JB/T 4392-1999 Method for determination of properties of water-soluble quenching medium for organic matter
Some standard content:
ICS25.200
J36
JB
Mechanical Industry Standard of the People's Republic of China
JB/T4392-1999
Water-soluble quenching medium for organic matter||tt| |Performance measurement method
Test method of characteristics on polymer quenchants1999-06-24 released
National Machinery Industry Bureau
Released
Implemented on 2000-01-01||tt ||JB/T4392—1999
Foreword
This standard is a revision of JB4392--87 "Method for determination of water solubility rate of organic matter and fire medium properties". Since the two standards GB1666-81 "Method for Determination of Specific Gravity of Plasticizers" and GB2954-82 "Method for Determination of pH Value of Synthetic Latex" have been invalidated, the relevant technical content in the original standards has been removed during the revision, and the relevant regulations have been Editorial changes have been made to the original standard, and the main technical content has not changed. This standard has replaced JB4392-87 since its implementation. This standard was proposed and centralized by the National Heat Treatment Standardization Technical Committee. The organization responsible for drafting this standard: Beijing Mechanical and Electrical Research Institute. The responsible drafters of this standard: Yang Shufan and Malan. This standard was first published on May 22, 1987. 1 Scope
Machinery Industry Standard of the People's Republic of China
Water-soluble quenching medium of organic matter
Performance determination method
Test method of characteristics on polymer quenchants This standard specifies the water-soluble quenching medium of organic matter Method for determination of fire media properties. This standard is applicable to the determination of the water solubility rate of organic matter and the technical performance of fire media. 2 Referenced standards
JB/T4392-1999
replaces JB4392-87
The provisions contained in the following standards constitute provisions of this standard by being quoted in this standard. At the time of publication, the editions indicated were valid. All standards are subject to revision and parties using this standard should explore the possibility of using the latest version of the standard listed below. GB/T1723-1993 Coating viscosity determination method GB/T1725--1979 Coating solid content determination 3 Appearance determination method
Visually inspect the appearance quality of the sample at room temperature (20~35℃). 3.1 Instruments and equipment
a) Glass measuring barrel: 500mL:
b) Mercury thermometer: 0~100℃ (or 0~50℃), graduation is 1℃; c) Beaker (or pond) Porcelain cup): greater than 500mL (containing test samples). 3.2 Measurement steps
3.2.1 Slowly pour the sample in the beaker into a dry and clean measuring barrel. 3.2.2 Place the graduated side of the measuring barrel towards the back (the non-scaled side facing forward), and perform visual inspection under normal light. Look at the scale line of the measuring barrel through the sample. If you can see it, it is transparent or translucent, and observe the purity of the sample. There should be no mixed substances such as turbidity and suspended matter. 3.2.3 Record the measured temperature at that time and the observation results as specified in 3.2.2. 4. Solid content determination method
The ratio of the weight of the material obtained after heating and drying the sample under certain temperature conditions to the weight of the sample, expressed as a percentage. This method is formulated with reference to GB/T1725-1979 Group 29. 4.1 Instruments and equipment
a) Balance: Sensitivity is 0.0001g (i.e. 0.1mg) b) Mercury thermometer: 0-200℃, graduation is 1℃; c) Weighing bottle: diameter 40mm, height 25mm ; Or a weighing bottle similar to this specification; d) Air blast constant temperature oven.
National Machinery Industry Bureau approved 2000-01-01 implementation on June 24, 1999
4.2 Measurement steps
JB/T4392—1999
4.2.1 Clean first Dry the weighing bottle in an oven at (100±2)℃ for 30 minutes, take it out and put it in a glass dryer to cool to room temperature, then weigh it on the balance. bZxz.net
4.2.2 Pour 1~1.5g sample into the weighing bottle, let the sample flow evenly across the bottom of the container, tightly cover the bottle cap, and weigh it on the balance. 4.2.3 Open the bottle Cap, put the bottle into a constant temperature drying oven, keep it at 100~110°C for 2.5 hours, take out the bottle, tightly cap it, place it in a dryer, cool to room temperature, and then weigh it on a balance. 4.3 Calculation method
Solid content , g;
W.—weight of sample and container after drying, g; W weight of sample and container before drying, g.
x100%
(1)
Take the average of the two samples as the test result. The relative error of the two samples should not be greater than 3%; if it is greater than 3%, a second repeat test should be performed.
