CN101504350B - Method for sealing sample room of mercury porosimeter - Google Patents
Method for sealing sample room of mercury porosimeter Download PDFInfo
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- CN101504350B CN101504350B CN2009101112639A CN200910111263A CN101504350B CN 101504350 B CN101504350 B CN 101504350B CN 2009101112639 A CN2009101112639 A CN 2009101112639A CN 200910111263 A CN200910111263 A CN 200910111263A CN 101504350 B CN101504350 B CN 101504350B
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- washer
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- pad
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Abstract
The invention discloses a method for sealing a sample room of a mercury injection apparatus and relates to technology for sealing the sample room of the mercury injection apparatus. The invention provides a method which has simple operation, can be repeatedly used, does not pollute a sample and is used for sealing the sample room of the mercury injection apparatus. A hollow annular washer is arranged between a plane of a polished mouth of a quartz glass sample cell of the mercury injection apparatus and a plane of a stainless steel contact component as an electrode; the size of the inside diameter and the outside diameter of the washer is the same as the polished mouth of the quartz glass sample cell; and the thickness of the washer is between 0.1 and 1.0 mm. The washer can be a molecular material washer, a soft metal washer or a graphite washer. The method adopts the washer to replace vacuum grease to realize the sealing of the sample room; and as the washer is a solid flake with a regular shape, the washer has good deformation and buffering capacity, is simple to operate, does not pollute the sample and can be repeatedly used. Moreover, as the thickness and the diameter of the washer are controllable, the quality of the injected mercury is relatively stable and the accuracy and the precision of the test are improved. Simultaneously, the method is safe and reliable and can prevent the sample cell breaking.
Description
Technical field
The present invention relates to a kind of technology that is used for sealing sample room of mercury porosimeter.
Background technology
Mercury injection apparatus is to utilize mercury intrusion method to measure the advanced instrument equipment of material internal microcosmic air hole structure, have that sample size is little, test result accurately and advantage such as good reproducibility.Mercury injection apparatus is measured the material pore structure and is divided into four steps: the notes mercury of the assembling of sample chamber, sample, boost gaging hole and step-down [Zhang Baoming, Zou Fangyong. Shandong chemical industry, 1997, (1): 47-50].During test when observing low pressure injection mercury in the sample cell mercury whether be full of sample cell adopting quartz glass generally speaking fully.The sealing of sample chamber is finished by ground plane, quartz glass samples pond with as the pressurization of the stainless steel contact assembly plane of electrode, the glass ground joint plane be coated with vacuum grease [Wang Yulong, Cao Zhenlei, Wang Yanzhong. Chinese papermaking, 2006,25 (3): 19-21].Can fill up the whole sample chamber in order to ensure mercury when annotating mercury at the low pressure station, vacuum tightness often needs to reach below the 1000.0 μ mHg, requires the vacuum grease thickness that is coated with suitable and can not be coated on the inside surface, in order to avoid contaminated samples influences test result.In addition, when screwing with following sample cell lid, firmly wants evenly on last sample cell lid, otherwise particularly (pressure can be up to 60000psi at high pressure in test process, about 4082.8atm) test the time causes that stress is concentrated and causes sample cell to break, test crash not only, and can cause mercury leakage pollution surrounding environment or high-pressure work station.
Because the actuating medium of mercury injection apparatus is the bigger liquid metal mercury of toxicity, needs the special messenger to operate generally speaking.Higher in the assembling process of sample chamber with the technical requirement of vacuum grease sealing, break if assemble improper the failure of an experiment or the sample cell of causing easily.The each experiment of vacuum grease all needs to smear again, owing to smear the inhomogeneous gas leakage that causes, then needs to clean again sample cell glass ground joint and stainless steel contact electrode assembly etc. sometimes; Thickness, position and the mass discrepancy of smearing during the vacuum grease sealing bigger at every turn, and then the mercury quality of influence injection.According to the principle of mercury injection apparatus working sample volume, keeping each empty sample cell to annotate the constant of mercury quality is the calculation sample volume, and the pacing items of physical quantitys such as the porosity relevant with volume, apparent density and real density.For the analytical test of precious sample or the few sample of amount, sample is pollution-free, guarantee disposable notes mercury success and keep sample cell notes mercury constant mass just to seem particularly important.
