CN104949865A - Multi-purpose sample digestion-gas absorption device - Google Patents
Multi-purpose sample digestion-gas absorption device Download PDFInfo
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- CN104949865A CN104949865A CN201410118883.6A CN201410118883A CN104949865A CN 104949865 A CN104949865 A CN 104949865A CN 201410118883 A CN201410118883 A CN 201410118883A CN 104949865 A CN104949865 A CN 104949865A
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Abstract
The invention discloses a multi-purpose sample digestion-gas absorption device which comprises a U-shaped absorption pipe and a reaction container, wherein a multihole glass plate is arranged on one side of the U-shaped absorption pipe, and a cooling device is arranged on the other side of the U-shaped absorption pipe; the reaction container is communicated with the pipe orifice on the side with the cooling device and is communicated with a liquid adding device and a bypass pipe; a cooling cover is arranged at the upper part of the reaction container; and a gas discharging pipe is arranged on the cooling cover and is detachably connected to the pipe orifice of the U-shaped absorption pipe. The experiment equipment of the multi-purpose sample digestion-gas absorption device is readily available; the reactions are carried out in a closed system, a digestion liquid is unlikely to volatilize and lose; furthermore, the reaction is full, and the temperature is controllable; the detection accuracy can be guaranteed, and the environment is pollution-free; and the multi-purpose sample digestion-gas absorption device is convenient to popularize and apply.
Description
Technical field
The present invention relates to chemical analysis instrument field, be specifically related to a kind of multiduty treatments of the sample-gas absorbing device.
background material
At the analysis detection field of material, collection gas carries out analysis and effectively can eliminate interference, improves the accuracy analyzing measurement result.As measured protein content in foodstuff (GB 5009.5-2010), usually first organic nitrogen is converted into Inorganic Ammonium, then adds alkali and steam ammonia, finally measure the content of ammonia to determine protein content; As everyone knows, the impact that the existence of sulphur is applied petroleum refining process and products thereof is larger, as corroding metal equipment, cause contaminated environment etc. in catalyst poisoning, use procedure, Ignition Lamp Method (GB/T380) is by sulfur dioxide absorption after organic sulfur burning, determining the content of sulphur by measuring content of sulfur dioxide, detecting accurately noiseless.
Existing gas absorbing device generally adopts condenser pipe or porous absorbent pipe or absorbing liquid, all there is difficult control of temperature, absorb incomplete problem, measurement result is caused to occur deviation, as GB Sulfur Dioxide In The Atmosphere assay method (HJ 482-2009) requires that temperature controls at 23-29 DEG C, but the environment temperature of test generally exceeds this scope; Many projects needing treatments of the sample to measure, as food protein mensuration (
gB5009.5-2010), conventional digestion method flask carries out in unlimited system, and digestion reagent is easily volatilized and loses and contaminated environment, and sample solution easily spills flask and loses, and cause metrical error large, accuracy rate is low.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of multiduty treatments of the sample-gas absorbing device, and burning sample temperature constant, does not affect burning rate, and digestive efficiency is high, and digestive juice is volatilization loss not easily, environmentally safe.
The present invention is achieved through the following technical solutions:
A kind of multiduty treatments of the sample-gas absorbing device, comprise side and be provided with porous plate, opposite side is provided with the U-shaped absorption tube of cooling device, and be communicated in the reaction vessel being provided with this side pipe mouth of cooling device, described reaction vessel is communicated with liquid-adding device and by-pass pipe, its top is provided with cooling dome, and described cooling dome is provided with escape pipe, the removable mouth of pipe being connected to U-shaped absorption tube of described escape pipe.
The further improved procedure of the present invention is, described cooling dome is double-layer glass structure or one week is double-layer glass structure, and liquid coolant inlet/outlet pipe is communicated with the cavity between double glazing.
Further improvement of the present invention mode is, described cooling dome and the connector of reaction vessel are that plug bush type is connected.
Further improvement of the present invention mode is, the connector place diameter of described cooling dome and reaction vessel is less than other position diameters.
Further improvement of the present invention mode is, escape pipe, liquid-adding device are communicated in cooling dome top respectively.
Further improvement of the present invention mode is, described cooling device is the U-shaped absorption tube of this section is double-layer glass structure, and liquid coolant inlet/outlet pipe is communicated with the cavity between double glazing.
