CN104587856B - A kind of compound method of calibrating gas - Google Patents
A kind of compound method of calibrating gas Download PDFInfo
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- CN104587856B CN104587856B CN201510062920.0A CN201510062920A CN104587856B CN 104587856 B CN104587856 B CN 104587856B CN 201510062920 A CN201510062920 A CN 201510062920A CN 104587856 B CN104587856 B CN 104587856B
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Abstract
The present invention relates to a kind of compound method of calibrating gas, belong to calibrating gas preparation technique field.The method includes several big steps such as raw material preparation, gas cylinder are pre-processed, proportioning is calculated, gas is prepared and is verified.The present invention is cooperated by gas dalton voltage divider principle and weight method, casts out the mistaken ideas by single method preparing calibrating gas in traditional distribution technology, based on quality, simplifies calculation procedure, greatlys save manpower and materials；The inventive method is simple and reliable, and the gas concentration of preparation is accurate, great commercial Application meaning.
Description
Technical field
The invention belongs to calibrating gas preparation technique field, and in particular to a kind of compound method of calibrating gas.
Background technology
Calibrating gas weighing method distribution is domestic and international most accurate air distributing method, because it is based on quality weighing,
The influence that gas temperature, pressure change and compressibility factor are brought to preparation result can be exempted in calibrating gas process for preparation, therefore originally
Method is International Organization for standardization（ISO）The standard method of the preparation normal mixture body of recommendation.But weighing method is in calibrating gas
The component pressure and quality of required filling in operation are then completely dependent on the theoretical calculation of actual gas.
There is certain, same N of such as nominal value in current China's calibrating gas market2—5ppmO2Standard Gases, difference is raw
Produce producer has the response of different value on same detecting instrument, although they are the legal reference materials of country；Even if same
The same concentrations gas of production, also because that can not be compared very well between batch difference, this explanation domestic standard makings amount is managed from country
The links such as specific production are managed to still need raising.Calibration standard gas is used alarm, more than its upper limit, just cannot the calibrating instrument upper limit.
There is minus deviation, the gas can be used reluctantly.Such as contract requirement N2-O210×10-6, it is assumed that for demarcating oxygen instrument higher limit,
The gas that the producer provides is necessarily less than 10 × 10-6, may refuse to receive more than value user, so being easy to manufacturer
Cause unnecessary loss.
In addition, such as preparing SO only with single method preparing calibrating gas in traditional distribution technology2And N2Gaseous mixture
During, if water in bottle point is exceeded, add SO2Dissolving can be caused, although now registration is increasing on balance, SO2Be not with
Gaseous state is present, and now then has a strong impact on the quality of product.
The content of the invention
The invention aims to solve the deficiencies in the prior art, there is provided a kind of compound method of calibrating gas, the party
Method is simple and reliable, and the gas concentration of preparation is accurate, great commercial Application meaning.
The technical solution adopted by the present invention is as follows：
A kind of compound method of calibrating gas, it is characterised in that comprise the following steps：
Step（1）, each component i, each group partial volume accounting Y be given according to orderi, gas cylinder volume VBottle, Balance Air and gas
Bottle species, gets out raw material, selected functional gas cylinder and reliable cylinder valve；
Step（2）, gas cylinder is pre-processed, heat and carry out vacuum displacement treatment；
Step（3）, standard device for making carries out precision application of vacuum, then from the unstrpped gas that inspection is qualified, will walk
Suddenly（1）Selected gas cylinder is connected to standard device for making, and to carry out pipeline displacement qualified, then each group distribution ratio is calculated, specifically
It is as follows：
By perfect condition：The satisfactory voltage division of component i：Pi=10×Yi；
Then temperature T during distribution is measured1, find the density p of now component ii；Meanwhile, temperature T during according to distribution1And
The satisfactory voltage division P of component ii, find the compressibility factor Z under the temperature and the pressurei, obtain total compression coefficient Zm = Yi；
Then the pressure to each component is modified, and obtains actual partial pressure P* i=PiZi/Zm；
Finally, the quality m of each component is obtainedi=P* i×VBottle×ρi；
Step（4）, open precision weighing apparatus precise and handle empty bottle well, accurately matched somebody with somebody using gravimetric method and partial pressure method
System, is filled with before and after every kind of component and weighs gas cylinder respectively, and the every kind of gas component quality being filled with is by being filled with gas cylinder before and after the component
The difference of quality determines；The each component in addition to Balance Air is first filled with, according to gauge pressure=absolute pressure-atmospheric pressure, is come in real time according to table
The actual partial pressure P of the voltage-controlled every kind of component of system* i, Balance Air to 10.5-11.0Mpa is finally filled with, meanwhile, during insufflation gas
The degree of accuracy of checking computations verification quality and actual partial pressure repeatedly, until required concentration standardized product is produced in completion, finally using accurate
Detecting instrument contrast verification result, if checking is correct, obtains qualified products.
