CN114264535A - Method for preparing solution of volatile solute - Google Patents
Method for preparing solution of volatile solute Download PDFInfo
- Publication number
- CN114264535A CN114264535A CN202111438742.9A CN202111438742A CN114264535A CN 114264535 A CN114264535 A CN 114264535A CN 202111438742 A CN202111438742 A CN 202111438742A CN 114264535 A CN114264535 A CN 114264535A
- Authority
- CN
- China
- Prior art keywords
- solute
- container
- weighing
- liquid
- bottle
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000005303 weighing Methods 0.000 claims abstract description 120
- 239000007788 liquid Substances 0.000 claims abstract description 108
- 238000002360 preparation method Methods 0.000 claims abstract description 25
- 239000002904 solvent Substances 0.000 claims abstract description 24
- 238000005086 pumping Methods 0.000 claims abstract description 20
- 238000012546 transfer Methods 0.000 claims description 28
- 238000004321 preservation Methods 0.000 claims description 16
- 238000007789 sealing Methods 0.000 claims description 11
- 238000000605 extraction Methods 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000741 silica gel Substances 0.000 claims description 6
- 229910002027 silica gel Inorganic materials 0.000 claims description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 5
- 235000011089 carbon dioxide Nutrition 0.000 claims description 5
- 238000007710 freezing Methods 0.000 claims description 5
- 230000008014 freezing Effects 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 11
- 238000001514 detection method Methods 0.000 abstract description 10
- 239000002775 capsule Substances 0.000 abstract description 4
- 239000004033 plastic Substances 0.000 abstract description 4
- 229920003023 plastic Polymers 0.000 abstract description 4
- 238000003908 quality control method Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 22
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 239000003708 ampul Substances 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000003988 headspace gas chromatography Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 238000000540 analysis of variance Methods 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 210000004907 gland Anatomy 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229920002379 silicone rubber Polymers 0.000 description 2
- 239000004945 silicone rubber Substances 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical compound CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 description 1
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012925 biological evaluation Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 150000004292 cyclic ethers Chemical class 0.000 description 1
- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 235000013773 glyceryl triacetate Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000000963 oxybis(methylene) group Chemical group [H]C([H])(*)OC([H])([H])* 0.000 description 1
- 229940113115 polyethylene glycol 200 Drugs 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229960002622 triacetin Drugs 0.000 description 1
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to the technical field of chemical industry, in particular to a preparation method of a volatile solute solution, which comprises the following steps: weighing a closed weighing container filled with a solvent; extracting a preset amount of solute in a liquid state; pumping the extracted solute into the weighing container; and weighing the weighing container after the solute is beaten in. The invention solves the weighing difficulty of volatile standard substances, avoids volatilization of main components in the weighing process, and simultaneously avoids instability of balance reading caused by volatilization, so that the weighing result is more accurate and infinitely close to the true value, the weighing accuracy is high, and the accuracy of the prepared solution is high. The standard substance has good uniformity through actual detection, and guarantees quality control and quantity detection in enterprises such as medical instruments, hollow capsules, plastic products and the like; the configuration accuracy and the detection reliability are greatly improved.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a preparation method of a volatile solute solution.
Background
Ethylene oxide is also called as ethylene oxide and dioxane, has CAS number of 75-21-8, molecular weight of 44.05 and structural formula of C2H4O, is the simplest cyclic ether, is colorless inflammable gas at normal temperature, is colorless and flowable liquid at the temperature of less than 10.7 ℃, has the smell of diethyl ether, is a medium-toxicity chemical product, is a very important fine chemical raw material, and is widely applied to the cosmetic industry, the pharmaceutical industry, medical disinfection, the rubber industry and the military.
The standards of the prior determination of ethylene oxide and propylene oxide in food contact materials and plastic products, the biological evaluation of residual ethylene oxide sterilization in medical instruments, the detection of residual ethylene oxide in gelatin hollow capsules and the like all relate to the preparation of ethylene oxide standard products.
Disclosure of Invention
The invention aims to provide a method for preparing a solution of a volatile solute, which aims to solve the technical problem of low weighing accuracy in the preparation of the solution of the volatile solute in the prior art.
In order to solve the technical problem, the preparation method of the volatile solute solution provided by the invention comprises the following steps:
weighing a closed weighing container filled with a solvent;
extracting a preset amount of solute in a liquid state;
pumping the extracted solute into the weighing container;
and weighing the weighing container after the solute is beaten in.
