CN2787290Y - Gas-liquid separating arrangement for chemical gas phase - Google Patents
Gas-liquid separating arrangement for chemical gas phase Download PDFInfo
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- CN2787290Y CN2787290Y CN 200520001620 CN200520001620U CN2787290Y CN 2787290 Y CN2787290 Y CN 2787290Y CN 200520001620 CN200520001620 CN 200520001620 CN 200520001620 U CN200520001620 U CN 200520001620U CN 2787290 Y CN2787290 Y CN 2787290Y
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Abstract
The utility model relates to a gas-liquid separating device for a chemical gas phase, which comprises a mixed reactor, a gas-liquid separating device and a carrier gas conveying pipe, wherein a gas mixer is arranged in a pipeline of a gas-phase output pipe of the gas-liquid separating device, and the carrier gas conveying pipe is connected with the gas mixer. The utility model can be used for chemical gas phase generating systems of various atomic spectrum instruments, effectively eliminates large amounts of gas bubbles generated in the generating process of the chemical gas phase and reduces content of water entering gas of an atomizer to be measured so as to enhance the signal-to-noise ratio of the instruments and effectively improves the detecting lower limits of the instruments. Adopting a gas mixing device with strong extracting force, the utility model can rapidly extract reaction generating gas in the gas-liquid separating device, and the reaction generating gas is uniformly mixed with carrier gas, so the utility model can obviously reduce the humidity of gas conveyed to the atomizer, the dew point of the gas is less than room temperature and the sensitivity and the stability of the instruments are obviously enhanced.
Description
Technical field
The utility model relates to a kind of gas-liquid separator and method thereof that atom spectrum is measured that be used for.
Background technology
The chemical gaseous phase genetic method is a kind of efficient sampling technique that extensively adopts during atom spectrum is measured, its general method is: the solution that will contain tested element mixes with reductant solution in suitable chemical environment, mixed liquid is fully reaction in the pipeline of certain size, the gas-liquid mixture that reaction forms is divided into two-phase in separator, wherein liquid phase flows out via the waste discharge pipeline, and gas phase then is sent in the atomizer by carrier gas and detects.Traditional chemical gas-phase generating apparatus promotes mixing material with carrier gas and flows in the gas-liquid separation device via reaction tube, and the gas after the gas-liquid separation is sent in the atomizer and detected.The process that its chemical gaseous phase takes place is: contain sour sample or current-carrying and reducing agent and pushed mixing reactor through sample/current-carrying carrier pipe and reducing agent carrier pipe by peristaltic pump respectively, the chemical gaseous phase reaction of formation takes place in mixing reactor, the carrier gas of product and the certain flow that imports through carrier gas inlet is mixed into the gas-liquid concurrent, and the gas-liquid concurrent flows in the gas-liquid separation device and is divided into gas, liquid two-phase.Wherein gas phase is sent in the atomizer and is detected, and liquid phase is discharged through the discard solution discharge port peristaltic pump.
The efficiency of transmission of tested element is near 100% when using this device, the detectability of tested element is significantly reduced, but this device is deposited following two point defects: contain a large amount of steam in the gas phase thing that obtains after (1) gas-liquid separation, and the existence meeting of these steam causes significant decay to signal, and reduce the stability of signal, therefore need to adopt baroque multistage water trap.From bibliographical information as can be known, dewater and can adopt the multi-stage gas-liquid separator, cyclonic separation or adopt means such as film separation, but wherein most of device only can be reduced to the dew point of gas a little less than room temperature, can not reach the best requirement that atom spectrum is measured.Has only employing " anti-branch " (Nafion, the Dupont product) film dewaters, can stablize at normal temperatures and obtain the gas that dew point is significantly less than room temperature, and the Nafion film itself costs an arm and a leg, in the process of anhydrating, consume a large amount of dry gas again, and service life is not long, and cost is too high from the economic angle; Nafion also can absorb alkaline hydride on the other hand, causes the decay of signal.Therefore, the present gas-liquid separation device that is applicable to chemical gaseous phase generation atom spectrum thought of convention nothing but still; (2) when content of organics is higher in the measured object, tend to generate a large amount of bubbles, reduced gas-liquid separation efficient, when serious even can damage instrument because of bubble enters atomizer.From bibliographical information as can be known froth breaking can adopt defoamer, porous plate such as stirs or ultrasonic at method.These methods all have certain elimination effect to common foam, but can not effectively eliminate a large amount of foams of the very tiny thickness of biological sample generation.