It is further preferred that described gas cylinder is aluminium alloy gas cylinder or carbon steel bottle.
If described component contains Cl2And/or HCl, then can not use aluminium alloy gas cylinder.
The principle of institute's foundation of the present invention：
In numerous gas equations, the preparation of gas mainly follows two laws：Dalton and Amagat theorems.
Dalton theorem is：The gas of certain volume, its stagnation pressure is each component partial pressure sum,P i =。
Amagat laws are then that under stagnation pressure, by each component sum, i.e., the cumulative volume of gas isV i =。
In being prepared in gas, some gases are such as：C3H6、C3H8、CO2、N2O、C2H6Deng critical temperature Tc relatively
Height, under with atmospheric pressure, usually 10.0MPa, easily forms liquefaction, if adopting by Amagat laws, in distribution higher
Under pressure, we cannot find gas compressibility factor, therefore, gas of the present invention is prepared and uses Dalton's law (of partial pressures), without making
Use Amagat laws.
The degree of accuracy of distribution is outside one's consideration for Standard Gases, user except the precision for being concerned about result, more concerned the standard of gas
Exactness, " accurate ", " uniform ", " stabilization " are gas key characters.Calibrating gas has the effect of " tracing to the source " and " arbitration ", gas
Prepare more accurate its uncertainty smaller.
Compared with prior art, its advantage is the present invention：
1. the present invention provides a kind of compound method of calibrating gas, and the method is simple and reliable, and the gas concentration of preparation is accurate,
Great commercial Application meaning.
2. calculate and cooperated by gas dalton voltage divider principle and weight method, cast out in traditional distribution technology by single
The mistaken ideas of method preparing calibrating gas, are such as preparing SO2And N2During gaseous mixture, if water in bottle point is exceeded, SO is added2Meeting
Cause dissolving, although now registration is increasing on balance, SO2It is not exist with gaseous state, now using the method for the present invention
Intuitively can be showed on pressure gauge, if SO2Dissolve, then pressure gauge will be stagnated and even returned when balance registration increases
Fall, this is not meet The Ideal-Gas Equation completely, whether the process for preparing gas such that it is able to judgement easily is reliable.Together
Reason, the method can be applied to show other adsorptivities, reactivity, deliquescent gas preparation process.
3. calculation procedure is simplified, and traditional distribution is calculated to be needed to consider a series of amendments such as compressibility factor and environment temperature,
I is based on based on quality company's method, the most of accuracy prepared calculating process, but do not influence result at all of removal, significantly
Save manpower and materials.
4. test and show, compressibility factor amendment must be used in distribution, can otherwise deviate 2%-10%, such as H2It is the standard at bottom
Gas.
Brief description of the drawings
Fig. 1 is the flow chart of the compound method of calibrating gas of the present invention.
Specific embodiment
With reference to embodiment, the present invention is described in further detail.
It will be understood to those of skill in the art that the following example is merely to illustrate the present invention, and should not be regarded as limiting this hair
Bright scope.In the examples where no specific technique or condition is specified, according to the technology or condition described by document in the art
Or carried out according to product description.Agents useful for same or the unreceipted production firm person of instrument, being can be by buying what is obtained
Conventional products.
Partial pressure method and use the weighing weighed that method prepared by calibrating gas of the present invention is calibrated using compressibility factor
Method, the container for using is the big ball of calibrated glass, and pressure is close to normal pressure, it is to avoid the uniformity of the gas that high pressure is caused,
The component of many activity has preferable inertia to glass surface simultaneously, can greatly reduce to outsourcing mark according to Static Volumetric Method
The dependence of quasi- gas, saves financial cost.
Air distributing device of the present invention is the conventional equipment used by the Static Volumetric Method distribution of this area.