Further improvement of the present invention mode is, described by-pass pipe lower end is communicated in the bottom of reaction vessel, and upper port is higher than reaction vessel, and described by-pass pipe is provided with B glass stopper.
Further improvement of the present invention mode is, the bottom of described U-shaped absorption tube is provided with the drain pipe for discharging liquid, and described drain pipe is provided with the C glass stopper for damming.
Further improvement of the present invention mode is, described liquid-adding device is separating funnel, and the drain pipe of described separating funnel is provided with the A glass stopper for damming.
Further improvement of the present invention mode is, this side pipe mouth that U-shaped absorption tube is provided with porous plate is communicated with air extractor.
The present invention compared with prior art has the following advantages:
One, the present invention is owing to being provided with cooling dome for reactor, and be provided with cooling device for U-shaped absorption tube, therefore, in use, according to the needs of the different sample of test, the liquid coolant of design temperature in one or two cooling device, can be carried wherein, thus control reaction and absorb temperature, guarantee that temperature meets examination criteria, improve the accuracy detected.
Such as, for the sample needing burning, first sample is placed in reaction vessel and burns, the gas of burning release, by cooling dome, the U-shaped absorption tube being provided with cooling device again through escape pipe inflow, enters absorbing liquid and absorbs after being cooled to design temperature.For another example, for the sample of hot digestion, the moieties after gasification meets cold liquefaction backflow in cooling dome, and digestive juice can be made repeatedly to gasify backflow, raising treatments of the sample rate.
Two, the present invention all carries out owing to reacting in airtight system, and detected material is volatilization loss not easily, can ensure the accuracy detected, environmentally safe, easy to utilize.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Fig. 2 is that the present invention measures sulfur content schematic diagram in fuel oil.
Fig. 3 is that the present invention measures atmospheric sulfur dioxide schematic diagram.
Embodiment
A kind of multiduty treatments of the sample-gas absorbing device as shown in Figure 1, comprise side and be provided with porous plate, opposite side is provided with the U-shaped absorption tube 1 of cooling device, and be communicated in the reaction vessel 2 being provided with this side pipe mouth of cooling device, reaction vessel 2 is communicated with liquid-adding device 4 and by-pass pipe 21, the top of reaction vessel 2 is provided with cooling dome 3, cooling dome 3 is provided with escape pipe 31, the removable mouth of pipe being connected to U-shaped absorption tube 1 of escape pipe 31, removable connection herein particularly by two connectors respectively sanding be then connected.Wherein, escape pipe 31, liquid-adding device 4 are communicated in the top of cooling dome 3 respectively, liquid-adding device 4 is separating funnel, in reaction vessel 2, sample or the reagent with example reaction is added by separating funnel during use, the drain pipe 41 of separating funnel is provided with for damming and the A glass stopper 62 of isolated air, ensure that the sealing of reaction environment.
Still as shown in Figure 1, cooling dome 3 is double-layer glass structure or one week is double-layer glass structure, and liquid coolant inlet/outlet pipe 52,51 is communicated with the cavity 5 between double glazing; In cavity 5, thermostatical circulating water (realizing this function by water circulating pump connection water delivering orifice 51 and a water inlet 52 in the present embodiment) is passed into before sample combustion or digestion, water temperature controls within the temperature range of sample test requirement, remain consistent by the reaction cavity temperature under cooling dome after recirculated water with water temperature, can not raise gradually along with the process of sample combustion, guarantee to react the constant of cavity temperature in whole experiment process.
Still as shown in Figure 1, cooling dome 3 and the connector of reaction vessel 2 are that plug bush type is connected, and cooling dome 3 is less than other position diameters with the connector place diameter of reaction vessel 2, and both interface sanding process, cooling dome 3 is enclosed within the collar extension of reaction vessel 2.
Still as shown in Figure 1, this side pipe mouth being provided with porous plate at U-shaped absorption tube 1 is communicated with air extractor, being pumped in absorbing liquid of gas uniform speed that sample produces can be collected, and cooling device is the double-layer glass structure being positioned at U-shaped absorption tube 1 side, inner layer glass tube is condenser pipe 11, the cavity 5 formed between layer glass plays the effect of control temperature, and liquid coolant inlet/outlet pipe 52,51 is communicated with cavity 5; The recirculated water passing into constant temperature in cavity 5 can change gas temperature in pipe, improves the absorption efficiency of absorbing liquid (such as; For the gas that high temperature not easily absorbs, the recirculated cooling water of frozen water or logical constant temperature can be loaded to reduce temperature so that absorbing liquid absorbs collection in the cavity of condenser pipe).