Summary of the invention
Purpose of the present invention be intended to provide a kind of easy and simple to handle, can reuse, contaminated samples not, be used for the method for sealing sample room of mercury porosimeter.
The method of sealing sample room of mercury porosimeter that is used for of the present invention is for to establish a hollow and annular pad on ground plane, mercury injection apparatus quartz glass samples pond with as the stainless steel contact assembly interplanar of electrode, the inner and outer diameter size of pad is with quartz glass samples Chi Mokouchu, thickness 0.1～1.0mm.
Pad can be macromolecular material pad, soft metal pad or Graphite pad etc.
Described macromolecular material is macromolecular material and their compound substances such as silicon rubber, rubber, plastics, nylon.
Described soft metal is copper, aluminium, silver, gold or lead etc.
The present invention adopts pad to replace vacuum grease to realize the sealing of sample chamber, and the stress of buffering sample chamber assembly in assembling process is concentrated, and prolongs the serviceable life of sample cell.Gasket material has good deformation and buffering ability, and size is suitable with quartz glass samples Chi Mokouchu.Because pad is the solid thin-sheet of regular shape, operate very simple, and can contaminated samples.Low as working pressure, reusable 5～20 times of pad, (60000psi) also can reuse 1～3 time under the high pressure.Because the thickness and the controllable diameter of pad, therefore the mercury quality of injecting is relatively stable.Like this, according to putting into the also corresponding raising of accuracy of annotating sample volume, porosity, apparent density and real density that the mercury qualitative difference calculates before and after the sample with precision.By with the gasket seal among the present invention and traditional vacuum grease sealing standard model being tested, the result shows peak shape and the not influence of peak position of testing collection of illustrative plates, reliable test result.In addition, use this encapsulating method,, the sample cell incident of breaking takes place seldom also in Hi-pot test even new start-up operates the computer.
Description of drawings
Fig. 1 is the user mode synoptic diagram of the embodiment of the invention.
The pad cut-open view that Fig. 2 adopts for the embodiment of the invention.
The pad floor map that Fig. 3 adopts for the embodiment of the invention.
Embodiment
The invention will be further described below by embodiment.
Embodiment 1: adopt U.S. Quan-tachrome company mercury injection apparatus, the formation of its sample chamber is seen Fig. 1, and corresponding with each label is respectively: quartz glass samples pond 1, last sample cell lid 2, O shape circle 3, sample cell ground 4, pad 5, stainless steel electrode contact assembly 6 and following sample cell lid 7.Fig. 2 is the cut-open view of pad 5, and Fig. 3 is the floor map of pad 5, and internal diameter is that A, external diameter are B, and thickness is H.Wherein A is consistent with the interior external diameter of sample cell ground respectively with B.With thickness H is in the middle of the silicon rubber pad 5 of 0.5mm is placed on sample cell ground 4 and stainless steel electrode contact assembly 6 sample chamber to be sealed.To the aperture is the porous SiO of 7.3 ± 0.5nm
2Standard model is tested, and the low pressure injection mercury pumpdown time that vacuum tightness reaches 1000.0 μ mHg is 12min, and the aperture that test result obtains is 7.36nm.
Embodiment 2: method of testing such as embodiment 1, and it is the nylon spacer of 0.1mm that thickness is adopted in sealing, and the low pressure pumpdown time is 13min, and the aperture that test obtains is 7.48nm.
Embodiment 3: method of testing such as embodiment 1, and it is the rubber sheet gasket of 1.0mm that thickness is adopted in sealing, and the low pressure pumpdown time is 10min, and the aperture that test obtains is 7.38nm.
Embodiment 4: method of testing such as embodiment 1, and it is the aluminium flake of 0.3mm that thickness is adopted in sealing, and the low pressure pumpdown time is 14min, and the aperture that test obtains is 7.42nm.
