CN206788130U - A kind of azeotropic distillation sampling device and the line measuring system for moisture content comprising the sampling device - Google Patents
A kind of azeotropic distillation sampling device and the line measuring system for moisture content comprising the sampling device Download PDFInfo
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Abstract
A kind of azeotropic distillation sampling device and the line measuring system for moisture content including the sampling device are the utility model is related to, wherein the azeotropic distillation sampling device includes：Cucurbit, closure and capillary；The closure is used for the jaw for sealing cucurbit；Wherein, cucurbit includes the first arm and the second arm, and the first arm and the second arm inside cucurbit body respectively by the through hole that cucurbit body top is set with connecting；Capillary includes the first capillary and the second capillary, and the outer surface of the first capillary is bonded with the inner surface of the first arm；Second capillary is bonded with the inner surface of the second arm.The utility model proposes azeotropic distillation sampling device and line measuring system for moisture content including the sampling device it is simple in construction, it is easy to operate, sample and karl Fischer reagent can be avoided to contact, quick and precisely measure sample moisture.
Description
Technical field
It the utility model is related to the sampling device during a kind of moisture measurement, and in particular to a kind of azeotropic distillation sample introduction dress
Put and the line measuring system for moisture content comprising the sampling device.
Background technology
Karl_Fischer method be to the specificity method that moisture measures in solid and fluid sample, be it is a kind of with
The chemical analysis of titration measuring moisture.Because the measurement result of Karl_Fischer method is reproducible, the degree of accuracy is high, therefore extensively
The general measure for food, medicine, chemical reagent and moisture in materials.The general principle of Karl_Fischer method is non-aqueous solution
In, iodine, sulfur dioxide and water are according to 1：1：1 stoichiometric reaction (i.e. karl Fischer reacts)；Therefore, can be according to disappearing
The amount of the material of the iodine of consumption calculates sample moisture content.According to the difference for producing iodine molecule mode, Karl_Fischer method can be divided into storehouse
Logical sequence method and the class of volumetric method two.Coulometry produces iodine molecule by being electrolysed, and volumetric method provides iodine molecule by the way that the solution containing iodine is added dropwise.
Comprising the material that side reaction can occur with karl Fischer reagent in some samples, line measuring system for moisture content is caused to miss
Difference.For example, the compound containing aldehyde ketone functional group, aldolisation, generation occur for the methanol easily and in karl Fischer reagent
Water, cause measurement result higher.For another example the sulfur-containing compound in crude oil, such as mercaptan, can with karl Fischer reagent
Redox reaction occurs for iodine, causes moisture measurement result higher.Also some samples, the solubility in karl Fischer reagent
Low, sample is added directly into titration cell, easily causes solution muddiness, layering, or contaminated electrode.Therefore, these samples are measured
Product, it is necessary to use special reagent or sample injection method.Using special reagent it is for instance possible to use the karr without methanol is taken
Not reagent, measure the moisture of the compound containing aldehyde ketone functional group and its mixture.It can for example be used and added using sample injection method
The method of thermal evaporation, make moisture effusion in sample and imported with carrier gas in karl Fischer titration cell, measure its moisture.But
It is that the moisture in sample may be remained partly in the base, it is impossible to effusion completely, cause moisture measurement Lower result；In addition, sample
Product are also possible to reaction of being decomposed in heating process, if product includes water, cause moisture measurement result higher.
Azeotropic distillation is also a kind of sample injection method.Its principle is dissolved a sample in organic solvent, such as toluene, is passed through
Heating makes sample dissolve or be partly dissolved, and water release is into organic solvent；When temperature is increased to particular value, water and organic solvent
Azeotropic mixture is formed, is passed into carrier gas in karl Fischer titration cell.The method titrated with karl Fischer, measure in azeotropic mixture
Contained moisture, so as to calculate sample moisture.
Existing azeotropic distillation sampling device is complicated, and cost is high；And the volume for distilling vial is excessive, sample water
Divide and be easily collected on superjacent headroom, cause moisture measurement error.Azeotropic distillation sample introduction-karl Fischer titrimetry
The method of moisture, blank solvent moisture, azeotropic mixture contained humidity, residual solution moisture is measured respectively, then according to mass balance
Sample contained humidity is calculated, process is complicated, and is not suitable for the sample that can be reacted with karl Fischer reagent.It is in addition, existing
Azeotropic distillation sampling device can not measure solid sample.In view of the above problems, at present the method for azeotropic distillation sample introduction in card
Using seldom in the practice of Er Feixiufa measurement moisture.
