CN100458402C - Accurate check weighing method of density for micro sample - Google Patents

Accurate check weighing method of density for micro sample Download PDF

Info

Publication number
CN100458402C
CN100458402C CNB2004100105033A CN200410010503A CN100458402C CN 100458402 C CN100458402 C CN 100458402C CN B2004100105033 A CNB2004100105033 A CN B2004100105033A CN 200410010503 A CN200410010503 A CN 200410010503A CN 100458402 C CN100458402 C CN 100458402C
Authority
CN
China
Prior art keywords
density
sample
compound liquid
quality
wiry
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.)
Expired - Fee Related
Application number
CNB2004100105033A
Other languages
Chinese (zh)
Other versions
CN1796971A (en
Inventor
侯明东
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Institute of Modern Physics of CAS
Original Assignee
Institute of Modern Physics of CAS
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Institute of Modern Physics of CAS filed Critical Institute of Modern Physics of CAS
Priority to CNB2004100105033A priority Critical patent/CN100458402C/en
Publication of CN1796971A publication Critical patent/CN1796971A/en
Application granted granted Critical
Publication of CN100458402C publication Critical patent/CN100458402C/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Abstract

The invention relates to a sample density high-accuracy measuring method, especially relating to a micro sample density high-accuracy measuring method, comprising: connecting a to-be-measured sample with a wire with a known accurate density less than the density of a dipping solution; immersing the sample-wire combined body in a compound solution with an accurate density, where the density of the compound solution is more than that of the wire but less than that of the sample; gradually and accurately regulating the mass of the wire until the sample-wire combined body is suspended in the compound solution; taking out the combined body and weighing them separately; and calculating the sample density by formula. The invention measures the sample density by floating technique and the outstanding character of the method is that it has a considerably high accuracy of measuring milligram-level micro sample density, able to be less than 0.5%.

