CN112557482A - Method for measuring trace moisture in liquefied methane chloride - Google Patents
Method for measuring trace moisture in liquefied methane chloride Download PDFInfo
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- CN112557482A CN112557482A CN202011286032.4A CN202011286032A CN112557482A CN 112557482 A CN112557482 A CN 112557482A CN 202011286032 A CN202011286032 A CN 202011286032A CN 112557482 A CN112557482 A CN 112557482A
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- 238000000034 method Methods 0.000 title claims abstract description 49
- FBBDOOHMGLLEGJ-UHFFFAOYSA-N methane;hydrochloride Chemical compound C.Cl FBBDOOHMGLLEGJ-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000005070 sampling Methods 0.000 claims abstract description 166
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 103
- 239000010959 steel Substances 0.000 claims abstract description 103
- 238000001514 detection method Methods 0.000 claims abstract description 22
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims description 40
- 239000010453 quartz Substances 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 238000003860 storage Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- 238000002347 injection Methods 0.000 claims description 8
- 239000007924 injection Substances 0.000 claims description 8
- 238000005868 electrolysis reaction Methods 0.000 claims description 7
- 238000011156 evaluation Methods 0.000 claims description 3
- 230000010287 polarization Effects 0.000 claims description 3
- 238000004448 titration Methods 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 238000012360 testing method Methods 0.000 abstract description 20
- 238000003869 coulometry Methods 0.000 abstract description 6
- 238000012544 monitoring process Methods 0.000 abstract description 6
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 6
- 238000007789 sealing Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 125000006850 spacer group Chemical group 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000004164 analytical calibration Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/42—Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte
- G01N27/44—Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte using electrolysis to generate a reagent, e.g. for titration
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- Health & Medical Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides a method for measuring trace moisture in liquefied methane chloride, and solves the technical problems of high difficulty and low precision in accurately measuring the trace moisture in the liquefied methane chloride in the prior art. The method comprises the following steps: (1) sampling by adopting a sampling steel cylinder, and (2) detecting by adopting a Karl Fischer moisture tester. The method for measuring trace moisture in liquefied methane chloride provided by the invention adopts a KF coulometry method, adjusts a sampling device, a sampling process, a sample introduction process and detection parameters, corrects the traditional Karl Fischer coulometry method, improves the precision and the accuracy of the detection method, and can meet the requirements of engineering acceptance test and daily product quality monitoring.
Description
Technical Field
The invention relates to a method for measuring trace moisture in liquefied methane chloride.
Background
The monochloromethane is an important chemical raw material, and the moisture content in the monochloromethane is an important index for evaluating the quality of products. With the improvement of chemical technology, the water content in the chloromethane can be reduced to below 10 PPM. The boiling point of the monochloromethane is-23.79 ℃, and the product is packaged, transported and sold by steel cylinders after being liquefied normally.
Since the methane chloride is liquefied gas, the accurate test of the moisture is difficult. The existing analytical test methods include phosphorus pentoxide absorption weighing method, Karl Fischer coulometry method, Karl Fischer volumetric method and electrolytic method; the phosphorus pentoxide absorption weighing method has poor accuracy and precision and low applicability; the electrolytic method is suitable for measuring the content of gaseous low moisture, is generally applied to the aspect of on-line test, is not suitable for measuring the moisture in liquefied gas, and has the problems that a test system needs a large amount of sample gas to purge and balance a test pipeline, standard gas is difficult to prepare, the difficulty of instrument calibration is high, and the Karl Fischer coulometry and the volumetric method are also applied to national and industrial standards for measurement.
In addition, due to the volatilization of the liquefied gas, a large amount of heat is absorbed, and the moisture in the sample generates a component discrimination phenomenon in the volatilization process, so that the moisture measurement value is low. And the gasification of the sample absorbs heat to cause the surface of the pipeline to agglutinate moisture in the air, thereby influencing the accuracy of the test.
The applicant has found that the prior art has at least the following technical problems:
1. in the prior art, the accurate test of trace moisture in liquefied monochloro methane has high difficulty and low precision.
