Some standard content:
National Standard of the People's Republic of China
Fatty alkyl trimethyl tertiary amines
Fatty alkyl dimethyl tertiary amines1Subject content and scope of application
CB/r15045---94
This standard specifies the classification, technical requirements, test methods, inspection rules and labeling, packaging, transportation and storage conditions of fatty alkyl dimethyl tertiary amines.
This standard applies to fatty alkyl dimethyl tertiary amines (N,N-dimethyl tertiary amines) prepared from fatty alcohols or fatty acids. This standard does not apply to fatty alkyl dimethyl amines prepared from carbonyl alcohols. The applicable tertiary amines are mainly used to prepare cationic surfactants, zwitterionic surfactants and nonionic surfactants. 2 Reference standards
GB5177.1 Rounding rules for the determination of alkylbenzene in the industry
GB 8170
3 Product classification
3.1 Structural formula
3.2 Classification and code
-12～C alkyl)
Fatty alkyl dimethyl amine is divided into six specifications according to the number of carbon atoms in the fatty alkyl group and the main component. Specifications and codes are as follows: Dialkyl dimethyl amine -
-12DMA
f: -/ -Tetraalkyl dimethyl tertiary amine ~ -12/14DMA -Hexaalkyl dimethyl tertiary amine
Octanealkyl dimethyl tertiary amine
-16DMA
Hexadecyl dimethyl amine (C16 is more than Cl.) Octadecadecyl dimethyl amine (Cis is more than Ce) Note: Products other than these six specifications are self-designed by the manufacturer. 3.3 Marking
16/18DMA
-18/16DMA
Product marking example:
Hexadecyl dimethyl tertiary amine is the main - hexadecyl dimethyl tertiary amine is the superior grade marked as \ tertiary amine 16/18DMA superior grade GB/T 15015\.
4 Technical requirements
The physical and chemical indicators of fatty alkyl dimethyl amine shall conform to the requirements of Table 1, approved by the State Bureau of Technical Supervision on April 12, 1994
Implementation on December 1, 1994
Color, Hazen
Amine content, %
Amine value
mgKOH/g
Primary and secondary amine content
Cir+CiAbzxz.net
Color, Hazen
Amine content, %
Amine value
mgKUH/g
Polyamine content
Main fraction"
Cra-Cu
Ca+Cua
Superior product
CB/r 15045-- 94
Table 1. Physical and chemical indicators of fatty alkyl dimethyl tertiary amine
First-class product
Qualified product
Colorless and transparentColorless to slightly poor
Light yellow and transparent
Transparent liquid
255~263
250263
Superior product
12/14[3MA
Colorless to yellow
Colorless and transparent
Transparent liquid
224-263
Qualified product
250~26 240~-260
221---260
Superior product
Colorless and transparent
202-~208
Superior product
First-class product
Qualified product
Superior product
First-class product
Light yellow transparent colorless and slightly yellow
Colorless~light yellow
Colorless and slightly yellow
Transparent liquid
198--208
177-~208
16/18DMA
First-class product
Colorless~slightly yellow Color~light yellow
195~206
190~206
Qualified product
190~210
1H3-189
179--189
Superior product
18/16DMA
Special color~slightly colorless~lightly felt
185195
150--155
Qualified product
161-189
Qualified product
175--195
5 Test method
GB/T 15045 94
In analysis, unless otherwise specified, analytically pure reagents and distilled water (conforming to the third-grade water in GB6682) should be used. 5.1 Determination of appearance
First measure the color and state of the sample in the sample bottle. 5.2 Determination of color
According to the procedure specified in GB5177.1, measure the absorbance of the platinum cobalt color standard and the molten tertiary amine sample at a wavelength of 373nm. 5.3 Determination of fatty alkyl methylamine content and amine value - 5.3.1 Principle
Titration method (arbitration method)
Add acetic anhydride to the fatty alkyl methylamine sample to acetylate the primary and secondary amines present, and then use a standard isopropanol-ethanol solution of hydrochloric acid for non-aqueous titration to measure the tertiary amine content and tertiary amine value. Reaction formula:
Amine RNH:+
5. 3.2 Reagents
-N+-H!
