CN104587856A - Method for preparing standard gas - Google Patents
Method for preparing standard gas Download PDFInfo
- Publication number
- CN104587856A CN104587856A CN201510062920.0A CN201510062920A CN104587856A CN 104587856 A CN104587856 A CN 104587856A CN 201510062920 A CN201510062920 A CN 201510062920A CN 104587856 A CN104587856 A CN 104587856A
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- gas
- component
- gas cylinder
- pressure
- quality
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Abstract
The invention relates to a method for preparing standard gas, belonging to the technical field of preparation of standard gas. The method comprises the following steps: preparing raw materials, performing gas cylinder pretreatment, calculating the ratio, preparing the gas, verifying and the like. The gas Dalton partial pressure principle and a weighing method are matched with each other, the misunderstanding that the standard gas is prepared according to a single method in the traditional gas preparation technology is avoided, the calculation step is simplified on the quality basis, and manpower and material resources are greatly saved; and moreover, the method disclosed by the invention is simple and reliable, the prepared gas is accurate in concentration and has high industrial application significance.
Description
Technical field
The invention belongs to calibrating gas preparation technique field, be specifically related to a kind of compound method of calibrating gas.
Background technology
The distribution of calibrating gas weighing method is the most accurate domestic and international air distributing method, because it is based on quality weighing, can exempt the impact that gas temperature, pressure change and compressibility factor are brought to preparation result in calibrating gas process for preparation, therefore this method is the standard method of the preparation normal mixture body that International Organization for Standardization is recommended.But the component pressure of weighing method required filling in calibrating gas operation and quality then rely on the theory calculate of actual gas completely.
There is certain problem in current China's calibrating gas market, the same N of such as nominal value
2-5ppmO
2standard Gases, there is the response of different value in different manufacturer on same detecting instrument, although they are national legal reference materials; Even if the same concentrations gas of same production, also because of can not comparison very well between batch difference, this illustrates that domestic standard makings amount is still needed from national management to links such as concrete productions raising.To warning calibration standard gas, exceed its upper limit, just cannot the calibrating instrument upper limit.Occur minus deviation, this gas can use reluctantly.As contract requirement N
2-O
210 × 10
-6, assuming that divide instrument higher limit for demarcating oxygen, the gas that the producer provides must be less than 10 × 10
-6, exceed this value user and may refuse to accept, so be easy to cause unnecessary loss to manufacturer.
In addition, in traditional distribution technology, only adopt single method preparing calibrating gas, as prepared SO
2and N
2in the process of gaseous mixture, exceed standard if water in bottle divides, add SO
2can dissolving be caused, although now on balance registration in increase, SO
2be not exist with gaseous state, now then have a strong impact on the quality of product.
Summary of the invention
The object of the invention is to solve the deficiencies in the prior art, provide a kind of compound method of calibrating gas, the method is simple and reliable, and the gas concentration of preparation is accurate, has commercial Application meaning.
The technical solution used in the present invention is as follows:
A compound method for calibrating gas, is characterized in that, comprises the steps:
Step (1), according to each component i, each volume components accounting Y that order provides
i, gas cylinder volume V
bottle, Balance Air and gas cylinder kind, get out raw material, selected functional gas cylinder and reliable cylinder valve;
Step (2), carries out pretreatment to gas cylinder, heats and carries out vacuum displacement process;
Step (3), standard device for making carries out precision application of vacuum, then selects the unstrpped gas be up to the standards, and gas cylinder selected for step (1) being connected to standard device for making, to carry out pipeline displacement qualified, then calculates each component proportion, specific as follows:
By perfect condition: the satisfactory voltage division of component i: P
i=10 × Y
i;
Then temperature T during distribution is measured
1, find the density p of now component i
i; Meanwhile, according to temperature T during distribution
1and the satisfactory voltage division P of component i
i, find the compressibility factor Z under this temperature and this pressure
i, obtain total compression coefficient Z
m=
y
i;
Then the pressure of each component is revised, obtain actual dividing potential drop P
* i=P
iz
i/ Z
m;
Finally, the quality m of each component is obtained
i=p
* i× V
bottle× ρ
i;
Step (4), open precision weighing apparatus precise and handle empty bottle well, adopt gravimetric method and point platen press to carry out accurate formulation, be filled with before and after often kind of component and weigh gas cylinder respectively, the often kind of gas component quality be filled with is determined by the difference of the quality being filled with gas cylinder before and after this component; First be filled with each component except Balance Air, according to gauge pressure=absolute pressure-atmospheric pressure, carry out the actual dividing potential drop P controlling often kind of component in real time according to gauge pressure
* i, be finally filled with Balance Air to 10.5-11.0Mpa, simultaneously, in insufflation gas process, repeatedly check the degree of accuracy of verification quality and actual dividing potential drop, produce desired concn standardized product until complete, finally adopt accurate detecting instrument contrast verification result, if checking is correct, then obtain qualified products.
