CN102253168A - Method and apparatus for producing mercury vapor with standard concentration - Google Patents
Method and apparatus for producing mercury vapor with standard concentration Download PDFInfo
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- CN102253168A CN102253168A CN2011101004129A CN201110100412A CN102253168A CN 102253168 A CN102253168 A CN 102253168A CN 2011101004129 A CN2011101004129 A CN 2011101004129A CN 201110100412 A CN201110100412 A CN 201110100412A CN 102253168 A CN102253168 A CN 102253168A
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Abstract
The invention discloses a method and an apparatus for producing mercury vapor with a standard concentration. The method comprises steps that a sample cell is vacuumized, added with liquid mercury or amalgam, and sealed; the sample cell is heated or cooled; a mercury vapor pressure in the sample cell is changed with the temperature, and pressure and temperature of the mercury vapor are detected by a pressure gauge; a mercury saturated vapor pressure is obtained from a mercury vapor saturated pressure and temperature parallel table according to the detected pressure and temperature; then a mercury saturated vapor concentration is obtained by calculating according to a formula; and mercury vapor with a standard concentration is obtained. A mercury vapor generator for calibration comprises a pressure gauge, a thermometer, a sample cell, refrigeration and heating equipment, liquid mercury or amalgam, and transparent quartz window. The invention has beneficial effects that the mercury vapor concentration is controlled by adjusting temperature, and the liquid mercury and the amalgam are all sealed in the sample cell, so as to avoid discharge to generate environment pollution, and simplify a structure of a current mercury vapor generator for environment monitoring calibration and an exhaust-gas treatment system.
Description
Technical field
The present invention relates to a kind of method and device thereof that produces the normal concentration mercury vapour.
Background technology
Coal-burning power plants etc. use coal in a large number and give off heavy metal-mercury.Mercury has very big harm to environment and human body, for monitoring the concentration of the mercury that discharges in the coal-fired flue-gas, existing many measuring methods and standard.Many surveying instruments have been developed on this basis.These instruments in use all need to calibrate and demarcate.Calibrating and demarcating mercury vapour measurement of concetration instrument produces normal concentration often with the mercury generator mercury vapour.At present the principle of mercury generator commonly used is that the heating liquid mercury produces mercury vapour, dilutes with the zero gas of accurate Control Flow then and carries mercury vapour carries out instrument to the calibration sample pond demarcation and calibration.Because mercury vapour is poisonous, must handle used mercurous zero gas, could discharge behind the mercury in absorption zero gas.So not only make instrument very complicated, also may produce pollution.It is necessary to develop a kind of not polluting the environment, and can change mercury vapour concentration as required, produce the method for normal concentration mercury vapour by mercury generator simple in structure.
Summary of the invention
The objective of the invention is provides a kind of and need not add method and the device thereof that liquid mercury produces the normal concentration mercury vapour at the surveying instrument timing signal in order to overcome the shortcoming that existing mercury takes place, to reduce and to eliminate mercury vapour and discharge the pollution that causes.
Ultimate principle of the present invention: in the airtight vacuum container that has liquid mercury or amalgam to exist, the space of vacuum tank can be full of the mercury vapour that is in state of saturation.The pressure of mercury vapour changes with the temperature variation of sample cell, and temperature raises, and the pressure of mercury vapour will correspondingly raise.The saturation temperature of mercury vapour saturation pressure correspondence can find from many documents, corresponding certain temperature has the saturation pressure and the temperature table of comparisons (seeing attached list: " the mercury vapour saturation pressure and the temperature table of comparisons ") of certain mercury saturated pressure mercury vapour, and certain temperature obtains corresponding mercury vapour saturation pressure value; And the saturation temperature of different mercury is corresponding different from mg/m
3Mercury vapour concentration for unit.Following formula has provided the relation that obtains mercury vapour concentration according to the mercury vapour saturation temperature:
Here ρ is a mercury vapour density, and M is the atomic weight of mercury, equals 200.59, and P is the mercury saturation vapour pressure, and Z is a compressibility factor, is less than or equal to 1, and R is a gas law constant, and T is a kelvin rating.