Disclosure of Invention
The invention aims to provide a method for measuring trace moisture in liquefied methane chloride. The method solves the technical problems of high difficulty and low precision in accurately testing trace moisture in liquefied methane chloride in the prior art. The technical effects that can be produced by the preferred technical scheme in the technical schemes provided by the invention are described in detail in the following.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a method for measuring trace moisture in liquefied methane chloride, which comprises the following steps:
(1) sampling
Sampling by adopting a sampling steel cylinder, wherein a sampling inlet valve and a sampling outlet valve are respectively arranged at two ends of the sampling steel cylinder, and a sampling inlet pipe and a sampling outlet pipe are respectively connected to the sampling inlet valve and the sampling outlet valve; the other end of the sampling outlet pipe is connected with a storage tank of methane chloride; the pressure of the outlet of the sampling outlet pipe is lower than that of the storage tank;
when sampling, sampling in a full-sealed mode, opening a needle valve on a sampling steel cylinder, then opening a sampling inlet valve and a sampling outlet valve, enabling the sample to flow out of a sampling port, pass through the sampling steel cylinder, enter a storage tank, flushing the sampling steel cylinder with a chloromethane sample, and then sampling;
when the sampling is stopped, closing the sampling outlet valve, the needle valve on the sampling steel cylinder and the sampling inlet valve in sequence to finish the sampling;
(2) detection of
The detection device is a Karl Fischer moisture tester for detection, and further comprises a steel cylinder bracket for obliquely placing a sampling steel cylinder, a weighing device arranged on the lower side of the steel cylinder bracket, an elastic quartz capillary tube and the Karl Fischer moisture tester; one end of the elastic quartz capillary tube extends into the sampling steel cylinder and is hermetically connected with the sampling steel cylinder, and the other end of the elastic quartz capillary tube extends into an electrolytic cell of the Karl Fischer moisture tester; a constant temperature device is arranged on the outer side of the elastic quartz capillary tube;
the working parameters of the Karl Fischer moisture tester are adjusted as follows: evaluation: 50 mv; dynamic range: 70 mv; maximum rate of electrolysis: 2240 mu g/min; minimum electrolysis rate 15ug/min, polarization cable: 10 uA; stopping drifting: 5 mu g/min; relative drift: 5 ug/min; starting drift: 20 ug/min; suspending titration: 10 s;
after the Karl Fischer moisture tester is stabilized, a detection device and a sampling steel cylinder are installed, and the initial weight W1 of the sampling steel cylinder is weighed; opening a needle valve of the sampling steel cylinder to start sample injection, and closing the needle valve of the sampling steel cylinder to stop sample injection after absolute moisture is displayed on a Karl Fischer moisture tester to be more than 300 ug; wiping the surface of the sampling steel cylinder, weighing the final weight W2 of the steel cylinder to obtain a sample amount, and inputting the sample amount into a Karl Fischer moisture tester to obtain a detection result.
Further, in the step (1), before sampling, the sampling steel cylinder is dried for at least 24 hours in a dryer;
further, in the step (1), during sampling, the sampling steel cylinder is shaken once at intervals of 1-3min, the water at the dead angle of the sampling steel cylinder is washed, and the process is repeated for 4-5 times.
Further, in the step (1), after the sampling is completed, the sampling steel cylinder is put into a dryer to be kept dry.
Further, in the step (1), during sampling, the sampling steel cylinder is arranged on the steel cylinder bracket; the steel bottle bracket comprises a workbench, a fixed support platform for installing a sampling steel bottle and a sliding support platform for installing the sampling steel bottle; the fixed supporting platform and the sliding supporting platform are both arranged on the workbench; the workbench is also provided with a plurality of linear guide rails; the bottom of the sliding support table is provided with a plurality of through holes; a sliding block matched with the linear guide rail is arranged in the through hole; and the linear guide rail is provided with a self-locking device.
Furthermore, an arc-shaped groove I matched with the appearance of the sampling steel cylinder is formed in the upper end of the sliding support platform, and two opposite side walls of the arc-shaped groove I are provided with ejection columns for fixing the sampling steel cylinder; the top column is in threaded connection with the sliding support platform; a buffer cushion is further arranged at one end of the top column close to the sampling steel cylinder; the top of the fixed support platform is provided with a second arc-shaped groove matched with the appearance of the sampling steel cylinder; the fixed supporting platform is fixed on the workbench through bolts.