Utility model content
In order to solve the above-mentioned technical problem, the utility model proposes a kind of azeotropic distillation sampling device and the sample introduction is included
The line measuring system for moisture content of device.
A kind of azeotropic distillation sampling device, including：Cucurbit, closure and capillary；The closure, which is used to seal, to be steamed
Evaporate the jaw of bottle；
Wherein, cucurbit includes the first arm and the second arm, and the first arm and the second arm pass through cucurbit bottle respectively
The through hole that body is set inside cucurbit body with connecting；
Capillary includes the first capillary and the second capillary, the outer surface of the first capillary and the inner surface of the first arm
Fitting；Second capillary is bonded with the inner surface of the second arm.
Further, cucurbit is cylindrical jaw bottle.
Further, closure is the closure with rubber spacer.
Further, arm is shaped as L-type, or outwards upwardly extends parabola shaped；And the shape of two arms
It is identical or different.
Further, the height of the positional distance cucurbit bottom of bottle where the through hole is more than or equal to cucurbit body height
2/3.
Further, close proximity to the inner bottom surface of cucurbit, the bottom surface of the second capillary is not stretched for the bottom surface of the first capillary
Enter inside body.
Further, above-mentioned azeotropic distillation feed arrangement also includes aluminium ingot and electric heater unit, and electric heating cover adds to aluminium ingot
Heat, the aluminium ingot can house the cucurbit.
Further, in the small rounding mesa-shaped in the big bottom in top, the side surface of aluminium ingot is formed the outer shape of the aluminium ingot
There is thermometer hole.
A kind of line measuring system for moisture content, including：Foregoing azeotropic distillation sampling device and moisture titration, the azeotropic
Distillation sampling device is connected by the second capillary with moisture titration.
Further, moisture titration includes stirring rotator and titration cell, and the azeotropic distillation sampling device passes through second
Capillary connects with the titration cell of moisture titration, and the titration cell rotates under the drive of stirring rotator.
The beneficial effects of the utility model：
1. the utility model proposes azeotropic distillation sampling device and line measuring system for moisture content, simple in construction, easy to operate, energy
Enough avoid sample and karl Fischer reagent from contacting, quick and precisely measure sample moisture.
2. the utility model proposes azeotropic distillation sampling device and line measuring system for moisture content, small volume, cucurbit jaw
Closure is detachable, easy to use；The access way of carrier gas is all low by polytetrafluoroethylene capillary, inwall residual moisture amount.
3. the utility model proposes azeotropic distillation sampling device and line measuring system for moisture content when measuring solid sample, with peace
Small jar bottle packaged sample, is placed in cucurbit and measures, and existing sampling device can not measure solid sample.
4. the utility model proposes azeotropic distillation sampling device and line measuring system for moisture content measurement sample when, first with moisture mark
Quasi- material calibration water transport efficiency (i.e. the rate of recovery), then measure sample moisture.With rate of recovery calibration measurement as a result, it is possible to realize
Accurate measurement, the measuring method than existing sampling device are simple.
5. the utility model proposes azeotropic distillation sampling device and line measuring system for moisture content in, both arms are located at the two of cucurbit
Side, in azeotropic distillation, below cucurbit, the temperature in cucurbit gradually reduces heater block from bottom to top.And distill
The through hole that bottle both sides are connected with both arms can try one's best close to liquid level, when the temperature of solution is increased to azeotropic point, azeotropic mixture (such as
The azeotropic mixture of toluene and water) easily exported by carrier gas, condensing reflux will not occur, therefore the temperature of solution need not be higher than azeotropic
Point, caused by solution temperature can be avoided higher sample it is easier by thermal decomposition the problem of.
Brief description of the drawings
Fig. 1 be the utility model proposes azeotropic distillation sampling device structural representation；
Fig. 2 be the utility model proposes the structural representation of aluminium ingot that includes of azeotropic distillation sampling device；
Fig. 3 be the utility model proposes line measuring system for moisture content structural representation；
Fig. 4 be the utility model proposes the obtained moisture rate of recovery calibration curve schematic diagram of line measuring system for moisture content measurement.