The utility model content
The purpose of this utility model is to address the aforementioned drawbacks, and provides a kind of energy gas-liquid separator froth breaking, efficient water-removing.
A kind of gas-liquid separator of the utility model, comprise mixing reactor, gas-liquid separation device and carrier gas carrier pipe, in the pipeline of the gas phase efferent duct of described gas-liquid separation device gas mixer is set, described carrier gas carrier pipe is connected with gas mixer.
Between mixing reactor and gas-liquid separation device, be provided with liquid atomiser.
Described liquid atomiser is ultrasonic nebulizer or two phase flow sprayer.
Described gas mixer comprises mixed air cavity and connected gas inlet pipe.
Described gas inlet pipe is vertical mutually with mixed air cavity or mutually at an angle, both center lines intersect or biasing mutually, and its gas inlet pipe must stretch into and mix in the air cavity.
Described mixed air cavity is sleeved on the gas phase efferent duct of gas-liquid separation device, and the bore of the port of export that mixes air cavity and gas phase efferent duct is less than the size of self main body.
Gas-liquid separator described in the utility model can be used for all kinds of atom spectrum instruments, comprise Atomic Absorption Spectrometer (AAS), Atomic Emission Spectrometer AES (AES), the chemical gaseous phase generation systems of inductively coupled plasma-mass spectrograph (ICP-MS) and AFS (AFS), whole device is installed in the front end of atomizer, can eliminate a large amount of bubbles that produce in the chemical gaseous phase generating process effectively, and reduce water content in the gas to be measured enter atomizer, thereby improved the signal to noise ratio of instrument, improved the lower limit that detects of instrument effectively.
Gas-liquid separator described in the utility model comprises a gas mixing device that draft is stronger, reaction in gas-liquid separation device generation gas can be extracted out rapidly and is evenly mixed with carrier gas, can significantly reduce the humidity that is sent to gas in the atomizer like this, its dew point is significantly less than room temperature, has significantly improved the sensitivity and the stability of instrument.
The gas dew point of actual measurement is shown in table 1, can find that the employed technology of the utility model has reached comparatively desirable water removal effect from table, and dehydration rate has reached 60%, a little less than the dehydration rate of Nafion pipe 75%.On this basis, we have also compared two kinds of modes that dewater to the influence that As measures, and the results are shown in Fig. 3, can find to adopt the fluorescence intensity of a section of traditional gas-liquid separation device minimum from figure; The fluorescence intensity of the b section that dewaters through the Nafion pipe is significantly improved; Increase again through Nafion pipe and the art of this patent fluorescence intensity ratio b section, but the fluorescent value of the d section that dewaters with simple use the art of this patent is fair substantially in conjunction with the c section that dewaters.This explanation as long as dehydration rate reaches 60% (this patent level), just can be eliminated in the gas to be measured vapor content to the influence of measurement result substantially for follow-up atomic fluorescence spectrophotometry.The method that this explanation this patent provides, can bring up to and adopt Nafion to manage identical level the sensitivity that atomic fluorescence is measured, consider the price of thousands of dollars of Nafion pipes itself and have more the carrier gas consumption of twice at least, water-eliminating method provided by the utility model obviously has more advantage.
Separator described in the utility model destroys the bubble of generation with the atomization of liquid, makes that no bubble accumulates in the gas-liquid separation device.Listed the result that high bubble sample and still sample dewater through gas-liquid separation described in the utility model in the table 2, after the sample that therefrom can find different foam content adopts gas-liquid separation device of the present utility model, can both keep the higher rate that dewaters, the rate that dewaters of just high bubble sample slightly reduces.And when using traditional gas-liquid separation device, a large amount of foams can directly directly overflow from gas outlet, gas-liquid separator upper end, head and shoulders above the measurement category of dew point hygrometer.The atomizer that adopts in this explanation the utility model is eliminated very effective to foam.