Therefore, the temperature of control sample cell just can obtain different mercury vapour concentration, for Calibration of measuring equipment provides standard.
Based on above-mentioned inventive principle, technical scheme of the present invention is: a kind of method that produces the normal concentration mercury vapour is characterized in that its concrete steps are:
1) earlier sample cell is vacuumized, add liquid mercury or amalgam then, sample cell is sealed fully again, the liquid mercury or the mercury in the amalgam that are in the sealed sample pond can part evaporate, and form mercury vapour in the space of sample cell;
2) by refrigerating and heating combined equipment sample cell is heated or cooling, along with the sample cell temperature variation, the mercury vapor pressure in the sample cell changes thereupon, and the pressure and temperature of mercury vapour is recorded by pressometer and temperature gauge,
From " the mercury vapour saturation pressure and the temperature table of comparisons ", obtain the saturated vapor pressure of mercury, basis then according to this measuring pressure and temperature
ρ is a mercury saturated vapor concentration in the formula, M is the atomic weight of mercury, equal 200.59, P is the mercury saturation vapour pressure, and Z is a compressibility factor, be less than or equal to 1, R is a gas law constant, and T is a kelvin rating, by the temperature of refrigerating and heating combined equipment to sample cell heating or cooling control sample cell, obtain different mercury saturated vapor concentration, for Calibration of measuring equipment provides the normal concentration mercury vapour.
Realize the device of the method for above-mentioned generation normal concentration mercury vapour, it is a kind of demarcation mercury vapour generator, be characterized in, it comprises pressometer, temperature gauge, sample cell, refrigerating and heating combined equipment, liquid mercury or amalgam and suprasil window, sample cell is one to be equipped with the airtight container of suprasil window, liquid mercury or amalgam place in the sample cell, are equipped with refrigerating and heating combined equipment under the sample cell, and sample cell is heated or cools off.
Described demarcation is the device of a usefulness current flow heats with refrigerating and heating combined equipment used in the mercury vapour generator, this device is for wrapping in the resistance wire zone of heating outside the sample cell, change heating current, change the temperature of sample cell, thereby the saturated vapour pressure of mercury in the change sample cell, and then changing mercury vapour concentration, described resistance wire zone of heating is equipped with heat-insulation layer outward, to keep the stable of sample cell temperature.
Described demarcation is the semiconductor refrigerating plant with refrigerating and heating combined equipment used in the mercury vapour generator, by changing the polarity of family's power supply on semiconductor cooling device, can realize cooling or heating to sample cell.
The invention has the beneficial effects as follows that mercury vapour concentration can control by regulating temperature, and liquid mercury or amalgam and mercury vapour all are sealed in the sample cell, can not discharge the generation environmental pollution, and can simplify the existing environment supervision instrument that is used for and demarcate with mercury vapour generator architecture and exhaust treatment system.
Description of drawings
Fig. 1 is apparatus of the present invention structural representation;
Fig. 2 is the embodiment of the invention 1 synoptic diagram;
Fig. 3 is the A-A sectional view of Fig. 2;
Fig. 4 is the embodiment of the invention 2 synoptic diagram.