Embodiment
For the purpose of this utility model, technical scheme and advantage is more clearly understood, below in conjunction with specific embodiment, and
Referring to the drawings, the utility model is further described.But those skilled in the art know, the utility model does not limit to
In accompanying drawing and following examples." first " or " second " for being mentioned in text etc. states, merely to technical characteristic is made a distinction,
Have no substantive limiting meaning.
The utility model proposes azeotropic distillation sampling device as shown in figure 1, azeotropic distillation sampling device is preferred for matching somebody with somebody
Close karl Fischer moisture titration measurement sample moisture.Azeotropic distillation sampling device includes：Cucurbit 8, closure 10
With capillary 11.
Cucurbit 8 is the jaw bottle of cylinder, and the body of jaw cucurbit 8 is glass material, those skilled in the art
It could be aware that, jaw cucurbit 8 can also be other bottleneck shapes or the cucurbit of other body shapes.Leaned on the top of body
The position of nearly jaw is provided with two and is located at the through holes of body both sides respectively, and surrounds each through hole outwards and seal upwards and extend
Arm, so as to form the jaw glass cucurbit with both arms.
Preferably, the height of the positional distance bottom of bottle where through hole is more than the 2/3 of body height, is so advantageous in azeotropic
The residual moisture of superjacent is reduced during distillation.
The internal diameter of the arm is less than the internal diameter of body, and the shape of arm can be L-type, such as right angle L-type is (such as Fig. 1 institutes
Show), or fillet L-type (as shown in Figure 3)；Can also be parabola shaped (not shown) that outwards upwardly extends, or other be in
The shape upwardly extended outside.The shape of two arms can be with identical, can also be different, such as arm is shaped as L-type, separately
One arm be shaped as outwards upwardly extending it is parabola shaped；Or arm is shaped as right angle L-type, another arm
Be shaped as fillet L-type.The material of arm can all be glass, or other are resistance to as the body of jaw cucurbit 8
The material of corrosion.Arm can be integrally formed with body, can also seal arm by modes such as meltings to be formed in body
Through hole.
In addition, the surface of the liquid held in jaw cucurbit 8 is less than or no more than the position where through hole.
The volume of jaw cucurbit 8 is preferably 15mL, and normal liquor capacity when measuring sample is about 10mL, at the top of superjacent
Spatial volume is no more than 5mL, so advantageously reduces residual moisture.
The closure 10 is used for the jaw of sealing jaws cucurbit 8, it is ensured that the sealing of system when sample introduction and sampling,
So as to prevent the material in solution from volatilizing in azeotropic distillation, the interference of ambient moisture is also reduced, ensures measurement accuracy.
Preferably, the closure 10 is the aluminium sealing cover with rubber spacer, this closure can ensure sample introduction and
The sealing of system during sampling, meanwhile, the aluminium sealing cover with rubber spacer is convenient to be dismantled, and has both facilitated disposable closure,
It is also convenient for removing the residual solution in jaw cucurbit 8, cleaning jaw cucurbit 8.
The capillary 11 is two.Wherein, the first capillary (calls in the following text from the arm of the body side of jaw cucurbit 8
One arm) and the through hole of the side extend into inside jaw cucurbit 8, by the carrier gas such as dry nitrogen be passed through jaw distillation
In bottle 8.First capillary is bonded with the inner wall sealing of the first arm.
Preferably, the bottom surface of the first capillary close proximity to jaw cucurbit 8 inner bottom surface, to facilitate in azeotropic distillation
Carrier gas is passed through solution bottom, fully contacted with solution.
Second capillary extend into jaw cucurbit from the arm (calling the second arm in the following text) of the body opposite side of jaw cucurbit 8
Near 8 another side through hole, to carry the carrier gas of azeotropic mixture output.The inner wall sealing of second capillary and the second arm
Fitting.
Preferably, the bottom surface of the second capillary is not stretched into inside body, fully to export the carrier gas for carrying azeotropic mixture.
Capillary 11 is preferably less than 0.5mm polytetrafluoroethylene capillary using internal diameter, and internal diameter is small, is advantageous to the abundant of water
Transfer, reduce tube wall absorption.Correspondingly, the internal diameter of the first arm and the second arm is less than 0.5mm, and can respectively with the first capillary
The outer surface palette of pipe and the second capillary.