Description

The method that tiny sampler density is accurately measured
Technical field:
The present invention relates to the pinpoint accuracy measuring method of sample rate, relate in particular to the measuring method of the pinpoint accuracy of tiny sampler density.
Background technology:
The amorphous material of heavy ion irradiation manifests a kind of anisotropic growth phenomenon at low temperatures.For distinguishing that whether this growth phenomenon follows the change of density, must carry out the accurate measurement of density.Because the size of irradiation sample generally is about 5mm * 1mm * 10 μ m, the about 0.4mg of weight, it also is very small changing if any density behind the irradiation, is difficult to survey.So in density measure, require to have extra high precision.
The conventional method of density measurement is that both are divided by then by the quality of Measuring Object and volume, and obtains the density of this object.Generally speaking, the measurement of quality can reach very high precision, but the measurement of volume is quite difficult, particularly to small sample or sample in irregular shape, is difficult to reach very high precision, thereby causes the tiny sampler density measure to become a difficult problem.
Summary of the invention:
The method that the objective of the invention is to avoid the deficiencies in the prior art part and provide a kind of tiny sampler density accurately to measure.Its feature be can be quality less than the density measure of the tiny sampler of 0.5mg to the precision that is better than 5 ‰.
Purpose of the present invention can be by realizing by the following technical solutions: the method that a kind of tiny sampler density is accurately measured, and its principal feature includes:
A. testing sample is connected with the tinsel of the known accurate density littler than compound liquid density.
B. tinsel is wrapped in and is immersed on the sample in the compound liquid of accurate demarcation density, compound liquid density is greater than described density of wires, and sample rate is greater than compound liquid density; The difference of thermostat temperature that compound liquid presets and breadboard room temperature is less than 1.0 ℃, to avoid the heat interchange between compound liquid liquid level and the air.
C. by to described tinsel progressively cutting diameter less than the filament of 0.05mm, thereby the quality wiry of progressively accurately adjusting known accurate density reaches and is wound with sample wiry presents the suspended state that neither rising does not also descend in compound liquid.
D. take out and be wound with sample wiry, sample and tinsel are accurately weighed respectively.
E. utilize following formula to calculate the density of testing sample:
D s＝M sD lD/[M sD-(D l-D)M]
Wherein: M sBe respectively the quality and the quality wiry of testing sample, D with M s, D and D lBe respectively the density of the density of testing sample, density wiry and compound liquid.
The scaling method of the accurate demarcation density of described compound liquid is:
A. with the highly purified metal sample of known density: golden Au, copper Cu, tantalum Ta, nickel, titanium Ti after one or more dispose an amount of aluminium wire respectively, are immersed in the compound liquid of density to be measured.
B. make it in the compound liquid of density to be measured, be suspended state.
C. take out metal sample and aluminium wire, and accurately weigh respectively.
D. utilize following formula computerized compound fluid density:
D l＝(M m+M Al)D mD Al/(M mD Al+M AlD m)
Wherein: D l, D mAnd D AlBe respectively the density of compound liquid, the density of used high pure metal and the density of aluminium.M mAnd M AlBe respectively the quality of used high pure metal and the quality of aluminium wire.Other symbolic significances are the same.As demarcating immersion liquid density with multiple metal, available least square method is tried to achieve average immersion liquid density.
The material wiry of the known density of the method that described tiny sampler density is accurately measured is aluminium Al.The compound liquid that described warp is accurately demarcated density is diiodomethane CH 2I 2, or be (CH 3) 2SnI 2, ClCBr 3, FCHI 2, FCBr 3, Br 3CNO 2, CHBr 3, Br 3CCH 2Br.
The invention has the beneficial effects as follows, this technology is come measuring samples density by flotation technique, the most outstanding characteristics of this method have quite high precision to the tiny sampler of milligram level, can be better than 0.5%, and the color density measuring method are bigger for small like this sample measurement error.Present technique also is applicable to the density measure of the sample of logarithm gram magnitude.
Description of drawings:
Be described in further detail below in conjunction with the most preferred embodiment shown in the accompanying drawing:
Fig. 1 is a small sample density measuring equipment structural representation of the present invention.Among the figure, 1 is the sample measurement cup, and 2 is thermostat water bath, and 3 is recirculated water, and 4 is testing sample, and 5 is high-purity aluminium wire, and 6 is immersion liquid.In the sample measurement cup immersion liquid is housed, the association of testing sample and aluminium wire should place immersion liquid, and thermostat water bath and recirculated water are for immersion liquid being remained on a stationary temperature.Be the suspended state of the association that can observe testing sample and aluminium wire, sample measurement cup and thermostat water bath are transparent.
Embodiment:
Fig. 1 provides the synoptic diagram of measurement mechanism.20 ℃ of diiodomethane density of liquid is 3.320g/cm 3, this density is greater than the density of metallic aluminium.Therefore, when aluminium is placed this liquid, aluminium will swim in the surface of liquid.And when the density of testing sample during greater than the diiodomethane density of liquid, sample will sink in diiodomethane liquid.If the aluminium wire of a suitable quantity is wrapped in the sample that is wound with aluminium wire is floated on a liquid, neither rise, also not sink.To reach this state exactly during density measure.Embodiment is as follows:
