technical jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Wuxi Chemical Industry Group Corporation. The main drafters of this standard are Gong Fuying, Feng Jing, Tan Xiangzhen, Zhang Hongguang and Cheng Xiaoming.0561
Wherein: V. -- Volume of potassium hydroxide ethanol standard titration solution consumed in blank test, mL; V: -- Volume of potassium hydroxide ethanol standard titration solution consumed in titration of sample, mL; Cs -- Concentration of potassium hydroxide ethanol standard titration solution, mol/L; (3)
0.0561 -- Mass of potassium hydroxide expressed in grams equivalent to 1.00mL potassium hydroxide ethanol standard titration solution [c(K0H)=1.000mol/L);
m -- Mass of sample, g.
Take the arithmetic mean of two parallel determinations as the result. 4.5.5 Allowable difference
The difference between two parallel determinations shall not exceed 3mgKOH/g. 4.6 Determination of Purity
4.6.1 Reagents and Materials
4.6.1.1 Carrier Gas and Auxiliary Gas
Carrier Gas: Nitrogen or Ammonia, purity greater than 99.9%; a.
Combustion Gas: Hydrogen, purity greater than 99.7%;
Combustion Auxiliary Gas: Secondary Purified Air.
4.6.1.2 Reagents and Materials Used in Preparing Chromatographic Columns a.
Fixed Liquid: SE-30+Decaethylene Glycol-20M; Carrier: 101 White Silylated Carrier. Particle Size 0.180.25mm (80~60 Mesh); b.
c. Solvent: Chloroform.
4.6.2 Instruments
4.6.2.1 Gas Chromatograph
Detector: Hydrogen Flame Ionization Detector. 4.6.2.2 Chromatographic column
a. Column tube: stainless steel tube or glass tube with an inner diameter of 3.5~4.0mm and a length of 2m. b. Filling material:
Ratio: carrier: stationary phase = 100:5 (polyethylene glycol-20M is 0.05%) (mass ratio) Method of coating stationary phase: weigh 1.25g methyl silicone SE-30 and 12.5mg polyethylene glycol-20M in a beaker, add 100mL chloroform to dissolve, add 25g of carrier, stir slightly, dry under infrared lamp or dry naturally. c. Filling method:
Plug the outlet end of the chromatographic column (the end connected to the detector) with a little glass wool, evacuate the outlet end, and load about 20g of stationary phase under gentle vibration, fill evenly and tightly, and then plug it with glass wool. d. Aging of chromatographic column
HG/T2310—92
Install the filled chromatographic column into the chromatographic column box, check the airtightness, pass nitrogen, gradually raise the temperature to 210℃, and age at 210℃ for more than 8 hours until the baseline is stable.
4.6.2.3 Sample injector: micro glass syringe. 4.6.2.4 Chromatographic data processor: recorder or integrator. 4.6.3 Analysis steps
4.6.3.1 Adjust the instrument
Adjust the instrument according to the following reference conditions:
Vaporization chamber temperature: 250℃;
Detection chamber temperature: 250℃;
Column box temperature: 170℃;
Nitrogen flow rate: 25~30ml/min;
Hydrogen flow rate: 25~30ml/min;
f. Air flow rate: 500ml/min;
gInjection volume: 0.02~0.1μl.
4.6.3.2 Calibration method: Corrected area normalization method. 4.6.3.3 Test: Adjust the instrument according to the above provisions. After the baseline is stable, use a micro glass syringe to inject the sample and use the chromatograph recorder or integrator to process and calculate the data according to the corrected area normalization method. 4.6.4 Calculation of analysis results
4.6.4.1 For each component X1, expressed as mass percentage, calculate according to formula (4): A,f
wherein, X, one-to-one corresponds to the content of component i, when X, is Xc12 alcohol represents purity, %; A corresponds to the chromatographic peak area of component i;
corresponds to the quantitative correction factor of the chromatographic peak of the component. The arithmetic mean of two parallel determinations is taken as the result. 4.6.4.2 Correction factor is calculated according to formula (5): fw
wherein: f—mass correction factor;
f's(w)
A, W, As, W. One is the peak area and mass of the analyte and the known chromatographic pure standard, respectively. 4.6.5 Allowable difference
The difference between two parallel determinations shall not be greater than 0.5%. 4.6.6 Detection limit
The minimum detection concentration is 0.05%.