When distilling sample introduction, the carrier gas such as dry nitrogen is passed through inside jaw cucurbit 8 from the first capillary, from the second capillary
Pipe flows out.
Further, above-mentioned azeotropic distillation feed arrangement also includes aluminium ingot 9 and electric heating cover 4, as shown in Figures 2 and 3, aluminium
Ingot 9 is placed on inside electric heating cover 4, and the aluminium ingot 9 is used to house above-mentioned jaw cucurbit 8, therefore electric heating cover 4 can pass through
Aluminium ingot 9 heats to jaw cucurbit 8.
In order to house jaw cucurbit 8, one or more accommodating holes are formed on the upper surface of aluminium ingot 9, each accommodating hole can
To house a jaw cucurbit 8.The interior shape of accommodating hole is as far as possible consistent with the body outer shape of jaw cucurbit 8, with
Ensure that jaw cucurbit 8 can be bonded with accommodating hole as far as possible, improve the efficiency of heating surface of aluminium ingot 9.
In addition, the side surface of aluminium ingot 9 can also form thermometer hole (not shown), the thermometer hole is used to place temperature measurer
Device, for being measured to the body surface temperature of jaw cucurbit 8, so as to control the heating-up temperature of electric heating cover 4.The survey
Warm instrument such as thermometer or temperature sensor.
Preferably, the outer shape of the aluminium ingot 9 is easy to the uniformly poly- of heat in the small rounding mesa-shaped in the big bottom in top
Collection, so as to uniformly be heated to the jaw cucurbit being contained in accommodating hole.
Electric heating cover 4 has the heat transfer part for surrounding or wrapping up the outer surface of aluminium ingot 9, so as to rapidly and uniformly by heat
Amount is delivered to aluminium ingot 9, and the jaw cucurbit 9 housed in the accommodating hole of aluminium ingot 9 is heated.
Preferably, in order to which heat transfer efficiency is high, the internal side surface shape of heat transfer part is identical with the outer surface shape of aluminium ingot 9,
But size is bigger, the outer surface of tight aluminium ingot 9 as far as possible.When aluminium ingot 9 is in the small rounding mesa-shaped in the big bottom in top, heat transfer
The inner side in portion is preferably also in rounding mesa-shaped.
The utility model proposes azeotropic distillation sampling device it is simple in construction, it is easy to use, and it is accurate to improve measurement
Degree and accuracy.
The utility model also proposed a kind of line measuring system for moisture content, as shown in figure 3, the line measuring system for moisture content includes：Altogether
Boiling distillation sampling device and moisture titration 5, the carrier gas flowed out from the second capillary of azeotropic distillation sampling device are passed through moisture
In titrator 5.
The moisture titration 5 is preferably Karl Fischer coulometric determination moisture titration 5.The Karl Fischer coulometric determination
Moisture titration 5 includes stirring rotator 6 and titration cell 7, and the carrier gas flowed out from the second capillary of azeotropic distillation sampling device is led to
In the titration cell 7 for entering moisture titration 5.The titration cell 7 is placed on stirring rotator 6, and can be 6 turns with stirring rotator
It is dynamic, so as to which when measuring moisture, carrier gas and the electrolyte in titration cell 7 that can make to be passed through in titration cell 7 are sufficiently mixed.
The device for measuring moisture also includes carrier gas supply department, and carrier gas supply department can be to supplying inside jaw cucurbit 8
Carrier gas.
When carrier gas is nitrogen, the carrier gas supply department includes nitrogen cylinder 1, molecular sieve drying pipe 2 and gas mass flow
Gauge 3.Nitrogen cylinder 1 is used to store nitrogen, and the nitrogen that molecular sieve drying pipe 2 exports to nitrogen cylinder 1 is dried, after drying
Nitrogen under the control of gas mass flow gauge 3, be passed through jaw cucurbit 9 from the first capillary of azeotropic distillation feed arrangement
It is internal.
When using the utility model proposes line measuring system for moisture content carry out moisture measurement, carrier gas is nitrogen, and solvent is toluene
During solvent, load a certain amount of toluene solvant in jaw cucurbit 8, sample is dissolved in toluene solvant, first is dissolved in sample
After benzene solvent, the solution in jaw cucurbit 8 is heated by electric heating cover 4 and aluminium ingot 9, is heated to the azeotropic temperature of water and toluene
Spend more than (about 85 DEG C), the azeotropic mixture of toluene and water is passed through Karl Fischer coulometric determination moisture with carrier gas (nitrogen) from the second arm
The titration cell 7 of titrator 5, titration cell 7 rotate under the drive of stirring rotator 6, and water content can titrate according to coulometry moisture
The electrolysis electricity of instrument calculates to obtain.