Further, preferably described gas cylinder is aluminium alloy gas cylinder or carbon steel bottle.
If described component is containing Cl
2and/or HCl, then can not use aluminium alloy gas cylinder.
the principle of institute of the present invention foundation:
In numerous gas equations, two laws are mainly followed in the preparation of gas: dalton and Amagat theorem.
Dalton's theorem is: the gas of certain volume, and its stagnation pressure is each component dividing potential drop sum,
p i =
.
Amagat law is then under stagnation pressure, and the cumulative volume of gas is by each component sum, namely
v i =
.
Due in gas preparation, some gas is as C
3h
6, C
3h
8, CO
2, N
2o, C
2h
6deng critical temperature Tc relatively high, under distribution pressure, be generally 10.0MPa, very easily form liquefaction, if adopt by Amagat law, under higher distribution pressure, we cannot find gas compressibility factor, therefore, gas preparation of the present invention adopts Dalton's law (of partial pressures), and does not use Amagat law.
The degree of accuracy of distribution is for Standard Gases, and user is except being concerned about the precision of result, and the more concerned degree of accuracy of gas, " accurately ", " evenly ", " stablizing " are gas key characters.Calibrating gas has " tracing to the source " and the effect of " arbitration ", and gas preparation its uncertainty more accurate is less.
compared with prior art, its beneficial effect is in the present invention:
1. the invention provides a kind of compound method of calibrating gas, the method is simple and reliable, and the gas concentration of preparation is accurate, has commercial Application meaning.
2. calculate and cooperatively interacted by gas dalton voltage divider principle and weight method, cast out the mistaken ideas by single method preparing calibrating gas in traditional distribution technology, as prepared SO
2and N
2in the process of gaseous mixture, exceed standard if water in bottle divides, add SO
2can dissolving be caused, although now on balance registration in increase, SO
2be not exist with gaseous state, now applying method of the present invention can show intuitively on Pressure gauge, if SO
2dissolve, then when balance registration increases, Pressure gauge will be stagnated and even fall after rise, and this does not meet The Ideal-Gas Equation completely, thus can judge that whether the process preparing gas is reliable easily.In like manner, the method can be applicable to show other adsorptivities, reactivity, deliquescent gas generation process.
3. simplify calculation procedure, tradition distribution calculates and needs to consider a series of correction such as compressibility factor and environment temperature, and my company's method, based on based on quality, removes major part preparation computational process, but do not affect the accuracy of result at all, greatly save manpower and materials.
4. experiment shows, must adopt compressibility factor correction, otherwise can depart from 2%-10%, as H in distribution
2for the calibrating gas at the end.
Accompanying drawing explanation
Fig. 1 is the flow chart of the compound method of calibrating gas of the present invention.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
It will be understood to those of skill in the art that the following example only for illustration of the present invention, and should not be considered as limiting scope of the present invention.Unreceipted concrete technology or condition person in embodiment, according to the technology described by the document in this area or condition or carry out according to product description.Agents useful for same or the unreceipted production firm person of instrument, being can by buying the conventional products obtained.
Point platen press that method prepared by calibrating gas of the present invention adopts compressibility factor to carry out calibrating and the weighing method that employing is weighed, the container adopted is the calibrated large ball of glass, pressure is close to normal pressure, the uniformity of the gas avoiding high pressure to cause, the component of many activity has good inertia to glass surface simultaneously, the dependence to outsourcing calibrating gas can be greatly reduced according to Static Volumetric Method, save financial cost.
