CN106769369B - Prepare container, the device and method of the organic mixed solution standard substance of volatility - Google Patents

Prepare container, the device and method of the organic mixed solution standard substance of volatility Download PDF

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Publication number
CN106769369B
CN106769369B CN201611117959.9A CN201611117959A CN106769369B CN 106769369 B CN106769369 B CN 106769369B CN 201611117959 A CN201611117959 A CN 201611117959A CN 106769369 B CN106769369 B CN 106769369B
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hole
plug
container
bottle
narrow
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CN106769369A (en
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王海峰
刘卫
张艾蕊
王海
宋小平
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National Institute of Metrology
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National Institute of Metrology
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/38Diluting, dispersing or mixing samples

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
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Abstract

The present invention relates to a kind of container, device and methods for preparing the organic mixed solution standard substance of volatility, wherein the container for preparing the organic mixed solution standard substance of volatility includes narrow-mouthed bottle, bottle cap, the first sealing-plug and the second sealing-plug;Wherein, bottle cap covers on the bottleneck of narrow-mouthed bottle, and Bottle cap top, which is equipped with, takes fluid through-hole and balance through-hole, and fluid through-hole and balance through-hole is taken to be connected to narrow-mouthed bottle inside;First sealing-plug can be placed on and take in fluid through-hole, and the second sealing-plug can be placed in balance through-hole.Technical solution proposed by the present invention can effectively inhibit the volatilization of volatile components in organic mixed solution standard substance process for preparation, also the volatilization of volatile components during organic mixed solution standard substance can be inhibited to dispense ensure that the accuracy of the organic configuration of mixed solution standard substance and packing process.

Description

Prepare container, the device and method of the organic mixed solution standard substance of volatility
Technical field
The present invention relates to a kind of glass containers, and in particular to a kind of appearance for preparing the organic mixed solution standard substance of volatility Device, device and method.
Background technique
The organic mixed solution standard substance of volatility generallys use gravimetric method to prepare, i.e., in volumetric flask or other containers In, the organic pure material of plurality of liquid is sequentially added, and weigh organic pure material quality of addition, according to the quality of every kind of pure material And its purity, calculate the content of the organic compound in mixed solution.The volatility of various fluid organic materials is different, addition sequence It is different, it is evaporate into environment during the preparation process or the quality in superjacent space has difference in container, so that gravimetric method is matched Result processed deviates the actual content of each organic compound.
When organic mixed solution is dispensed into ampoule bottle, solution usually is extracted from container bottom with a tubule and is distributed to ampoule Bottle, is then sealed with flame rapidly, repeats the process, realizes continuous packing.The disadvantages of the method are as follows in preparation process, in container Superjacent headspace becomes larger, the stronger component evolution of volatility, and constituent content decline in solution deviates gravimetric method and prepares As a result, simultaneously between the bottle of standard substance each component content uniformity be deteriorated.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of volatility organic mixed solution standard substances of preparing Container, device and method.Technical solution proposed by the present invention is as follows.
A kind of container preparing the organic mixed solution standard substance of volatility, which includes narrow-mouthed bottle, bottle cap, first close Blocking and the second sealing-plug;Wherein, bottle cap covers on the bottleneck of narrow-mouthed bottle, and Bottle cap top, which is equipped with, takes fluid through-hole and balance through-hole, Fluid through-hole and balance through-hole is taken to be connected to narrow-mouthed bottle inside;First sealing-plug can be placed on and take in fluid through-hole, the second sealing-plug It can be placed in balance through-hole.
Further, the container further includes taking liquid plug and balanced plug, takes liquid plug that can be placed on and takes in fluid through-hole, balanced plug It can be placed in balance through-hole.
Further, taking fluid through-hole is tapped through hole, and the first sealing-plug is solid thread plug, and taking liquid plug is hollow thread Plug.
Further, balance through-hole is tapped through hole, and the second sealing-plug is solid thread plug, and balanced plug is hollow thread Plug.
Further, round tube is equipped in hollow thread plug.
Further, the round tube lower end in liquid plug is taken to be equipped with filter screen.