+CH,000H
+CH,CUOH
Hydrochloric acid (GB622), e(HCI)=D.2mol/Lisolanol-Z, alcohol standard solution: acetic anhydride (GR 677)!
Isol (HG/T 31167);
Ethylene glycol.
5.3.3 Instruments
Precision acidity meter, graduation ≤ 0.05pH, equipped with glass electrode (such as type 231) and calomel electrode (such as type 232) or composite electrode; a.
Electromagnetic stirrer with a stirring rod wrapped in polytetrafluoroethylene; microburette, graduation 0.02ml, 5ml. 1.Beaker, 50.
Graduating cylinder, 50ml.
Test procedure
Weigh 0.2ml of the melted mixed sample (accurate to 0.1m) into a 50mL beaker, slowly add 10ml of acetic anhydride (if solid matter appears in the sample, it needs to be heated and melted on a warm electric stove), mix well, and place it at room temperature for 15min. Then add 30mL of isopropanol solution, put it on a stirrer, immerse the calibrated glass electrode and calomel electrode of the titrator into the liquid, turn on the electromagnetic stirrer and adjust the speed appropriately, use the hydrochloric acid isoflurane glycol standard solution (5.3.2) for potentiometric titration, draw the titration curve, take the maximum jump of the potential value as the integral point, and record the corresponding volume (V,).
5.3.5 Calculation of test results
GB/T15045—
The tertiary amine content (X,) is expressed as mass percentage and calculated according to formula (1). The amine value (T) of the amine is expressed as milligram potassium hydroxide per gram (mgKOH/g) and calculated according to formula (2).
T=YG.X 56.1
Wherein: V-
is the volume of hydrochloric acid standard solution consumed in titrating the sample, mL; the concentration of hydrochloric acid standard solution, mol/l;
1——mass of the sample>t
M——molar mass of tertiary amine (determined according to 5.4), g/mol56.1-molar mass of potassium hydroxide (KOH), mg/rmmol. The average value of the parallel determination results is taken as the result, and the value is retained to the unit place. 5.3.6 The difference in the content of amine between two parallel determination results should not be greater than 0.7%, and the difference in the value of tertiary amine should not be less than 1.5mgK()H/g. 5.4 Determination of the content, average relative molecular weight and relative components of fatty alkyl dimethyl tertiary amines 5.4.1 Principle
Gas-liquid chromatography
· (2)
The sample is separated by gas-liquid chromatography with a packed column. The amine content, average relative molecular weight and relative components are calculated from the peak area of the obtained chromatogram. 5.4.2 Reagents
Ether (GB12591)
b. Anhydrous ethanol (GB678);
c. Methane (GB 682);
Reference sample: fatty alkyl dimethyl tertiary amines of known chain length. A product of known composition can be used as a reference sample to test the performance of the chromatogram:
Carrier gas: nitrogen;
f. Fuel gas: hydrogen:
Combustion gas air, supplied by cylinder gas or air compressor. 5. 4.3 Instruments
Chromatographic instrument with flame ionization detector and programmed temperature riser: a.
Chromatographic column,The column tube is made of stainless steel or glass double column, with a length of 0.5~～1.5 m, an inner diameter of 2~4 mm, and a carrier of Chiranusorh WAW DMCS or 405 silanized white carrier with a particle size of 150~180 μm, coated with 5%~~10% potassium hydroxide and 5%~10% Apiezon grease (Apiezon 1.), and pre-aging is required for 5~~10 h before the experiment. The chromatographic peaks of different carbon chain fatty alkyl dimethyl amines are required to be well separated!
Data processing machine or electronic integrator;
Recorder:
Syringe, 5 or 10μL.
5.4.4 Experimental procedure
Setting of chromatographic analysis conditions
Column temperature: The program temperature is used, the initial temperature is 90~120℃. The heating rate is 4~6℃/min, and the final temperature is 270~290℃! Injection port temperature 290~320C;
Carrier gas flow rate: about 50ml/min
d. Gas flow rate: about 50mL/min;
e. Oxygen-supporting gas base: about 500mL/min.