With reference to specific example illustrate the utility model proposes line measuring system for moisture content measuring method.
Embodiment 1：The measure of the water transport efficiency of azeotropic distillation sampling device
Moisture titration 5 is opened, operating measurement method, instrument enters holding state after pre- titration.Electric heating cover 4 adds
Heat to the temperature of aluminium ingot 9 is 90 DEG C.10mL toluene is added in the jaw cucurbit 8, with Sealing plierses by the closure with rubber spacer
10 fix.The aspirated switch of nitrogen cylinder 1 is opened, setting nitrogen flow is 50mL/min, and nitrogen is gentle through molecular sieve drying pipe 2
Weight flowmeter 3 is passed through jaw cucurbit 8 from the first arm.Jaw cucurbit 8 is put into the accommodating hole of aluminium ingot 9, passed through
Electric heating cover 4 is heated.Minor amount of water and toluene in toluene form azeotropic mixture, and moisture is passed through from the second arm with nitrogen carrier gas
The titration cell 7 of titrator 5.The drift value of moisture titration 5 gradually reduces, until being less than 10 μ g/min.On moisture titration 5
Click on " Sample ", start sample introduction process.A certain amount of liquid is added at the rubber spacer of closure 10 with syringe rapidly
Moisture standards material.Water and toluene in sample form azeotropic mixture, and the titration cell 7 of moisture titration 5, instrument are passed through with nitrogen carrier gas
Device electrolysis iodine participates in karl Fischer reaction, records electrolysis electricity, and calculate water content (in terms of mg).
According to the Instrument measuring value and actual value of moisture standards water content of materials, water transport efficiency is calculated, i.e. moisture returns
Yield.Add the liquid moisture standards material of different quality, the moisture rate of recovery corresponding to measure, moisture rate of recovery formula such as formula
(1)。
In above formula, Recovery is the moisture rate of recovery of azeotropic distillation sampling device, %；
mH2O,CRMBe Karl Fischer coulometric determination moisture titration measure moisture standards material water content, mg；
CH2O,CRMIt is the moisture certificate value of liquid moisture standards material, mg/g；
mCRMIt is the quality of liquid moisture standards material, g.
According to the moisture measurement of moisture standards material value-rate of recovery result, map and be fitted, obtain moisture rate of recovery school
Directrix curve.
Embodiment 2：The measure of the water transport efficiency of azeotropic distillation sampling device
Moisture titration 5 is opened, operating measurement method, instrument enters holding state after pre- titration.Electric heating cover 4 adds
Heat to the temperature of aluminium ingot 9 is 90 DEG C.10mL toluene is added in the jaw cucurbit 8, with Sealing plierses by the closure with rubber spacer
10 fix.The aspirated switch of nitrogen cylinder 1 is opened, setting nitrogen flow is 50mL/min, and nitrogen is gentle through molecular sieve drying pipe 2
Weight flowmeter 3 is passed through jaw cucurbit 8 from the first arm.Jaw cucurbit 8 is put into the accommodating hole of aluminium ingot 9, passed through
Electric heating cover 4 is heated.Minor amount of water and toluene in toluene form azeotropic mixture, and moisture is passed through from the second arm with nitrogen carrier gas
The titration cell 7 of titrator 5.The drift value of moisture titration 5 gradually reduces, until being less than 10 μ g/min.On moisture titration 5
Click on " Sample ", start sample introduction process.The rapid liquid moisture for adding 1mL at the rubber spacer of closure 10 with syringe
Standard substance GBW 13513.Water and toluene in sample form azeotropic mixture, and the titration of moisture titration 5 is passed through with nitrogen carrier gas
Pond 7, instrument electrolysis iodine participate in karl Fischer reaction, record electrolysis electricity, and it is 1.114mg that water content, which is calculated,.
According to the Instrument measuring value and actual value of moisture standards water content of materials, water transport efficiency is calculated, i.e. moisture returns
Yield (formula (1)).