Air distributing device of the present invention is this area Static Volumetric Method distribution conventional equipment used.
Before calibrating gas preparation, clearly must understand the contract requirement of user, this point, no matter from technical standpoint or security standpoint, all must not have a bit general idea.Otherwise the economy trouble that even secure context is many will be caused to suffer from, the link of contract review should be paid much attention to for this reason.Generally, user's specification gas order needs to provide: constituent species (title of gas), concentration of component (partial volume concentration v/v, mass concentration m/m etc., not do not illustrate it is then volumetric concentration), pressure (except liquid gas), gas cylinder volume, following concrete case:
embodiment 1
N
2
—10%CO 8L/Al
Its information transmitted is:
1, this bottle of calibrating gas is with N
2for spirit or title Balance Air (sometimes representing with english abbreviation bal, meaning balance);
2,10% concentration representing volume shared by CO in calibrating gas, N
2account for 90%
3, CO represents the component CO gas contained in calibrating gas;
4,8L is the volume of gas cylinder;
5, Al represents aluminium alloy gas cylinder.
And to carbon steel bottle, contract is write usually " T ", what represent as " T40 " is the carbon steel bottle of 40L.Although this abbreviation does not have regular standard regulation, generally adopt in the industry.
the calculating of this contract gas:
The stagnation pressure of conventional this bottle of gas is: 10.0Mpa.
By perfect condition:
The satisfactory voltage division of CO: Pco=10 × 10%=1.0Mpa,
N
2satisfactory voltage division: P
n2=10 × (100-10) %=9.0Mpa;
Temperature when supposing distribution is: 20 DEG C,
The density (usually representing with ρ) of CO: 1.16g/l when 20 DEG C
N when looking into 20 DEG C
2density: 1.25g/l
Remarks: above-mentioned source digital is in BOC gas data table;
Look into 20 DEG C, the compressibility factor (z of CO under 1.0Mpa
co): 15 DEG C, 0.9959; 50 DEG C, 0.9988;
Adopt interpolation method, difference: (0.9988-0.9959)/35=0.0000725;
So 20 DEG C, under 1.0Mpa pressure, compressibility factor:
Z
co=0.995+0.0000725×(20-15)=0.99536；
In like manner, look into 20 DEG C, N under 9.0 Mpa
2compressibility factor (Z
n2): 1.00243.
So:
Z
m=Y
coZ
co+Y
N2Z
N2=0.99536×10%+1.00243×90%=0.90318。
Revised result:
P
*co=P
coZ
co/Z
m=1.0×0.99536/0.90318=1.102Mpa；
P
* N2=P
N2Z
N2/Z
m=9.0×1.00243/0.90318=9.9890Mpa。
So:
The quality of CO is: P
*co × V × ρ
co=1.102 × 8 × 1.16=102.2656g;
N
2quality be: P
* n2× V × ρ
n2=9.9890 × 8 × 1.25=998.90g.
step:
A gas cylinder carries out pretreatment, heats and carries out vacuum displacement process; Balance Air and gas cylinder kind, get out raw material, selected functional gas cylinder and reliable cylinder valve; Write down the quality of empty bottle;
It is local atmospheric pressure that B fills high-purity CO Pressure gauge display 1.102-0.1=1.02 Mpa(0.1, can adjust, absolute pressure=gauge pressure+atmospheric pressure according to actual conditions), write down the gas cylinder quality charging CO;
C fills high-purity N
2to 10.5Mpa, write down and charge N
2gas cylinder quality, meanwhile, in insufflation gas process, repeatedly check the degree of accuracy of verification quality and actual dividing potential drop, produce desired concn standardized product until complete, finally adopt accurate detecting instrument contrast verification result, if checking is correct, then obtain qualified products.
Practical operation balanced gas can adopt XP155KS electronic balance, and inflatable body limit, limit weighs.If the amount that the first component adds is different with the theoretical amount calculated, if not the reason of such as weighing, raw material, just need not adjustment repeatedly, the quality calculating next component based on the first component can be adopted.
