Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/T2545-93
Sixteen
Published on September 25, 1993
Ministry of Chemical Industry of the People's Republic of China
Implemented on July 1, 1994
W Chemical Industry Standard of the People's Republic of China
Subject Content and Scope of Application
HG/T2545-93
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage of hexadecanol. This standard applies to the production of hexadecanol from natural oils and fats through esterification and high-pressure hydrogenation to mixed fatty alcohols, and then through distillation. Molecular formula: CH(CHz)1CH2OH
Relative molecular mass: 242.45 (according to the international relative atomic mass in 1989) Reference standards
GB/T601
Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents Preparation of preparations and products used in chemical reagent test methods GB/T603
GB1250
GB3143
Expression and determination methods of limit values Color of liquid chemical products Colorimetric method (Hazen unit - platinum-cobalt color number)
GB/T6365
GB/T6678
GB/T6679
ZB/T17027
3 Technical requirements
Determination of free alkalinity and free acidity of surfactants Titration method General rules for sampling of chemical products
General rules for sampling of solid chemical products
Octadecanol
3.1 Appearance: White granular or flaky solid at room temperature. 3.2 The quality of hexadecanol shall meet the requirements of the following table: Item
Melting point, ℃
Melting color, (Hazen unit platinum-cobalt) Color number Acid value, mgKOH/g
Saponification value, mgKOH/g
Iodine value, gI/100g
Hydroxy value, mgKOH/g
Hexadecanol content, %
Alkanes, %
Approved as a superior product by the Ministry of Chemical Industry of the People's Republic of China on September 25, 1993
2 28~235
47.5~51.5
First-class products
225235
Qualified products
46.0~52.0
225~240
1994-07-01 implementation
W.4 Test method
HG/T2545—93
The reagents and water used in this standard shall be analytical reagents and distilled water or water of equivalent purity unless otherwise specified. The standard solution preparations and products used in this standard shall be prepared in accordance with the provisions of GB/T601 and GB/T603 unless otherwise specified.
4.1 Determination of Melting Point
4.1.1 Summary of Method
By heating, the sample in the melting point tube is gradually raised from a temperature lower than the initial melting temperature to the final melting temperature. The final melting temperature is visually observed to determine the melting point of the sample. 4.1.2 Instruments and Equipment
4.1.2.1 Melting Point Tube
A capillary tube made of neutral hard glass, sealed at one end, with an inner diameter of 0.9~1.1mm, a wall thickness of 0.10~0.15mm, and a length determined by the upper end being higher than the water bath liquid level after installation (about 100mm). 4.1.2.2 Thermometer
Mercury thermometer (GB514): 30~100℃, graduation value 0.2℃; 4.1.2.3 Tall beaker: 600mL;
4.1.2.4 Magnetic heating stirrer.
4.1.3 Melting point determination device
Figure 1 Melting point determination device
1—Magnetic heating stirrer, 2—Beaker; 3—Capillary; 4—Fixed clamp, 5—Thermometer4.1.4 Analysis steps
Grind the sample into the finest powder possible and put it into a clean and dry melting point tube. Take a dry glass tube about 800mm long and stand it upright on a glass plate. Drop the melting point tube containing the sample into it several times until the sample in the melting point tube shrinks to 2-3mm high, and start stirring and heating. When the temperature of the distilled water rises to about 10℃ lower than the specified melting point, use a rubber ring to attach the melting point tube containing the sample to the thermometer so that the sample end of the melting point tube is at the same level as the middle of the mercury ball. The mercury ball of the thermometer should be in the middle of the distilled water cup. Control the heating rate to about 1℃ per minute. The final temperature when the sample is completely melted is the melting point of hexadecanol. 4.1.5 Calculation of analysis results
HG/T254593
Take the arithmetic mean of the results of two parallel determinations as the determination result, and the difference between the two parallel determination results shall not be greater than 0.2℃. 4.2 Melting color determination
After the solid sample placed in a glass beaker is heated and melted in a water bath, proceed according to the provisions of GB3143 standard. 4.3 Determination of acid value
Perform according to the provisions of GB/T6365, titrate until the pink color does not fade for 30s. Take the arithmetic mean of the results of two parallel determinations as the determination result, and the difference between the two parallel determination results shall not be greater than 0. 01 mg KOH/g.
4.4 Determination of saponification value
4.4.1 Summary of method
Excess alkali neutralizes the acid in the sample and reacts with the esters in the sample for saponification. After the reaction is completed, the remaining alkali is neutralized with acid. 4.4.2 Reagents and solutions
4.4.2.1 Neutral anhydrous ethanol: neutralize with alkali until it is neutral to phenolphthalein. 4.4.2.2 Potassium hydroxide ethanol solution: 30g/L. 4.4.2.3 Standard hydrochloric acid titration solution: c(HC1)=0.5mol/L. 4.4.2.4 Phenol indicator solution: 10g/L.
