CN109884218A - The preparation facilities and method of arsine gas standard substance in a kind of nitrogen - Google Patents
The preparation facilities and method of arsine gas standard substance in a kind of nitrogen Download PDFInfo
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- CN109884218A CN109884218A CN201910297006.2A CN201910297006A CN109884218A CN 109884218 A CN109884218 A CN 109884218A CN 201910297006 A CN201910297006 A CN 201910297006A CN 109884218 A CN109884218 A CN 109884218A
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Abstract
The invention belongs to the development preparation fields of gas reference material, more particularly, to the preparation facilities and method of arsine gas standard substance in a kind of nitrogen.The gaseous arsine with specific severe toxicity is set to keep liquid in transfer process by the way of cooling and liquid nitrogen gasification purging, avoid a possibility that its leakage causes the accident noresidue transfer completely simultaneously, the purge gas used simultaneously is diluent gas, it will not influence preparation result, total nitrogen use level can obtain in such a way that mass comparator measures, and ensure that accuracy.This method operates safe and convenient, and accuracy is high, and arsine gas standard substance has good homogeneity and stability in nitrogen obtained.
Description
Technical field
The invention belongs to the development preparation fields of gas reference material, more particularly, to arsine gas standard in a kind of nitrogen
The preparation facilities and method of substance.
Background technique
Standard substance (RM) reference material (RM): being that one kind has determined that there is one or more enough
The substance or material of uniform characteristic value, as " measurer " in analysis measurement industry, in calibration measurement instrument and device, evaluation
It measures analysis method, measurement of species or material property value and examines the operating technology of analysis personnel horizontal, and in production process
The fields such as the quality control of middle product play indispensable role.The characteristic of standard substance magnitude and basic demand include accurate
Property, uniformity and stability, the standard substance of different stage have different requirements to its uniformity and stability and purposes.
Standard substance can be pure or mixed gas, liquid or solid.In analytical chemistry, standard substance is the main of chain of tracing to the source
Component units.Arsenic hydride is a kind of colourless, hypertoxic fuel gas, in certain specific environments, such as in submarine cabin, to arsenic
Hydrogen concentration has certain permissible value (GJB11).To ensure officers and men's life security, the arsine gas concentration in cabin is carried out
Detection is necessary.The detection method of arsenic hydride is wherein given in GJB533.8, needs one when making standard trisquare
The arsine gas of series standard concentration, but arsine gas standard substance has not been reported at present, and since arsine gas contains
There is severe toxicity, in preparation and preservation, safety problem easily occur, is also not suitable for preparing using conventional method.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of preparation facilities of arsine gas standard substance in nitrogen and
Method, this method operate safe and convenient, and accuracy is high, and in nitrogen obtained arsine gas standard substance have it is good
Good homogeneity and stability.
The complete technical solution of the present invention includes:
A kind of preparation facilities of arsine gas standard substance in nitrogen is inventor provided first, which includes mixing
Bottle shifts bottle, stock bottle, liquid nitrogen bottle, machinery rolling mixing mechanism, cooling bath, triple valve and mass comparator.
Wherein, stock bottle is placed in cooling bath, and cooling bath is integrally placed on mass comparator；Liquid nitrogen bottle is placed in another quality
On comparator；
It shifts bottle one end and stock bottle and liquid nitrogen bottle is connected by triple valve, other end connection mixes bottle, mixes and set below bottle
There is mechanical rolling mixing mechanism；
Machinery rolls mixing mechanism and includes the bracket of two sides, and more roller bearings being connected on bracket, mixes bottle and is placed in
On roller bearing.