A. with testing sample 4 with than immersion liquid 6 diiodomethane (CH 2I 2) metal aluminum filament 5 of the known accurate density that density is little connects.Used aluminium wire is 99.999% high-purity aluminium wire, and its diameter depends on the size of the sample quality of density to be measured.Sample can use thicker aluminium wire when heavy, causes adhering to of bubble in order to avoid the aluminium wire of use is long.In addition, also should there be a kind of diameter only to be the aluminium wire of 0.05mm, as adjusting the quality of twining aluminium wire.
B. metal aluminum filament 5 is wrapped in the compound liquid 6 diiodomethane (CH that are immersed on the sample 4 through accurate demarcation density 2I 2) in, this compound liquid 6 diiodomethane (CH 2I 2) density greater than the density of described metal aluminum filament 5, and less than the density of sample 4.
C. reach the sample 4 that is wound with metal aluminum filament 5 by the quality of progressively accurately adjusting the metal aluminum filament 5 of known accurate density and in compound liquid 6, present the suspended state that neither rising does not also descend.Adjusting metal aluminum filament 5 method for quality is that progressively cutting diameter only is the aluminium wire of 0.05mm.The long diameter of 1mm is that the aluminium wire quality of 0.05mm only is 5.29 micrograms, and the adjustment that cut a few microgram quality at 0.1mm realization zero point has no difficulty.When the quality of adjusting winding aluminium wire 5 suspends the sample 4 that is wound with metal aluminum filament 5, should make aluminium wire peaceful long short earlier, cut unnecessary aluminium wire then gradually, finally reach the state of suspension.
D. take out the sample 4 that is wound with metal aluminum filament 5, sample 4 and metal aluminum filament 5 are accurately weighed respectively.
E. utilize following formula to calculate the density of testing sample 4:
D s＝M sD lD Al/[M sD Al-(D l-D Al)M Al]
Wherein: M sAnd M AlBe respectively the quality of testing sample and the quality of metal aluminum filament 5, D s, D AlAnd D lBe respectively the density of testing sample, the density of metal aluminum filament 5 and the density of immersion liquid.
In the process of measuring, following factor has measurement result and seriously influences: the chemical stability of immersion liquid, the temperature fluctuation of immersion liquid, the generation of convection current, the shape and size of sample, dirt on the sample and bubble, chemical reaction between immersion liquid and testing sample or corrosion.
Temperature control is very important, and the convection current that immersion liquid is faint can have great influence to sample and aluminium wire association floating.Therefore, sample measurement cup 1 must place the water-bath 2 of constant temperature.Moreover, should there be air-conditioning in whole room, and it is identical with water temperature to regulate the room temperature.The temperature three of the room temperature in room, the water temperature of water-bath and immersion liquid is consistent as much as possible, between the temperature difference should can prevent the convection current of immersion liquid effectively less than 1.0 ℃.The wellability of sample also has certain influence, and the adhering to of micro-bubble is with the measurement result that leads to errors.So should examine bubble-free adhering to when the association of sample and aluminium wire is placed immersion liquid.The selection of immersion liquid should be avoided the generation of chemical reaction.
Practical measuring examples:
What table 1 provided is one of many examples of measuring.
The example that table 1 sample rate is measured
Measuring condition: 21.95 ℃ of Al silks of temperature density 2.698g/cm 3Immersion liquid density 3.3250g/cm 3
Sample composition Sample quality (mg) Al yarn quality (mg) Sample rate (the g/cm that calculates 3)
Fe 80B 20 0.1417 0.3292 7.2267
Fe 80B 20 0.1770 0.3858 6.7382
Co 75Si 15B 10 0.1718 0.4089 7.4405
Ni 78Si 8B 14 0.1603 0.3889 7.6228
Al yarn quality measuring error Δ M Al/ M AlInfluence to the testing sample density measure:
ΔD s/D s＝{(D l-D Al)/[(M s/M Al+1)D Al-D l]}ΔM Al/M Al
With the Fe that measures 80B 20Be example, Δ M Al/ M Al=0.2%, Δ D then s/ D s=0.22%.
Immersion liquid density error Δ D l/ D lInfluence to the testing sample density measure:
ΔD s/D s＝{(M s+M Al)D Al/[(M s+M Al)D Al-M AlD l]}ΔD l/D l
Fe still to measure 80B 20Be example, Δ D l/ D l=0.03%, Δ D then s/ D s=0.22%.
The mensuration of immersion liquid density
The density of the highly purified metal assay immersion liquid of available known density, as: Au, Cu, Ta, Ni, Ti etc.These metals obtain high purity easily.And, provided their accurate density in the document, referring to table 2.
Table 2 is used to measure the density of the high purity metal of immersion liquid density
Element Density (g/cm 3)
Au 19.281
Cu 8.933
Ta 16.670
Ni 8.907
Ti 4.508
Ask the used formula of density of immersion liquid as follows:
D l＝(M m+M Al)D mD Al/(M mD Al+M AlD m)
Wherein: D l, D mAnd D AlBe respectively the density of immersion liquid, the density of used high pure metal and the density of aluminium.M mAnd M AlBe respectively the quality of used high pure metal and the quality of aluminium wire.Used high pure metal should have 99.999% purity, and its density is known.Therefore, measure the M that is in suspended state mAnd M AlCan obtain the density D of immersion liquid lIn addition, also needing accurately, the density of grasp immersion liquid concerns with variation of temperature.
The immersion liquid that other are available
Except diiodomethane (CH 2I 2) can be used as outside the immersion liquid, following organometallics is also available, referring to table 3.
Other organometallicss of the immersion liquid that table 3 can be used
Molecular formula Molecular weight Density Fusing point Boiling point
(CH 3) 2SnI 2 402.57 2.872 43(30) 228
ClCBr 3 287.19 2.71 55 158-9
CH 2I 2 267.87 3.3254 6 181
FCHI 2 285.84 3.1969 -34 100
FCBr 3 270.76 2.7648 106
Br 3CNO 2 297.74 2.7930 10.25 89-90
CHBr 3 252.75 2.8899 8.3 149.5
Br 3CCH 2Br 345.67 2.8748 0 112