Embodiment 5: method of testing such as embodiment 1, and it is the Graphite pad of 0.7mm that thickness is adopted in sealing, and the low pressure pumpdown time is 11min, and the aperture that test obtains is 7.38nm.
Embodiment 6: method of testing such as embodiment 1, and it is the multiple aluminium foil pad of the low foaming of low-density polyethylene (LDPE) of 0.6mm that thickness is adopted in sealing, and the low pressure pumpdown time is 11min, and the aperture that test obtains is 7.35nm.
Comparative Examples: method of testing such as embodiment 1, with vacuum grease sample room of mercury porosimeter is sealed, the low pressure pumpdown time is 12min, the aperture that test obtains is 7.38nm.
Claims (3)
1. a method that is used for sealing sample room of mercury porosimeter is characterized in that on ground plane, mercury injection apparatus quartz glass samples pond and establishes a hollow and annular pad as the stainless steel contact assembly interplanar of electrode the sample chamber is sealed; The inner and outer diameter size of described pad is with quartz glass samples Chi Mokouchu, and the thickness of pad is 0.1～1.0mm, and pad is macromolecular material pad, soft metal pad or Graphite pad.
2. a kind of method that is used for sealing sample room of mercury porosimeter as claimed in claim 1 is characterized in that described macromolecular material is silicon rubber, rubber, plastics, nylon and their compound substance.
3. a kind of method that is used for sealing sample room of mercury porosimeter as claimed in claim 1 is characterized in that described soft metal is copper, aluminium, silver, gold or plumbous.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101112639A CN101504350B (en) | 2009-03-13 | 2009-03-13 | Method for sealing sample room of mercury porosimeter |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101112639A CN101504350B (en) | 2009-03-13 | 2009-03-13 | Method for sealing sample room of mercury porosimeter |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101504350A CN101504350A (en) | 2009-08-12 |
| CN101504350B true CN101504350B (en) | 2011-01-26 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009101112639A Expired - Fee Related CN101504350B (en) | 2009-03-13 | 2009-03-13 | Method for sealing sample room of mercury porosimeter |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2037413U (en) * | 1988-10-12 | 1989-05-10 | 浙江省玉环县沙鳝密封器材厂 | Composite sealing ring |
| CN2252913Y (en) * | 1996-07-30 | 1997-04-23 | 北京清华大学太阳能电子厂 | Sealing ring with wave-shape inner wall |
| CN2606349Y (en) * | 2003-04-07 | 2004-03-10 | 石油大学(华东)石仪科技实业发展公司 | Pressure differential mercury instrument |
| CN1514228A (en) * | 2002-12-31 | 2004-07-21 | 中国石油化工股份有限公司 | Void structure instrument |
| CN1673762A (en) * | 2005-04-26 | 2005-09-28 | 重庆大学 | Gasinsulation combined electric device local discharge analog experimental apparatus and experimental method |
| CN1696546A (en) * | 2004-05-14 | 2005-11-16 | 宁波天生密封件有限公司 | Sealing gasket and manufacturing method |
-
2009
- 2009-03-13 CN CN2009101112639A patent/CN101504350B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2037413U (en) * | 1988-10-12 | 1989-05-10 | 浙江省玉环县沙鳝密封器材厂 | Composite sealing ring |
| CN2252913Y (en) * | 1996-07-30 | 1997-04-23 | 北京清华大学太阳能电子厂 | Sealing ring with wave-shape inner wall |
| CN1514228A (en) * | 2002-12-31 | 2004-07-21 | 中国石油化工股份有限公司 | Void structure instrument |
| CN2606349Y (en) * | 2003-04-07 | 2004-03-10 | 石油大学(华东)石仪科技实业发展公司 | Pressure differential mercury instrument |
| CN1696546A (en) * | 2004-05-14 | 2005-11-16 | 宁波天生密封件有限公司 | Sealing gasket and manufacturing method |
| CN1673762A (en) * | 2005-04-26 | 2005-09-28 | 重庆大学 | Gasinsulation combined electric device local discharge analog experimental apparatus and experimental method |
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| CN101504350A (en) | 2009-08-12 |
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Granted publication date: 20110126 Termination date: 20140313 |