Further, before the preset amount of the solute in the liquid state is extracted, the method further comprises the following steps: the best effect is achieved when the operating environment temperature is below-4 ℃, a sealed solute bottle containing liquid solute is placed in a heat preservation container, and the temperature in the heat preservation container is lower than the boiling temperature of the solute, so that the solute in the solute bottle is kept in a liquid state. The heat retainer can also be an ice bag or dry ice.
Further, the step of extracting a preset amount of solute in a liquid state specifically comprises the following steps: inserting a needle of a liquid transferring device into a solute bottle, extracting a preset amount of solute, inverting the solute bottle and the liquid transferring device to enable the needle of the liquid transferring device to be higher than the liquid in the solute bottle, operating the liquid transferring device to extract a preset amount of gas, and rapidly pulling out the needle of the liquid transferring device from the solute bottle.
Further, the step of extracting the solute with the preset amount specifically comprises the following steps: and pumping a small amount of solute into the liquid transfer device, pumping the solute in the liquid transfer device back into the solute bottle, and pumping a preset amount of solute into the liquid transfer device.
Further, the method also comprises the following steps after weighing the weighing container with the solute injected into the weighing container: using a pipettor to extract all liquid in the weighing container;
the liquid in the liquid transfer device is driven into a preparation container containing a preset amount of solvent.
Further, the method for extracting all liquid in the weighing container by using the pipettor specifically comprises the following steps: and inserting the pipette needle into the weighing container for extraction, and pulling out the pipette needle from the weighing container when the pressure in the weighing container is less than the external atmospheric pressure.
Further, the method for extracting all liquid in the weighing container by using the pipettor specifically comprises the following steps: the method comprises the steps of inserting a pipette needle into a weighing container for extraction, after all liquid is extracted, continuing to operate the pipette to extract gas with a preset amount, inverting the pipette and the weighing container to enable the pipette to be below the weighing container, and rapidly pulling out the pipette needle from the weighing container.
Further, the preparation method of the heat-insulating container comprises the following steps: putting an object into a container filled with liquid, so that the liquid in the container partially submerges the object, putting the container into a refrigerator for freezing until the liquid is completely solidified, taking the container out of the refrigerator, taking the object out of the container, and forming the container into the heat-preservation container, wherein the container is internally provided with a groove.
Further, weigh the container including weighing the bottle and sealed lid, sealed lid is established in the opening of weighing the bottle and is located will weigh the bottle and seal, and the material of sealed lid is silica gel.
Further, the step of pumping the extracted solute into the weighing container comprises the following steps: and pumping the extracted solute into a weighing container by using a liquid transfer device, inserting a needle of the liquid transfer device into the weighing container, positioning the needle above the liquid level in the weighing container, and pumping the solute in the liquid transfer device into the weighing container.
By adopting the technical scheme, the invention has the following beneficial effects:
the method for preparing the solution of the volatile solute solves the weighing difficulty of volatile standard substances, avoids volatilization of main components in the weighing process, and avoids instability of balance reading caused by volatilization, so that the weighing result is more accurate and infinitely close to the true value, the weighing accuracy is high, and the prepared solution is high in accuracy. The standard substance has good uniformity through actual detection, and guarantees quality control and quantity detection in enterprises such as medical instruments, hollow capsules, plastic products and the like; the configuration accuracy and the detection reliability are greatly improved.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The present invention will be further explained with reference to specific embodiments.
The preparation method of the solution of the volatile solute provided by the embodiment comprises the following steps:
weighing a closed weighing container filled with a solvent;
extracting a preset amount of solute in a liquid state;
pumping the extracted solute into the weighing container;
and weighing the weighing container after the solute is beaten in.
In the solution preparation method provided by this embodiment, the weighing container containing the solvent is weighed, the liquid solute is pumped into the weighing container, so that the solute is dissolved in the solvent, the weighing container is weighed, and the weight of the extracted solute can be obtained by comparing the two weights of the weighing container. This embodiment adopts and squeezes the solute into the mode of weighing after the solvent for the solute dissolves to the solvent after, has reduced the volatilization of solute, the operation of being convenient for, it is high to weigh the accuracy, and the solution accuracy of configuration is high. The invention is suitable for preparing the solution of volatile solute, in particular to the solute which is gaseous at normal temperature, such as ethylene oxide and the like.
