Guidance on the determination of physico-chemical properties of pesticides—Part 19：Boiling point
Some standard content:
ICS65.020
Agricultural Industry Standard of the People's Republic of China
NY/T1860.19—2010
Guidance on the dctermination of physico-chemical properties of pesticides Part 19:Boiling point
Published on May 20, 2010
Implemented on September 1, 2010
Published by the Ministry of Agriculture of the People's Republic of China
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NY/T1860 "Guidelines for the Determination of Physical and Chemical Properties of Table Pharmacology" is a series of standards, with a total of 22 parts: - Part 1 pH value:
Part 2: Acidity (alkalinity): bzxZ.net
-- Part 3: Appearance:
- Part 4: Qualitative properties of the original drug;
- Part 5: UV/visible absorption: · Part 6: Explosion;
- Part 7: Solubility in water
- Part 8: Octanol/water partition coefficient: --- Part 9 Part; Hydrolysis:
-· Part 10: Oxidation-reduction/chemical incompatibility-Part 11: Flash point;
-Part 12: Fire point;
-—· Part 13: Miscibility with non-polar organic solvents;-Part 14: Saturated vapor pressure;
-Part 15: Solid flammability;
Part 16: Corrosiveness to packaging materials;-Part 17: Density;
-Part 18: Specific rotation;
Part 19: Boiling point;
Part 20: Melting point;
-Part 21: Viscosity;
-Part 22: Solubility.
This part is Part 19 of the "Guidelines for the Determination of Physical and Chemical Properties of Pesticides". This part was proposed and approved by the Crop Management Department of the Ministry of Agriculture. This part was drafted by: Pesticide Control Institute of the Ministry of Agriculture and China Agricultural University. The main drafters of this part: Chen Tiechun, Wu Xuemin, Bo Rui, Xu Yan, and Zhu Shengxiang. http:
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NY/T1860.19—2010
1 Scope
Test methods for determination of physical and chemical properties of pesticides
Part 19: Boiling point
This part specifies the basic requirements for the test method and test report writing for the determination of boiling point of pesticides. This part is applicable to the determination of boiling point of pure pesticides and pesticide technical materials for the application of pesticide registration. 2 Normative references
NY/T1860.19—2010
The following documents are indispensable for the application of this article. For documents with a reference date, the version with a reference date does not apply to the documents. This is an undated document, the latest version of which (including all amendments) applies to this document. (GB/T616-2006 General method for determination of boiling range of chemical reagents (JSO) 6353-1:1982.NEQ) JG130 Working glass liquid thermometer
JG272 Empty box barometer Dog Empty box barometer
3 Requirements
The boiling point of pure pesticides and cooling drugs should be determined by appropriate methods: When the boiling point is between 0℃ and 300℃, GBT616-2006 or liquid bath capillary method can be used; when the boiling point is between 20℃ and 300℃, metal block capillary method can be used; when the boiling point is between 20℃ and 1000℃, differential thermal analyzer (TDA) can be used; when the boiling point is between 100℃ and 1000℃, differential scanning calorimeter (LSC) can be used. 4 Test method
4.1 Principle of the method
The boiling point of the sample is determined by measuring the boiling temperature when the sample temperature rises to the same level as that under one atmosphere. 4.2 GB/T616—2006 General method for determination of boiling range of chemical reagents 4.3 Liquid bath capillary method
4.3.1 Apparatus
4.3.1.1 Three-necked round-bottom flask: 500ml, main neck length about 230mm, 4.3.1.2 Sample tube, maximum outer diameter 5inm. 4.3.1.3 Capillary tube: about 100tmm long, inner diameter about 1mm, wall thickness 9.2tmm~0.3mm. 4.3.1.4 Rubber tube: with air outlet pin on the outside. 4.3.1.5 Measuring thermometer: internal standard single-bulb thermometer, graduation value 0.1℃. The range is suitable for the boiling point temperature of the sample to be measured. 4.3.1.6 Auxiliary thermometer: the graduation value is 1. 4.3.2 Instrument installation
As shown in Figure 1, connect the three-necked flask, sample tube, capillary tube and measuring hygrometer with rubber runners, the lower end of the measuring thermometer is 20mm away from the condensation surface of the test tube, and the middle of the mercury ball of the hygrometer is in contact with the end of the sample tube containing the sample. Attach the auxiliary thermometer to the measuring hygrometer, so that the mercury ball is about 40mm away from the mercury ball of the measuring thermometer. Inject about 1/2 of its volume of silicon dioxide into the flask. 4.3.3 Determination
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NY/T 1860.19—2010
Vent hole; D—temperature flask:-auxiliary thermometer; F—oil bath G—a test tube
flask, R
rubber stopper; C—
outer diameter 5mm, capillary band, about 1Dmm long, inner diameter about 1mm, thickness 0.2mm~0.3mmru1l-side tube.
Figure 1 Schematic diagram of boiling point determination device by liquid bath capillary method After the sample is dried and crushed, it is loaded into the capillary with the end melted, and the capillary is dropped in the capillary tube for about 700min to make it compact. After compaction, the sample height is about 3min, and the capillary with the melted capillary 1cm away from the lower end is inserted into the sample tube so that the wooden end is immersed below the liquid surface. When the bath liquid is heated up (about 3℃/min) to 10℃ lower than the expected boiling point under stirring, the capillary is inserted into the appropriate position and the heating rate is reduced to 1%/min. When it approaches the boiling point, bubbles will form quickly and continuously at the end of the capillary. When the bubbles suddenly disappear and the temperature at which the liquid surface rises in the capillary is the boiling point. Record the room temperature and air pressure at the same time. 4.3.4 Correction of the effect of air pressure on the boiling point of the sample When the positive pressure difference does not exceed 25kPa, the standard trace point is calculated according to formula (1): tu -1f×ap
Where:
—standard boiling point, in degrees Celsius (℃); the difference between standard pressure and ambient pressure, in Pascals (kPa); A
——the rate of change of boiling point with pressure, in degrees Celsius per ton of Pascal (℃/kPa)-boiling point, in degrees Celsius ().