5 Density (or specific quantity) determination method
5.1 Instruments and equipment
a) Precision density meter (precision hydrometer): graduation is 0.001; b) Mercury thermometer: 0~ 100℃, the graduation is 1℃; c) Glass measuring cylinder: 500mL;
d) Constant temperature water bath: Control the thermometer to have a graduation of 1℃. 5.2 Measurement steps
5.2.1 After adjusting the sample temperature to 20°C, pour about 500mL into a dry and clean glass measuring cylinder along the glass rod. Hold the upper end of a dry and clean density meter (hydrometer) and slowly place it into a bubble-free sample. After it is still, read the reading at the contact point between the lowest point of the liquid surface concave and the hydrometer (the line of sight and the lowest point of the liquid level must be at the same level when reading), and read accurately to 0.001. 5.2.2 Make the measuring barrel horizontal, and the density meter ( Hydrometer) should not touch the inside wall of the measuring barrel. 5.2.3 Record the liquid temperature during the test. The standard temperature during measurement is (20±1)°C. 6 Viscosity determination method
6.1 Method A
This method is formulated with reference to the GB/T1723-1993 Group 29 Zhongtu-1 viscometer method. Using the Tu-1 viscometer, expressed in s, the time required for a certain amount of sample to flow out from a hole of a specified diameter at a certain temperature when the outflow volume is 50mL is used as the measured conditional viscosity value (s). Tu-1 viscometer is used to measure the water solubility rate of organic substances and fire media with a viscosity value of not less than 20s.
6.1.1 Instruments and Equipment
a) Tu-! Viscometer (QND-1));
b) Mercury thermometer: 0~50℃, graduation is 1℃; c) Stopwatch: graduation is 0.1s;
d) Bearing bottle: 50mL measuring cup.
6.1.2 Measurement steps
JB/T4392—1999
6.1.2.1 The inside of the viscometer must be cleaned before measurement. Wipe the inside of the viscometer clean with gauze, and dry it in the air or use cold air. Blow dry; observe the viscometer leakage tip against the light and it should be clean. Then place the viscometer in the water bath cover and insert the stopper. 6.1.2.2 Stir the sample larger than 100mL evenly, adjust the sample temperature to (25±1)°C, then pour the sample into the viscometer, and adjust the horizontal screw to make the liquid level coincide with the marking line. 6.1.2.3 In order to allow the bubbles in the sample to escape, it should be kept still for a moment, then cover the lid and insert a thermometer. Adjust the water bath temperature to keep the sample crystal at (25±1).
6.1.2.4 Place a 50mL beaker (with a score line) under the viscometer leak. When the sample temperature meets the requirements, quickly lift the stopper. When the sample flows from the leak to the bottom of the cup, immediately start the stopwatch. When the sample in the cup reaches the 50mL mark, stop the stopwatch immediately, and the time (s) required for the sample to flow into 50mL of the cup is the conditional viscosity value of the sample. The difference between two measured values ??for the same batch of samples should not be greater than 3% of the average value. 6.2 Method B
This method uses a rolling falling ball viscometer to measure the viscosity of the water-soluble rate fire medium of organic matter at different temperatures. The measurement results are expressed in terms of dynamic viscosity\. When measuring the viscosity of the sample, the free falling time of the ball should be no less than 30 seconds. 6.2.1 Test equipment
a) Rolling ball viscometer RN50-1;
b) Super thermostat: the maximum temperature difference of the constant temperature field is 0.01℃ c) Stopwatch: the graduation value is 0.1s ;
d) Physical level: graduation value is 0.1g:
e) Webster balance;
f) Hair dryer;
g) Absolute ethanol .