Standard Gases preparation is one and seems simple, but very complicated work, need comprehensive professional technique and very careful working attitude, require that each participant wants harmonious and coordinates simultaneously, mutual prompting, the calibration etc. of strict cylinder treatment, material quality control, preparation accurately the selecting of instrument, measuring equipment, the gas that such guarantee is allotted accurately, evenly, reliable, otherwise full of mistakes, there is security incident even sometimes.In addition, gas makers-up needs unceasing study, enriches, and constantly finds new situation, summing up experience when preparing, and has only so, pin of could standing firm in the industry.
More than show and describe general principle of the present invention and principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and description just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof
.
Claims (3)
1. a compound method for calibrating gas, is characterized in that, comprises the steps:
Step (1), according to each component i, each volume components accounting Y that order provides
i, gas cylinder volume V
bottle, Balance Air and gas cylinder kind, get out raw material, selected functional gas cylinder and reliable cylinder valve;
Step (2), carries out pretreatment to gas cylinder, heats and carries out vacuum displacement process; Balance Air and gas cylinder kind, get out raw material, selected functional gas cylinder and reliable cylinder valve;
Step (3), standard device for making carries out precision application of vacuum, then selects the unstrpped gas be up to the standards, and gas cylinder selected for step (1) being connected to standard device for making, to carry out pipeline displacement qualified, then calculates each component proportion, specific as follows:
By perfect condition: the satisfactory voltage division of component i: P
i=10 × Y
i;
Then temperature T during distribution is measured
1, find the density p of now component i
i; Meanwhile, according to temperature T during distribution
1and the satisfactory voltage division P of component i
i, find the compressibility factor Z under this temperature and this pressure
i, obtain total compression coefficient Z
m=
y
i;
Then the pressure of each component is revised, obtain actual dividing potential drop P
* i=P
iz
i/ Z
m;
Finally, the quality m of each component is obtained
i=p
* i× V
bottle× ρ
i;
Step (4), open precision weighing apparatus precise and handle empty bottle well, adopt gravimetric method and point platen press to carry out accurate formulation, be filled with before and after often kind of component and weigh gas cylinder respectively, the often kind of gas component quality be filled with is determined by the difference of the quality being filled with gas cylinder before and after this component; First be filled with each component except Balance Air, according to gauge pressure=absolute pressure-atmospheric pressure, carry out the actual dividing potential drop P controlling often kind of component in real time according to gauge pressure
* i, be finally filled with Balance Air to 10.5-11.0Mpa, simultaneously, in insufflation gas process, repeatedly check the degree of accuracy of verification quality and actual dividing potential drop, produce desired concn standardized product until complete, finally adopt accurate detecting instrument contrast verification result, if checking is correct, then obtain qualified products.
2. the compound method of calibrating gas according to claim 1, is characterized 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, is characterized in that, if described component is containing Cl
2and/or HCl, then can not use aluminium alloy gas cylinder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510062920.0A CN104587856B (en) | 2015-02-06 | 2015-02-06 | A kind of compound method of calibrating gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510062920.0A CN104587856B (en) | 2015-02-06 | 2015-02-06 | A kind of compound method of calibrating gas |
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|---|---|
| CN104587856A true CN104587856A (en) | 2015-05-06 |
| CN104587856B CN104587856B (en) | 2017-06-27 |
Family
ID=53114113
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106568795A (en) * | 2015-10-12 | 2017-04-19 | 哈尔滨理工大学 | Melt hydrogen detector calibrating method and device |
| 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 |
| 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 |
| 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 |
| CN111744423A (en) * | 2019-03-29 | 2020-10-09 | 中国石油天然气股份有限公司 | Preparation device and preparation method of standard mixed gas |
| CN114878069A (en) * | 2022-05-06 | 2022-08-09 | 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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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111744423A (en) * | 2019-03-29 | 2020-10-09 | 中国石油天然气股份有限公司 | Preparation device and preparation method of standard mixed gas |
| CN114878069A (en) * | 2022-05-06 | 2022-08-09 | 中国计量科学研究院 | Pressure standard source, pressure standard source preparation equipment and pressure calibration method |
| 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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| CN104587856B (en) | 2017-06-27 |
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