Preferably, the solute is ethylene oxide. The solvent is water. The solvent can also be DMSO, polyethylene glycol 200, glycerol triacetate, toluene, dichloromethane, isooctane, etc.
Specifically, when the ambient temperature is less than-4 ℃, when the extracted solute is driven into the weighing container by the liquid transfer device, the needle of the liquid transfer device is positioned above the liquid level in the weighing container, so that the needle is prevented from contacting with the liquid in the weighing container, and the weighing precision can be improved. Before the needle is pulled out of the weighing container, the needle is contacted with the bottle wall of the weighing container to remove the residual liquid on the needle tip.
On the basis of the above embodiment, further, before the preset amount of the solute in the liquid state is extracted, the method further includes the following steps: the method comprises the steps of placing a sealed solute bottle containing liquid solute in a heat preservation container, wherein the heat preservation container can be an ice box or dry ice, and the temperature in the heat preservation container is lower than the boiling temperature of the solute so as to keep the solute in the solute bottle in a liquid state. The heat preservation container can make the solute in the solute bottle keep for liquid, avoids weighing in-process solute to volatilize to be convenient for draw the solute.
Specifically, the preparation method of the heat-insulating container comprises the following steps: putting an object into a container filled with liquid, so that the liquid in the container partially submerges the object, putting the container into a refrigerator for freezing until the liquid is completely solidified, taking the container out of the refrigerator, taking the object out of the container, and forming the container into the heat-preservation container, wherein the container is internally provided with a groove. The method is adopted to conveniently and rapidly prepare the heat preservation container, the heat preservation container can be an ice bag or dry ice, preferably, the object can be a bottle body, a weight is placed in the bottle body, liquid in the container can be water, the bottle body is placed in the water in the container, so that two thirds of the height of the bottle body is submerged, the container is placed in a refrigerator to be frozen until the water is solidified into ice, the container is taken out of the refrigerator, then the bottle body is taken out of the container, and after the bottle body is taken out, the part of the container, which is used for accommodating the bottle body, is formed into a groove shape, namely the heat preservation container.
On the basis of the above embodiment, further, the extracting a preset amount of the solute in the liquid state specifically includes the following steps: inserting a needle of a liquid transferring device into a solute bottle, extracting a preset amount of solute, inverting the solute bottle and the liquid transferring device to enable the needle of the liquid transferring device to be higher than the liquid in the solute bottle, operating the liquid transferring device to extract a preset amount of gas, and rapidly pulling out the needle of the liquid transferring device from the solute bottle. Inverting the solute bottle and the pipette means the solute bottle is up and the pipette is down. After inversion, the needle head of the liquid shifter can be positioned above the liquid in the solute bottle, air in the solute bottle is continuously extracted to enter the needle head, and then the needle head is pulled out of the solute bottle. The reason why the operation mode is adopted is that after the needle of the liquid transfer device is pulled out of the solute bottle, the solute in the liquid transfer device is partially gasified and volatilized due to the high temperature of the external air, and the volatilized gas is sprayed out through the needle. And after adopting above-mentioned operation, the outside one section distance of syringe needle is the air, when volatilizing gas in the pipettor passes through the outside blowout of syringe needle, the first-selected spun is the inside air of syringe needle, just from the blowout in the pipettor when the air blowout is finished volatilizing gas, has reduced the blowout of volatilizing gas in the pipettor to if the operator operation when faster, can realize in the pipettor volatilizing gas when not blowout promptly by being squeezed into weigh the container in, thereby reduced the volatilization of weighing in-process solute.
The pipette in the present invention may be a syringe or a pipette gun having a needle, and preferably, the pipette is a syringe.
On the basis of the above embodiment, further, the extracting the solute by the preset amount specifically includes the following steps: and pumping a small amount of solute into the liquid transfer device, pumping the solute in the liquid transfer device back into the solute bottle, and pumping a preset amount of solute into the liquid transfer device. Because the liquid temperature in the solute bottle is lower, the pipettor temperature is higher, can lead to liquid solute to volatilize because of the temperature becomes high after the pipettor extracts liquid solute. In the embodiment, during operation, a small amount of solute is extracted into the liquid transfer device, the temperature in the liquid transfer device is reduced due to the lower temperature of the solute, the solute in the liquid transfer device is volatilized into gas, the gaseous solute in the liquid transfer device is pumped back into the solute bottle, the liquid solute with the preset amount is extracted into the solute bottle, and the liquid solute cannot be volatilized as gas after entering the liquid transfer device due to the temperature reduction of the liquid transfer device, so that the volatilization of the solute is reduced.