Using above-mentioned apparatus, a kind of preparation method of arsine gas standard substance in nitrogen, this method are inventor provided
Specifically include 1) cleaning device, 2) metering and transfer, 3) mix and etc., specifically:
1) cleaning device
First to including mixing the air-channel systems such as bottle, transfer bottle, connecting line, triple valve to clean, removal wherein may be used
The impurity of calibrating can be interfered, the high pure nitrogen after cleaning using purity greater than 99.999% is purged, and is driven away therein
Gas then vacuumizes entire air-channel system；
2) metering and transfer
The wherein transfer and metering of arsenic hydride raw material: arsenic hydride raw material is placed in stock bottle, and stock bottle is placed in quality and compares
Reading M on instrument, before writing down transfer0(unit is gram), and the access between triple valve and stock bottle is opened, in a manner of injection
A certain amount of arsenic hydride is injected in transfer bottle, the access between triple valve and stock bottle is closed, the reading M after writing down transfer1
(unit is gram), the quality for shifting arsenic hydride in bottle at this time is M=M0-M1。
The transfer and metering of nitrogen: nitrogen cylinder is placed on electronic scale, the reading m before writing down transfer0(unit is gram), opens
Access between triple valve and nitrogen cylinder, nitrogen enter triple valve, and drive the arsenic hydride raw material of liquid to enter and mix room, then
A certain amount of nitrogen is continuously added, the access between triple valve and nitrogen cylinder is closed, the reading m after writing down transfer1(unit is
Gram), the quality of nitrogen transfer at this time is m=m0-m1.Complete the transfer and metering of arsenic hydride raw material and nitrogen.
3) it mixes
After the completion of transfer, mechanical rolling mixing mechanism is opened, roller bearing starts turning, and mixing bottle is driven to start turning.Mixed
As the temperature rises for arsenic hydride in even bottle, starts to gasify, and mixes with nitrogen.
4) it stores
After inspection is satisfied the criteria, calibrating gas is injected in steel cylinder, calculates the saturated vapour pressure P of arsenic hydride at room temperature0,
And the partial pressure P of the arsenic hydride in steel cylinder in stored calibrating gas is made to be lower than P0。
For the accuracy for guaranteeing obtained gas reference material, to preparing the pure of arsenic hydride raw material used in standard substance
Degree detection, can use existing method for detecting purity such as gas chromatography, Karl Fischer coulometric determination, ICPMS method, ion color
The purity of the methods of spectrometry or DSC measurement arsenic hydride raw material.
After mixing, uniformity testing is carried out to standard substance using GC-ICP-MS direct-injection technique, stability is examined
It examines.
It is equipped with coolant liquid in cooling bath, the arsenic hydride stored in stock bottle is maintained at liquid.
The present invention compared with the existing technology the advantages of be: this method has filled up domestic blank, using cooling and liquid nitrogen gas
The mode for changing purging makes the gaseous arsine with specific severe toxicity keep liquid in transfer process, avoids its leakage and causes the accident
A possibility that noresidue transfer completely simultaneously, while the purge gas used is diluent gas, will not influence preparation as a result, total
Nitrogen use level can mass comparator measure by way of obtain, ensure that accuracy.By being deposited lower than saturated vapor pressure
The mode of storage ensure that calibrating gas has good time stability.
Detailed description of the invention
Fig. 1 is the preparation facilities structural schematic diagram of arsine gas standard substance in nitrogen.
In figure: 1- mixing bottle, 2- transfer bottle, 3- stock bottle, 4- liquid nitrogen bottle, 5- machinery rolling mixing mechanism, 6- cooling bath,
7- triple valve, 8- coolant liquid, 9- liquid arsenic hydride, 10- liquid nitrogen, 11,12- be mass comparator, 13- bracket, 14- roller bearing.
Specific embodiment
The present invention will be further described with reference to the accompanying drawings and detailed description.
The preparation facilities of arsine gas standard substance in a kind of nitrogen, as shown in Figure 1, the device includes mixing bottle 1, transfer
Bottle 2, stock bottle 3, liquid nitrogen bottle 4, machinery roll mixing mechanism 5, cooling bath 6, triple valve 7 and the first mass comparator 11, second
Mass comparator 12.
Stock bottle 3 is placed in cooling bath 6, and coolant liquid 8 is housed in cooling bath 6, the arsenic hydride 9 stored in stock bottle is kept
In liquid, cooling bath is integrally placed on mass comparator 11, and stock bottle connects triple valve 7.Liquid nitrogen bottle 4 is placed in the first mass and compares
On instrument 12, memory is placed with liquid nitrogen 10.Liquid nitrogen bottle 4 connects triple valve 7.