Before calibrating gas is prepared, it is necessary to be expressly understood that the contract requirement of user, no matter this point from technical standpoint or pacifies
Full angle sees must not all there be a bit general idea.The trouble trouble that will otherwise cause economic even secure context many, should height for this
Degree payes attention to the link of contract review.Generally, user's specification gas order needs to be given：Constituent species（The name of gas
Claim）, concentration of component（Partial volume concentration v/v, mass concentration m/m etc., are then volumetric concentrations without explanation）, pressure（Liquid gas
Except）, gas cylinder volume, following concrete case：
Embodiment 1
N2—10%CO 8L/Al
Its transmission information be：
1st, this bottle of calibrating gas is with N2It is spirit or Balance Air（Sometimes represented with english abbreviation bal, meaning balance）；
2nd, 10% the concentration of volume shared by CO in calibrating gas, N are represented2Account for 90%
3rd, CO represents the component CO gases contained in calibrating gas；
4th, 8L is the volume of gas cylinder；
5th, Al represents aluminium alloy gas cylinder.
And to carbon steel bottle, contract generally writes " T ", what such as " T40 " was represented is the carbon steel bottle of 40L.This abbreviation is not although have
Regular standard regulation, but generally use in the industry.
The calculating of this contract gas：
Routinely the stagnation pressure of this bottle of gas is：10.0Mpa.
By perfect condition：
The satisfactory voltage division of CO：Pco=10 × 10%=1.0Mpa,
N2Satisfactory voltage division：PN2=10×（100-10）%=9.0Mpa；
Assuming that temperature during distribution is：20 DEG C,
The density of CO at 20 DEG C（Generally represented with ρ）：1.16g/l
N when looking into 20 DEG C2Density:1.25g/l
Remarks:Above-mentioned source digital is in BOC gas data tables；
Look into 20 DEG C, under 1.0Mpa CO compressibility factor (zco):15℃、0.9959；50℃、0.9988；
Using interpolation method, difference：(0.9988-0.9959)/35=0.0000725；
So 20 DEG C, under 1.0Mpa pressure, compressibility factor：
Zco=0.995+0.0000725×(20-15)=0.99536；
Similarly, 20 DEG C are looked into, N under 9.0 Mpa2Compressibility factor (ZN2):1.00243。
So：
Zm=YcoZco+YN2ZN2=0.99536×10%+1.00243×90%=0.90318。
Revised result：
P*co=PcoZco/Zm=1.0×0.99536/0.90318=1.102Mpa；
P* N2 =PN2ZN2/Zm=9.0×1.00243/0.90318=9.9890Mpa。
So：
The quality of CO is：P*co×V×ρco=1.102×8×1.16=102.2656g；
N2Quality be：P* N2×V×ρN2=9.9890×8×1.25=998.90g。
Step：
A gas cylinders are pre-processed, and heat and carry out vacuum displacement treatment；Balance Air and gas cylinder species, get out raw material,
Selected functional gas cylinder and reliable cylinder valve；Write down the quality of empty bottle；
B fills high-purity CO pressure gauges display 1.102-0.1=1.02 Mpa（0.1 is local atmospheric pressure, can be according to actual feelings
Condition is adjusted, absolute pressure=gauge pressure+atmospheric pressure）, write down the gas cylinder quality for charging CO；
C fills high-purity N2To 10.5Mpa, write down and charge N2Gas cylinder quality, meanwhile, checked repeatedly during insufflation gas
The degree of accuracy of verification quality and actual partial pressure, until required concentration standardized product is produced in completion, finally using accurate detecting instrument
Contrast verification result, if checking is correct, obtains qualified products.
Practical operation balanced gas can use XP155KS electronic balances, be weighed in inflatable body.What the first component was added
If amount and the theoretical amount for calculating are different, if not the reason for such as weighing, raw material, adjustment that just need not be repeatedly can be adopted
To calculate the quality of next component based on the first component.
Standard Gases preparation is one and seems simple, but sufficiently complex work, it is desirable to have comprehensive professional technique and ten
Divide careful working attitude, while require that each participant harmonious will coordinate, mutually prompting, strict cylinder treatment, material quality
Control, accurate selection, the calibration of measuring equipment for preparing instrument etc., so just can guarantee that the gas allotted is accurate, uniform, reliable,
It is otherwise full of mistakes, or even it some times happens that security incident.Additionally, gas makers-up need to constantly learn, enrich, when preparing not
Disconnected to find new situation, summing up experience is had only in this way, the pin that could stand firm in the industry.