Further, in the step (2), the constant temperature device is a water bath device.
Further, in the step (2), when the moisture content in the methane chloride is less than 20mg/Kg, the sample feeding amount of the Karl Fischer moisture tester is 5-10 g; when the moisture content in the methane chloride is more than 20mg/Kg, the sample amount of the Karl Fischer moisture tester is 2-5 g.
Based on the technical scheme, the embodiment of the invention can at least produce the following technical effects:
the method for measuring trace moisture in liquefied methane chloride provided by the invention adopts a KF coulometry method, adjusts a sampling device, a sampling process, a sample introduction process and detection parameters, corrects the traditional Karl Fischer coulometry method, improves the precision and the accuracy of the detection method, and can meet the requirements of engineering acceptance test and daily product quality monitoring.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic structural view (front view) of a cylinder holder according to an embodiment of the present invention;
FIG. 2 is a schematic structural view (top view) of a cylinder holder according to an embodiment of the present invention;
FIG. 3 is a schematic structural view (side view) of a cylinder holder according to an embodiment of the present invention;
FIG. 4 is a schematic diagram of the connection during a test state according to an embodiment of the present invention;
FIG. 5 is a schematic view of the connection between the sampling steel cylinder and the elastic quartz capillary tube during the detection in the embodiment of the present invention.
In the figure: 1. a work table; 2. fixing the support; 3. a sliding support table; 4. a linear guide rail; 5. a slider; 6. a first arc-shaped groove; 7. a top pillar; 8. a second arc-shaped groove; 9. sampling a steel cylinder; 10. an elastic quartz capillary tube; 11. a card sleeve; 12. fixing a nut; 13. a sealing gasket; 14. a plastic spacer; 15. karl fischer moisture tester; 16. a weighing device; 17. a steel cylinder bracket; 18. a water bath device; 19. a drying tube; 20. an electrolytic cell.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
As shown in fig. 1:
example 1:
as shown in fig. 1-5:
the structure of the cylinder holder 17 employed:
the steel bottle bracket comprises a workbench 1, a fixed support 2 for installing a sampling steel bottle 9 and a sliding support 3 for installing the sampling steel bottle 9; the fixed supporting platform 2 and the sliding supporting platform 3 are both arranged on the workbench 1; the workbench 1 is also provided with a plurality of linear guide rails 4; the bottom of the sliding support 3 is provided with a plurality of through holes; a sliding block 5 matched with the linear guide rail 4 is arranged in the through hole; and a self-locking device is arranged on the linear guide rail 4.
An arc-shaped groove I6 matched with the shape of the sampling steel cylinder 9 is formed in the upper end of the sliding support 3, and top columns 7 for fixing the sampling steel cylinder 9 are arranged on two opposite side walls of the arc-shaped groove I6; the top column 7 is in threaded connection with the sliding support 3; a buffer cushion is arranged at one end of the top pillar 7 close to the sampling steel cylinder 9, so that the sampling steel cylinder 9 is prevented from being damaged when being fixed; the top of the fixed support 2 is provided with a second arc-shaped groove 8 matched with the shape of the sampling steel cylinder 9; the fixed supporting platform 8 is fixed on the workbench 1 through bolts.
The invention provides a method for measuring trace moisture in liquefied methane chloride, which comprises the following steps:
(1) sampling
Sampling by adopting a sampling steel bottle 9, drying the sampling steel bottle 9 in at least a dryer for 24 hours before sampling, and installing the sampling steel bottle 9 on a steel bottle bracket 17 during sampling; a sampling inlet valve and a sampling outlet valve are respectively arranged at two ends of the sampling steel cylinder 9, and a sampling inlet pipe and a sampling outlet pipe are respectively connected to the sampling inlet valve and the sampling outlet valve; the other end of the sampling outlet pipe is connected with a storage tank of methane chloride; the pressure of the outlet of the sampling outlet pipe is lower than that of the storage tank;
specifically, the other end of the sampling and sample-out pipe is connected with a storage tank of methane chloride through a storage tank steel cylinder; the pressure in the sampling steel cylinder 9 is about 10kg generally, and the other end of the sampling outlet pipe is connected with a storage tank steel cylinder with the pressure lower than the pressure of the sampling steel cylinder 9, so that the pressure at the outlet of the sampling outlet pipe is lower than the pressure of the storage tank.
