CN104049045A - Gas phase needle maintenance method for high-viscosity or high-freezing point substances - Google Patents
Gas phase needle maintenance method for high-viscosity or high-freezing point substances Download PDFInfo
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- CN104049045A CN104049045A CN201410215756.8A CN201410215756A CN104049045A CN 104049045 A CN104049045 A CN 104049045A CN 201410215756 A CN201410215756 A CN 201410215756A CN 104049045 A CN104049045 A CN 104049045A
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Abstract
The invention discloses a gas phase needle maintenance method for high-viscosity or high-freezing point substances. The method comprises the following four steps: 1, selecting a low-viscosity solvent as a solvent for gas chromatographic detection; 2, taking out a sample introduction needle and cleaning the sample introduction needle with the low-viscosity solvent 5 to 8 times by using an automatic cleaning device before sample introduction; 3, cleaning the sample introduction needle with the low-viscosity solvent more than 10 times immediately after completion of sample introduction; and 4, regularly detecting and cleaning the sample introduction needle in a period from completion of usage of the sample introduction needle to next-time usage of the sample introduction needle. The gas phase needle maintenance method for high-viscosity or high-freezing point substances provides cleaning steps and cleaning pace for gas phase needles from all the aspects, can realize effective, regular and real-time cleaning and maintenance of gas phase needles at regular intervals, effectively improves the usage efficiency of gas phase needles, enhances experimental accuracy, effectively saves experimental time, prolongs the service life gas phase needles and saves experimental cost.
Description
Technical field
The gas phase pin maintaining method that the present invention relates to a kind of high viscosity or high-solidification point material, belongs to chemical area of maintenance.
Background technology
Gas phase auto injection pin is parts very crucial in gas phase, is also the parts that frequency of utilization is the highest, and it is related to accuracy and the precision of test.Good use habit and maintenance mode can effectively ensure stable long-term test.In test process, often can run into a lot of problems.
Liquid substance equally, high viscosity or high-solidification point (0-25 DEG C) material, in the time of gas phase quantitative test, can run into the amount that residual, the material of material in sample introduction needle enter gassy system analysis and can not reappear, use for a long time and there will be that sample introduction needle piston is astringent even to be blocked.
At present, we investigate repetition sample introduction, and whether 6 pin sample introduction measured matter peak area RSD meet≤2.0%.If can not meet, it is likely the problem of sample introduction needle.Need maintenance clean.In existing laboratory, may just adopt interim use then just to expect cleaning or safeguarding, not have systematic maintaining method, therefore, studying the gas phase pin maintaining method of a kind of high viscosity or high-solidification point material, is the easily problem of ignorance of worker of chemical field, the damage that may bring sample introduction needle.
Summary of the invention
The object of this invention is to provide the gas phase pin maintaining method of a kind of high viscosity or high-solidification point material, to solve in above-mentioned prior art a still unsolved difficult problem.
The technical solution used in the present invention is: the gas phase pin maintaining method of a kind of high viscosity or high-solidification point material, and its innovative point is: the maintaining method of described gas phase pin comprises first, second and third and four steps;
Described first step is that the solvent using while selecting gas chromatographic detection is low viscosity solvent;
Described second step, for taking out sample introduction needle, adopts automatic flushing device to use for 5～8 times low viscosity solvent to clean before sampling; Described the 3rd step used low viscosity solvent to clean more than 10 times for after having tested immediately; Described the 4th step is between operating period next time, to make regular check on cleaning sample introduction needle after use finishes.
Further, the material of described high-solidification point is solidifying point at the material of 0～50 degree Celsius.
Further, described high-viscosity material is 2-(2-(2-methoxy ethoxy) ethoxy) acetic acid or the bromo-2-butine of 1-.
Further, described high-solidification point material is the chloro-4-fluoroaniline of di-tert-butyl dicarbonate, 3-or 3-methyl isophthalic acid-phenyl-2-phosphorylation alfin-1-oxide.
Further, the low viscosity solvent of selecting in described first step is do not react with measured matter and in chromatogram, do not produce the low viscosity solvent disturbing.
Further, described low viscosity solvent is methenyl choloride, methylene chloride, acetone, methyl alcohol, acetonitrile, normal hexane or normal heptane.
Further, described in, making regular check on middle sample introduction needle occurs when piston has some setbacks or foreign matter is residual cleaning; Described cleaning, for first using hot water ultrasonic cleaning, is then used methyl alcohol ultrasonic cleaning, finally uses normal hexane ultrasonic cleaning.
Beneficial effect: the gas phase pin maintaining method of this high viscosity of the present invention or high-solidification point material; the cleaning step of gas phase pin is provided in all its bearings and has cleaned rhythm; effectively regularly real-time cleaning and maintenance of the carrying out of rule; accomplish effectively to improve on the one hand the service efficiency of gas phase pin; increase experiment accuracy rate; effectively save experimental period; extend on the other hand the serviceable life of gas phase pin; save experimental cost; set about from details drop; economize on resources, protection of the environment, realizes sustainable economic development.
Embodiment
Implementation column below can make those skilled in the art more fully understand the present invention, but does not therefore limit the present invention among described scope of embodiments.
embodiment 1
Laboratory sample is the bromo-2-butine of 1-, and selection low viscosity solvent is normal hexane, has both reduced the viscosity of measured object, avoids solvent and measured matter to react simultaneously and produces and disturb in chromatogram.
