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1CS 13. 300
National Standard of the People's Republic of China
GB/T28111—2011
Test method of ester emulsifier for emulsion explosive2011-12-30Issued
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of ChinaStandardization Administration of the People's Republic of China
2012-08-01Implementation
This standard was drafted in accordance with the rules of CB/T1.1-2009. This standard was proposed and managed by the National Technical Committee for the Administration of Dangerous Chemicals (SAC/TC251). GB/T28111—2011
The drafting units of this standard are the Quality and Technical Supervision Bureau of Tanbei City, Anhui Province, and the Institute of Blasting Technology of the China Coal Research Institute. The main drafters of this standard are: Ting Hai, Wang Jiwen, Wang Jifeng, Zhang Guangfeng, Song Jialiang, Xia Bin, Zheng Zhensheng. TTKANYKAcA
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Test methods for ester emulsifiers for emulsion explosives GB/T 28111—2011
This standard specifies the sample preparation and appearance, acid value, saponification value, hydroxyl value, moisture and kinematic viscosity test methods for ester emulsifiers for emulsion explosives.
This standard is applicable to the test of ester emulsifiers for emulsion explosives. 2 Normative references
The following documents are indispensable for the application of this document. For all dated references, only the dated version applies to this document. For all undated references, the latest version (including all amendments) applies to this document. GB/T601 Preparation of standard titration solution for chemical reagents GB/T1884 Laboratory determination of density of crude oil and liquid petroleum products (densitometer method) GB/T3143 Color determination of liquid chemical products (Hazen unit - platinum-cobalt color number) GB/T8170 Numerical rounding rules and expression and determination of limit values 3 Sample preparation
Stir the sample (warm if necessary) with a stainless steel stirrer and take 500 samples from it for test. 4 Appearance test
4.1 Instruments and equipment
4.1.1 Colorimetric tube: 25 mL.
4.1.2 Constant temperature water bath.
4.1.3 Glass cone: 10 mm.
4.2 Test procedure
4.2.1 Take 20 mL of emulsifier, put it in a colorimetric tube, and warm it in a water bath at 50°C and 5°C for 10 min. Remove and drain the water outside the colorimetric tube. Observe visually under natural light and record the observed phenomena. 4.2.2 Insert the glass into the emulsifier liquid surface at a depth of 5 cm, lift the glass and drop it to 0.4 m above the liquid surface, so that the emulsifier flows down, observe the flow condition visually and record the observed phenomena. 4.3 Conclusion
Report the observed phenomena of the sample (whether it is uniformly transparent, without suspended particles and foreign matter, and whether it is a uniform thin strip when flowing down). 1
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GB/T 28111-—2011
5 Acid value (A) test
5.1 Titration method
5.1.1 Principle
Use phenolic acid as an indicator and titrate with standard sodium hydroxide solution to calculate the number of potassium hydroxide points required to neutralize 1 part of the emulsifier. This method is applicable to the determination of single-type ester emulsifiers. 5.1.2 Instruments and reagents
5.1.2.1 Analytical balance: accuracy 0.1mg. 5.1.2.2 Dimensional flask: 250mL.
5.1.2.3 Burette: 25mL, basic type.
5.1.2.4 Sodium hydride standard solution: 0.1mol/1., prepared and calibrated according to the provisions of GB/T601. 5.1.2.5 Phenolic acid: 10g/L 95% ethanol (volume fraction) solution. 5.1.2.6 Neutral ethanol: Take an appropriate amount of 95% (volume fraction) ethanol, add a few drops of phenol (add 4 drops per 200mL) as an indicator, and neutralize with hydroxide standard solution (5.1.2.4) until it turns pink. 5.1.3 Test procedure
Weigh about 10g of the emulsifier sample into a conical flask, add 100mL of neutral ethanol, and shake to dissolve the sample completely (warm it if necessary). Add 4 to 5 drops of phenol and titrate with sodium hydroxide standard solution until it turns pink. 5.1.4 Result expression
The acid value of the sample is calculated according to formula (1):
Where:
A_VXeX56.1
The acid value of the sample, in milligrams per gram (mg/g), calculated as potassium hydroxide: The volume of sodium hydroxide standard solution consumed in the titration, in milliliters (m=): The concentration of the sodium hydroxide solution, in moles per liter (rmol/L); 56.1
The molar mass of sodium hydroxide, in grams per mole (g/mol): 2
The mass of the sample, in grams ().
The calculation result shall be retained to one decimal place, and the data processing shall be carried out in accordance with the requirements of B/T 8170. The arithmetic mean of the two test results shall be taken as the test result.