Embodiment
A kind of demarcation uses the mercury vapour generator by shown in Figure 1, it comprises pressometer 1, temperature gauge 2, sample cell 3, refrigerating and heating combined equipment 4, liquid mercury or amalgam 5 and suprasil window 7, sample cell 3 is one to be equipped with the airtight container of suprasil window 6, liquid mercury 5 places in the sample cell, sample cell is equipped with refrigerating and heating combined equipment 43 times, and sample cell 3 is heated or cools off.The concrete steps that produce the method for normal concentration mercury vapour are:
1) earlier sample cell 3 is vacuumized, add liquid mercury or amalgam 5 then, sample cell 3 is sealed fully again, the liquid mercury or the amalgam 5 that are in the sealed sample pond can partly flash to gaseous mercury 6, form mercury vapour in the space of sample cell;
2) by refrigerating and heating combined equipment sample cell is heated or cooling, along with sample cell 3 temperature variation, the mercury vapor pressure in the sample cell changes thereupon, and the pressure and temperature of mercury vapour is by pressometer 1 and temperature gauge 2
Record, according to this measuring pressure and temperature from subordinate list: obtain the saturated vapor pressure of mercury " the mercury vapour saturation pressure and the temperature table of comparisons ", then basis
ρ is a mercury saturated vapor concentration in the formula, M is the atomic weight of mercury, equal 200.59, P is the mercury saturation vapour pressure, and Z is a compressibility factor, be less than or equal to 1, R is a gas law constant, and T is a kelvin rating, by the temperature of refrigerating and heating combined equipment to sample cell heating or cooling control sample cell, obtain different mercury saturated vapor concentration, for Calibration of measuring equipment provides the normal concentration mercury vapour.
For example: the mercury that can look into according to subordinate list is that corresponding saturation pressure is 1.85*10-4mmHg at 0 ℃, be equivalent to 0.024605Pa, the atomic weight M of mercury is 200.59g/mol, gas law constant R=8.3145J/mol.k, T=273.16K(0 ℃), get Z=1, the density that then can obtain mercury vapour is 2.1731mg/m3.
When the calibration measurements instrument, incident measuring light 8 incides in the sample cell through transparent quartz window, is absorbed by the mercury vapour in the sample cell, and transmission measurement light 9 will be decayed, and its decay size is relevant with the mercury vapour concentration in the sample cell.So just can be used for demarcating the mercury measurement instrument.
Embodiment 1:
Described demarcation is the device of a usefulness current flow heats with refrigerating and heating combined equipment used in the mercury vapour generator, as shown in Figure 2, this device is for wrapping in the resistance wire zone of heating 10 outside the sample cell, change heating current, change the temperature of sample cell, thereby change the saturated vapour pressure of mercury in the sample cell, and then change mercury vapour concentration, described resistance wire zone of heating is equipped with heat-insulation layer 11 outward, as shown in Figure 3, and to keep the stable of sample cell temperature.
Embodiment 2:
By shown in Figure 4, because sample cell can not seal fully, the long-time vacuum of back sample cell of using can descend, cause pressure in the sample cell that records to be not equal to the saturation pressure of mercury vapour, for eliminating the influence that vacuum descends, increased exhaust tube 12 on sample cell 3, valve 13 is housed on the exhaust tube, the back connects vacuum pump 14.After vacuum descends, can open valve, start vacuum pump sample cell is vacuumized, valve-off stops vacuum pump then, keeps the vacuum of sample cell.
Embodiment 3:
When demarcating very low concentration, because the liquefaction pressure of mercury is very low, mercury vapour concentration corresponding to mercury saturation pressure corresponding under the room temperature may be too high, at this moment, with demarcating with refrigerating and heating combined equipment used in the mercury vapour generator among Fig. 1 is the semiconductor refrigerating plant, by changing the polarity of semiconductor cooling device power supply, can be to cooling of sample cell polarity or heating.