Triple valve 7 is also connected with transfer bottle 2, and the connection of transfer 2 other side of bottle mixes bottle 1, mixes and is equipped with mechanical roll below bottle 1
Mixing mechanism 5, machinery roll the bracket 13 that mixing mechanism 5 includes two sides, and more roller bearings 14 being connected on bracket, mix
Bottle 1 is placed on roller bearing 14.
To prepare 100 × 10-6In the nitrogen of mol/mol for arsine gas standard substance, to method disclosed by the invention
It is further described.
The preparation method of arsine gas standard substance in presently disclosed nitrogen specifically includes metering, turns
Move, mix etc., the accuracy to guarantee obtained gas reference material first, it is necessary to the purity symbol of guarantee preparation raw material first
It closes and requires, therefore existing purity detecting can be used to the purity detecting for preparing arsenic hydride raw material used in standard substance
The methods of method such as gas chromatography, Karl Fischer coulometric determination, ICPMS method, the chromatography of ions or DSC measures arsenic hydride raw material
Purity.
Then to including mixing the air-channel systems such as bottle, transfer bottle, connecting line, triple valve to clean, removal wherein may be used
The impurity of calibrating can be interfered, the high pure nitrogen after cleaning using purity greater than 99.999% is purged, and is driven away therein
Gas then vacuumizes entire air-channel system.
The transfer and metering of arsenic hydride raw material: arsenic hydride raw material is placed in the stock bottle in cooling bath, and cooling bath is placed in matter
It measures on comparator, the reading M before writing down transfer0(unit is gram), and the access between triple valve and stock bottle is opened, with injection
Mode by liquid arsenic hydride be transferred to transfer bottle in, as the reading M of mass comparator1=M0Stop injection at -0.07793 gram,
Close the access between triple valve and stock bottle.
The transfer and metering of nitrogen: liquid nitrogen bottle is placed on mass comparator, the reading m before writing down transfer0(unit thousand
Gram), the access between triple valve and liquid nitrogen bottle is opened, liquid nitrogen enters triple valve, and gasifies rapidly, drives the arsenic hydride of liquid former
Material, which enters, mixes bottle, although liquid nitrogen gasification at this time is nitrogen, but still has rather low temperature, cooling arsenic hydride raw material is allowed to
Liquid is kept, the liquid nitrogen that gasification is added is continued thereafter with, as the reading m of mass comparator1=m0When -280.13g, triple valve is closed
Access between liquid nitrogen bottle.Complete the transfer and metering of arsenic hydride raw material and nitrogen.
After the completion of transfer, mechanical rolling mixing mechanism is opened, roller bearing starts turning, and mixing bottle is driven to start turning.Mixed
As the temperature rises for arsenic hydride in even bottle, starts to gasify, and mixes with nitrogen.
After mixing, uniformity testing is carried out to standard substance using GC-ICP-MS direct-injection technique, stability is examined
It examines.
After inspection is satisfied the criteria, calibrating gas is injected in standard steel cylinder specified in GB5099, calculates arsenic hydride in room
Saturated vapour pressure P under temperature0, and the partial pressure P of the arsenic hydride in steel cylinder in stored calibrating gas is made to be lower than P0, use is this
Mode can make the arsenic hydride in prepared calibrating gas keep gaseous state at normal temperature, improve the stability of gas.
Since arsenic hydride is gaseous state at normal temperature and has severe toxicity, to avoid the leakage of gaseous arsine in transfer process from making
A possibility that at safety accident, the present invention makes it keep liquid in transfer process by the way of cooling, avoids its leakage.Together
When by way of liquid nitrogen gasification driving purging, the purging driving capability of the existing gas of low temperature nitrogen after liquid nitrogen gasification guarantees arsenic
Change the complete noresidue transfer of hydrogen, and low temperature is kept so that the arsenic hydride of transfer process is maintained at liquid more than the boiling point of arsenic hydride
State.The purge gas for further ensuring safety, while using is diluent gas, will not influence preparation as a result, total simultaneously
Nitrogen use level can mass comparator measure by way of obtain, ensure that accuracy.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, it is all according to the present invention
Technical spirit any simple modification to the above embodiments, change and equivalent structural changes, still fall within skill of the present invention
In the protection scope of art scheme.