On the basis of the above embodiment, further, after weighing the weighing container with the solute therein, the method further includes the following steps:
preferably the ambient temperature should be controlled below 4 ℃.
Using a pipettor to extract all liquid in the weighing container;
the liquid in the liquid transfer device is driven into a preparation container containing a preset amount of solvent.
In this embodiment, all the liquid in the weighing container is transferred to the preparation container and diluted to a predetermined density.
Further, after the preparation container is diluted to a preset concentration, the preparation container is refrigerated for a preset time, the solution in the preparation container is subpackaged into ampoule bottles, and then the ampoule bottles are sealed by melting and stored in a freezing way.
On the basis of the above embodiment, further, after the liquid in the pipette is driven into the preparation container containing the preset amount of the solvent, the method further includes the following steps: the weighing container was cleaned with a solvent, and the cleaned liquid was transferred into a preparation container. Preferably, the weighing vessel is repeatedly cleaned a number of times to ensure that the solute in the weighing vessel is transferred into the dispensing vessel.
On the basis of the above embodiment, further, the extracting all the liquid in the weighing container by using the pipette specifically includes the following steps: and inserting the pipette needle into the weighing container for extraction, and pulling out the pipette needle from the weighing container when the pressure in the weighing container is less than the external atmospheric pressure. Because the solvent is pumped into the weighing container, the internal pressure of the weighing container is increased, and when the liquid in the weighing container is pumped out, the internal pressure of the weighing container is ensured to be negative (namely, the internal pressure of the container is less than the external atmospheric pressure), so that the gas in the weighing container can be prevented from being sprayed out after the needle head is pulled out.
On the basis of the above embodiment, further, the extracting all the liquid in the weighing container by using the pipette specifically includes the following steps: the method comprises the steps of inserting a pipette needle into a weighing container for extraction, after all liquid is extracted, continuing to operate the pipette to extract air with a preset amount, inverting the pipette and the weighing container to enable the pipette to be below the weighing container, and rapidly pulling out the pipette needle from the weighing container. Because the pipettor extracts the air of the preset amount, a section of distance in the needle head is the air, when the pipettor needle head is pulled out and is transferred, when the solute in the pipettor is volatilized and is outwards sprayed, the air in the pipettor needle head is outwards sprayed, and the volatilization of the solute is reduced.
On the basis of the embodiment, further, the weighing container comprises a weighing bottle body and a sealing cover, the sealing cover is arranged at the opening of the weighing bottle body to seal the weighing bottle body, and the sealing cover is made of silica gel. The sealed lid of silica gel is convenient for pipettor syringe needle and is inserted into the extraction and squeeze into, and convenient operation is applicable to the solution's of solvent for water preparation. The solute bottle can also adopt the structural form of a bottle body and a silica gel sealing cover. Preferably, the sealing cover is composed of a silicone rubber and an aluminum gland, the silicone rubber being located at the center of the aluminum gland.
The solution prepared by the method provided by the invention is detected by a headspace gas chromatography method and evaluated by an analysis of variance method, and the result uniformity is good. Therefore, the compound can be used as a standard substance, can greatly improve the reliability and the accuracy, and has important significance for detecting and analyzing the quantity transmission and quality control of a laboratory.
The solvent is water, the solute is ethylene oxide as a preferred embodiment, and the preparation process comprises the following steps:
step a: preparing a heat preservation container: putting a heavy object into the bottle body, putting the bottle body into a container filled with water to submerge the bottle body to two thirds of the height, putting the container into a refrigerator to freeze until the water freezes, taking out the completely solidified container from the refrigerator, taking out the solidified bottle body from the container, and forming a groove in the container.
Step b: taking out the solute bottle containing volatile ethylene oxide from the refrigerator, and inserting the solute bottle into the groove in the container for later use;
step c: transferring a certain amount of solvent (water) into a weighing container (a headspace glass bottle with a silica gel sealing cover), and putting the weighing container on a balance to return to zero;
step d: and (3) extracting a certain amount of solute in the solute bottle, quickly pumping the solute into a weighing container (a headspace glass bottle containing a blank aqueous solvent) (the room temperature in the operation process needs to be less than or equal to 4 ℃ or in a refrigeration house), and weighing.