Subordinate list: the mercury vapour saturation pressure and the temperature table of comparisons
The saturated vapour pressure of mercury under different temperatures
| Temperature/℃ | Vapor pressure/mmHg | Temperature/℃ | Vapor pressure/mmHg | Temperature/℃ | Vapor pressure/mmHg |
| -38.0 | 1.45×10 -6 | 122.0 | 0.8198 | 282.0 | 164.39 |
| -36.0 | 1.97×10 -6 | 124.0 | 0.9004 | 284.0 | 172.21 |
| -34.0 | 2.66×10 -6 | 126.0 | 0.9882 | 286.0 | 180.34 |
| -32.0 | 3.59×10 -6 | 128.0 | 1.084 | 288.0 | 188.79 |
| -30.0 | 4.78×10 -6 | 130.0 | 1.186 | 290.0 | 197.57 |
| -28.0 | 6.30×10 -6 | 132.0 | 1.298 | 292.0 | 206.70 |
| -26.0 | 8.28×10 -6 | 134.0 | 1.419 | 294.0 | 216.17 |
| -24.0 | 1.08×10 -5 | 136.0 | 1.551 | 296.0 | 226.00 |
| -22.0 | 1.40×10 -5 | 138.0 | 1.692 | 298.0 | 236.21 |
| -20.0 | 1.81×10 -5 | 140.0 | 1.845 | 300.0 | 246.80 |
| -18.0 | 2.32×10 -5 | 142.0 | 2.010 | 302.0 | 257.78 |
| -16.0 | 2.98×10 -5 | 144.0 | 2.188 | 304.0 | 269.17 |
| -14.0 | 3.80×10 -5 | 146.0 | 2.379 | 306.0 | 280.98 |
| -12.0 | 4.81×10 -5 | 148.0 | 2.585 | 308.0 | 293.21 |
| -10.0 | 6.06×10 -5 | 150.0 | 2.807 | 310.0 | 305.89 |
| -8.0 | 7.62×10 -5 | 152.0 | 3.046 | 312.0 | 319.02 |
| -6.0 | 9.54×10 -5 | 154.0 | 3.303 | 314.0 | 332.62 |
| -4.0 | 1.19×10 -4 | 156.0 | 3.578 | 316.0 | 346.70 |
| -2.0 | 1.49×10 -4 | 158.0 | 3.873 | 318.0 | 361.26 |
| 0.0 | 1.85×10 -4 | 160.0 | 4.189 | 320.0 | 376.33 |
| 2.0 | 2.28×10 -4 | 162.0 | 4.528 | 322.0 | 391.92 |
| 4.0 | 2.76×10 -4 | 164.0 | 4.890 | 324.0 | 408.04 |
| 6.0 | 3.35×10 -4 | 166.0 | 5.277 | 326.0 | 424.71 |
| 8.0 | 4.06×10 -4 | 168.0 | 5.689 | 328.0 | 441.94 |
| 10.0 | 4.90×10 -4 | 170.0 | 6.128 | 330.0 | 459.74 |
| 12.0 | 5.88×10 -4 | 172.0 | 6.596 | 332.0 | 478.13 |
| 14.0 | 7.06×10 -4 | 174.0 | 7.095 | 334.0 | 497.12 |
| 16.0 | 8046×10 -4 | 176.0 | 7.626 | 336.0 | 516.74 |
| 18.0 | 1.009×10 -3 | 178.0 | 8.193 | 338.0 | 537.00 |
| 20.0 | 1.201×10 -3 | 180.0 | 8.796 | 340.0 | 557.90 |
| 22.0 | 1.426×10 -3 | 182.0 | 9.436 | 342.0 | 579.45 |
| 24.0 | 1.691×10 -3 | 184.0 | 10.116 | 344.0 | 601.69 |
| 26.0 | 2.000×10 -3 | 186.0 | 10.839 | 346.0 | 624.64 |
| 28.0 | 2.359×10 -3 | 188.0 | 11.607 | 348.0 | 648.30 |
| 30.0 | 2.777×10 -3 | 190.0 | 12.423 | 350.0 | 672.69 |
| 32.0 | 3.261×10 -3 | 192.0 | 13.287 | 352.0 | 697.83 |
| 34.0 | 3.823×10 -3 | 194.0 | 14.203 | 354.0 | 723.73 |
| 36.0 | 4.471×10 -3 | 196.0 | 15.173 | 356.0 | 750.43 |
| 38.0 | 5.219×10 -3 | 198.0 | 16.200 | 358.0 | 777.92 |
| 40.0 | 6.079×10 -3 | 200.0 | 17.287 | 360.0 | 806.23 |
| 42.0 | 7.067×10 -3 | 202.0 | 18.437 | 362.0 | 835.38 |
| 44.0 | 8.200×10 -3 | 204.0 | 19.652 | 364.0 | 865.36 |
| 46.0 | 9.497×10 -3 | 206.0 | 20.936 | 366.0 | 896.23 |
| 48.0 | 0.01098 | 208.0 | 22.292 | 368.0 | 928.02 |
| 50.0 | 0.01267 | 210.0 | 23.723 | 370.0 | 960.66 |
| 52.0 | 0.01459 | 212.0 | 25.233 | 372.0 | 994.34 |
| 54.0 | 0.01677 | 214.0 | 26.826 | 374.0 | 1028.9 |
| 56.0 | 0.01925 | 216.0 | 28.504 | 376.0 | 1064.4 |
| 58.0 | 0.02206 | 218.0 | 30.271 | 378.0 | 1100.9 |