5.1.5 Repeatability
The difference between the two test results of the same sample and the same analyst shall not be greater than 2.5% of the average value. 5.1.6 Reproducibility
The difference between the results of the same sample measured in two different laboratories shall not be greater than 6.5% of the average value. 5.2 Potentiometric titration
5.2.1 Principle
Using the pH electrode as the indicator, titrate with standard potassium hydroxide isopropanol solution to the endpoint potential, and calculate the acid value of the sample according to the volume of potassium hydroxide solution consumed.
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This method is applicable to the determination of composite ester emulsifiers. 5.2.2 Instruments and reagents
5.2.2.1 Potentiometric titrator: accuracy not less than ±10mV. 5.2.2.2 Glass electrode,
5.2.2.3 Glycerol electrode,
5.2.2.4 Analytical balance: accuracy 0.1mg. Full set tube: 25mL,
5.2. 2. 5
5. 2. 2. 8
Beaker: 50mL100mL.
Volume flask: 500tnL.
Isol: analytical grade.
Ethyl acetate: analytical grade,
5. 2. 2. 9
5, 2. 2. 10
5. 2. 2. 11
5. 2. 2. 12
Ethanol: 5% (volume fraction),
GE/T28111--2011
pH 9. 18 Standard buffer solution: weigh 1. 90 & borax (reference reagent), dilute to 500 mL volumetric flask with distilled water. Potassium hydroxide isopropanol solution: 0.1mol/L. Weigh 3.0% potassium hydroxide and add it to 500mL isopropanol, boil slightly for 10 min, let stand for 48 h, take the supernatant, store in a reagent bottle, seal and store, calibrate according to the provisions of GB/T 601. 5.2.3 Instrument calibration
Instrument calibration is carried out according to the following steps:
Assume that the instrument is connected to the power supply for 301i, adjust the temperature
Pour an appropriate amount of standard buffer solution into the burning standard, put it in the electric field, and stir it positively: c) Adjust the temperature compensator to the actual temperature of the liquid, press the reading switch, and adjust the calibrator to make the indicated value 9.18 d) Press the reading switch again, the indicated value should be correct, and the calibration is completed. 5.2.4 Test procedure
The test is carried out according to the following steps:
Turn on the instrument and preheat for 30min, adjust the dew point: weigh about 10g of emulsifier sample into a conical flask, add 100mL of acetaldehyde, shake to dissolve the sample completely (warm it if necessary) b)
and add a small amount of ethyl acetate;
c) Turn on the stirrer for titration. At the beginning, control the titration speed to about 0.2mL/min, and continue until each drop is 0 .1mI. When the potential value changes by 30mV, reduce the titration speed to 0.05mL/min, and stop when the end potential is reached. d) Rinse the electrode with alcohol water, wipe it dry, and record the reading of the burette; perform a blank test using 100mL of ethanol as blank according to the above procedure. e
5.2.5 Result expression
The acid value of the sample is calculated according to formula (2):
A=-V)XGX56. 1
A\-the acid value of the sample (in terms of potassium hydride). The unit is milligram per gram (mg/g). --·The volume of potassium oxychloride dissolved in alcohol consumed in the titration, the unit is milliK (m)V.
The volume of potassium hydroxide isopropanol solution consumed in the blank test, in liters (mL): TTTKANYKACA
GB/T 28111—2011
The concentration of potassium hydroxide isopropanol solution, in moles per liter (mo1/L) 56.1——The molar mass of potassium hydroxide, in grams per mole (g/mo1>; -The mass of the sample, in grams (g).
The result of the calculation shall be retained to one decimal place, and the data shall be processed in accordance with the requirements of GB/T8170. The arithmetic mean of the two test results shall be taken as the test result.
5.2.6 Reproducibility
The difference between the two determination results of the same sample and the same analyst shall not be greater than 8.5% of the average value. 5.2.7 Reproducibility
|For the same sample, the difference between the results obtained in two different laboratories should not be greater than 18.9% of the average value. 6 Saponification value (X) test
6.1 Principle
Sodium hydroxide in ethanol reacts with the ester group in the sample, and then the remaining alkali is neutralized with standard hydrochloric acid solution. The saponification value of the sample is calculated from the difference in the volume of acid consumed by the blank and the sample. 6.2 Instruments and reagents
6.2.1 Analytical balance: accuracy 0.1mB.
6.2.2 Plate balance accuracy 0.5g.
6.2.3 Conical flask: 250ml.a
6. 2. 4 Burette: 25 mL, knocking type
6. 2.5 Pipette: 25 mL.
6.2.6 Spherical condenser: outer tube length 300 mm, 6.2.7 Ethanol: 95% (volume fraction)
6.2.B Sodium hydroxide ethanol solution: 0.5 mol/L, weigh 24 g of sodium hydroxide, add appropriate amount of ethanol to dissolve and release to 1000 mL. Place in a rubber stopper glass bottle and let stand for 24 hours, then pour the upper clear liquid into a glass bottle and seal it for storage. 6.2.9 Hydrochloric acid standard solution: analytical grade, concentration 0.5 01/L. Prepare and calibrate according to the provisions of GB/T601. 6.3 Test procedure
The test is carried out according to the following steps:
Weigh 2. 5 g of sample (accurate to 0.000 1 g) Add the conical flask. b) Use a pipette to accurately add 25 mL of sodium hydroxide ethanol solution, install a condenser, heat to a slight boil in a constant temperature water bath, and reflux for 30 minutes.