In the present embodiment, by-pass pipe 21 lower end is communicated in the bottom of reaction vessel 2, and by-pass pipe 21 is provided with B glass stopper 61, and need the sample of distillation digestion for some, can connect steam generator on by-pass pipe 21, time no, standby B glass stopper 61 seals.Require that the upper port of by-pass pipe 21 is higher than reaction vessel 2, if it is highly lower, liquid in reaction vessel 2 can backflow the interior impact detection of by-pass pipe 21 (such as: when by-pass pipe 21 connects steam generator, the liquid that distillation produces can backflow in steam generator through by-pass pipe 21, and causing sample to run off affects testing result).
In the present embodiment, be provided with the drain pipe 12 for discharging liquid in the bottom of U-shaped absorption tube 1, be convenient to sampling absorbing liquid and pipe blow-through, drain pipe 12 is provided with the C glass stopper 6 for damming.
Structure of the present invention is simple, can combinationally use, such as, when measuring Protein in Food (as shown in Figure 1), first U-shaped absorption tube 1 is removed from this device, getting commercially available fresh milk 10.00g adds in reaction vessel 2, adds 0.2 g copper sulphate, 0.6 g potassium sulfate and 20 mL sulfuric acid by separating funnel, closes A, B glass tube 62,61, the temperature of cooling dome 3 controls at 50 DEG C, reaction vessel 2 is placed in digestion extremely blueness on electric furnace.U-shaped absorption tube 1 is connected with escape pipe 31, water emptying in cooling dome 3, NaOH is added from separating funnel NaOH(and prepare by GB 5009.5-2010), measure the content of the ammonia discharged, calculate Protein Content in Milk.Sample determination precision: replication 6 sample sizes are 3.5%, and relative standard deviation is less than 1.6%.
Entirety of the present invention is easy to use, such as, when measuring sulfur content (as shown in Figure 2) in fuel oil, first in little spirit lamp, add 3.00ml ethanol and 1.00g simulation fuel oil, little spirit lamp is placed in reaction vessel 2, U-shaped absorption tube 1 loads formaldehyde absorbent 5.00ml, by A, B, C glass stopper 62, 61, 6 close, light spirit lamp, the thermostatted water of 40 DEG C is passed in cooling dome 3, 25 DEG C of thermostatted waters are passed in condenser pipe 11, the side that U-shaped absorption tube 1 is provided with porous plate connects air extractor (air extractor of this experiment is aspiration pump 7), burning gases are gathered by the speed of evacuation of 0.5L/min, after having burnt, open C glass stopper 6, U-shaped absorption tube 1 is cleaned with distilled water, and constant volume is in 10.00ml color comparison tube, according to the required reagent of Sulfur Dioxide In The Atmosphere National Standard Method (HJ 482-2009) method preparation, and measurement result.Sample determination precision: 100.00ppm standard model, replication 6 relative standard deviations are less than 2.5%; Accuracy: measure 6 100ppm concentration of analog samples, measured value is 97.0ppm ± 1.0(x ± SD).
The present invention can also be used alone, such as, only need by being used alone U-shaped absorption tube 1 shown in Fig. 3 when measuring atmospheric sulfur dioxide: first, close C glass stopper 6, add absorbing liquid (configuring by GB HJ 482-2009), by the recirculated water by 25 DEG C in condenser pipe 11, the side that U-shaped absorption tube 1 is provided with porous plate connects air extractor (air extractor of this experiment is aspiration pump 7), to bleed 60min, open C glass stopper 6 and collect absorbing liquid and detect with 0.5L/min speed.Estimating precision: the sulphuric dioxide standard model of 0.101 μ g/ml, repeated relative standard deviation is less than 1.5%, and repeatability relative standard deviation is less than 3.2%.