| 60.0 | 0.02524 | 220.0 | 32.133 | 380.0 | 1138.4 |
| 62.0 | 0.02883 | 222.0 | 34.092 | 382.0 | 1177.0 |
| 64.0 | 0.03287 | 224.0 | 36.153 | 384.0 | 1216.6 |
| 66.0 | 0.03740 | 226.0 | 38.318 | 386.0 | 1257.3 |
| 68.0 | 0.04251 | 228.0 | 40.595 | 388.0 | 1299.1 |
| 70.0 | 0.04825 | 230.0 | 42.989 | 390.0 | 1341.9 |
| 72.0 | 0.05469 | 232.0 | 45.503 | 392.0 | 1386.1 |
| 74.0 | 0.06189 | 234.0 | 48.141 | 394.0 | 1431.3 |
| 76.0 | 0.06993 | 236.0 | 50.909 | 396.0 | 1477.7 |
| 78.0 | 0.07889 | 238.0 | 53.812 | 398.0 | 1525.2 |
| 80.0 | 0.08880 | 240.0 | 56.855 | 400.0 | 1574.1 |
| 82.0 | 0.1000 | 242.0 | 60.044 | 430.0 | 2464 |
| 84.0 | 0.1124 | 244.0 | 63.384 | 460.0 | 3715 |
| 86.0 | 0.1261 | 246.0 | 66.882 | 490.0 | 5420 |
| 88.0 | 0.1413 | 248.0 | 70.543 | 520.0 | 7691 |
| 90.0 | 0.1582 | 250.0 | 74.375 | 550.0 | 10650 |
| 92.0 | 0.1769 | 252.0 | 78.381 | 600.0 | 17381 |
| 94.0 | 0.1976 | 254.0 | 82.568 | 650.0 | 26972 |
| 96.0 | 0.2202 | 256.0 | 86.944 | 700.0 | 39908 |
| 98.0 | 0.2453 | 258.0 | 91.518 | 750.0 | 56894 |
| 100.0 | 0.2729 | 260.0 | 96.296 | 800.0 | 78516 |
| 102.0 | 0.3032 | 262.0 | 101.28 | 850.0 | 105199 |
| 104.0 | 0.3366 | 264.0 | 106.48 | (900.0 critical point) | 137499 |
| 106.0 | 0.3731 | 266.0 | 111.91 | 950.0 | 172201 |
| 108.0 | 0.4132 | 268.0 | 117.57 | 1000.0 | 220780 |
| 110.0 | 0.4572 | 270.0 | 123.47 | 1050.0 | 272156 |
| 112.0 | 0.5052 | 272.0 | 129.62 | 1100.0 | 332348 |
| 114.0 | 0.5576 | 274.0 | 136.02 | 1150.0 | 396188 |
| 116.0 | 0.6150 | 276.0 | 142.69 | 1200.0 | 468768 |
| 118.0 | 0.6776 | 278.0 | 149.64 | 1250.0 | 548264 |
| 120.0 | 0.7457 | 280.0 | 156.87 | 1300.0 | 635284 |
Claims (5)
1. a method that produces the normal concentration mercury vapour is characterized in that, its concrete steps are:
1) earlier sample cell is vacuumized, add liquid mercury or amalgam then, sample cell is sealed fully again, the liquid mercury that is in the sealed sample pond can part evaporate, and forms mercury vapour in the space of sample cell;
2) by refrigerating and heating combined equipment sample cell is heated or cooling, along with the sample cell temperature variation, the mercury vapor pressure in the sample cell changes thereupon, and the pressure and temperature of mercury vapour is recorded by pressometer and temperature gauge,
From " the mercury vapour saturation pressure and the temperature table of comparisons ", obtain the saturated vapor pressure of mercury, basis then according to this measuring pressure and temperature
ρ is a mercury saturated vapor concentration in the formula, M is the atomic weight of mercury, equal 200.59, P is the mercury saturation vapour pressure, and Z is a compressibility factor, be less than or equal to 1, R is a gas law constant, and T is a kelvin rating, by the temperature of refrigerating and heating combined equipment to sample cell heating or cooling control sample cell, obtain different mercury saturated vapor concentration, for Calibration of measuring equipment provides the normal concentration mercury vapour.