(5)
W.bzsoso.coI4
4.7 Determination of alkane content
HG/T2310-92
C12 alcohol chromatogram
1-C1o alcohol; 2-C14 alkane; 3-C12 alcohol; 4-C16 alkane The sum of the contents of each carbon chain alkane component in the sample is the alkane content. Follow the provisions of 4.6.1 to 4.6.4.2 in the purity determination method. 4.7.1 Allowable difference
The difference between two parallel determination values shall not be greater than 0.3%. 5 Inspection rules
5.1 Dodecanol shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that each batch of dodecanol shipped from the factory meets the requirements of this standard.
5.2 The user has the right to inspect and accept dodecanol in accordance with the provisions of this standard. 5.3 Each batch of products leaving the factory shall be accompanied by a quality certificate, which includes: manufacturer name, product name, grade, production date, batch number, net weight, proof that the product quality complies with this standard and the number of this standard. 5.4 Sampling shall be carried out in accordance with the provisions of GB6678, and the total amount of samples shall not be less than 500g. 5.5 Melt and mix the samples taken; put equal amounts into two clean and dry bottles with ground stoppers, and paste labels on the bottles, indicating the manufacturer name, product name, grade, batch number and sampling date. One bottle is for inspection and the other bottle is kept for two months for future reference. 5.6 If one of the indicators in the test results does not meet the requirements of this standard, dodecanol should be taken from twice the amount of packaging containers for re-testing. Even if only one indicator in the re-test results 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 objections to the product quality, they can negotiate to resolve the issue, or conduct arbitration in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection".
6 Marking, packaging, transportation and purchase and storage
6.1 Marking: The packaging container of dodecanol should have obvious and firm markings, including: manufacturer name, product name, trademark, production date, grade, batch number, net weight, and this standard number. 6.2 Packaging: Dodecanol should be packed in firm, dry, clean galvanized barrels or aluminum barrels, with a net weight of 160kg per barrel. 6.3 Transportation: The barrel cover must be tightly sealed during transportation to avoid leakage. 6.4 Storage: Dodecanol should be stored in a dry and ventilated warehouse. The storage period is 1 year from the date of leaving the factory. 6
Additional instructions:
HG/T2310-92
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 technical jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard is drafted by Wuxi Chemical Industry Group Corporation. The main drafters of this standard are Gong Fuying, Feng Jing, Tan Xiangzhen, Zhang Hongguang and Cheng Xiaoming.5mg polyethylene glycol-20M is dissolved in a beaker, 100mL chloroform is added to dissolve, 25g of carrier is added, and after a little stirring, it is dried under an infrared lamp or dried naturally. c Filling method:
Plug the outlet end of the chromatographic column (the end connected to the detector) with a little glass wool, evacuate the outlet end, and load about 20g of the stationary phase under gentle vibration, fill evenly and tightly, and then plug it with glass wool. d. Aging of chromatographic column
HG/T2310—92
Put the filled chromatographic column into the chromatographic column box, check the air tightness, pass nitrogen, gradually heat to 210℃, and age at 210℃ for more than 8h until the baseline is stable.
4.6.2.3 Injector: micro glass syringe. 4.6.2.4 Chromatographic data processor: recorder or integrator. 4.6.3 Analysis steps
4.6.3.1 Adjust the instrument
Adjust the instrument according to the following reference conditions:
Vaporization chamber temperature: 250℃;
Detection chamber temperature: 250℃;
Column box temperature: 170℃;
Nitrogen flow rate: 25~30ml/min;
Hydrogen flow rate: 25~30ml/min;
f. Air flow rate: 500ml/min;
gInjection volume: 0.02~0.1μl.