Claims (10)
1. multiduty treatments of the sample-gas absorbing device, it is characterized in that: comprise side and be provided with porous plate, opposite side is provided with the U-shaped absorption tube (1) of cooling device, and be communicated in the reaction vessel (2) being provided with this side pipe mouth of cooling device, described reaction vessel (2) is communicated with liquid-adding device (4) and by-pass pipe (21), its top is provided with cooling dome (3), described cooling dome (3) is provided with escape pipe (31), the removable mouth of pipe being connected to U-shaped absorption tube (1) of described escape pipe (31).
2. a kind of multiduty treatments of the sample-gas absorbing device as claimed in claim 1, it is characterized in that: described cooling dome (3) is for double-layer glass structure or one week are for double-layer glass structure, and liquid coolant inlet/outlet pipe (52,51) is communicated with the cavity (5) between double glazing.
3. a kind of multiduty treatments of the sample-gas absorbing device as claimed in claim 1 or 2, is characterized in that: described cooling dome (3) and the connector of reaction vessel (2) are that plug bush type is connected.
4. a kind of multiduty treatments of the sample-gas absorbing device as claimed in claim 3, is characterized in that: described cooling dome (3) is less than other position diameters with the connector place diameter of reaction vessel (2).
5. the multiduty treatments of the sample-gas absorbing device of the one as described in claim 1 or 3, is characterized in that: escape pipe (31), liquid-adding device (4) are communicated in cooling dome (3) top respectively.
6. a kind of multiduty treatments of the sample-gas absorbing device as claimed in claim 1, it is characterized in that: described cooling device is the U-shaped absorption tube (1) of this section is double-layer glass structure, liquid coolant inlet/outlet pipe (52,51) is communicated with the cavity (5) between double glazing.
7. a kind of multiduty treatments of the sample-gas absorbing device as claimed in claim 1, it is characterized in that: described by-pass pipe (21) lower end is communicated in the bottom of reaction vessel (2), upper port is higher than reaction vessel (2), and described by-pass pipe (21) is provided with B glass stopper (61).
8. a kind of multiduty treatments of the sample-gas absorbing device as claimed in claim 1, it is characterized in that: the bottom of described U-shaped absorption tube (1) is provided with the drain pipe (12) for discharging liquid, and described drain pipe (12) is provided with the C glass stopper (6) for damming.
9. a kind of multiduty treatments of the sample-gas absorbing device as claimed in claim 1, is characterized in that: described liquid-adding device (4) is separating funnel, and the drain pipe (41) of described separating funnel is provided with the A glass stopper (62) for damming.
10. a kind of multiduty treatments of the sample-gas absorbing device as claimed in claim 1, is characterized in that: this side pipe mouth that U-shaped absorption tube (1) is provided with porous plate is communicated with air extractor.
Priority Applications (1)
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CN201410118883.6A CN104949865A (en) | 2014-03-27 | 2014-03-27 | Multi-purpose sample digestion-gas absorption device |
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CN201410118883.6A CN104949865A (en) | 2014-03-27 | 2014-03-27 | Multi-purpose sample digestion-gas absorption device |
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CN201410118883.6A Withdrawn CN104949865A (en) | 2014-03-27 | 2014-03-27 | Multi-purpose sample digestion-gas absorption device |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107340288A (en) * | 2016-12-31 | 2017-11-10 | 青岛大学 | A kind of equipment for detecting air formaldehyde concentration |
CN108640485A (en) * | 2018-04-18 | 2018-10-12 | 南京卡佛科学仪器有限公司 | A kind of production method of porous glass plate for gas absorption tube |
-
2014
- 2014-03-27 CN CN201410118883.6A patent/CN104949865A/en not_active Withdrawn
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107340288A (en) * | 2016-12-31 | 2017-11-10 | 青岛大学 | A kind of equipment for detecting air formaldehyde concentration |
CN107340288B (en) * | 2016-12-31 | 2023-06-27 | 青岛大学 | Equipment for detecting formaldehyde concentration in air |
CN108640485A (en) * | 2018-04-18 | 2018-10-12 | 南京卡佛科学仪器有限公司 | A kind of production method of porous glass plate for gas absorption tube |
CN108640485B (en) * | 2018-04-18 | 2020-11-03 | 南京卡佛科学仪器有限公司 | Method for manufacturing porous glass plate for gas absorption tube |
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Application publication date: 20150930 |