When the preparation concentration is 2000 mug/mL, a 2mL injector is needed to accurately absorb 1.2mL of ethylene oxide (about 1 g), the ethylene oxide is quickly injected into a headspace bottle with blank solvent water (the room temperature is not more than 4 ℃ in the operation process or the operation is carried out in a cold storage), the mixture is slightly shaken (the liquid is not required to be attached to a headspace cover), so that the ethylene oxide raw material is fully dissolved into the solvent, the mixture is placed on a balance, and after the degree is stable, the indication value is recorded.
The liquid in the weighing container is transferred into a 500mL volumetric flask (the weighing amount is 1g, the concentration is 2000 mug/mL) by using a 20mL syringe (with a 80mm needle head), the weighing container (a headspace bottle structure) needs to be cleaned for more than or equal to 5 times by using a blank hydrosolvent, the blank hydrosolvent needs to contact with a bottle cap as little as possible during the first three times, and the blank hydrosolvent needs to be fully shaken after being injected into the solvent during the last two times of cleaning by using the solvent, and then the whole weighing container is transferred into a preparation container (volumetric flask) for constant volume.
Step e: the solution poured into the weighing container was transferred into a preparation container (volumetric flask with empty white water) by a syringe, and diluted to a target volume and a constant volume.
Step f: subpackaging the solution standard substance in the preparation container into ampoule bottles, sealing by melting by using an ampoule bottle sealing machine, and freezing for storage.
Step g: and extracting a certain amount of samples from the finished product by adopting a random number table method, taking two characters from each sample, detecting by adopting a headspace gas chromatography (FID), and evaluating the uniformity by adopting an analysis of variance method.
The following is that the solvent is water, the solute is ethylene oxide solution to detect, namely, 11 samples are extracted from the finished product by a random number table method, each sample takes two characters, headspace gas chromatography (FID) is adopted to detect, variance analysis is adopted to evaluate the uniformity, and the uniformity of the sample is judged by comparing the F test value with the F critical value. The ethylene oxide homogeneity test in water is shown in table 1 below:
TABLE 1
The above data show that the homogeneity of the ethylene oxide characteristic values in water passes the F test, indicating that the homogeneity of the standard is good.
In conclusion, the standard solution preparation method provided by the invention solves the weighing difficulty of volatile standard substances, avoids volatilization of main components in the weighing process, and simultaneously avoids instability of balance reading caused by volatilization, so that the weighing result is more accurate and infinitely approaches to the true value; the standard substance has good uniformity through actual detection, and guarantees quality control and quantity detection in enterprises such as medical instruments, hollow capsules and plastic products. The configuration accuracy and the detection reliability are greatly improved.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A method of preparing a solution of a volatile solute comprising the steps of:
weighing a closed weighing container filled with a solvent;
extracting a preset amount of solute in a liquid state;
pumping the extracted solute into the weighing container;
and weighing the weighing container after the solute is beaten in.
2. The method for preparing a solution of a volatile solute of claim 1 further comprising, before extracting a predetermined amount of solute in a liquid state, the steps of:
and placing a sealed solute bottle containing liquid solute in a heat preservation container, wherein the temperature in the heat preservation container is lower than the boiling temperature of the solute, and the heat preservation container can be an ice bag or dry ice. The best effect is achieved by keeping the ambient temperature below-4 ℃ so that the solute in the solute bottle is kept in a liquid state.
3. A method of preparing a solution of a volatile solute according to claim 2, wherein the extracting of a predetermined amount of solute in liquid state comprises the steps of:
the environment temperature is controlled below-4 ℃, a needle of the liquid transferring device is inserted into the solute bottle, a preset amount of solute is extracted, the solute bottle and the liquid transferring device are inverted, the needle of the liquid transferring device is higher than the liquid height in the solute bottle, the liquid transferring device is operated to extract a preset amount of gas, and the needle of the liquid transferring device is rapidly pulled out of the solute bottle.