4.6.3.2 Calibration method: Corrected area normalization method. 4.6.3.3 Test: Adjust the instrument according to the above provisions. After the baseline is stable, use a micro glass syringe to inject the sample and use the chromatograph recorder or integrator to process and calculate the data according to the corrected area normalization method. 4.6.4 Calculation of analysis results
4.6.4.1 For each component X1, expressed as mass percentage, calculate according to formula (4): A,f
wherein, X, one-to-one corresponds to the content of component i, when X, is Xc12 alcohol represents purity, %; A corresponds to the chromatographic peak area of component i;
corresponds to the quantitative correction factor of the chromatographic peak of the component. The arithmetic mean of two parallel determinations is taken as the result. 4.6.4.2 Correction factor is calculated according to formula (5): fw
wherein: f—mass correction factor; bZxz.net
f's(w)
A, W, As, W. One is the peak area and mass of the analyte and the known chromatographic pure standard, respectively. 4.6.5 Allowable difference
The difference between two parallel determinations shall not be greater than 0.5%. 4.6.6 Detection limit
The minimum detection concentration is 0.05%.
（5）
W.bzsoso.coI4
4.7 Determination of alkane content
HG/T2310-92
C12 alcohol chromatogram
1—C1o alcohol; 2—C14 alkane; 3—C12 alcohol; 4—C16 alkane The sum of the contents of each carbon chain alkane component in the sample is the alkane content. Follow the provisions of 4.6.1 to 4.6.4.2 in the purity determination method. 4.7.1 Allowable difference
The difference between two parallel determination values shall not be greater than 0.3%. 5 Inspection rules
5.1 Dodecanol shall be inspected by the quality inspection department of the manufacturer, and the manufacturer shall ensure that each batch of dodecanol shipped from the factory meets the requirements of this standard.
5.2 The user has the right to inspect and accept dodecanol in accordance with the provisions of this standard. 5.3 Each batch of products leaving the factory shall be accompanied by a quality certificate, which includes: manufacturer name, product name, grade, production date, batch number, net weight, proof that the product quality complies with this standard and the number of this standard. 5.4 Sampling shall be carried out in accordance with the provisions of GB6678, and the total amount of samples shall not be less than 500g. 5.5 Melt and mix the samples taken; put equal amounts into two clean and dry bottles with ground stoppers, and paste labels on the bottles, indicating the manufacturer name, product name, grade, batch number and sampling date. One bottle is for inspection and the other bottle is kept for two months for future reference. 5.6 If one of the indicators in the test results does not meet the requirements of this standard, dodecanol should be taken from twice the amount of packaging containers for re-testing. Even if only one indicator in the re-test results 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 objections to the product quality, they can negotiate to resolve the issue, or conduct arbitration in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection".
6 Marking, packaging, transportation and purchase and storage
6.1 Marking: The packaging container of dodecanol should have obvious and firm markings, including: manufacturer name, product name, trademark, production date, grade, batch number, net weight, and this standard number. 6.2 Packaging: Dodecanol should be packed in firm, dry, clean galvanized barrels or aluminum barrels, with a net weight of 160kg per barrel. 6.3 Transportation: The barrel cover must be tightly sealed during transportation to avoid leakage. 6.4 Storage: Dodecanol should be stored in a dry and ventilated warehouse. The storage period is 1 year from the date of leaving the factory. 6
Additional instructions:
HG/T2310-92
This standard was 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 technical jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Wuxi Chemical Industry Group Corporation. The main drafters of this standard are Gong Fuying, Feng Jing, Tan Xiangzhen, Zhang Hongguang and Cheng Xiaoming.5mg polyethylene glycol-20M is dissolved in a beaker, 100mL chloroform is added to dissolve, 25g of carrier is added, and after a little stirring, it is dried under an infrared lamp or dried naturally. c Filling method:
Plug the outlet end of the chromatographic column (the end connected to the detector) with a little glass wool, evacuate the outlet end, and load about 20g of the stationary phase under gentle vibration, fill evenly and tightly, and then plug it with glass wool. d. Aging of chromatographic column
HG/T2310—92
Put the filled chromatographic column into the chromatographic column box, check the air tightness, pass nitrogen, gradually heat to 210℃, and age at 210℃ for more than 8h until the baseline is stable.