Claims (4)

1. the method accurately measured of a tiny sampler density, its feature includes:
A. testing sample is connected with the tinsel of the known accurate density littler than compound liquid density;
B. tinsel is wrapped in and is immersed on the sample in the compound liquid of accurate demarcation density, compound liquid density is greater than described density of wires, and sample rate is greater than compound liquid density; The difference of thermostat temperature that compound liquid presets and breadboard room temperature is less than 1.0 ℃;
C. by to described tinsel progressively cutting diameter less than the filament of 0.05mm, thereby the quality wiry of progressively accurately adjusting known accurate density reaches and is wound with sample wiry presents the suspended state that neither rising does not also descend in compound liquid;
D. take out and be wound with sample wiry, tinsel and sample are accurately weighed respectively;
E. utilize following formula to calculate the density of testing sample:
D s＝M sD lD/[M sD-(D l-D)M]
Wherein: M sBe respectively the quality and the quality wiry of testing sample, D with M s, D and D lBe respectively the density of the density of testing sample, density wiry and compound liquid.
2. the method that tiny sampler density as claimed in claim 1 is accurately measured is characterized in that the scaling method of the accurate demarcation density of described compound liquid is:
A. with the highly purified metal sample of known density: golden Au, copper Cu, tantalum Ta, nickel, titanium Ti after one or more dispose an amount of aluminium wire respectively, are immersed in the compound liquid of density to be measured;
B. make it in the compound liquid of density to be measured, be suspended state;
C. take out metal sample and aluminium wire, and accurately weigh respectively;
D. utilize following formula computerized compound fluid density:
D l＝(M m+M Al)D mD Al/(M mD Al+M AlD m)
Wherein: D l, D mAnd D AlBe respectively the density of compound liquid, the density of used high pure metal and the density of aluminium.M mAnd M AlBe respectively the quality of used high pure metal and the quality of aluminium wire.
3. the method that tiny sampler density as claimed in claim 1 is accurately measured, the material wiry that it is characterized in that described known density is aluminium Al.
4. the method that tiny sampler density as claimed in claim 1 is accurately measured, the compound liquid that the described warp of its feature is accurately demarcated density is diiodomethane CH 2I 2, or be (CH 3) 2SnI 2, ClCBr 3, FCHI 2, FCBr 3, Br 3CNO 2, CHBr 3, Br 3CCH 2Br.
CNB2004100105033A 2004-12-27 2004-12-27 Accurate check weighing method of density for micro sample Expired - Fee Related CN100458402C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNB2004100105033A CN100458402C (en) 2004-12-27 2004-12-27 Accurate check weighing method of density for micro sample