4. A method of preparing a solution of volatile solutes according to claim 3, characterized in that the extraction of a predetermined amount of solutes comprises in particular the steps of:
and pumping a small amount of solute into the liquid transfer device, pumping the solute in the liquid transfer device back into the solute bottle, and pumping a preset amount of solute into the liquid transfer device.
5. The method for preparing a solution of a volatile solute according to claim 1, further comprising the following steps after weighing the weighing container after the solute is beaten in:
using a pipettor to extract all liquid in the weighing container;
the liquid in the liquid transfer device is driven into a preparation container containing a preset amount of solvent.
6. A method of preparing a solution of a volatile solute according to claim 5, wherein the step of using a pipette to extract all of the liquid in the weighing container comprises the steps of:
and inserting the pipette needle into the weighing container for extraction, and pulling out the pipette needle from the weighing container when the pressure in the weighing container is less than the external atmospheric pressure.
7. A method of preparing a solution of a volatile solute according to claim 5, wherein the step of using a pipette to extract all of the liquid in the weighing container comprises the steps of:
the method comprises the steps of inserting a pipette needle into a weighing container for extraction, after all liquid is extracted, continuing to operate the pipette to extract gas with a preset amount, inverting the pipette and the weighing container to enable the pipette to be below the weighing container, and rapidly pulling out the pipette needle from the weighing container.
8. The method for preparing a solution of a volatile solute according to claim 2, wherein said method for preparing a thermal container comprises the steps of:
putting an object into a container filled with liquid, so that the liquid in the container partially submerges the object, putting the container into a refrigerator for freezing until the liquid is completely solidified, taking the container out of the refrigerator, taking the object out of the container, and forming the container into the heat-preservation container, wherein the container is internally provided with a groove; or an ice bag or dry ice may be substituted.
9. The method for preparing a solution of a volatile solute according to claim 1, wherein the weighing container includes a weighing bottle and a sealing cap, the sealing cap is disposed at an opening of the weighing bottle to seal the weighing bottle, and the sealing cap is made of silica gel.
10. A method of preparing a solution of volatile solutes according to claim 1, wherein pumping the extracted solutes into the weighing receptacle comprises the steps of:
and pumping the extracted solute into a weighing container by using a liquid transfer device, inserting a needle of the liquid transfer device into the weighing container, positioning the needle above the liquid level in the weighing container, and pumping the solute in the liquid transfer device into the weighing container.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111438742.9A CN114264535A (en) | 2021-11-29 | 2021-11-29 | Method for preparing solution of volatile solute |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111438742.9A CN114264535A (en) | 2021-11-29 | 2021-11-29 | Method for preparing solution of volatile solute |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114264535A true CN114264535A (en) | 2022-04-01 |
Family
ID=80825851
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111438742.9A Pending CN114264535A (en) | 2021-11-29 | 2021-11-29 | Method for preparing solution of volatile solute |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114264535A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102247901A (en) * | 2011-04-14 | 2011-11-23 | 山东电力研究院 | Measuring flask used for preparation of volatile standard solution and application method thereof |
| CN103728164A (en) * | 2012-10-16 | 2014-04-16 | 辽宁奥克化学股份有限公司 | Method for preparing epoxy compound standard solution and method for measuring concentration of epoxy compound |
| CN105259014A (en) * | 2015-11-04 | 2016-01-20 | 中国汽车技术研究中心 | VOCs solution measuring method and standard gas preparation method |
| CN106769369A (en) * | 2016-12-07 | 2017-05-31 | 中国计量科学研究院 | Prepare container, the device and method of the organic mixed solution standard substance of volatility |
| CN106908545A (en) * | 2017-03-23 | 2017-06-30 | 苏州桓晨医疗科技有限公司 | A kind of detection method of minimal residue oxirane |
| CN107860853A (en) * | 2017-12-15 | 2018-03-30 | 吉林化工学院 | A kind of needle type extraction device and its application method for concentrating volatile benzene homologues |