Further, the container is glass container.
Further, the bottleneck outer peripheral edge of narrow-mouthed bottle is equipped with external screw thread, and the inner peripheral of bottle cap is equipped with internal screw thread, and bottle cap passes through The opening is set on the bottleneck of narrow-mouthed bottle, the external screw thread of narrow-mouthed bottle bottleneck and the screw-internal thread fit of bottle cap.
A kind of device preparing the organic mixed solution standard substance of volatility, the device include two as described in preceding any one Container, wherein the first container in two containers is mixed solution supply container, and second container is equalizing reservoir;First holds The balance through-hole of device is connected with the balance through-hole of second container;Automatic-packaging takes fluid through-hole to extract first from the first container The organic mixed solution standard substance of the volatility in the narrow-mouthed bottle of container is dispensed;The fluid through-hole that takes of second container is to open Put state.
A method of the organic mixed solution standard substance of volatility being prepared, this method is using two as described in preceding any one Container, described two containers be the first container and second container, include the following steps:
Step S11: it is individually contained with ampoule bottle each volatile in the mixed organic pure material of plurality of liquid of needs The organic pure material of liquid, and calculate with Subtraction method the quality of the organic pure material of each volatile liquid;
Step S12: the ampoule of the organic pure material of volatile liquid will be respectively loaded with from the bottleneck of the narrow-mouthed bottle of the first container Bottle is put into the narrow-mouthed bottle of the first container, and takes fluid through-hole in the narrow-mouthed bottle of the first container with long syringe needle by the first container Syringe is separately added into the organic pure material of remaining liquid, and weighs respectively;The first appearance is placed in fluid through-hole in taking for the first container First sealing-plug of device places the second sealing-plug of the first container in the balance through-hole of the first container;The first container is rocked, is made The each ampoule bottle being put into narrow-mouthed bottle is broken, and the organic pure material of liquid contained in all ampoule bottles and first holds The organic pure material of liquid being added in the narrow-mouthed bottle of device is uniformly mixed, and the organic mixed solution standard substance of volatility is prepared;
Step S13: step S11 and step S12 is repeated, to prepare in the narrow-mouthed bottle of second container and the first container The identical organic mixed solution standard substance of volatility in narrow-mouthed bottle;
Step S14: the balance through-hole of the first container is connected to the balance through-hole of second container, and second container takes fluid through-hole For open state;Automatic-packaging has from the volatility in the narrow-mouthed bottle for taking fluid through-hole to extract the first container of the first container Machine mixed solution standard substance is dispensed into each sub-bottling.
Beneficial effects of the present invention: container, the dress of the preparation organic mixed solution standard substance of volatility proposed by the present invention It sets and method, the volatilization of volatile components in organic mixed solution standard substance process for preparation can be effectively inhibited, can also be pressed down It is formed with the volatilization of volatile components during machine mixed solution standard substance dispenses, ensure that organic mixed solution standard substance is matched Set and dispense the accuracy of process.Although headspace becomes larger in addition, the liquid level of thin mouth vial reduces during packing, But the composition of organic matter does not change in gas phase, liquid and gas are in equilibrium state always, therefore the composition of liquid phase does not have Change, the liquid composition for being assigned to ampoule bottle is kept constant, it is ensured that between the bottle of the organic mixed solution standard substance of liquid uniformly Property.
Detailed description of the invention
Fig. 1 is that the structure of the glass container proposed by the present invention for the organic mixed solution standard substance preparation of volatility is shown It is intended to;
Fig. 2 is the central, threaded through-hole of bottle cap proposed by the present invention and the schematic diagram of side tapped through hole;
Fig. 3 a is the structural schematic diagram of the solid thread plug of center through hole proposed by the present invention;
Fig. 3 b is the structural schematic diagram of the solid thread plug of side through hole proposed by the present invention;
Fig. 4 a is the structural schematic diagram of center through hole hollow circular-tube thread plug proposed by the present invention;
Fig. 4 b is the structural schematic diagram of side through hole hollow circular-tube thread plug proposed by the present invention;
Fig. 5 is the structural schematic diagram of additional equilibrium bottle standard solution proposed by the present invention packing;
Fig. 6 is the method flow diagram of the preparation organic mixed solution standard substance of volatility proposed by the present invention;
Fig. 7 is the correlation data using mixed solution each component measurement result and conventional method prepared by the present invention.