4.4.3 Apparatus
4.4.3.1 Conical flask: 250mL (ground mouth, boron-free and alkali-resistant); 4.4.3.2 Water bath or hot plate.
4.4.4 Analysis steps
Weigh 5g of sample, accurate to 0.0002g, and place it in a ground-mouth conical flask. Use a pipette to take 25mL of potassium hydroxide ethanol solution, install a reflux condenser, and place it in a water bath. The water bath temperature should not be lower than 95℃. Heat and reflux for 1h. Rinse the condenser wall with 10mL 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 colorless end point. Perform a blank test at the same time.
4.4.5 Calculation of analysis results
The saponification value X (mgKOH/g) is calculated according to formula (1): X
(V.-V)·c1X0. 0561×1 000
(Vo-V)·ciX56.1
Where: V. —The volume of the standard hydrochloric acid solution consumed in the blank test, mL; V1—The volume of the standard hydrochloric acid solution consumed in the titration sample, mL; Ci——The actual concentration of the standard hydrochloric acid solution, mol/L; 0.0561-
(1)
—The mass of potassium hydroxide in grams equivalent to 1.00mL of the standard hydrochloric acid solution [c(HC1)=1.000mol/L);
m——The mass of the sample, g.
Take the arithmetic mean of the results of two parallel determinations as the determination result. The difference between the two parallel determination results shall not be greater than 0.3 mg KOH/g.
4.5 Determination of iodine value
4.5.1 Summary of the method
Excess iodine chloride reacts with the sample. After the reaction is completed, potassium iodide is added to precipitate iodine, and then titrated with a standard sodium thiosulfate solution.
4.5.2 Reagents and solutions
4.5.2.1 Carbon tetrachloride or chloroform;
4.5.2.2 Glacial acetic acid;
4.5.2.3 Potassium iodide solution: 150g/L;
HG/T2545-93
4.5.2.4 Iodine chloride glacial acetic acid solution (Wei's solution): 16.2g/L, dissolved in 16.2g iodine chloride in 1L glacial acetic acid. Or weigh 13g iodine and dissolve it in 1L glacial acetic acid, and pass dry chlorine gas until the solution changes from brown to orange-red. Before and after passing chlorine gas, calibrate according to blank determination. The number of milliliters consumed by 0.1mol/L sodium thiosulfate standard titrant should be twice the former, otherwise it needs to be adjusted.
4.5.2.5 Sodium thiosulfate standard titration solution: c (NazS20s) = 0.1 mol/L. 4.5.2.6 Starch indicator solution: 10 g/L.
4.5.3 Analysis steps
Weigh 5 g of sample accurately to 0.0002 g in an iodine volumetric flask, add 25 mL of carbon tetrachloride or chloroform to dissolve, and accurately transfer 25 mL of Wei's solution.0mL, cover the bottle stopper, seal the bottle mouth with potassium iodide solution, shake it slowly, and place it in the dark at room temperature for 1h. After taking it out, add 25mL potassium iodide solution and 50mL water, and titrate it with sodium thiosulfate standard titration solution until it turns light yellow, then add about 1mL starch indicator solution, and continue titrating until the blue disappears as the end point.
At the same time, perform a blank test.
4.5.4 Calculation of analysis results
The iodine value X2 (gl/100g) is calculated according to formula (2): X2 =V):cX0.126 9
(Vo-V)c2X12.69
Where: V. —The volume of sodium thiosulfate standard titration solution consumed in the blank test, mL; V2The volume of sodium thiosulfate standard titration solution consumed by the sample, mL; C2——The actual concentration of the sodium thiosulfate standard titration solution, mol/L; (2)
0.1269——The mass of iodine in grams equivalent to 1.00mL of sodium thiosulfate standard titration solution [c(NazS20s)=1.000mol/L);
——The mass of the sample, g.
The arithmetic mean of the results of two parallel determinations is taken as the determination result. The difference between the two determination results shall not be greater than 0.1gI/100g. 4.6 Determination of hydroxyl value
4.6.1 Summary of the method
Alcohol and excess acetylating agent react. After the reaction is completed, water is added to hydrolyze the remaining acetic anhydride, and then the generated acetic acid is neutralized with alkali.