General principle of the invention and principal character and advantages of the present invention has been shown and described above.The technology of the industry
Personnel it should be appreciated that the present invention is not limited to the above embodiments, simply explanation described in above-described embodiment and specification this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appending claims and its
Equivalent thereof.
Claims (3)
1. a kind of compound method of calibrating gas, it is characterised in that comprise the following steps：
Step（1）, each component i, each group partial volume accounting Y be given according to orderi, gas cylinder volume VBottle, Balance Air and gas cylinder kind
Class, gets out raw material, selected functional gas cylinder and reliable cylinder valve；
Step（2）, gas cylinder is pre-processed, heat and carry out vacuum displacement treatment；
Step（3）, standard device for making carries out precision application of vacuum, then from the unstrpped gas that inspection is qualified, by step（1）
Selected gas cylinder is connected to standard device for making, and to carry out pipeline displacement qualified, then each group distribution ratio is calculated, specific as follows：
By perfect condition：The satisfactory voltage division of component i：Pi=10×Yi；
Then temperature T during distribution is measured1, find the density p of now component ii；Meanwhile, temperature T during according to distribution1And component
The satisfactory voltage division P of ii, find the compressibility factor Z under the temperature and the pressurei, obtain total compression coefficient Zm = Yi；
Then the pressure to each component is modified, and obtains actual partial pressure P* i=PiZi/Zm；
Finally, the quality m of each component is obtainedi=P* i×VBottle×ρi；
Step（4）, the empty bottle that precision weighing apparatus precise is handled well is opened, accurate formulation is carried out using gravimetric method and partial pressure method,
It is filled with before and after every kind of component and weighs gas cylinder respectively, the every kind of gas component quality being filled with is by being filled with the quality of gas cylinder before and after the component
Difference determine；The each component in addition to Balance Air is first filled with, according to gauge pressure=absolute pressure-atmospheric pressure, is come in real time according to gauge pressure control
Make the actual partial pressure P of every kind of component* i, Balance Air to 10.5-11.0Mpa is finally filled with, meanwhile, during insufflation gas repeatedly
The degree of accuracy of checking computations verification quality and actual partial pressure, until required concentration standardized product is produced in completion, finally using precisely detection
Instrument contrast verification result, if checking is correct, obtains qualified products.
2. the compound method of calibrating gas according to claim 1, it is characterised in that described gas cylinder is aluminium alloy gas cylinder
Or carbon steel bottle.
3. the compound method of calibrating gas according to claim 2, it is characterised in that if described component contains Cl2
And/or HCl, then can not use aluminium alloy gas cylinder.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106568795A (en) * | 2015-10-12 | 2017-04-19 | 哈尔滨理工大学 | Melt hydrogen detector calibrating method and device |
| CN108241039A (en) * | 2016-12-23 | 2018-07-03 | 中核陕西铀浓缩有限公司 | The preparation facilities and preparation method of a kind of instrument calibration fluorination hydrogen mixed gas |
| CN108267278A (en) * | 2017-12-05 | 2018-07-10 | 洛阳双瑞特种装备有限公司 | The method for carrying out leak test to pressure vessel using the gaseous mixture of ammonia nitrogen |
| CN108031314A (en) * | 2017-12-11 | 2018-05-15 | 苏州金宏气体股份有限公司 | A kind of mixed gas preparation method |
| CN108760421A (en) * | 2018-05-11 | 2018-11-06 | 杭州贝斯特气体有限公司 | The manufacturing process of gas reference material in nitrogen |
| CN111744423B (en) * | 2019-03-29 | 2022-08-02 | 中国石油天然气股份有限公司 | Preparation device and preparation method of standard mixed gas |
| CN114878069B (en) * | 2022-05-06 | 2024-01-26 | 中国计量科学研究院 | Pressure standard source, pressure standard source preparation equipment and pressure calibration method |
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| CN201324604Y (en) * | 2008-12-11 | 2009-10-14 | 大连光明特种气体有限公司 | Standard automatic distributing device for mixed gas |
| CN102500253A (en) * | 2011-11-09 | 2012-06-20 | 西南化工研究设计院 | Novel device for distributing standard gas |
| CN203043861U (en) * | 2013-01-20 | 2013-07-10 | 廊坊黎明气体有限公司 | Standard gas distribution device |
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