Description of symbols: the thin mouth vial of 1-;2- external screw thread;3- internal screw thread;4- bottle cap;5- central, threaded through-hole;6- The solid thread plug of center through hole;7- center through hole hollow circular-tube thread plug;The first round tube of 71-;The side 8- tapped through hole;9- side through hole Solid thread plug;10- side through hole hollow circular-tube thread plug;The second round tube of 101-;11- filter screen;The thin mouth vial of 12-.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, and reference Attached drawing, the present invention is described in more detail.In a particular embodiment, using the material of container as glass material, pass through screw thread phase Present invention is described for the mode mutually cooperated, but as known to those skilled in the art, and the invention is not limited to attached drawings and following Embodiment.
A kind of container preparing the organic mixed solution standard substance of volatility proposed by the present invention, as shown in Figure 1.The container It can be glass container, but as known to those skilled in the art, which can also be made of other materials.
The container includes thin mouth vial 1 and bottle cap 4.
The volume of thin mouth vial 1 is, for example, 500mL, 1L etc..The internal diameter of thin 1 bottleneck of mouth vial is less than thin mouth glass The internal diameter at 1 other positions of glass bottle.The bottleneck outer peripheral edge of thin mouth vial 1 is equipped with external screw thread 2.
4 bottom opening of bottle cap can be set on the bottleneck of thin mouth vial 1.The inner peripheral of bottle cap 4 is equipped with internal screw thread 3, carefully The external screw thread 2 of mouth 1 bottleneck of vial can be fitted close with the internal screw thread 3 of bottle cap 4.Preferably, the outer spiral shell of thin 1 bottleneck of mouth vial The internal screw thread 3 of line 2 and bottle cap 4 is same nominal diameter.Narrow-mouthed bottle is filled in it will be understood by those skilled in the art that can also use The bottle cap of bottleneck or the bottle cap for screwing in narrow-mouthed bottle bottleneck.
4 top center position of bottle cap is equipped with central, threaded through-hole 5, and the position of 4 top offset from center of bottle cap is equipped with side screw thread Through-hole 8, certainly, the position of central, threaded through-hole 5 and side tapped through hole 8 also can change, as long as guaranteeing that the central, threaded is logical Hole 5 and side tapped through hole 8 can be communicated with the inside of thin mouth vial 1.
Central, threaded through-hole 5 is mainly when packaged convenient for the liquid inside the thin mouth vial 1 as solution supply bottle Outflow, and convenient for sucking air as the thin mouth vial 12 of equilibration flask;Side tapped through hole 8 mainly when packaged with balance Bottle cooperation is with the air pressure in balance solution supply bottle, and guarantees uniformity between the bottle of the organic mixed solution standard substance of liquid, As shown in Figure 2 and Figure 5.Preferably, the internal diameter of the central, threaded through-hole 5 of bottle cap 4 is 10mm, the internal diameter of side tapped through hole 8 Size is 3mm.
The central, threaded through-hole 5 equipped with the solid thread plug 6 of center through hole and center through hole hollow circular-tube thread plug 7, As shown in Fig. 3 a and Fig. 4 a, the central location of center through hole hollow circular-tube thread plug 7 is equipped with the first round tube 71, under the first round tube 71 There is filter screen 11 at end, as shown in Figure 5;The external screw thread of the solid thread plug 6 of center through hole and center through hole hollow circular-tube thread plug 7 External screw thread can be fitted close with the internal screw thread of central, threaded through-hole 5, it is preferable that the external screw thread of the solid thread plug 6 of center through hole External screw thread with center through hole hollow circular-tube thread plug 7 is same nominal diameter with the internal screw thread of central, threaded through-hole 5.