4.6.2.3 Injector: micro glass syringe. 4.6.2.4 Chromatographic data processor: recorder or integrator. 4.6.3 Analysis steps
4.6.3.1 Adjust the instrument
Adjust the instrument according to the following reference conditions:
Vaporization chamber temperature: 250℃;
Detection chamber temperature: 250℃;
Column box temperature: 170℃;
Nitrogen flow rate: 25~30ml/min;
Hydrogen flow rate: 25~30ml/min;
f. Air flow rate: 500ml/min;
gInjection volume: 0.02~0.1μl.
4.6.3.2 Calibration method: Corrected area normalization method. 4.6.3.3 Test: Adjust the instrument according to the above provisions. After the baseline is stable, use a micro glass syringe to inject the sample and use the chromatograph recorder or integrator to process and calculate the data according to the corrected area normalization method. 4.6.4 Calculation of analysis results
4.6.4.1 For each component X1, expressed as mass percentage, calculate according to formula (4): A,f
wherein, X, one-to-one corresponds to the content of component i, when X, is Xc12 alcohol represents purity, %; A corresponds to the chromatographic peak area of component i;
corresponds to the quantitative correction factor of the chromatographic peak of the component. The arithmetic mean of two parallel determinations is taken as the result. 4.6.4.2 Correction factor is calculated according to formula (5): fw
wherein: f—mass correction factor;
f's(w)
A, W, As, W. One is the peak area and mass of the analyte and the known chromatographic pure standard, respectively. 4.6.5 Allowable difference
The difference between two parallel determinations shall not be greater than 0.5%. 4.6.6 Detection limit
The minimum detection concentration is 0.05%.
（5）
W.bzsoso.coI4
4.7 Determination of alkane content
HG/T2310-92
C12 alcohol chromatogram
1—C1o alcohol; 2—C14 alkane; 3—C12 alcohol; 4—C16 alkane The sum of the contents of each carbon chain alkane component in the sample is the alkane content. Follow the provisions of 4.6.1 to 4.6.4.2 in the purity determination method. 4.7.1 Allowable difference
The difference between two parallel determination values shall not be greater than 0.3%. 5 Inspection rules
5.1 Dodecanol shall be inspected by the quality inspection department of the manufacturer, and the manufacturer shall ensure that each batch of dodecanol shipped from the factory meets the requirements of this standard.
5.2 The user has the right to inspect and accept dodecanol in accordance with the provisions of this standard. 5.3 Each batch of products leaving the factory shall be accompanied by a quality certificate, which includes: manufacturer name, product name, grade, production date, batch number, net weight, proof that the product quality complies with this standard and the number of this standard. 5.4 Sampling shall be carried out in accordance with the provisions of GB6678, and the total amount of samples shall not be less than 500g. 5.5 Melt and mix the samples taken; put equal amounts into two clean and dry bottles with ground stoppers, and paste labels on the bottles, indicating the manufacturer name, product name, grade, batch number and sampling date. One bottle is for inspection and the other bottle is kept for two months for future reference. 5.6 If one of the indicators in the test results does not meet the requirements of this standard, dodecanol should be taken from twice the amount of packaging containers for re-testing. Even if only one indicator in the re-test results 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 objections to the product quality, they can negotiate to resolve the issue, or conduct arbitration in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection".