The table 1. difference water content in the gaseous mixture under the mode (carrier gas and reaction generate gas) that dewaters
| Mode dewaters | Do not remove under the water condition | Remove under the water condition | Dehydration rate (%) | ||
| Water partial pressure (mmHg) | Dew point (℃) | Water partial pressure (mmHg) | Dew point (℃) | ||
| Example one a | 16.2 | 18.7 | 6.4 | 4.8 | 60 c |
| Nafion a，b | 16.2 | 18.7 | 4.0 | -2.0 | 75 c |
The flow-rate ratio that a, this moment are reacted gas generating amount and carrier gas is about 1: 2, and these group data obtain during for continuous the operation.
The inside and outside throughput ratio of b, Nafion pipe is 1: 2;
C, dehydration rate=(do not remove water partial pressure under the water condition-remove water partial pressure under the water condition) ÷ does not remove water partial pressure * 100% under the water condition.
The different samples of table 2. adopt the water removal effect behind the utility model gas-liquid separator example two
a
| Mode dewaters | Do not remove under the water condition | Remove under the water condition | Dehydration rate (%) | ||
| Water partial pressure (mmHg) | Dew point (℃) | Water partial pressure (mmHg) | Dew point (℃) | ||
| High bubble sample b | 11.6 | 13.5 | 4.0 | -2.0 | 64 c |
| Still sample | 11.2 | 13.0 | 3.8 | -2.5 | 66 c |
The flow-rate ratio that a, this moment are reacted gas generating amount and carrier gas is about 1: 2, and these group data are to obtain in intermitten operation (moving 30 seconds stopped 10 seconds) time;
B, high bubble sample obtain after family expenses hand cleanser water is diluted at 1: 2000;
C, dehydration rate=(do not remove water partial pressure under the water condition-remove water partial pressure under the water condition) ÷ does not remove water partial pressure * 100% under the water condition.
Description of drawings
Fig. 1 is the schematic diagram of an embodiment of gas-liquid separator described in the utility model;
Fig. 2 is the schematic diagram of another embodiment of gas-liquid separator described in the utility model;
Fig. 3 is the schematic diagram of an embodiment of the separator gas mixer shown in Fig. 1 and Fig. 2;
Fig. 4 is the vertical view of Fig. 3;
Fig. 5 is the schematic diagram of the 2nd embodiment of the separator gas mixer shown in Fig. 1 and Fig. 2;
Fig. 6 is the vertical view of Fig. 5;
Fig. 7 is the schematic diagram of the 3rd embodiment of gas mixer of the separator shown in Fig. 1 and Fig. 2;
Fig. 8 is the vertical view of Fig. 7.
The specific embodiment
Referring to Fig. 1, gas-liquid separator described in the utility model comprises mixing reactor 5, gas-liquid separation device 6 and carrier gas carrier pipe 4.In the pipeline of the gas phase efferent duct 7 of described gas-liquid separation device 6 gas mixer 11 is set, described carrier gas carrier pipe 4 is connected with gas mixer 11.The process that its chemical gaseous phase takes place is, contain sour sample and reducing agent and pushed mixing reactor 5 through current-carrying carrier pipe 2 and reducing agent carrier pipe 1 by peristaltic pump 3 respectively, the chemical gaseous phase reaction of formation takes place in mixing reactor 5, product enters and is divided into gas, liquid two-phase in the gas-liquid separation device 6, wherein gas phase is through gas phase efferent duct 7 body blenders 11, send in the atomizer after the carrier gas of the certain flow that imports with carrier gas carrier pipe 4 mixes and detect, liquid phase is discharged by peristaltic pump 3 through waste discharge mouth 8,9.
Referring to Fig. 2, the further improvement of separator described in the utility model is to be provided with liquid atomiser 10 between mixing reactor 5 and gas-liquid separation device.The gas-liquid concurrent is through liquid atomiser 10 atomizings, and droplet enters in the gas-liquid separation device 6.
Described liquid atomiser 10 can be ultrasonic nebulizer or two phase flow sprayer.