The side tapped through hole 8 is equipped with the solid thread plug 9 of side through hole and side through hole hollow circular-tube thread plug 10, such as Fig. 3 b With shown in Fig. 4 b, the central location of side through hole hollow circular-tube thread plug 10 is equipped with the second round tube 101;The solid thread plug 9 of side through hole External screw thread and the external screw thread of side through hole hollow circular-tube thread plug 10 can be fitted close with the internal screw thread of side tapped through hole 8;Side The external screw thread of the external screw thread of the solid thread plug 9 of through-hole and side through hole hollow circular-tube thread plug 10 with the interior spiral shell of side tapped through hole 8 Line is same nominal diameter.
It is retouched using process combination Fig. 1 to Fig. 6 of the glass container preparation organic mixed solution standard substance of volatility It states.
Step S11, the weighing of the organic pure material of volatile liquid: with assay balance first ampoule of precise in order The bottle quality of bottle moves into the first volatile liquid organic pure material in ampoule bottle, seals first ampoule bottle with sealing machine, The gross mass of first ampoule bottle after precise sealing, the gross mass subtract the bottle quality of the first ampoule bottle and the bottle of fusing After cap quality, the quality of the organic pure material of the first volatile liquid is obtained.In the same manner, successively that other are several The organic pure material of mixed volatile liquid is needed to enclose in ampoule bottle respectively, and it is organic to calculate separately out each volatile liquid The quality of pure material.
Step S12, the preparation of the organic mixed solution standard substance of volatility: to be loaded with volatile liquid organic pure by each The ampoule bottle of substance is put into thin mouth vial 1, screws in the solid thread plug 6 of center through hole in the central, threaded through-hole 5 of bottle cap 4, In side, tapped through hole 8 screws in the solid thread plug 9 of side through hole, then bottle cap 4 is spun on the outer of thin mouth vial 1 by its internal screw thread 3 On screw thread 2;Then the solid thread plug 6 of center through hole is removed from central tapped through hole 5, long needle applicator is used to draw as molten The long syringe needle of the small organic pure material of liquid of the first volatility of matter, long needle applicator passes through central, threaded through-hole 5, minute hand Head cannot encounter bottle cap 4 and thin mouth vial 1, can not be inserted into the solution in thin mouth vial 1, as close as possible to solute liquid At above face, the organic pure material of the small liquid of the first volatility in long needle applicator is slowly injected into thin mouth vial 1 It is interior, after to be implanted, long needle applicator is taken out, the solid thread plug 6 of center through hole is spun on central, threaded through-hole 5 again On.
Before and after the small organic pure material of liquid of the first volatility is added, thin mouth vial is weighed with assay balance respectively 1 quality, the quality of the small organic pure material of liquid of the first volatility that addition is calculated with Subtraction method.According to identical Method sequentially adds other several organic pure materials of liquid for needing mixed volatility small, and it is organic to calculate each liquid The quality of pure material, until whole organic pure materials of liquid are added and weigh and finish.Thin mouth vial 1 is acutely rocked, makes to be put into Each ampoule bottle it is broken, and all ampoule bottles in contain organic pure material and thin mouth vial 1 in it is all molten Matter is uniformly mixed.
Wherein, the content of certain organic compound is calculated as follows in mixed solution:
In formula (1):
xi,0--- the content of i-th kind of organic compound, % in mixed solution;
Purityi--- the purity of i-th kind of organic pure material, %;
mi--- the quality of i-th kind of organic pure material, g in mixed solution;
--- the gross mass of mixed solution, g.
Step S13, it the preparation of equilibration flask: is prepared according to abovementioned steps S11 and step S12, then in thin mouth vial 12 With the organic mixed solution of volatility identical in thin mouth vial 1.
Step S14, it is hollow that center through hole the connection of sealed in unit: is screwed in the central, threaded through-hole 5 of thin mouth vial 1 Round tube thread plug 7 screws in center through hole hollow circular-tube thread plug 7 in the central, threaded through-hole 5 of thin mouth vial 12;Thin mouth glass The lower end of first round tube 71 of the lower end and thin mouth vial 12 of the first round tube 71 of glass bottle 1 reaches bottom of bottle, under the first round tube The filter screen 11 at end is used to filter ampoule bottle fragment;The upper end of first round tube 71 of thin mouth vial 1 and ampoule bottle automatic packaging The Liquid sample introduction pipe of machine connects, and the upper end exposure of the first round tube 71 of thin mouth vial 12 is in air.