4.6.2 Reagents and solutions
4.6.2.1 Neutral anhydrous ethanol: neutralize with alkali until it is neutral to phenolphthalein; 4.6.2.2 Acetylation reagent: anhydrous pyridine: acetic anhydride = 4 + 1 (freshly prepared); 4.6.2.3 Potassium hydroxide ethanol standard titration solution: c (KOH) = 0.5 mol/L. The preparation method of potassium hydroxide ethanol standard titration solution is shown in 4.4.2.2. Calibration method: weigh 3g of standard potassium hydrogen phthalate that has been dried to constant weight at 105-110℃, weigh to 0.0001g, dissolve in 80mL of carbon dioxide-free water, add 2 drops of phenolphthalein indicator solution, and titrate with the prepared potassium hydroxide ethanol standard titration solution until the solution turns pink. At the same time, perform a blank test and calculate the concentration of the potassium hydroxide ethanol standard titration solution according to the following formula. 4
HG/T2545—93
Cs-（V, -V)×0.2042
Wherein: Cs—
-Concentration of potassium hydroxide ethanol standard titration solution, mol/Lm
Mass of potassium hydrogen phthalate, g;
Vi——Amount of potassium hydroxide solution, mL, V2—Amount of potassium hydroxide solution used in blank test, mL;—Mass of potassium hydrogen phthalate expressed in grams equivalent to 1.00mL of potassium hydroxide standard titration solution [c(KOH）=1.000mol/L], g.
4.6.2.4 Phenol indicator solution: 10g/L.
4.6.3 Analysis steps
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 the funnel on the bottle mouth, put it into a 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 it to room temperature, add 2mL of water from the funnel mouth, shake it well, and then put it into a glycerol bath at 96-99℃, and heat to hydrolyze for 5min. Take it out and cool it 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 pink color lasts for 30s without fading as the end point. Perform a blank test at the same time.
4.6.4 Calculation of analysis results
The hydroxyl value X (mgKOH/g) is calculated according to formula (3): Xx = (V.-V) · cX0. 056 1X1000m
(Vo—Vs)cgX56.1
Wherein: V. is the volume of the standard potassium hydroxide ethanol titration solution consumed in the blank test, mLV: the volume of the standard potassium hydroxide ethanol titration solution consumed in the titration sample, mL; Cs is the concentration of the standard potassium hydroxide ethanol titration solution, mol/L; (3)
is the mass of potassium hydroxide expressed in grams equivalent to 1.00mL of the standard potassium hydroxide ethanol titration solution [c (KOH) = 1.000mol/L];
is the mass of potassium hydroxide expressed in grams equivalent to 0.0561—
of the standard potassium hydroxide ethanol titration solution;
is the mass of the sample, g.
The arithmetic mean of the results of two parallel determinations shall be taken as the determination result. The difference between the two parallel determination results shall not be greater than 3 mg KOH/g.
4.7 Determination of content
4.7.1 Reagents and materials
4.7.1.1 Carrier gas and auxiliary gas
Carrier gas: nitrogen or hydrogen, purity greater than 99.9%a.
Combustion gas: hydrogen, purity greater than 99.7%;
c. Combustion gas: secondary purified air.
4.7.1.2 Reagents and materials used in the preparation of chromatographic columnsa.
Stationary liquid: methyl silicone (SE-30) + polyethylene glycol-20M = 100 + 1. Carrier: 101 white silanized carrier: particle size 0.18 ~ 0.25mm (80 ~ 60 mesh), (produced by Shanghai Reagent Factory); c. Solvent: chloroform.
4.7.2 Instruments
4.7.2.1 Gas chromatograph
HG/T254593
Detector: hydrogen flame ionization detector, minimum detection concentration 0.05%. 4.7.2.2 Chromatographic column
a. Column: stainless steel tube or glass tube with inner diameter of 3.5~4.0mm and length of 2m. b. Filler: carrier: stationary liquid = 100:5 (mass ratio). Method of coating stationary liquid: weigh 1.25g methyl silicone (SE-30) and 12.5mg polyethylene glycol-20M in a beaker, add 100mL chloroform to dissolve, add 25g carrier, stir slightly, and dry under infrared lamp or dry naturally. c. Filling method: plug the outlet of the chromatographic column (connected to the detector) with a little glass wool, evacuate the outlet, and add about 20g of the stationary phase under gentle vibration. Fill evenly and tightly, and then plug it with glass wool. d. Aging of the chromatographic column: load the filled column into the chromatographic column box, check the air tightness, pass nitrogen, gradually heat to 210℃, and age at 210℃ for more than 8 hours until the baseline is stable. 4.7.2.3 Injector
Micro glass syringe.
4.7.2.4 Chromatographic data processor
Recorder or integrator.
4.7.3 Analysis steps
4.7.3.1 Adjust the instrument
Adjust the instrument according to the following reference conditions
Vaporization chamber temperature: 250~300℃;
Detection chamber temperature: 250~300℃;
Column box temperature: 180~200℃;
Nitrogen flow rate: 25~30mL/min;
Hydrogen flow rate: 25~30mL/min;
Air flow rate: 400mL/min;
Sample dilution: sample + solvent = 1+5,
Injection volume: 0.02~0.1μL.