Referring to Fig. 3 to Fig. 6, described gas mixer 11 comprises mixed air cavity 12 and gas inlet pipe 13.Described gas inlet pipe 13 is vertical mutually with mixed air cavity 12 or mutually at an angle, both center lines intersect or biasing mutually, and its gas inlet pipe 13 must stretch into and mix in the air cavity 12, to the center.
Referring to Fig. 7 and Fig. 8, described mixed air cavity 12 is sleeved on the gas phase efferent duct 7 of gas-liquid separation device 6, and the bore of the port of export that mixes air cavity 12 and gas phase efferent duct 7 is less than the size of self main body.
Enumerate several combinations below, and its effect be described:
1, embodiment 1, promptly there is not atomizer, the gas mixing device that gas mixer 11 adopts both center lines of Fig. 3,4 gas inlet pipes 13 and mixed air cavity 12 to setover mutually, because big flow carrier gas produces cyclone at gas mixer 11 middle parts, cause big negative pressure, chemical gaseous phase in the gas-liquid separation device of its underpart take place can be produced the complete suction gas mixer of gas 11 tops that contain element to be measured, detect with sending among the atomizer A after carrier gas mixes.
Above-mentioned gas-liquid separation device is shown in table 3 to the raising effect of AFS signal sensitivity.Can find from table no matter said apparatus is to detecting arsenic or antimony, all having played the effect that improves sensitivity really.The measurement stability and the detection limit that use this device back arsenic, two kinds of elements of antimony have been provided in the table 4, as can be known, use said apparatus from table, the detection limit of two kinds of elements has reached the ppt level, and use traditional device, the detectability of these two kinds of elements is generally arsenic:＜20ppt; Antimony:＜40ppt.This illustrates the performance that above-mentioned gas-liquid separation device can very effective raising gas phase generation atom spectrum instrument.
The raising effect of 1 pair of AFS signal sensitivity of table 3. embodiment
| Measure element | Blank AFS value | AFS value under the 10ppb | The raising rate | ||
| Traditional approach | Embodiment 1 | Traditional approach | Embodiment 1 | ||
| Arsenic | 228 | 206 | 2267 | 3781 | 74％ |
| Antimony | 538 | 391 | 3408 | 4972 | 60％ |
aRaising rate=[(AFS value under the back 10ppb that dewaters-the blank AFS value in back dewaters)-(the AFS value-preceding blank AFS value dewaters under the 10ppb before dewatering)] ÷ (AFS value-blank AFS value before dewatering under the preceding 10ppb that dewaters) * 100%
The raising effect of 1 pair of AFS signal stabilization of table 4. embodiment
| Measure element | blank | 4ppb | 6ppb | 8ppb | 10ppb | Standard deviation | Detection limit/ppt | |
| Embodiment 1 | Arsenic | 633 | 4058 a | 5561 a | 7596 a | 9421 a | 2.25 | 7.2 |
| Antimony | 491 | 2947 a | 4546 a | 6357 a | 8153 a | 2.20 | 8.1 |
aData have been deducted blank
2, liquid atomiser 10 adopts the two phase flow atomising device, gas mixer 11 adopts gas inlet pipe 13 shown in Fig. 3,4 and mixed air cavity 12 mutual blenders at an angle, because big flow carrier gas produces negative pressure at gas mixer 11 middle parts, chemical gaseous phase in the gas-liquid separation device of its underpart take place can be produced the complete suction gas mixer of gas 11 tops that contain element to be measured, detect with sending among the atomizer A after carrier gas mixes.
AFS when above-mentioned gas-liquid separation device is measured height bubble sample the results are shown in the following table 5.From table, can find, originally the height bubble sample that can't measure, after using said apparatus, the linearly dependent coefficient of four variable concentrations standard specimen measured values has reached 1.00, detect and be limited to 14.3ppt, a little more than the 7.2ppt of above-mentioned still sample, even be better than the detection limit 20ppt of still sample under traditional gas-liquid separation device, this illustrates that this kind gas-liquid separation device can be good at satisfying the requirement that the measurement of gas phase generation atom spectrum instrument has the bubble sample.