Claims (5)
1. the preparation facilities of arsine gas standard substance in a kind of nitrogen, which is characterized in that the device includes mixing bottle (1), is turned
It moves bottle (2), stock bottle (3), liquid nitrogen bottle (4), machinery rolls mixing mechanism (5), and cooling bath (6), triple valve (7) and quality compare
Instrument (11 and 12)；
Wherein, stock bottle (3) is placed in cooling bath (6), and cooling bath (6) is integrally placed on mass comparator (11)；Liquid nitrogen bottle (4)
It is placed on another mass comparator (12)；
Bottle (2) one end is shifted by triple valve (7) connection stock bottle (3) and liquid nitrogen bottle (4), other end connection mixes bottle (1), mixes
Mechanical rolling mixing mechanism (5) is equipped with below even bottle (1).
2. the preparation facilities of arsine gas standard substance in a kind of nitrogen according to claim 1, which is characterized in that described
Mechanical roll mixing mechanism (5) include the bracket (13) of two sides, and more roller bearings (14) being connected on bracket mix bottle
(1) it is placed on roller bearing (14).
3. the preparation facilities of arsine gas standard substance in a kind of nitrogen according to claim 1, which is characterized in that described
Cooling bath in (6) be equipped with coolant liquid (8).
4. the preparation method of arsine gas standard substance in a kind of nitrogen, this method specifically includes 1) cleaning device, 2) metering with
Transfer, 3) mix step, which is characterized in that specifically:
1) cleaning device
First to including mixing the air-channel systems such as bottle, transfer bottle, connecting line, triple valve to clean, removal wherein can be competent
The impurity for disturbing calibrating, the high pure nitrogen after cleaning using purity greater than 99.999% are purged, and gas therein is driven away,
Then entire air-channel system is vacuumized；
2) metering and transfer
The wherein transfer and metering of arsenic hydride raw material: arsenic hydride raw material is placed in stock bottle, and stock bottle is placed on mass comparator,
Reading M before writing down transfer0, and the access between triple valve and stock bottle is opened, by a certain amount of arsenic in a manner of injection
In hydrogen injection transfer bottle, the access between triple valve and stock bottle is closed, the reading M after writing down transfer1, arsenic in bottle is shifted at this time
The quality for changing hydrogen is M=M0-M1；
The transfer and metering of nitrogen: nitrogen cylinder is placed on electronic scale, the reading m before writing down transfer0(unit is gram), opens threeway
Access between valve and nitrogen cylinder, nitrogen enter triple valve, and drive the arsenic hydride raw material of liquid to enter and mix room, continue thereafter with
A certain amount of nitrogen is added, closes the access between triple valve and nitrogen cylinder, the reading m after writing down transfer1(unit is gram), this
When nitrogen transfer quality be m=m0-m1, complete the transfer and metering of arsenic hydride raw material and nitrogen；
3) it mixes
After the completion of transfer, mechanical rolling mixing mechanism is opened, roller bearing starts turning, and mixing bottle is driven to start turning, and is mixing bottle
As the temperature rises for interior arsenic hydride, starts to gasify, and mixes with nitrogen.
5. the preparation method of arsine gas standard substance in a kind of nitrogen according to claim 4, which is characterized in that the party
Method further include include 4) store, specifically:
After inspection is satisfied the criteria, calibrating gas is injected in steel cylinder, calculates the saturated vapour pressure P of arsenic hydride at room temperature0, and make
The partial pressure P for obtaining the arsenic hydride in steel cylinder in stored calibrating gas is lower than P0。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910297006.2A CN109884218A (en) | 2019-04-12 | 2019-04-12 | The preparation facilities and method of arsine gas standard substance in a kind of nitrogen |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114130435A (en) * | 2020-09-04 | 2022-03-04 | 中国石油天然气股份有限公司 | Quantitative ring for gas transfer and gas transfer method |
| CN114184446A (en) * | 2021-12-21 | 2022-03-15 | 中国计量科学研究院 | Volatile organic gas standard substance preparation system capable of weighing on line |
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| CN114184446A (en) * | 2021-12-21 | 2022-03-15 | 中国计量科学研究院 | Volatile organic gas standard substance preparation system capable of weighing on line |
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