Rinse the inside of the condenser tube and the lower part of the part connected to the conical flask (including the stopper) with about 20 mL of ethanol, add 3 to 5 drops of phenol, and titrate with standard hydrochloric acid solution while it is hot until the pink color just disappears + heat to zero. If the solution turns pink again, titrate again until the pink color fades.
d) Carry out a blank test according to the above procedure.
6.4 Expression of results
The saponification value of the sample is calculated according to formula (3):
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Wherein:
X=(Vo-V)xe×56.1
The saponification value of the sample (calculated as potassium hydroxide), the unit is gram per gram (mg/g): The volume of the acid standard dissolved sugar consumed in the blank test, the unit is milliliter (mL): The concentration of the acid solution, the unit is mole per liter (mal/IL); 56.1--the molar mass of potassium hydroxide, the unit is gram per mole (g/mo1); n
The mass of the sample, the unit is gram (α).
GB/T 28111--2011
The calculation result shall retain - decimal places, and the data shall be processed in accordance with the requirements of GB/T8170. The arithmetic mean of the two test results shall be taken as the test result.
6.5 Repeatability
The difference between the results of the same sample and the same analyst should not be greater than 0.7% of the average value. 6.6 Reproducibility
The difference between the results of two opposite samples measured in two different laboratories should not be greater than 2.9% of the average value. 7 Hydroxyl Value () Test - Acetic Anhydride Method
7.1 Principle
The hydroxyl groups in the sample are esterified with acetic anhydride pyridine solution, and then the excess acetic anhydride is hydrolyzed and neutralized and titrated with sodium hydroxide standard solution. The hydroxyl value of the sample is calculated by the difference between the volume of sodium hydroxide dissolved in the blank and the volume of sodium hydroxide dissolved in the sample. 7.2 Instruments and Reagents
7.2.1 Analytical Balance: Accuracy 0.1 mg: 7.2.2 Conical flask: 250 mL, with ground joint, clean and dry before use. 7.2.3 Burette: 50 mL, basic type.
7.2.4 Pipette: one with a capacity of 15 mL and one with a capacity of 25 mL. 7.2.5 Spherical condenser: outer tube length 300 mm, with ground joint, clean and dry before use. 7.2.6 Pyridine: local temperature is 114.5 ℃ ~115.5 ℃. 7.2.7 Acetic anhydride: content not less than 97%, analytical grade. Acetic anhydride pyridine solution: mix 1 volume of acetic anhydride with 10 volumes of pyridine under cooling, store in a brown glass bottle with a ground stopper 7.2.8
, store in a sealed container, and measure the color of the solution with platinum diamond according to GR/T3113. If the color of the solution exceeds 200 Haze 5 units, it cannot be used. 7.2.9 Sodium hydroxide solution: 0.5 mol/L, prepared and calibrated according to the provisions of GB/T601 7.2.10 Phenolic acid: 10 g/L, 95% ethanol (volume fraction) solution. 7.3 Test procedure
The operation should be carried out in a ventilated room, and the waste should meet the discharge standards. The test is carried out in the following steps:
a) Weigh about 1.6 of the sample into a conical bottle with dry media: b) Carefully transfer 15 mL of acetic anhydride pyridine solution into the conical bottle, wet the joint of the condenser with pyridine and connect it to the conical bottle. Swirl to mix the contents of the bottle evenly. S
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GB/T 28111-2011
Heat the conical flask in a boiling water bath for 1 hour, shake and mix for 1 minute every 10 minutes or so, the contents of the flask should be below the water surface, add 2 mL of water into the conical flask through the condenser and shake and mix. Heat in a boiling water bath for 5 minutes. d)
Take out the conical flask together with the condenser and cool it to below 30°C. Add 70 mL of water through the condenser, remove the cold tube, and rinse the ground glass joint with water.
Pipette 25 mL of sodium hydroxide solution into the conical flask, add 4 drops of phenolic acid indicator, shake quickly, and use sodium hydroxide standard solution to determine until pink. The end point is that it does not fade for 15 minutes. According to the above procedure, replace the sample with 2 to 3 drops of water to make a blank test. g
7.4 Result Expression
The hydroxyl value of the sample is calculated according to formula (4):
Wherein:
I_(VV)XcX56. 1+A
…Hydroxy value of the sample (in terms of group oxide), in milligrams per gram (mz/g) V.