| CN111656082A (en) * | 2018-01-12 | 2020-09-11 | 亚致力气体科技有限公司 | Thermal cascade for cryogenic storage and transport of volatile gases |
-
2021
- 2021-11-29 CN CN202111438742.9A patent/CN114264535A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102247901A (en) * | 2011-04-14 | 2011-11-23 | 山东电力研究院 | Measuring flask used for preparation of volatile standard solution and application method thereof |
| CN103728164A (en) * | 2012-10-16 | 2014-04-16 | 辽宁奥克化学股份有限公司 | Method for preparing epoxy compound standard solution and method for measuring concentration of epoxy compound |
| CN105259014A (en) * | 2015-11-04 | 2016-01-20 | 中国汽车技术研究中心 | VOCs solution measuring method and standard gas preparation method |
| CN106769369A (en) * | 2016-12-07 | 2017-05-31 | 中国计量科学研究院 | Prepare container, the device and method of the organic mixed solution standard substance of volatility |
| CN106908545A (en) * | 2017-03-23 | 2017-06-30 | 苏州桓晨医疗科技有限公司 | A kind of detection method of minimal residue oxirane |
| CN107860853A (en) * | 2017-12-15 | 2018-03-30 | 吉林化工学院 | A kind of needle type extraction device and its application method for concentrating volatile benzene homologues |
| CN111656082A (en) * | 2018-01-12 | 2020-09-11 | 亚致力气体科技有限公司 | Thermal cascade for cryogenic storage and transport of volatile gases |
Non-Patent Citations (1)
| Title |
|---|
| 李玲 等: "生物学实验技术", 30 November 2001, 湖南科学技术出版社, pages: 8 - 15 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Scholander | Analyzer for accurate estimation of respiratory gases in one-half cubic centimeter samples | |
| Scholander et al. | Micro gasometric determination of dissolved oxygen and nitrogen | |
| Riley et al. | A bubble method for estimation of PCO2 and PO2 in whole blood | |
| Suurkuusk et al. | Design and testing of an improved precise drop calorimeter for the measurement of the heat capacity of small samples | |
| JP3279320B2 (en) | Liquid container | |
| US4557899A (en) | Water-in-oil testing apparatus | |
| CN103743647A (en) | Device and method for rapidly determining content of nitrogen in edible vegetable oil | |
| CN114264535A (en) | Method for preparing solution of volatile solute | |
| CN105547909B (en) | Component volatile depth de gassed solution compound method and vapour-pressure test method | |
| Christiansen et al. | tion of Molecular Weight of some Specimens of Potassium Hyaluronate | |
| CN103512780B (en) | A kind of Acid Hydrolytic Hydrocarbon preparation facilities and lossless collection method thereof | |
| Friis-Hansen | The measurement of deuterium oxide at low concentrations by the gradient tube method | |
| Pettenkofer | XXIX.—Volumetric estimation of atmospheric carbonic acid | |
| US3536106A (en) | Method for measurement and transfer of small fluid volumes | |
| US3478575A (en) | Liquid dilatometer | |
| SU1749772A1 (en) | Method for determining density of substances and device | |
| CN203732396U (en) | Device for quickly determining nitrogen content in edible vegetable oil | |
| Schütz | Experiments on foam time. Part I. The method of measuring foam time and some experiments with saponin and methyl cellulose | |
| US3180132A (en) | Method for calibrating microanalytical instruments and apparatus therefor | |
| Page et al. | Stability study of nitroglycerin sublingual tablets | |
| CN207887188U (en) | A kind of reagent bottle | |
| Ferguson | The many uses of disposable plastic hypodermic syringes− A shot in the arm for small equipment budgets | |
| US3402597A (en) | Method and apparatus for the determination of the molecular weight of organic chemical compounds | |
| US4521377A (en) | Flow through gas analyzer | |
| Gupta et al. | Analysis of Physicochemical Aspects of Milk |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
Address after: Room 801, building 5, Changzhou inspection and testing industrial park, Changzhou City, Jiangsu Province 213000 Applicant after: Changzhou Manhag Testing Technology Co.,Ltd. Address before: 213000 Black Peony Science Park, Tianning District, Changzhou City, Jiangsu Province Applicant before: Manhag Testing Technology Co.,Ltd. |
|
| CB02 | Change of applicant information | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20230913 Address after: 101100 second floor, building 63, No. 15, Jingsheng South 4th Street, Jinqiao Science and technology industrial base, Tongzhou Park, Zhongguancun Science and Technology Park, Tongzhou District, Beijing Applicant after: Beijing Manhattan Biotechnology Co.,Ltd. Address before: Room 801, building 5, Changzhou inspection and testing industrial park, Changzhou City, Jiangsu Province 213000 Applicant before: Changzhou Manhag Testing Technology Co.,Ltd. |
|
| TA01 | Transfer of patent application right |