2. realization produces the device of the method for normal concentration mercury vapour according to claim 1, it is a kind of demarcation mercury vapour generator, it is characterized in that, it comprises pressometer, temperature gauge, sample cell, cooling-heating device, liquid mercury and suprasil window, sample cell is one to be equipped with the airtight container of suprasil window, liquid mercury places in the sample cell, is equipped with refrigerating and heating combined equipment under the sample cell, and sample cell is heated or cools off.
3. the device of the method for generation normal concentration mercury vapour according to claim 2, it is characterized in that, described demarcation is the device of a usefulness current flow heats with refrigerating and heating combined equipment used in the mercury vapour generator, this device changes heating current for wrapping in the resistance wire zone of heating outside the sample cell, changes the temperature of sample cell, thereby the saturated vapour pressure of mercury in the change sample cell, and then changing mercury vapour concentration, described resistance wire zone of heating is equipped with heat-insulation layer outward, to keep the stable of sample cell temperature.
4. a kind of method that produces the normal concentration mercury vapour according to claim 1, it is characterized in that, described demarcation is the semiconductor refrigerating plant with refrigerating and heating combined equipment used in the mercury vapour generator, change the polarity of semiconductor cooling device power supply, can make the semiconductor refrigerating heating combined equipment sample cell heating or cooling.
5. according to the device of the method for the described generation normal concentration of claim 2 mercury vapour, it is characterized in that, increased exhaust tube on the described sample cell, valve is housed on the exhaust tube, the back connects vacuum pump.
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| CN105372191A (en) * | 2015-10-22 | 2016-03-02 | 燕山大学 | Gaseous elemental mercury spectrum monitoring method and monitoring device thereof |
| CN105698151A (en) * | 2016-01-11 | 2016-06-22 | 中国科学院上海光学精密机械研究所 | Controllable low-temperature mercury vapor source for ultrahigh vacuum system |
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| CN109541102A (en) * | 2018-11-20 | 2019-03-29 | 中广核研究院有限公司 | A kind of device and method of volatile organic matter vapour pressure measurement |
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| CN105698151A (en) * | 2016-01-11 | 2016-06-22 | 中国科学院上海光学精密机械研究所 | Controllable low-temperature mercury vapor source for ultrahigh vacuum system |
| CN106040110A (en) * | 2016-05-25 | 2016-10-26 | 北京雪迪龙科技股份有限公司 | Mercuric chloride reduction heating chamber and mercury vapor generating device and method by using heating chamber |
| CN106525554A (en) * | 2016-12-16 | 2017-03-22 | 上海华川环保科技有限公司 | High-concentration gaseous mercury generator |
| CN109541102A (en) * | 2018-11-20 | 2019-03-29 | 中广核研究院有限公司 | A kind of device and method of volatile organic matter vapour pressure measurement |
| CN116008024A (en) * | 2022-12-09 | 2023-04-25 | 华能重庆珞璜发电有限责任公司 | Preparation device and preparation method of zero-valent mercury standard gas |
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