6 Marking, packaging, transportation and purchase and storage
6.1 Marking: The packaging container of dodecanol should have obvious and firm markings, including: manufacturer name, product name, trademark, production date, grade, batch number, net weight, and this standard number. 6.2 Packaging: Dodecanol should be packed in firm, dry, clean galvanized barrels or aluminum barrels, with a net weight of 160kg per barrel. 6.3 Transportation: The barrel cover must be tightly sealed during transportation to avoid leakage. 6.4 Storage: Dodecanol should be stored in a dry and ventilated warehouse. The storage period is 1 year from the date of leaving the factory. 6
Additional instructions:
HG/T2310-92
This standard was 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 technical jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Wuxi Chemical Industry Group Corporation. The main drafters of this standard are Gong Fuying, Feng Jing, Tan Xiangzhen, Zhang Hongguang and Cheng Xiaoming.5 Melt and mix the sample; put equal amounts into two clean and dry bottles with ground stoppers, paste labels on the bottles, indicate the manufacturer name, product name, grade, batch number and sampling date, one bottle for inspection, and the other bottle for two months for reference. 5.6 If one of the indicators in the inspection results does not meet the requirements of this standard, dodecanol should be re-tested from twice the amount of packaging containers. Even if only one indicator in the re-test results does not meet the requirements of this standard, the entire batch of products is unqualified. 5.7 When the supply and demand parties have objections to the product quality, they can negotiate to resolve the issue, or conduct arbitration in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection".
6 Marking, packaging, transportation and storage
6.1 Marking: The packaging container of dodecanol should have obvious and firm markings, including: manufacturer name, product name, trademark, production date, grade, batch number, net weight, and this standard number. 6.2 Packaging: Dodecanol should be packed into firm, dry and clean galvanized barrels or aluminum barrels, with a net weight of 160kg per barrel. 6.3 Transportation: The barrel cover must be tightly sealed during transportation to prevent leakage. 6.4 Storage: Dodecanol should be stored in a dry and ventilated warehouse. The storage period is 1 year from the date of leaving the factory. 6
Additional instructions:
HG/T2310—92
This standard was 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 technical jurisdiction of the Beijing Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by Wuxi Chemical Industry Group Corporation. The main drafters of this standard are Gong Fuying, Feng Jing, Tan Xiangzhen, Zhang Hongguang and Cheng Xiaoming. 75 Melt and mix the sample; put equal amounts into two clean and dry bottles with ground stoppers, paste labels on the bottles, indicate the manufacturer name, product name, grade, batch number and sampling date, one bottle for inspection, and the other bottle for two months for reference. 5.6 If one of the indicators in the inspection results does not meet the requirements of this standard, dodecanol should be re-tested from twice the amount of packaging containers. Even if only one indicator in the re-test results does not meet the requirements of this standard, the entire batch of products is unqualified. 5.7 When the supply and demand parties have objections to the product quality, they can negotiate to resolve it, or conduct arbitration in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection".
6 Marking, packaging, transportation and storage
6.1 Marking: The packaging container of dodecanol should have obvious and firm markings, including: manufacturer name, product name, trademark, production date, grade, batch number, net weight, and this standard number. 6.2 Packaging: Dodecanol should be packed into firm, dry and clean galvanized barrels or aluminum barrels, with a net weight of 160kg per barrel. 6.3 Transportation: The barrel cover must be tightly sealed during transportation to prevent leakage. 6.4 Storage: Dodecanol should be stored in a dry and ventilated warehouse. The storage period is 1 year from the date of leaving the factory. 6
Additional instructions:
HG/T2310—92
This standard was 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 technical jurisdiction of the Beijing Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by Wuxi Chemical Industry Group Corporation. The main drafters of this standard are Gong Fuying, Feng Jing, Tan Xiangzhen, Zhang Hongguang and Cheng Xiaoming. 7
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