6.2.2 Measurement steps
6.2.2.1 Place the instrument on the experimental platform, and then adjust the horizontal screw so that the water bubble in the level is located in the center circle 6.2.2.2 Temperature adjustment: The constant-temperature water in the constant-temperature space is supplied through the circulation of the super thermostat. The inlet and outlet water pipes are connected to the inlet and outlet liquid pipes of the super thermostat respectively, and the magnetic amplitude of the contact thermometer on the super thermostat is adjusted according to the required temperature. 6.2.2.3 Selection of test balls: The instrument is equipped with a total of five test balls, which are numbered 1, 2, 3, 4, and 5 according to their diameters. Among them, No. 1 to 4 are glass balls and No. 5 is a steel ball. . The density and constant of each ball are provided in the instrument instruction manual. 6.2.2.4 Before starting the experiment, the measuring tube, test ball, funnel plug, stopper, and gasket must be dry and oil-free (wash with absolute ethanol before testing, and then blow dry. However, the hair dryer cannot blow hot air onto the level) 6.2. 2.5 Inject the sample along the inner wall of the measuring tube, and the liquid level should be about 15mm lower than the top of the measuring tube. Use test ball pliers to gently clamp the selected test ball into the measurement tube, put the funnel stopper on, and then screw on the measurement tube cap (there should be no bubbles in the measurement tube), wait until the temperature of the constant temperature space reaches the measurement requirement temperature ±1 ℃, keep it at constant temperature for 15~30min before measurement. 6.2.2.6 Determine the falling time of the test ball: Put the viscometer in the working position (note that the head of the positioning shaft is inserted into the shaft seat and tightly sealed). When the test ball drops to the annular measuring line m, start the stopwatch. When it reaches the measurement line m, stop timing. Record the time when the test ball falls (at the moment of starting and stopping the stopwatch, the circular measurement lines should overlap front and back when observing). Then rotate the viscometer body 180°, let the test ball fall 3
JB/T4392-1999
to the top of the measurement tube, and then return the body to the working state for another measurement. , do it three times in total, and take the average of the three times. 6.2.3 Calculation of viscosity
Calculate the viscosity according to formula (2):
n=K(pP.)T
where: ——
- of the sample Dynamic viscosity, Pa·s
K——-Test ball constant,
mPa-s
g/cm\.s
P——-Sample density, g /cm';
p—density of test ball, g/cm;
T—average time of test ball falling, 5.
Acidity and alkalinity pH value determination method
The pH value of the sample at (23±1)℃.
(2)
Dip a strip of precision test paper (gradation of 0.5) into the sample to be measured, take it out after 0.5 seconds and compare it with the standard color plate to get the pH value. 8 Refractive index measurement method
8.1 Measurement principle
According to the different propagation speeds of light in different media, the refractive index is also different. Through the determination of the refractive index of water-soluble organic matter media , the concentration range of the sample can be measured. 8.2 Instruments and equipment
a) Abbe refractometer;
b) Super thermostat: The maximum temperature difference of the constant temperature field is 0.01°C. 8.3 Measurement steps
8.3.1 The refractometer should be calibrated before starting the measurement. The refractive index of water at 20℃ is 1.3330; a standard glass block can also be used for calibration. 8.3.2 Before starting the measurement, the light correction mirror and refractor should be wiped clean with ethanol to avoid leaving other substances that may affect the measurement accuracy. 8.3.3 The refractometer should be placed in a place with sufficient light, and constant temperature water should be passed through it to keep the calibration mirror at a constant temperature. Use a dripping filter tube to add the sample to the frosted surface of the light calibration mirror, making sure it is evenly distributed without bubbles and fills the field of view. Turn the prism locking handle and hold for several minutes. Adjust the knob of the calibration lens to separate the field of view into light and dark parts. Turn the compensator to eliminate the rainbow and make the dividing line between light and dark clear and align it on the cross line. Record the reading according to the scale scale. The reading should be accurate to the third decimal place, and the fourth place is an estimate. Alternately align the dividing line at the intersection of the crosshairs from one side and then the other, and repeat observing and recording the readings three times. The difference between each reading should not be greater than 0.0005, and the average of the readings is the refractive index of the sample. 9 Conductivity measurement method
9.1 Measurement principle
Utilizes the water solubility rate of organic matter at the same temperature and different concentrations. The ions in the fire medium sample have different conductive capabilities under the action of the electric field, that is Different conductivities can be used to measure the concentration range of the sample. 9.2 Instruments and equipment
a) Conductivity meter: the basic error is less than or equal to 1.5%; b) Super thermostat: the maximum temperature difference of the constant temperature field is 0.01℃; c) Several 100mL beakers;
d) DJS -1 platinum black electrode:
e) distilled water.