Side through hole hollow circular-tube thread plug 10 is screwed in the side tapped through hole 8 of thin mouth vial 1, in thin mouth vial 12 Side tapped through hole 8 in screw in side through hole hollow circular-tube thread plug 10, the side through hole hollow circular-tube thread plug 10 of thin mouth vial 1 The second round tube of same root 101 is shared with the side through hole hollow circular-tube thread plug 10 of thin mouth vial 12,101 one end of the second round tube It protrudes into thin mouth vial 1, the other end protrudes into thin mouth vial 12, and thin mouth vial 1 passes through the second round tube 101 and thin mouth glass Glass bottle 12 is connected to.
Step S15, the distribution and encapsulation of solution: ampoule bottle automatic-packaging extracts the distribution of the solution in thin mouth vial 1 Into the ampoule bottle of 5mL volume, every bottle of 2mL solution, then with flame to the ampoule bottle Quick seal that solution is housed;It is so continuous Solution, encapsulation are distributed, until complete soln packing finishes.
When ampoule bottle automatic-packaging extracts the solution in thin mouth vial 1, negative pressure is formed in thin mouth vial 1, by It is connected to by the second round tube 101 with thin mouth vial 12 in thin mouth vial 1, the upper end of the first round tube 71 of thin mouth vial 12 In air, air enters from the first round tube 71 of thin mouth vial 12 at this time for exposure, forms bubble and escapes liquid level, into thin mouth Second round tube 101 of vial 12 enters the second round tube 101 of thin mouth vial 1 via pipeline, maintains in thin mouth vial 1 Air pressure balance.
In addition, into thin mouth vial 12 air after hold-up, into thin 12 superjacent top of mouth vial Portion space forms consistent with the air of thin 1 superjacent headspace of mouth vial;Therefore although thin mouth during packing The liquid level of vial 1 reduces, and headspace becomes larger, but the composition of organic matter does not change in gas phase, and liquid and gas are always Composition in equilibrium state, therefore liquid phase does not change, and the liquid composition for being assigned to ampoule bottle is kept constant, it is ensured that liquid Uniformity between the bottle of organic mixed solution standard substance.
Explanation is compared so that three kinds prepare the method for the organic mixed solution standard substance of volatility as an example below, these three Method is that conventional method, the method with equilibration flask packing and ampoule bottle proposed by the present invention weigh volatile organic matter respectively With the method dispensed with equilibration flask.
(1) conventional method prepares the organic mixed solution standard substance of volatility
The sequence to grow from weak to strong by volatility sequentially adds the tert-butyl alcohol, ethyl alcohol, first into the thin mouth vial that volume is 1L Alcohol, methyl tertiary butyl ether(MTBE) (MTBE) and glycol dimethyl ether (DME) each 20mL, and have with each liquid of assay balance precise The quality of machine pure material.Then 900mL isooctane and correct amount is added.Bottle cap is screwed on, solution is shaken up.A piece round tube is worn Meticulous mouth vial bottle cap, round tube lower end connect sealing machine Liquid sample introduction mouth close to bottle bottom, round tube upper end.When packing, take out Taking 2mL solution to distribute to capacity is to be sealed with flame rapidly in 5mL ampoule bottle, repeats the process, realizes continuous packing.It is divided into 500 standard solution are filled, are divided into 14 parts, about 35 every part by the sequencing of packing.From the 1st, 3,5,7,9,11,12 and 1 is respectively extracted in 14 parts, with the content of the gas chromatographic detection tert-butyl alcohol, ethyl alcohol, methanol and MTBE.Contained according to each organic compound The gravimetric method preparation value and gas-chromatography measured value of amount, calculate the volatile quantity of each organic compound, specific formula is as follows:
In formula (2):