4.3.5 Calculation of the correction value of the thermometer reading (1)
If the fully immersed thermometer is used for retrograde measurement, the part of the mercury column of the thermometer that is exposed outside the liquid should be corrected. The correction value of the part of the mercury column of the thermometer that is exposed outside the liquid is calculated according to formula (2): A = 0.000 16n X (t - tg)
Where:
Temperature correction value, in degrees Celsius (); ...The number of scales of the thermometer D that are submerged below the liquid surface; Machine-observed temperature, that is, the reading of the thermometer, in degrees Celsius (); Auxiliary thermometer temperature, that is, the reading on the thermometer, in degrees Celsius (). 2
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NY/T 1860. 19—2010
The temperature after correction in Article 4.3.4 is added to this correction value to obtain the boiling point of the sample, which is calculated according to formula (3): ts: : t - At + t
Where:
t,- --Boiling point, in degrees Celsius ():
t-Observed temperature, i.e. the reading of thermometer D, in degrees Celsius ((\):: --Overflow correction value, in degrees Celsius (℃): A-Variation of boiling point with air pressure, in degrees Celsius (℃) 4.4 Metal block capillary method
4.4.1 Instrument
The metal block capillary method boiling point determination device is shown in Figure 2, where. If the automatic determination method is adopted. Thermometer A can be replaced by a thermoelectric sensor, while the thermometer C uses a photoelectric sensor. 4.4.1.1 Metal heating block: The H part is empty, forming a small cavity. There are four small windows made of heat-resistant glass on the side of the small cavity wall, which are at right angles, A sun mirror is set up in front of one of the small windows. As shown in E in Figure 2. 4.4.1.2 Metal socket: There are 2 or more holes on it, which are used to place capillaries. As shown in G in Figure 2. 4.4.1.3 Adjustable power electrical heating system: It is composed of multiple adjustable resistors to adjust the heating rate. As shown in D in Figure 24.4.1.4 Capillary: About 100mm long, inner diameter about 1mm, wall thickness 0.2mm-~0.3nm. 4.4.1.5 Measuring piece thermometer: Internal standard single-ball thermometer, graduation value 0.1℃. The range is suitable for the boiling point temperature of the sample being measured. 4.4.1.6 Lamp: Use Ding to provide light source to observe the changes in the sample. A
A Hao Du Ji.4.4.2 Determination of the capillary tube: TF resistance: metal heating block; wick-metal insert. Figure 2 Schematic diagram of the boiling point determination device of the metal block capillary tube method The capillary tube is filled with the sample in the same way as in 4.3.3. When the metal heating block is heated to 10℃ lower than the expected boiling point at a rate of 3%/min, the capillary tube is inserted into the small chamber in the metal heating block, and the heating rate is reduced to 1℃/min. When it approaches the boiling point, the end of the capillary tube will bubble rapidly and continuously. When the bubble suddenly disappears, the temperature at which the liquid rises in the capillary tube is the boiling point. 4.5 Differential Thermal Analysis (DTA) Method 4.5.1 Principle of the Method The sample and the standard substance are heated or cooled according to the same temperature control program. By recording the temperature of the endothermic (gasification) peak when the sample undergoes phase transition on the temperature baseline, the boiling point is obtained. 4.5.2 Instrument
Differential thermal analyzer. Basic parameters:
Measuring range: 20℃~-1000℃;
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NY/T 1860.19—2010
Heating rate: 0℃/min~100%/min;
Accuracy: ±0.2℃,
4.5.3 Determination
Grind the sample and standard reference material to 100~~200℃, weigh appropriate amount of sample and reference material and put them into the sample furnace, heat or cool according to the same temperature control program, and the program temperature rise (fall) is preferably 10℃/min~15%/min. When the sample undergoes a phase transition, its change will cause an endothermic (melting) or exothermic (condensation) drop on the temperature recording baseline. The temperature at which the peak appears is the boiling point of the sample. 4.6 Differential Scanning Calorimetry (DSC) Method
4.6.1 Principle of the Method
The sample and the standard substance are heated according to the same temperature control program. By recording the energy baseline, when the sample undergoes a phase transition, the temperature at which the change causes an endothermic (vaporization) peak is the boiling point. 4.6.2 Instrument
Differential Scanning Calorimeter, basic parameters:
Range: 2 000μV;
Measurement range: -100℃1000%;
Heating rate: 1℃/min~30℃/min;
Accuracy: ±0.2℃.
4.6.3 Determination
Heat the test object and the standard substance according to the same temperature control procedure. The energy required to maintain the same temperature of the test object and the reference object will be different when the test object undergoes mechanical transformation. The entropy of the phase transformation will cause an endothermic (gasification) peak on the energy input baseline. Record the temperature corresponding to the peak value, which is the temperature of the test object. boiling point. 5 Test report
The report should provide sufficient details, including at least the following: 1) Sample description: It should include the name, purity, specification, batch number, source, and production period of the pesticide sample to be tested. The characteristics of the sample packaging/sealing system should be clearly stated, such as the type, shape and color of the packaging material. 2) Test conditions: It should include ambient temperature, pressure, reagents, bath liquid, instruments, etc. 3) Test method: The test method used should be described. 4) Test results: It should include the test results
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NY/T 1860.19-2010
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People's Republic of China
Standards for the packaging industry
Test Guidelines for the Determination of Physical and Chemical Properties of Pesticides
Part 19: Boiling Point
NY:T 1860.19 -2070
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