5.4.4.2 Chromatographic analysis
GB/T 15045-94
Use a syringe to inject a sufficient amount of sample into the chromatograph to obtain a chromatogram with appropriate peak height. Qualitative analysis: Under the same operating conditions, the chromatographic peak of the sample is qualitatively analyzed according to the retention time of the reference tertiary amine chromatographic peak! a.
Finition: When the chromatographic peaks of each carbon chain fetal aliphatic alkyl dimethyl tertiary amine are well separated, the peak area normalization method is used for analysis. b.
5.4.5 Calculation of test results
5.4.5.1 The mass fraction (B,) of each carbon chain fatty alkyl dimethyl tertiary amine is calculated according to formula (3): 4×100
Wherein: 3,——the mass percentage of carbon chain fatty alkyl dimethyl tertiary amine; A,—the peak area of carbon chain fatty alkyl methyl tertiary amine; A—the sum of the peak areas of each chain fatty alkyl dimethyl tertiary amine and non-tertiary amine. 5.4.5.2 The content of fatty alkyl dimethyl tertiary amine (X,) is expressed as mass percentage and calculated according to formula (4): X, = ER.
5. 4.5. 3 The average relative molecular weight (M,) of fatty alkyl dimethyl tertiary amine is calculated according to formula (5): M,
Wherein: M,—the theoretical relative molecular weight of carbon chain fatty alkyl monomethyl tertiary amine, and the values of M are shown in Table 2.
Table 2 Theoretical composition of fatty alkyl dimethyl tertiary amines of various carbon chains Fatty alkyl carbon number
(3))
(4)
(5)
157.3171.3185.3199.4213.4227.4241.5255.5269.5283.5197.6311,6325,65.4.5.4 The main component of fatty alkyl dimethyl tertiary amine is expressed by the mass percentage of the soil component (B). The average value of the parallel determination results is taken as the result, and the value is retained to the unit place. 5.4.6 Precision
The difference between the average relative molecular weight of the parallel determination results of fatty alkyl dimethyl tertiary amine should not exceed 1; the difference between the parallel determination results of the total amount of tertiary amine and the main component should not exceed 0.7% respectively.
5.5 Determination of primary and secondary amine content
5.5.1 Principle
Add salicylaldehyde to the mixed amines. The primary amine reacts with salicylaldehyde to form salicylaldehyde. Compared with secondary and tertiary amines, it is a very weak amine. Therefore, the mixture is titrated in a non-aqueous solvent with standard hydrochloric acid to measure the sum of the amine values of the secondary and tertiary amines. Subtract the amine value of the secondary amine measured in 5.3 from this amine value to obtain the secondary amine value, and the secondary amine content can be calculated. Subtract the sum of the amine values of the secondary and tertiary amines from the total amine value to obtain the primary amine value, and the primary amine content can be calculated. 5.5.2 Reagents
In addition to those listed in 5.3.2, add salicylaldehyde. 5.5.3 Instruments
As listed in 5.3.3.
5.5.4 Test procedure
GB/T 15045—94
Weigh 0.20.3g of melted and mixed sample (accurate to 0.1mg) in a 50ml beaker, add 30mL isopropanol, 5mL salicylaldehyde, put in a stirring sample, stir thoroughly, place at room temperature for 30min, then use hydrochloric acid isopropanol-ethylene glycol standard solution (5.3.2a) for potentiometric titration, draw the titration curve, take the maximum potential jump as the end point, and record the corresponding volume (V,). Use the same procedure, but without adding salicylaldehyde, to measure the volume (V,) of the hydrochloric acid standard solution consumed by the total amine. 5.5.5 Calculation of test results
The amine values of secondary and tertiary amines (S,) are calculated according to formula (6); the total rubber value (S) is calculated according to formula (7). The secondary amine content (X) and primary amine content (X,) are expressed as mass fractions and calculated according to formulas (8) and (9) respectively. S.=Yaci X 56.1
S, = Yaci × 56. 1
(Sr-T)× M
(S, -S,) X M.