Δxi--- the volatile quantity of i-th of organic compound, %;
xi--- the content of i-th of organic compound, g in the mixed solution of gas Chromatographic Determination;
xi,0--- the gravimetric method Configuration Values of the content of i-th kind of organic compound, g in mixed solution;
(2) method with equilibration flask packing prepares the organic mixed solution standard substance of volatility
The sequence to grow from weak to strong by volatility sequentially adds the tert-butyl alcohol, ethyl alcohol, first into the thin mouth vial that volume is 1L Alcohol, methyl tertiary butyl ether(MTBE) (MTBE) and glycol dimethyl ether (DME) each 20mL, and it is organic pure with each liquid of balance precise The quality of substance.Then 900mL isooctane and correct amount is added.Bottle cap is screwed on, solution is shaken up.Take another thin mouth glass Bottle is prepared and forms identical mixed solution.Two thin mouth vial is connected, gas pressure balancing in bottle is kept.Extract thin mouth Solution is distributed to ampoule bottle in vial, is sealed with flame rapidly, and the process is repeated, and realizes continuous packing.It is divided into and fills 500 marks Quasi- solution is divided into 14 parts, about 35 every part by the sequencing of packing.It is each from the 1st, 3,5,7,9,11,12 and 14 part 1 is extracted, with the content of the gas chromatographic detection tert-butyl alcohol, ethyl alcohol, methanol and MTBE.According to the weight of each organic compound content Method preparation value and gas-chromatography measured value calculate the volatile quantity of each organic compound according to formula (2).
(3) ampoule bottle weighs volatile organic matter and the method with equilibration flask packing prepares the organic mixed solution mark of volatility Quasi- substance
The ethyl alcohol of 20mL is encapsulated in ampoule bottle by the method according to the invention, with the matter of Subtraction method precise ethyl alcohol Ampoule bottle equipped with ethyl alcohol is put into thin mouth vial 1 by amount;In the same manner, 20mL methanol, MTBE and DME are individually enclosed in In ampoule bottle, weighing, and be put into thin mouth vial 1.The 20mL tert-butyl alcohol, its matter of precise are added into thin mouth vial 1 Amount;Then 900mL isooctane, and precise its quality are added into thin mouth vial 1.Thin mouth vial 1 is acutely rocked, is made Ampoule bottle is smashed, and solute is uniformly mixed in organic matter and narrow-mouthed bottle in ampoule bottle.
With identical preparation method, preparation forms identical fluid organic material mixed solution, is stored in thin mouth vial 12 In.Thin mouth vial 1 and thin mouth vial 12 are connected according to foregoing description (reference can be made to shown in Fig. 5), keep gas pressure in bottle Dynamic balance.It extracts solution in thin mouth vial to distribute to ampoule bottle, be sealed with flame rapidly, repeat the process, realize continuous point Dress.It is divided into and fills 500 standard solution, be divided into 14 parts, about 35 every part by the sequencing of packing.From the 1st, 3,5,7,9, 11,1 is respectively extracted in 12 and 14 parts, with the content of the gas chromatographic detection tert-butyl alcohol, ethyl alcohol, methanol and MTBE.According to each organic The gravimetric method preparation value and gas-chromatography measured value of compounds content calculate the volatile quantity of each organic compound according to formula (2).
The standard sample that above-mentioned three kinds different preparation methods obtain, volatility Comparative result are as shown in Figure 7.
Fig. 7 left data is using the mixed solution standard substance of customary preparation methods preparation, the 1st part of methanol volatile quantity It is 2.801%, the 14th part of methanol volatile quantity is 4.073%, and the difference of volatile quantity is 1.272%, it can be seen that packing sequence is got over Rearward, volatile quantity increases;The volatile quantity of methanol and MTBE are maximum, and in the 14th part, the volatile quantity of methanol and MTBE are respectively 4.073% and 4.968%.