9.3 Measurement steps
JB/T 43921999
9.3.1 Before measuring, observe whether the meter needle points to zero, and adjust the screw on the meter head to make the meter needle point to zero. 9.3.2 After turning on the power, turn on the power switch and let it warm up for a few minutes until the pointer is completely stable. 9.3.3 Select the range switch to the required measurement range. If the conductivity of the sample is not known in advance, the range switch must be selected to the maximum conductivity measurement range, and then lowered step by step. 9.3.4 Clamp the electrode with an electrode clamp and fix it on the electrode rod. 9.3.5 Insert the electrode plug into the electrode socket, tighten the fastening screw on the socket, and then immerse the electrode into the beaker containing the sample. 9.3.6 Turn the calibration regulator to make the indication full (the electrode plug should be inserted into the electrode socket during calibration). 9.3.7 Turn the switch to the "measuring plate". The indication number at this time multiplied by the multiple of the range switch is the actual conductivity of the sample. 9.3.8 After the measurement, wash the electrode with distilled water for reuse next time. 10 Method for determination of cooling curve of dilute solution of water-soluble quenching medium of organic matter This method is suitable for the determination of the cooling capacity of dilute solution (water dropability rate of organic matter). The first stage of the supply state of the fire medium is a concentrated liquid. When used, it can be released into falling liquid of different concentrations according to process needs. ) 10.1 Silver probe thermocouple method
Install the silver probe equipped with the thermocouple on an appropriate heat-resistant steel pipe support rod, heat it to 800°C with a tubular resistance furnace, hold it for a few minutes, and then put it into the Measure the sample (the time should not exceed 1 s). Make sure the probe is located in the middle of the container. The drop in temperature of the probe is reflected by the thermocouple installed in the center. Connect it to the specified recorder and record the temperature/time curve. and speed/temperature curve. 10.2 Devices and tools
The measuring device adopts a quenching medium cooling rate tester, including an automatic operating system composed of a tubular resistance furnace for heating, a sample container, instruments for recording and data processing, and electrical devices. 10.2.1 Heating electric furnace
tubular resistance furnace (without controlled atmosphere). The heating furnace body should maintain a uniform temperature in the heating zone within a length of 100mm. The probe should be located in the middle of the heating zone, and the temperature fluctuation range of the probe should not exceed ±2°C. 10.2.2 The test probe
can be composed of a Φ20mm spherical or cylindrical silver probe body of a certain specification (purity is 99.9%) and a thermocouple installed in the center.
a) The thermocouple is a nickel-chromium-silica electric heating wire. Its hot contact should be located at the geometric center of the probe, and the cooling point should be 0℃: b) The available outer diameter of the thermocouple support tube is Φ10mm and the wall thickness is 1mm. The length of the stainless steel tube should be no less than twice the length of the furnace, and the thermocouple should be insulated from the support tube:
c) The thermocouple should be firmly fixed at the center of the silver probe; d) The silver operating head and support The pipes are connected together with threads or special fastening nuts and fixed on the bracket of the heating device. 10.2.3 Recorder
A recording instrument with a full-scale amplitude of 250mm, a full-scale time of 0.6s, a TY function recorder for temperature/time, an XY function recorder for speed and temperature, an indication accuracy of 0.5%, and a measurement sensitivity of 1%. JB/T4392—1999
10.2.4 Thermocouple temperature indicator is 0~1300℃, and the reading accuracy is 0.5%. 10.2.5 Container for media samples
1000mL beaker for chemical analysis.
10.3 Operation sequence
10.3.1 Place 1000mL sample in the container, stir and heat on the heater to the specified temperature, then place it under the tubular resistance furnace and adjust the placement position to ensure that the probe falls into the sample being measured, and the lower end of the probe rod is 15~20mm away from the liquid surface. 10.3.2 The silver probe is heated to (800±2)℃ in the resistance furnace, and then maintained for 3~5 minutes. Stop heating, and check that the TY and XY instruments should be in normal operation. When the sample is stationary, the switch is turned on, and the probe is automatically put into the container. At the same time, the instrument records the temperature, time, and speed/temperature curve.
10.4 Correction of the device
10.4.1 The potential of the nickel-chromium-nickel silicon thermocouple is calibrated with a platinum-platinum blunt standard thermocouple, and the error should be within the allowable range before use. 10.4.2 For the new probe, use distilled water as the standard liquid and repeatedly measure its sensitivity and repeatability. The difference in seconds from 800 to 400°C should not be greater than 0.5s
10.4.3. Probe repair method
After every five curves are measured, the surface of the probe should be lightly rubbed with No. 800~1000 gold steel sandpaper to show its luster. When the repaired probe cannot correctly represent the cooling curve, it should be stopped from use.
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