In above formula, mH2O,CRMIt is the water content of the moisture standards material of Karl Fischer coulometric determination moisture titration measure,
1.114mg；
CH2O,CRMIt is the moisture certificate value of liquid moisture standards material, 1.110mg/g；
Recovery is the moisture rate of recovery of azeotropic distillation sampling device, 97.2%；
Different volumes and the liquid moisture standards material of different in moisture content are measured respectively so that moisture covers
(0.055mg~10mg) scope, moisture rate of recovery calibration curve is obtained, as shown in Figure 4.
Embodiment 3：The measure of sample moisture and calculating
Moisture titration 5 is opened, operating measurement method, instrument enters holding state after pre- titration.Electric heating cover 4 adds
Heat to the temperature of aluminium ingot 9 is 90 DEG C.10mL toluene is added in the jaw cucurbit 8, with Sealing plierses by the closure with rubber spacer
10 fix.The aspirated switch of nitrogen cylinder 1 is opened, setting nitrogen flow is 50mL/min, and nitrogen is gentle through molecular sieve drying pipe 2
Weight flowmeter 3 is passed through jaw cucurbit 8 from the first arm.Jaw cucurbit 8 is put into the accommodating hole of aluminium ingot 9, passed through
Electric heating cover 4 is heated.Minor amount of water and toluene in toluene form azeotropic mixture, and moisture is passed through from the second arm with nitrogen carrier gas
The titration cell 7 of titrator 5.The drift value of moisture titration 5 gradually reduces, until being less than 10 μ g/min.On moisture titration 5
Click on " Sample ", start sample introduction process.A certain amount of liquid is added at the rubber spacer of closure 10 with syringe rapidly
Sample.Water and toluene in sample form azeotropic mixture, and the titration cell 7 of moisture titration 5, instrument electrolysis iodine are passed through with nitrogen carrier gas
Participate in karl Fischer reaction, record electrolysis electricity, and calculate water content (in terms of mg).
Moisture rate of recovery formula according to embodiment 1, sample moisture content measurement result is substituted into, obtains corresponding moisture
The rate of recovery.Then sample moisture content correction value is calculated according to moisture measurement result and the moisture rate of recovery, such as formula (2).
In above formula, mH2O,Sample' it is sample moisture content correction value, mg；
mH2O,SampleBe Karl_Fischer method measure sample moisture content, mg；
Recovery is the moisture rate of recovery of azeotropic distillation sampling device, %.
Then sample moisture is calculated according to sample moisture content correction value and sample quality, such as formula (3).
In above formula, CH2O,SampleIt is the moisture of sample, mg/g；
mH2O,sample' be Karl Fischer coulometric determination moisture titration measure sample moisture content correction value, mg；
mSampleIt is the quality of sample, g.
Above-mentioned is measuring method when measuring fluid sample moisture.When measuring solid sample, 2mL is put into by sample
With fire sealing after ampoule bottle；Then the ampoule bottle equipped with sample is put into jaw cucurbit 8, adds toluene solvant, started altogether
Boiling distillation.When toluene solvant azeotropic distillation finishes, i.e., the drift value of moisture titration 5 firmly rocks pincers less than after 10 μ g/min
Mouth cucurbit 8, crushes ampoule bottle, and solid sample is dissolved or is partly dissolved by toluene, and following moisture and toluene form azeotropic
Thing, it is passed through titration cell 7 and carries out moisture measurement.
Embodiment 4：The measure of crude oil moisture and calculating
Moisture titration 5 is opened, operating measurement method, instrument enters holding state after pre- titration.Electric heating cover 4 adds
Heat to the temperature of aluminium ingot 9 is 90 DEG C.10mL toluene is added in the jaw cucurbit 8, with Sealing plierses by the closure with rubber spacer
10 fix.The aspirated switch of nitrogen cylinder 1 is opened, setting nitrogen flow is 50mL/min, and nitrogen is gentle through molecular sieve drying pipe 2
Weight flowmeter 3 is passed through jaw cucurbit 8 from the first arm.Jaw cucurbit 8 is put into the accommodating hole of aluminium ingot 9, passed through
Electric heating cover 4 is heated.Minor amount of water and toluene in toluene form azeotropic mixture, and moisture is passed through from the second arm with nitrogen carrier gas
The titration cell 7 of titrator 5.The drift value of moisture titration 5 gradually reduces, until being less than 10 μ g/min.On moisture titration 5
Click on " Sample ", start sample introduction process.The rapid crude oil for adding 1mL at the rubber spacer of closure 10 with syringe.It is former
Water and toluene in oil form azeotropic mixture, and the titration cell 7 of moisture titration 5 is passed through with nitrogen carrier gas, and instrument electrolysis iodine participates in card
Er Feixiu reacts, and records electrolysis electricity, and it is 1.150mg that water content, which is calculated,.