Data among Fig. 7 are using the mixed solution standard substance prepared with equilibration flask, and the 1st part of methanol volatile quantity is 1.793%, the 14th part of methanol volatile quantity is 2.069%, although volatile quantity is increased with packing back, Difference is only 0.276%, better than conventional method;14th part of methanol volatile quantity (2.069%) is than the 14th part of conventional method (4.073%) low;Illustrate the volatilization of volatile organic matter during can inhibiting packing with the method dispensed with equilibration flask.
Data on the right side of Fig. 7 are using the mixed solution standard substance of scheme proposed by the present invention preparation, i.e. ampoule bottle claims It measures volatile organic matter and is dispensed with equilibration flask, the 1st part of methanol volatile quantity is 1.2%, and the 14th part of methanol volatile quantity is 1.387%, although volatile quantity increased, and difference is only 0.187% with packing back, than conventional method and Method with equilibration flask packing is low;14th part of methanol volatile quantity (1.387%) is than conventional method (4.073%) and with equilibration flask The method for dispensing (2.069%) is low;Illustrate to weigh volatile organic matter using ampoule bottle proposed by the present invention and with equilibration flask point The method of dress can effectively inhibit the volatilization of volatile organic matter during preparing and dispensing, improve mixed solution standard substance Bottle between uniformity and definite value result accuracy.
More than, embodiments of the present invention are illustrated.But the present invention is not limited to above embodiment.It is all Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in guarantor of the invention Within the scope of shield.

Claims (20)

1. a kind of device for preparing the organic mixed solution standard substance of volatility, which is characterized in that the device includes two containers, The container includes narrow-mouthed bottle, bottle cap, the first sealing-plug and the second sealing-plug;Wherein, bottle cap covers on the bottleneck of narrow-mouthed bottle, bottle cap Top, which is equipped with, takes fluid through-hole and balance through-hole, and fluid through-hole and balance through-hole is taken to be connected to narrow-mouthed bottle inside;First sealing-plug energy It is placed on and takes in fluid through-hole, the second sealing-plug can be placed in balance through-hole;
Wherein, the first container in two containers is mixed solution supply container, and second container is equalizing reservoir;The first container Balance through-hole is connected with the balance through-hole of second container;Automatic-packaging takes fluid through-hole to extract the first container from the first container Narrow-mouthed bottle in the organic mixed solution standard substance of the volatility dispensed;Second container takes fluid through-hole for open shape State.
2. the apparatus according to claim 1, which is characterized in that the container further includes taking liquid plug and balanced plug, takes liquid plug It can be placed on and take in fluid through-hole, balanced plug can be placed in balance through-hole.
3. the apparatus of claim 2, which is characterized in that taking fluid through-hole is tapped through hole, and the first sealing-plug is solid Thread plug, taking liquid plug is hollow thread plug.
4. device according to claim 2 or 3, which is characterized in that balance through-hole is tapped through hole, and the second sealing-plug is real Heart thread plug, balanced plug are hollow thread plug.
5. device according to claim 3, which is characterized in that be equipped with round tube in hollow thread plug.
6. device according to claim 5, which is characterized in that the round tube lower end in liquid plug is taken to be equipped with filter screen.
7. device according to claim 1 or 2, which is characterized in that the container is glass container.
8. device according to claim 1 or 2, which is characterized in that the bottleneck outer peripheral edge of narrow-mouthed bottle is equipped with external screw thread, bottle cap Inner peripheral be equipped with internal screw thread, bottle cap is set on the bottleneck of narrow-mouthed bottle by the opening of bottle cap, the external screw thread of narrow-mouthed bottle bottleneck With the screw-internal thread fit of bottle cap.
9. device according to claim 4, which is characterized in that be equipped with round tube in hollow thread plug.
10. device according to claim 9, which is characterized in that the round tube lower end in liquid plug is taken to be equipped with filter screen.