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNB2004100105033A CN100458402C (en) 2004-12-27 2004-12-27 Accurate check weighing method of density for micro sample

Publications (2)

Publication Number Publication Date
CN1796971A CN1796971A (en) 2006-07-05
CN100458402C true CN100458402C (en) 2009-02-04

Family

ID=36818184

Family Applications (1)

Application Number Title Priority Date Filing Date
CNB2004100105033A Expired - Fee Related CN100458402C (en) 2004-12-27 2004-12-27 Accurate check weighing method of density for micro sample

Country Status (1)

Country Link
CN (1) CN100458402C (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105486352B (en) * 2016-01-14 2019-08-16 广东工业大学 A kind of comprehensive detection device and method of shell equivalent features information

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1383141A1 (en) * 1986-10-29 1988-03-23 Институт Геологии И Геохимии Горючих Ископаемых Ан Усср Method of determining density of solid bodies
CN2082412U (en) * 1990-04-08 1991-08-07 中国人民解放军信息工程学院 Intelligent measuring device for solid density
US6637265B1 (en) * 2000-09-19 2003-10-28 Fast Forward Devices, Llc Apparatus for measuring physical properties of matter

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1383141A1 (en) * 1986-10-29 1988-03-23 Институт Геологии И Геохимии Горючих Ископаемых Ан Усср Method of determining density of solid bodies
CN2082412U (en) * 1990-04-08 1991-08-07 中国人民解放军信息工程学院 Intelligent measuring device for solid density
US6637265B1 (en) * 2000-09-19 2003-10-28 Fast Forward Devices, Llc Apparatus for measuring physical properties of matter

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
悬浮法测定高相对密度试样的密度. 梅寅年.稀有金属材料与工程，第1期. 1979 *
自动固体密度计的研究. 王永洪，孙振东，冯正鸣，王洁，范世福.分析仪器，第2期. 1994 *

Also Published As

Publication number Publication date
CN1796971A (en) 2006-07-05

Similar Documents

Publication Publication Date Title
CN2938074Y (en) Liquid surface tension coefficient measuring instrument
CN207570970U (en) New liquid surface tension coefficient analyzer
CN211262376U (en) Soft package lithium ion battery gas production testing arrangement
CN100458402C (en) Accurate check weighing method of density for micro sample
CN203858181U (en) Novel liquid surface tension coefficient tester
Henins Precision density measurement of silicon
CN105067481A (en) Digital mud specific gravity tester and testing method
CN2504625Y (en) Liquid surface tension coefficient analyzer
Tyler et al. Portable Analyzer for Determination of Dissolved Oxygen in Water. Application of Rapid-Dropping Mercury Portable Analyzer for Determination of Dissolved Oxygen in Water. Application of Rapid-Dropping Mercury Electrode
US4944183A (en) Level gauge for liquid helium
CN205027631U (en) A device that is used for surveing in aqueous object quality
CN202383040U (en) Hydrostatic balance
CN2816762Y (en) Magnetic balancer
US2722838A (en) Device for determining the composition of sodium-lead alloy
CN207487758U (en) Buoy measuring device and buoy volume measuring system
CN215492968U (en) Electronic densimeter for liquid
US2716596A (en) Determination of tin on tinplate
CN215640707U (en) Measuring device for gas production rate of silicon-based negative electrode slurry
CN212748620U (en) Baume meter
CN219552186U (en) Experimental device for measuring liquid surface tension based on pull-off method
CN201285364Y (en) Linear scale bydrostatic balance
CN217717383U (en) Differential thermal thermogravimetric analyzer for electric field
CN101887002A (en) Liquid surface tension coefficient measuring apparatus
CN213515928U (en) Weighing data acquisition device
CN215727514U (en) Setting time detection device for cement production and processing

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
C17 Cessation of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20090204

Termination date: 20131227