During sampling, sampling is carried out in a full-sealed mode, a needle valve on a sampling steel cylinder 9 is opened, then a sampling inlet valve and a sampling outlet valve are opened, a sample flows out from a sampling port, passes through the sampling steel cylinder, enters a storage tank, shakes the sampling steel cylinder 9 once at intervals of 1-3min, washes water in a dead angle of the sampling steel cylinder 9, repeats for 4-5 times, and then samples are carried out again;
when the sampling is stopped, closing the sampling outlet valve, the needle valve on the sampling steel cylinder 9 and the sampling inlet valve in sequence to finish the sampling; after sampling, putting the sampling steel cylinder 9 into a dryer to keep dry;
(2) detection of
The adopted detection device is a Karl Fischer moisture tester for detection, and the detection device also comprises a steel cylinder bracket 17 (the structure of the steel cylinder bracket 17 is described in detail in the foregoing), a weighing device 16 (preferably an electronic balance) arranged at the lower side of the steel cylinder bracket 7, an elastic quartz capillary tube 10 and a Karl Fischer moisture tester 15, wherein the sampling steel cylinder 9 is obliquely arranged; one end of the elastic quartz capillary tube 10 extends into the sampling steel cylinder 9 and is hermetically connected with the sampling steel cylinder 9, and the other end of the elastic quartz capillary tube 10 extends into an electrolytic cell 20 of a Karl Fischer moisture tester 15; a water bath device 18 is arranged on the outer side of the elastic quartz capillary tube 10; the electrolytic cell 20 is connected with a drying pipe 19, and an arrow a in fig. 4 is an emptying direction.
The sealing connection mode of the elastic quartz capillary tube 10 and the sampling steel cylinder 9 is shown in fig. 5, and specifically comprises the following steps:
a cutting sleeve 11 and a fixed nut 12 are arranged on the outer side of the elastic quartz capillary tube 10 in sequence, and a sealing gasket 13 and a plastic spacer 14 are additionally arranged between the cutting sleeve 11 and the sampling steel cylinder 9 for sealing when sealing connection is carried out.
The working parameters of the Karl Fischer moisture tester are adjusted as follows: evaluation: 50 mv; dynamic range: 70 mv; maximum rate of electrolysis: 2240 mu g/min; minimum electrolysis rate 15ug/min, polarization cable: 10 uA; stopping drifting: 5 mu g/min; relative drift: 5 ug/min; starting drift: 20 ug/min; suspending titration: 10 s;
after the Karl Fischer moisture tester 15 is stabilized, a detection device and the sampling steel cylinder 9 are installed, and the initial weight W1 of the sampling steel cylinder 9 is weighed; opening the needle valve of the sampling steel cylinder 9 to start sample injection, and closing the needle valve of the sampling steel cylinder 9 to stop sample injection after the absolute moisture displayed on the Karl Fischer moisture tester 15 is more than 300 ug; wiping the surface of the sampling steel cylinder 9 and wiping the sampling needle, quickly weighing the final weight W2 of the sampling steel cylinder 9, obtaining the sample amount by adopting a decrement method, inputting the sample amount into a Karl Fischer moisture tester 15, and obtaining a detection result.
Second, experimental example:
1. the method for measuring the moisture content of the liquid monochloromethane product was subjected to a precision test according to the method described in example 1, seven different monochloromethane products were taken, 7 samples were taken, seven tests were performed for each batch, and the corresponding standard deviations were calculated, and the test results are shown in table 1.