4.7.3.2 Quantitative method
Modified area normalization method.
4.7.3.3 Test
Adjust the instrument according to the above reference conditions. 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 modified area normalization method.
4.7.4 Calculation of analysis results
4.7.4.1 For each component X, (%) is calculated according to formula (4): Xi
Ar·fL×100wwW.bzxz.Net
ZAt·f
·(4)
Where: X is the content of the corresponding component i. When X is Xel6, it represents the purity of hexadecanol. When X is X, it represents the alkane content; A is the area of the chromatographic peak corresponding to the component i; f is the quantitative correction factor of the chromatographic peak corresponding to the component i. 4.7.4.2 Quantitative correction factor: measured with known chromatographically pure samples, calculated according to formula (5): 6
W.bzsoso.coI Where: w is the weight correction factor,
HG/T2545-93
f'w)_A,·W
f's(w)A,W,
Ai, W1, As, W- are the peak areas and weights of the analyte and the known chromatographically pure standard respectively. The arithmetic mean of the results of two parallel determinations is taken as the determination result, and the difference between the two parallel determination results shall not exceed 0.5%. Figure 2 Chromatogram of Ci alcohol
1-Ci alcohol, 2-C alkane, 3-C alcohol, 4-C2 alkane, 5-C18 alcohol (5)
W.bzsoso.coI4.8 Determination of alkane content
HG/T2545-93
The sum of the contents of each carbon chain alkane component in the sample is the alkane content. The determination method is carried out in accordance with the provisions of 4.7.
4.8.1 Calculation of analysis results
The alkane content (%) corresponding to component i is calculated according to formula (4). The total alkane content (%) in the sample is calculated according to formula (6): XRH-
Where: X--total alkane content in the sample; XiRH-alkane content corresponding to component i in the sample. SXT
The arithmetic mean of the results of two parallel determinations is taken as the determination result. The difference between the results of two parallel determinations shall not be greater than 0.3%. 5 Inspection rules
5.1 This product is inspected by the quality supervision and inspection department of the manufacturer. The manufacturer shall ensure that the various technical indicators of the products leaving the factory meet the requirements of this product standard and attach a quality certificate in a certain format. The content of the quality certificate includes product name, product grade, product batch number, net weight, factory date and standard number. All technical indicators listed in this standard are type inspection items, among which melting point, melting color, acid value, saponification value, iodine value, content and alkane are factory inspection items. Under normal circumstances, type inspection shall be carried out at least once a month. 5.2 When leaving the factory, any number of the same grade is a batch. The sampling method shall be carried out in accordance with Articles 6.4 and 6.6 of GB/T6678, and the sampler shall be carried out in accordance with Article 2.2 of GB/T6679.
The total amount of the sample shall not be less than 500g. The selected samples shall be mixed and put into two clean and dry bottles with ground stoppers in equal amounts. Labels shall be affixed to the bottles. One bottle is for inspection and the other bottle is kept for one year for future reference. The content of the sample label includes: product name, batch number, grade, sampling date and sampler. 5.3 The test results shall be determined according to the GB1250 rounded value comparison method. If one of the test results does not meet the requirements of this standard, samples shall be taken from twice the amount of packaging for re-inspection. Even if only one of the re-inspection results does not meet the requirements of this standard, the entire batch of products shall be unqualified.
For products that have exceeded the storage period, the manufacturer shall conduct re-inspection according to the product standard requirements before leaving the factory. Only qualified re-inspection can leave the factory. 5.4 The user has the right to inspect and accept the product quality according to this standard. During the storage period, if the supply and demand parties have any objections to the product quality, they shall promptly raise them and resolve them through negotiation or ask the arbitration unit to conduct arbitration analysis. 6 Marking, packaging, transportation and storage
6.1 Each package shall be painted with a clear and firm mark of the manufacturer's name, product name, trademark, product grade, product batch number, production date, standard number, and product net weight.
6.2 The product shall be packed in a dry and clean woven bag lined with a plastic bag. The mouth of the inner plastic bag is sewn with the mouth of the woven bag, and the average net weight of each bag is 25±0.1kg.
6.3 Handle with care during transportation to avoid damage caused by collision with hard objects. 6.4 The product should be stored in a dry and ventilated warehouse. The storage period is 1 year from the date of leaving the factory. W.bzsoso.coIAdditional instructions:
HG/T2545—93
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, Zhang Hongguang, Yang Pushian, Cheng Xiaoming, and Zhu Xiufen. 9
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.