11. a kind of method for preparing the organic mixed solution standard substance of volatility, which is characterized in that this method uses two appearances Device, the container include narrow-mouthed bottle, bottle cap, the first sealing-plug and the second sealing-plug;Wherein, bottle cap covers on the bottleneck of narrow-mouthed bottle, Bottle cap top, which is equipped with, takes fluid through-hole and balance through-hole, and fluid through-hole and balance through-hole is taken to be connected to narrow-mouthed bottle inside;First sealing Plug, which can be placed on, to be taken in fluid through-hole, and the second sealing-plug can be placed in balance through-hole;Described two containers are the first container and the Two containers, include the following steps:
Step S11: it is individually contained with ampoule bottle and needs each volatile liquid in the mixed organic pure material of plurality of liquid Organic pure material, and calculate with Subtraction method the quality of the organic pure material of each volatile liquid;
Step S12: the ampoule bottle for being respectively loaded with the organic pure material of volatile liquid is put from the bottleneck of the narrow-mouthed bottle of the first container Enter in the narrow-mouthed bottle of the first container, and takes fluid through-hole in the narrow-mouthed bottle of the first container with long needle injection by the first container Device is separately added into the organic pure material of remaining liquid, and weighs respectively;The first container is placed in fluid through-hole in taking for the first container First sealing-plug places the second sealing-plug of the first container in the balance through-hole of the first container;The first container is rocked, makes to be put into Each ampoule bottle in narrow-mouthed bottle is broken, and the liquid organic pure material and the first container contained in all ampoule bottles The organic pure material of liquid being added in narrow-mouthed bottle is uniformly mixed, and the organic mixed solution standard substance of volatility is prepared;
Step S13: step S11 and step S12 is repeated, to prepare the thin mouth with the first container in the narrow-mouthed bottle of second container The identical organic mixed solution standard substance of volatility in bottle;
Step S14: the balance through-hole of the first container is connected to the balance through-hole of second container, and the fluid through-hole that takes of second container is to open Put state;Automatic-packaging is organic mixed from the volatility in the narrow-mouthed bottle for taking fluid through-hole to extract the first container of the first container Solution reference material is closed to be dispensed into each sub-bottling.
12. according to the method for claim 11, which is characterized in that the container further includes taking liquid plug and balanced plug, takes liquid Plug, which can be placed on, to be taken in fluid through-hole, and balanced plug can be placed in balance through-hole.
13. according to the method for claim 12, which is characterized in that taking fluid through-hole is tapped through hole, and the first sealing-plug is real Heart thread plug, taking liquid plug is hollow thread plug.
14. method according to claim 12 or 13, which is characterized in that balance through-hole is tapped through hole, the second sealing-plug For solid thread plug, balanced plug is hollow thread plug.
15. according to the method for claim 13, which is characterized in that be equipped with round tube in hollow thread plug.
16. according to the method for claim 15, which is characterized in that the round tube lower end in liquid plug is taken to be equipped with filter screen.
17. method according to claim 11 or 12, which is characterized in that the container is glass container.
18. method according to claim 11 or 12, which is characterized in that the bottleneck outer peripheral edge of narrow-mouthed bottle is equipped with external screw thread, The inner peripheral of bottle cap is equipped with internal screw thread, and bottle cap is set on the bottleneck of narrow-mouthed bottle by the opening of bottle cap, outside narrow-mouthed bottle bottleneck The screw-internal thread fit of screw thread and bottle cap.
19. according to the method for claim 14, which is characterized in that be equipped with round tube in hollow thread plug.
20. according to the method for claim 19, which is characterized in that the round tube lower end in liquid plug is taken to be equipped with filter screen.
CN201611117959.9A 2016-12-07 2016-12-07 Prepare container, the device and method of the organic mixed solution standard substance of volatility Expired - Fee Related CN106769369B (en)

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CN110470616A (en) * 2018-05-10 2019-11-19 北京清测科技有限公司 Sampling device, mercury analysis system and mercury analysis method
CN108758323B (en) * 2018-06-21 2023-07-25 盛密科技(上海)有限公司 Gas cylinder and method for configuring standard cylinder gas
CN111068574A (en) * 2018-10-18 2020-04-28 中国石油天然气股份有限公司 Volatile liquid mixing device, mixing and weighing device and weighing method
CN114264535A (en) * 2021-11-29 2022-04-01 曼哈格检测技术股份有限公司 Method for preparing solution of volatile solute

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