AFS result when de-watering apparatus is measured height bubble sample among table 5. embodiment 2
| Measure element | blank | 4ppb | 6ppb | 8ppb | 10ppb | Standard deviation | Linearly dependent coefficient | Detection limit/ppt |
| Arsenic | 223 | 549 a | 1405 a | 2258 a | 2761 a | 1.32 | 1.00 | 14.3 |
A, data have been deducted blank
B, high bubble sample are to obtain after the family expenses hand cleanser is diluted with the standard liquid that contains trace arsenic at 1: 2000;
3, liquid atomiser 10 adopts the two phase flow atomising device, gas mixer 11 adopts gas inlet pipe 13 shown in Fig. 5,6 and mixed air cavity 12 mutual blenders at an angle, because big flow carrier gas produces negative pressure at gas mixer 11 middle parts, chemical gaseous phase in the gas-liquid separation device of its underpart take place can be produced the complete suction gas mixer of gas 11 tops that contain element to be measured, detect with sending among the atomizer A after carrier gas mixes.
4, liquid atomiser 10 adopts the two phase flow atomising device, gas mixer 11 adopts Fig. 7,8 described structures, promptly mix air cavity 12 and be sleeved on the gas phase efferent duct 7 of gas-liquid separation device 6 structure that the center line of the center line of gas inlet pipe 13 and mixed air cavity 12 is setovered mutually.Because tangential inflow is prolonged in big flow carrier gas in M2, produce strong negative pressure at top small nozzle place, chemical gaseous phase in the gas-liquid separation device of its underpart take place can be produced the complete suction of the gas top that contain element to be measured, detect with sending among the atomizer A after carrier gas mixes.
Claims (6)
1, gas-liquid separator, comprise mixing reactor (5), gas-liquid separation device (6) and carrier gas carrier pipe (4), it is characterized in that in the pipeline of gas phase efferent duct (7) of described gas-liquid separation device (6) gas mixer (11) being set, described carrier gas carrier pipe (4) is connected with gas mixer (11).
2, separator according to claim 1 is characterized in that being provided with liquid atomiser (10) between mixing reactor (5) and gas-liquid separation device.
3, separator according to claim 2 is characterized in that described liquid atomiser (10) is ultrasonic nebulizer or two phase flow sprayer.
4,, it is characterized in that described gas mixer (11) comprises mixed air cavity (12) and connected gas inlet pipe (13) according to claim 1,2 or 3 described separators.
5, separator according to claim 4, it is characterized in that described gas inlet pipe (13) is vertical mutually with mixed air cavity (12) or mutually at an angle, both center lines intersect or biasing mutually, and its gas inlet pipe (13) must stretch in the mixed air cavity (12).
6, separator according to claim 4 is characterized in that described mixed air cavity (12) is sleeved on the gas phase efferent duct (7) of gas-liquid separation device (6), and the bore of the port of export that mixes air cavity (12) and gas phase efferent duct (7) is less than the size of self main body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200520001620 CN2787290Y (en) | 2005-01-26 | 2005-01-26 | Gas-liquid separating arrangement for chemical gas phase |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200520001620 CN2787290Y (en) | 2005-01-26 | 2005-01-26 | Gas-liquid separating arrangement for chemical gas phase |
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| CN2787290Y true CN2787290Y (en) | 2006-06-14 |
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| CN 200520001620 Expired - Lifetime CN2787290Y (en) | 2005-01-26 | 2005-01-26 | Gas-liquid separating arrangement for chemical gas phase |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100371052C (en) * | 2005-01-26 | 2008-02-27 | 北京吉天仪器有限公司 | Gas-liquid separator |
| CN103878694A (en) * | 2012-12-21 | 2014-06-25 | 株式会社荏原制作所 | Gas liquid separating device and grinding device |
-
2005
- 2005-01-26 CN CN 200520001620 patent/CN2787290Y/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100371052C (en) * | 2005-01-26 | 2008-02-27 | 北京吉天仪器有限公司 | Gas-liquid separator |
| CN103878694A (en) * | 2012-12-21 | 2014-06-25 | 株式会社荏原制作所 | Gas liquid separating device and grinding device |
| CN103878694B (en) * | 2012-12-21 | 2019-01-11 | 株式会社荏原制作所 | Gas-liquid separation device and grinding device |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Effective date of abandoning: 20080227 |
|
| C25 | Abandonment of patent right or utility model to avoid double patenting |