Moisture rate of recovery calibration curve according to embodiment 2, sample moisture content measurement result is substituted into, obtained corresponding
The moisture rate of recovery (formula (2)).
In above formula, mH2O,SampleBe Karl_Fischer method measure water content in crude oil, 1.150mg；
Recovery is the moisture rate of recovery of azeotropic distillation sampling device, is learnt by Fig. 4 as 96.9%；
mH2O,Sample' it is sample moisture content correction value, 1.187mg.
Then sample moisture (formula (3)) is calculated according to sample moisture content correction value and sample quality.
In above formula, mH2O,sample' it is the sample moisture content correction value that Karl Fischer coulometric determination moisture titration determines,
1.187mg；
mSampleIt is the quality of sample, 0.9215g；
CH2O,SampleIt is the moisture of crude oil, 1.288mg/g.
More than, embodiment of the present utility model is illustrated.But the utility model is not limited to above-mentioned implementation
Mode.All any modification, equivalent substitution and improvements within the spirit and principles of the utility model, done etc., should be included in
Within the scope of protection of the utility model.
Claims (10)
1. a kind of azeotropic distillation sampling device, it is characterised in that azeotropic distillation sampling device includes：Cucurbit, closure and hair
Tubule；The closure is used for the jaw for sealing cucurbit；
Wherein, cucurbit includes the first arm and the second arm, and the first arm and the second arm are respectively by cucurbit body
The through hole that portion is set inside cucurbit body with connecting；
Capillary includes the first capillary and the second capillary, and the outer surface of the first capillary and the inner surface of the first arm paste
Close；Second capillary is bonded with the inner surface of the second arm.
2. device according to claim 1, it is characterised in that cucurbit is cylindrical jaw bottle.
3. device according to claim 1 or 2, it is characterised in that closure is the closure with rubber spacer.
4. device according to claim 3, it is characterised in that arm is shaped as L-type, or the parabolic outwards upwardly extended
It is linear；And the shape of two arms is identical or different.
5. device according to claim 3, it is characterised in that the height of the positional distance cucurbit bottom of bottle where the through hole
2/3 of degree more than or equal to cucurbit body height.
6. device according to claim 3, it is characterised in that interior bottom of the bottom surface of the first capillary close proximity to cucurbit
Face, the bottom surface of the second capillary are not stretched into inside body.
7. device according to claim 3, it is characterised in that above-mentioned azeotropic distillation feed arrangement also includes aluminium ingot and electricity adds
Thermal, electric heating cover heat to aluminium ingot, and the aluminium ingot can house the cucurbit.
8. device according to claim 7, it is characterised in that the outer shape of the aluminium ingot is fallen in the big bottom in top is small
Round table-like, the side surface of aluminium ingot is formed with thermometer hole.
9. a kind of line measuring system for moisture content, it is characterised in that the line measuring system for moisture content includes：Such as any one of claim 1 to 8
Described azeotropic distillation sampling device and moisture titration, the azeotropic distillation sampling device are dripped by the second capillary and moisture
Determine instrument connection.
10. system according to claim 9, it is characterised in that moisture titration includes stirring rotator and titration cell, described
Azeotropic distillation sampling device is connected by the second capillary with the titration cell of moisture titration, and the titration cell is in stirring rotator
Drive lower rotate.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109100465A (en) * | 2017-06-21 | 2018-12-28 | 中国计量科学研究院 | A kind of azeotropic distillation sampling device and the line measuring system for moisture content comprising the sampling device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109100465A (en) * | 2017-06-21 | 2018-12-28 | 中国计量科学研究院 | A kind of azeotropic distillation sampling device and the line measuring system for moisture content comprising the sampling device |
| CN109100465B (en) * | 2017-06-21 | 2024-04-12 | 中国计量科学研究院 | Azeotropic distillation sampling device and moisture measurement system comprising same |
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