TABLE 1 moisture content in monochloromethane test results (mg/kg)
Table 1 shows that, in the test of trace moisture content in liquefied monochloromethane by the determination method in example 1, the influence of each link such as a sampling steel cylinder, a sampling pipeline, a sample injection pipeline, sampling, sample injection and the like on the test result is removed, and the instrument detection parameters are optimized, so that the test precision (relative standard deviation is 0.45% -3.10%) is greatly improved, and conditions are laid for accurate determination of trace moisture in liquefied monochloromethane.
2. The method of on-line comparison was applied to verify the reliability of the determination method in example 1.
The online equipment adopts the principle of phosphorus pentoxide absorption electrolysis method to test the water concentration in gaseous chloromethane, and the instrument is provided by Spain Alasong and has stronger reliability. Laboratory test results are now compared with on-line results and their relative deviations are calculated. The detailed results are shown in Table 2.
TABLE 2 comparison of the determination method and on-line monitoring results in example 1
| Sample (I) | 1 | 2 | 3 | 4 | 5 | 6 |
| Results of prior monitoring (mg/kg) | 0.00090 | 0.00076 | 0.00064 | 0.00092 | 0.00459 | 0.00572 |
| Example 1 monitoring results (mg/kg) | 0.00085 | 0.00079 | 0.00067 | 0.00095 | 0.00463 | 0.00581 |
| Relative deviation (%) | 5.71 | 3.87 | 4.58 | 3.21 | 0.87 | 1.56 |
As shown in Table 2, the relative deviation between the measurement method in example 1 and the on-line test result is 0.087% -8.09%, and the measurement results of the two devices and methods have no significant difference. The accuracy and feasibility of the method can thus be demonstrated from the above data. Therefore, the method can be used for testing and monitoring the trace moisture in the liquid methane chloride.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention.
Claims (8)
1. A method for measuring trace moisture in liquefied methane chloride is characterized in that: the method comprises the following steps:
(1) sampling
Sampling by adopting a sampling steel cylinder, wherein a sampling inlet valve and a sampling outlet valve are respectively arranged at two ends of the sampling steel cylinder, and a sampling inlet pipe and a sampling outlet pipe are respectively connected to the sampling inlet valve and the sampling outlet valve; the other end of the sampling outlet pipe is connected with a storage tank of methane chloride; the pressure of the outlet of the sampling outlet pipe is lower than that of the storage tank;
when sampling, sampling in a full-sealed mode, opening a needle valve on a sampling steel cylinder, then opening a sampling inlet valve and a sampling outlet valve, enabling the sample to flow out of a sampling port, pass through the sampling steel cylinder, enter a storage tank, flushing the sampling steel cylinder with a chloromethane sample, and then sampling;
when the sampling is stopped, closing the sampling outlet valve, the needle valve on the sampling steel cylinder and the sampling inlet valve in sequence to finish the sampling;
(2) detection of
The detection device is a Karl Fischer moisture tester for detection, and further comprises a steel cylinder bracket for obliquely placing a sampling steel cylinder, a weighing device arranged on the lower side of the steel cylinder bracket, an elastic quartz capillary tube and the Karl Fischer moisture tester; one end of the elastic quartz capillary tube extends into the sampling steel cylinder and is hermetically connected with the sampling steel cylinder, and the other end of the elastic quartz capillary tube extends into an electrolytic cell of the Karl Fischer moisture tester; a constant temperature device is arranged on the outer side of the elastic quartz capillary tube;
the working parameters of the Karl Fischer moisture tester are adjusted as follows: evaluation: 50 mv; dynamic range: 70 mv; maximum rate of electrolysis: 2240 mu g/min; minimum electrolysis rate 15ug/min, polarization cable: 10 uA; stopping drifting: 5 mu g/min; relative drift: 5 ug/min; starting drift: 20 ug/min; suspending titration: 10 s;
after the Karl Fischer moisture tester is stabilized, a detection device and a sampling steel cylinder are installed, and the initial weight W1 of the sampling steel cylinder is weighed; opening a needle valve of the sampling steel cylinder to start sample injection, and closing the needle valve of the sampling steel cylinder to stop sample injection after absolute moisture is displayed on a Karl Fischer moisture tester to be more than 300 ug; wiping the surface of the sampling steel cylinder, weighing the final weight W2 of the sampling steel cylinder to obtain a sample amount, and inputting the sample amount into a Karl Fischer moisture tester to obtain a detection result.