First take out sample introduction needle, before sampling, adopt automatic flushing device to use for 5 times low viscosity solvent to clean, then use sample introduction needle to carry out sample introduction, then after having tested, using immediately low viscosity solvent to clean 10 times properly places afterwards, prevent from producing solidification phenomenon after measured matter residual in pin is due to solvent evaporates, easy disposable breaking or bending pin piston when used next time, finally make regular check on cleaning step, general, 1-2 days when frequency of utilization is high, general use inspection in 3-4 days once, observe sample introduction needle and whether occur the phenomenon that piston has some setbacks, whether there is atrament to remain in pin, simulation sample introduction is whether spray liquid is vertical.
If while finding that foreign matter or piston have some setbacks, first use hot water ultrasonic cleaning, then use methyl alcohol ultrasonic cleaning, finally with normal hexane ultrasonic cleaning.
The sample introduction needle of the present embodiment, undertaken after a series of maintaining by this method, obviously increase service time, generally can use 2～3 years, the present embodiment effectively improves the service efficiency of gas phase pin on the one hand, increases experiment accuracy rate, effectively saves experimental period, extend on the other hand the serviceable life of gas phase pin, save experimental cost.
embodiment 2
Laboratory sample is di-tert-butyl dicarbonate, and selection low viscosity solvent is normal heptane, and the selection of low viscosity solvent had both reduced the viscosity of measured object, avoids solvent and measured matter to react simultaneously and produces and disturb in chromatogram.
First take out sample introduction needle, before sampling, adopt automatic flushing device to use for 6 times low viscosity solvent to clean, then use sample introduction needle to carry out sample introduction, then after having tested, using immediately low viscosity solvent to clean 20 times properly places afterwards, prevent from producing solidification phenomenon after measured matter residual in pin is due to solvent evaporates, easy disposable breaking or bending pin piston when used next time, finally make regular check on cleaning step, general, 1-2 days when frequency of utilization is high, general use inspection in 3-4 days once, observe sample introduction needle and whether occur the phenomenon that piston has some setbacks, whether there is atrament to remain in pin, simulation sample introduction is whether spray liquid is vertical.
If while finding that foreign matter or piston have some setbacks, first use hot water ultrasonic cleaning, then use methyl alcohol ultrasonic cleaning, finally with normal hexane ultrasonic cleaning.
The sample introduction needle of the present embodiment, undertaken after a series of maintaining by this method, obviously increase service time, generally can use 2～3 years, the present embodiment effectively improves the service efficiency of gas phase pin on the one hand, increases experiment accuracy rate, effectively saves experimental period, extend on the other hand the serviceable life of gas phase pin, save experimental cost.
Claims (7)
1. a gas phase pin maintaining method for high viscosity or high-solidification point material, is characterized in that: the maintaining method of described gas phase pin comprises first, second and third and four steps; Described first step is that the solvent using while selecting gas chromatographic detection is low viscosity solvent; Described second step, for taking out sample introduction needle, adopts automatic flushing device to use for 5～8 times low viscosity solvent to clean before sampling;
Described the 3rd step used low viscosity solvent to clean more than 10 times for after having tested immediately;
Described the 4th step is between operating period next time, to make regular check on cleaning sample introduction needle after use finishes.
2. the gas phase pin maintaining method of high viscosity according to claim 1 or high-solidification point material, is characterized in that: the material of described high-solidification point is solidifying point at the material of 0～50 degree Celsius.
3. the gas phase pin maintaining method of high viscosity according to claim 1 or high-solidification point material, is characterized in that: described high-viscosity material is 2-(2-(2-methoxy ethoxy) ethoxy) acetic acid or the bromo-2-butine of 1-.
4. the gas phase pin maintaining method of high viscosity according to claim 1 or high-solidification point material, is characterized in that: described high-solidification point material is the chloro-4-fluoroaniline of di-tert-butyl dicarbonate, 3-or 3-methyl isophthalic acid-phenyl-2-phosphorylation alfin-1-oxide.
5. the gas phase pin maintaining method of high viscosity according to claim 1 or high-solidification point material, is characterized in that: the low viscosity solvent of selecting in described first step is do not react with measured matter and in chromatogram, do not produce the low viscosity solvent disturbing.
6. the gas phase pin maintaining method of high viscosity according to claim 1 and 2 or high-solidification point material, is characterized in that: described low viscosity solvent is methenyl choloride, methylene chloride, acetone, methyl alcohol, acetonitrile, normal hexane or normal heptane.
7. the gas phase pin maintaining method of high viscosity according to claim 1 or high-solidification point material, is characterized in that: described in make regular check on middle sample introduction needle and occur when piston has some setbacks or foreign matter is residual cleaning; Described cleaning, for first using hot water ultrasonic cleaning, is then used methyl alcohol ultrasonic cleaning, finally uses normal hexane ultrasonic cleaning.
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| CN201410215756.8A CN104049045A (en) | 2014-05-21 | 2014-05-21 | Gas phase needle maintenance method for high-viscosity or high-freezing point substances |
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| CN201410215756.8A CN104049045A (en) | 2014-05-21 | 2014-05-21 | Gas phase needle maintenance method for high-viscosity or high-freezing point substances |
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Application publication date: 20140917 |