56. 1 × 10
..........( 6 )
.+..( 8)
Wherein: M, M1-- are the molar masses of secondary amine and primary amine respectively (obtained by subtracting 14 and 28 from the molar mass of tertiary amine measured in accordance with 5.4 respectively), g/mol,
are the total amine value, (secondary and tertiary) amine value and tertiary amine value respectively, mgKOH/g; L: V--
is the volume of the hydrochloric acid standard solution consumed for titrating the total amine, mL; t.. the concentration of the hydrochloric acid standard solution mol/L; m.-. the mass of the sample used for determining the secondary amine and tertiary amine values; m.-- is the mass of the sample used for determining the total amine value, &56.1-- is the millimolar mass of potassium hydroxide (KOH), nig/mmol. The average value of two equal determinations is taken as the result, and the value is rounded to the unit. 6 Inspection rules
6.1 Inspection classification
6.1. 1 The tertiary amine content, primary amine content and color value specified in Chapter 1 are the factory inspection items. All factory inspection items must be inspected when the product is delivered for acceptance and inspected by the quality supervision agency. The manufacturer should ensure that all fatty alkyl dimethyl tertiary amine products shipped meet all technical requirements of this standard.
6. 1.2 Type inspection
All technical requirements and indicators specified in this standard shall be inspected in the following situations: a.
When there are changes or abnormalities in the production process, equipment, materials, and catalysts: b. When the quality supervision agency or the user unit proposes a type inspection requirement: c. Normal production should be subject to type inspection every three months. 6.2 Batching and sampling rules
GB/T15045-94
6.2.1 Fatty alkyl methyl amines are delivered and sampled in batches, and products of the same type, specification, and batch number delivered at one time constitute a delivery batch.
6.2.2 Products must pass the factory inspection and be issued with a certificate of conformity before they can leave the factory. The receiving department shall accept the goods based on the certificate of conformity and may, if necessary, be inspected according to 6. 2. 3 Sampling acceptance.
6.2.3 Sampling
Determine the sample size according to the batch size according to Table 3, and randomly select sample barrels from the batch. Table 3
Batch size (number of barrels)
51~150
151~500
Batch size (number of barrels)
Use a dry and clean sampling tube with a diameter of about 15mm, insert it to the 5/6 depth of each sample barrel to extract equal amounts of samples, and the total sample size shall not be less than 1.5kg.
6.2.4 Mix the selected samples carefully and put them into three clean, dry brown bottles respectively. The product name, specifications, markings, batch number, and sampling date should be indicated on the sealed labels. The delivery parties shall each hold one copy for inspection, and the third copy shall be kept by the delivery party for arbitration inspection. 6.3 Judgment rules
The test result data shall first be rounded to the same effective digit as the technical requirement value in accordance with the provisions of GB8170, and then compared with the plate limit value specified in the technical requirements to determine whether the test batch of products is qualified or unqualified. If one indicator in the test result does not meet the standard, it shall be re-tested from the double-volume sample barrel A. If the re-test result is still unqualified, the batch of products shall be judged as unqualified.
If the two parties to the delivery cannot reach an agreement due to different test results, they may ask the arbitration institution for arbitration, and the result shall be the final basis. 7 Marking, packaging, transportation and storage
7.1 The outer wall of the packaging barrel shall be marked with paint or self-adhesive label paper, and the pattern and text shall be clear and correct. Indicate: product name, product specifications, grade, manufacturer, production date, batch number, net weight, and flammable mark. 7.2 Fatty alkyl and methyl tertiary amines shall be packaged in containers that are not corrosive and can ensure strength. 7.3. During the shipment, the products should be handled with care and avoid collision. The loading and unloading personnel should wear labor protection articles to avoid skin burns. 7.4 Fatty alkyl mono-tertiary amines are inflammable, so they should be stored in a well-ventilated warehouse, avoid exposure to the sun, and stay away from fire sources. Under the specified packaging and transportation conditions, the product shelf life is one year. Additional remarks:
This standard is proposed by China Light Industry General Association.
This standard is under the jurisdiction of the National Surfactant Detergent Standardization Center. This standard was drafted by the Daily Chemical Industry Science Research Institute of the Ministry of Light Industry. The main drafters of this standard are Yao Yao, Peng Xianqun, and Zhu Chuanjia.
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