2. The method for measuring trace moisture in liquefied monochloromethane according to claim 1, wherein: in the step (1), the sampling steel cylinder is dried for at least 24 hours in a dryer before sampling.
3. The method for measuring trace moisture in liquefied monochloromethane according to claim 1, wherein: in the step (1), during sampling, the sampling steel cylinder is shaken once at intervals of 1-3min, the water at the dead angle of the sampling steel cylinder is washed, and the process is repeated for 4-5 times.
4. The method for measuring trace moisture in liquefied monochloromethane according to claim 1, wherein: in the step (1), after sampling is finished, the sampling steel cylinder is put into a dryer to be dried.
5. The method for measuring trace moisture in liquefied monochloromethane according to claim 1, wherein: in the step (1), during sampling, the sampling steel cylinder is arranged on the steel cylinder bracket; the steel bottle bracket comprises a workbench, a fixed support platform for installing a sampling steel bottle and a sliding support platform for installing the sampling steel bottle; the fixed supporting platform and the sliding supporting platform are both arranged on the workbench; the workbench is also provided with a plurality of linear guide rails; the bottom of the sliding support table is provided with a plurality of through holes; a sliding block matched with the linear guide rail is arranged in the through hole; and the linear guide rail is provided with a self-locking device.
6. The method for measuring trace moisture in liquefied monochloromethane according to claim 5, wherein: an arc-shaped groove I matched with the appearance of the sampling steel cylinder is formed in the upper end of the sliding support platform, and two opposite side walls of the arc-shaped groove I are provided with ejection columns for fixing the sampling steel cylinder; the top column is in threaded connection with the sliding support platform; a buffer cushion is further arranged at one end of the top column close to the sampling steel cylinder; the top of the fixed support platform is provided with a second arc-shaped groove matched with the appearance of the sampling steel cylinder; the fixed supporting platform is fixed on the workbench through bolts.
7. The method for measuring trace moisture in liquefied monochloromethane according to claim 1, wherein: in the step (2), the constant temperature device is a water bath device.
8. The method for measuring trace moisture in liquefied monochloromethane according to claim 1, wherein: in the step (2), when the moisture content in the methane chloride is less than 20mg/Kg, the sample amount of a Karl Fischer moisture tester is 5-10 g; when the moisture content in the methane chloride is more than 20mg/Kg, the sample amount of the Karl Fischer moisture tester is 2-5 g.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5179024A (en) * | 1991-05-30 | 1993-01-12 | Harald Dahms | Sealed vials containing improved karl fischer solutions, and process for water determination using these vials |
| JPH09251017A (en) * | 1996-03-15 | 1997-09-22 | Mitsubishi Chem Corp | Moisture content measurement method using karl fisher's reagent |
| CN102928365A (en) * | 2012-10-26 | 2013-02-13 | 上海天科化工检测有限公司 | Dynamic calibrating device and method in process of measuring micro-moisture in gas by using optical method |
-
2020
- 2020-11-17 CN CN202011286032.4A patent/CN112557482A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5179024A (en) * | 1991-05-30 | 1993-01-12 | Harald Dahms | Sealed vials containing improved karl fischer solutions, and process for water determination using these vials |
| JPH09251017A (en) * | 1996-03-15 | 1997-09-22 | Mitsubishi Chem Corp | Moisture content measurement method using karl fisher's reagent |
| CN102928365A (en) * | 2012-10-26 | 2013-02-13 | 上海天科化工检测有限公司 | Dynamic calibrating device and method in process of measuring micro-moisture in gas by using optical method |
Non-Patent Citations (3)
| Title |
|---|
| 毕鹏禹等: "卡尔费休库仑法测定微量水的装置改进", 《分析化学》 * |
| 沈治荣 等: "卡尔费休库仑滴定法测定液化一氯甲烷中微量水分", 《四川化工》 * |
| 王川等: "弹性石英毛细管和卡尔费休库仑法测定乙烯、丙烯中微量水", 《石油化工》 * |
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Application publication date: 20210326 |