The volume of sodium hydroxide standard solution consumed in the blank test, in milliliters (nI); The volume of sodium hydroxide standard solution consumed in the sample, in liters (tmI): The concentration of standard sodium hydroxide solution, in moles per liter (mot/I); The molar mass of potassium hydroxide, in grams per mole (g/mal): The mass of the sample, in grams (g)
-…The acid value of the sample, in grams per gram (m), calculated as potassium hydroxide (4)
The calculation result is retained to one decimal place. The data processing is carried out in accordance with the requirements of CB/18170. The arithmetic half-mean of the two test results is taken as the test result.
7.5 Repeatability
The difference between the two determination results of the same sample and the same analyst should not be greater than 1.4% of the average value. 7.6 Reproducibility
The difference between the results of the same sample in two different experiments shall not exceed 3.7% of the average value. 8 Water (w) test - azeotropic distillation method
8.1 Principle
The water in the sample forms an azeotrope with formaldehyde and is distilled out. After the oil and water are separated, the volume of water is read and the water content is calculated.
8.2 Instruments and reagents
8.2.1 Analytical balance: accuracy 0.1mg.
8.2.2 Moisture analyzer: flask volume 500mL, condenser length 250mm~300mm, with ground joint 8.2.3 Electric heating jacket or oil bath.
8.2.4 Toluene: analytical grade, treated according to method F before use: add 2 liters of water to every 100mL of toluene, distill, cut off the azeotrope formed by the distillation head water and toluene, and then collect the formaldehyde fraction for testing. 8.3 Test procedure
The operation should be carried out in a fume hood, and the waste should be discharged in compliance with the standards. 6
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The test is carried out in the following steps:
a) Weigh about 50g of the sample, put it into a flask, and add 250mL~300mL of toluene. b) Connect the moisture receiver and condenser, and pass cooling water. GB/T281112011
Heat the flask with an electric heating jacket or oil bath to reflux the contents of the flask until the toluene outflow in the receiver disappears (2 or 3 drops per second) and no water separates from the surface: stop heating. d) Wait for the receiver to cool to room temperature, and read the reading after the water in the receiving tube is clearly separated, and read accurately to 0.02 mL. 8.4 Expression of results
The moisture content of the sample is expressed in %, and is calculated according to formula (5): wexy
Wherein:
The mass fraction of water in the sample, %,
—Density of water, take 1, unit is gram per cubic centimeter (g/cmn): V——·Volume of water in the receiver, unit is milliliter (mL); -Mass of the sample, unit is gram ().
The calculation result shall be retained to one decimal place, and the data processing shall be carried out in accordance with the requirements of (B/T8170). The arithmetic mean of the two test results shall be taken as the test result.
8.5 Reproducibility
For the same sample, the difference between the results obtained by the same analyst in two different laboratories shall not be greater than 0.9 of the average value.8.6 Reproducibility
For the same sample, the difference between the results obtained in two different laboratories shall not be greater than 1.3 of the average value.9 Kinematic viscosity (v)
9.1 Principle
At a constant temperature, first determine the dynamic viscosity of the sample, and then convert it to its kinematic viscosity at the same temperature.9.2 Instrument
9.2.1 The measurement accuracy of the viscometer shall not be less than ±5%.9.2.2 Super thermostat: control accuracy ±0.1°C.9.2.3 Thermometer: accuracy 0.1°C.
9. 3 Test procedure
The test is carried out in the following steps:
Test preparation
Turn on the power supply of the viscometer, adjust to zero, and start the thermostat to keep the temperature constant at the specified temperature. Determine the dynamic viscosity of the sample according to the requirements of the viscometer manual. If necessary, adjust the range so that the reading is 40% to 0% of the full volume difference: and determine the dynamic viscosity of the sample under this condition.
b) Determine the dynamic viscosity of the sample under the above determination conditions. c) The density β of the sample is determined according to GB/T 1884. TTKNTKACA
GB/T 28111—2011
Result Expression
The kinematic viscosity of the sample is calculated according to formula (6):
Where:
The kinematic viscosity of the sample, in units of square meters per second (m/s);——The dynamic viscosity of the sample, in units of Pascal seconds (Pa s); PThe density of the sample, in units of grams per cubic meter (kg/m\). 6)
The calculation result shall be rounded to three decimal places, and the data shall be processed in accordance with the requirements of GB/1 8170. The arithmetic mean of the two test results shall be taken as the test result.
9.5 Repeatability
For the same sample, the difference between the two test results of the same analyst shall not exceed 5.9% of the average value. 9.6
Reproducibility
The difference between the results of the same sample measured in two different laboratories shall not exceed 12.2% of the average value. 10
Test report
The test report shall include the following contents:
All information required for identification of the sample:
The method adopted;
The results obtained and the method of expression:
Test conditions;
Any operation not specified in this standard and any situation that may affect the results.
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