CN107860768A - Sulfide detection means in a kind of mud sample with efficient absorption function - Google Patents

Sulfide detection means in a kind of mud sample with efficient absorption function Download PDF

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Publication number
CN107860768A
CN107860768A CN201711089769.5A CN201711089769A CN107860768A CN 107860768 A CN107860768 A CN 107860768A CN 201711089769 A CN201711089769 A CN 201711089769A CN 107860768 A CN107860768 A CN 107860768A
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China
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detection means
detector
absorption function
efficient absorption
mud sample
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CN201711089769.5A
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CN107860768B (en
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应忠真
孙秀梅
胡红美
金衍健
郝青
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Zhejiang Marine Fisheries Research Institute
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Zhejiang Marine Fisheries Research Institute
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Plasma & Fusion (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention provides sulfide detection means in a kind of mud sample with efficient absorption function, including detector, experiment frame, unit detection means and lowering or hoisting gear, experiment frame is fixedly mounted in the top of detector, unit detection means includes reaction bulb, reaction bulb is placed on lowering or hoisting gear, the present invention is compact-sized, it is easy to operate, the rational deployment of unit detection means can be realized by detector and experiment frame, overall structure stability is strong, on the one hand the floor space of device is reduced, on the other hand four groups of unit detection means can be operated simultaneously, accelerate detection procedure, and pass through the barrier effect of plastics sieve plate, improve the absorbed effect of hydrogen sulfide gas.

Description

Sulfide detection means in a kind of mud sample with efficient absorption function
Technical field
The present invention relates to sulfide detection device technology field, sulphur in specially a kind of mud sample with efficient absorption function Compound detection means.
Background technology
Sulfurous organic compound in soil can produce inorganic sulphide during anaerobic decomposition.Sulfate is in reduction-state Under the conditions of, also it can be generated sulfide by microbial action.Sulfide meets acid and produces hydrogen sulfide, the easy loss of hydrogen sulfide to air In, stink is produced, and toxicity is very big.It can be acted on the disulfide bond in human inner cell's pigment, oxidizing ferment and such material, Cellular oxidation process is influenceed, cell tissue anoxic is caused, jeopardizes the life of people.Therefore, sulfide is a weight of soil monitoring Want index.
The assay method of sulfide in the existing soils and sediments in China, including iodimetric titration, ion selective electrode method, methylene Base indigo plant AAS etc., referring especially to《Water and effluent monitoring analysis method(The third edition)》With《Marine monitoring specification the 5th Point:Sediment analysis》(GB17378.5-2007).Iodimetric titration is applied to the higher soils and sediments sample of measure sulfide content Product, but sensitivity is low.Its principle is that in acid condition, sulfide acts on excessive iodine, remaining iodine sodium thiosulfate Solution titrates, the amount consumed according to hypo solution, derives the content of sulfide.Ion selective electrode method determines sulphur During compound, detection limit is low compared with iodimetric titration, but the current-responsive due to electrode has exponent relation with sulphion concentration, so being more suitable for The larger sample of sulfide content span is determined, when sulfide content is generally relatively low, its current-responsive effect is bad, stability Difference, it is also easy to produce larger error.And it is found through experiments that, the silver-colored sulfur electrode that domestic manufacturers are produced is not directed to sulphur before dispatching from the factory Ion application is corrected, so in addition to custom-made, mostly can not Accurate Determining sulfite ion concentration.Inlet electrode price is held high It is expensive, at the same there is also be not easy to use, less stable the shortcomings of.According to above-mentioned, existing detection method typically uses methylene Blue AAS, sub-methyl blue spectrum analysis have the characteristics that easy to operate, strong applicability, high sensitivity, extensive utilization In the measure of sulfide.
In sub-methyl blue spectrum analysis determines sample sulfide, the sulfide in sample changes into gaseous hydrogen sulfide, The hydrogen that cured in the absorption tube that develops the color absorbs developer and fully absorbed, and chromogenic reaction occurs, and generation is a kind of more stable and limpid Yellow-brownish solution, there is absorption maximum characteristic at 400nm.But conventional colour developing absorption tube assimilation effect is poor so that the sulphur measured Compound concentration is relatively low, influences the accuracy of measurement.
The content of the invention
It is an object of the invention to provide sulfide detection means in a kind of mud sample with efficient absorption function, to solve The problem of being proposed in above-mentioned background technology.
To achieve the above object, the present invention provides following technical scheme:Sulphur in a kind of mud sample with efficient absorption function Peace is fixed on compound detection means, including detector, experiment frame, unit detection means and lowering or hoisting gear, the top of the detector Experiment frame is filled, the unit detection means includes nitrogen comb, and the nitrogen comb connects outside nitrogen by the first rubber tube Tank, the port of export of the nitrogen comb are fixedly connected with the entrance point of needle-valve flowmeter, the port of export socket of the needle-valve flowmeter There is the second rubber tube, second rubber sleeve is connected to a side bottleneck of reaction bulb, and the reaction bulb is three-necked flask, and its Another side bottleneck ground dropping funel, the top bottleneck ground connection condenser west tube of the reaction bulb, the straight type condensation Pipe sleeve is connected to the 3rd rubber tube, and the 3rd rubber sleeve is connected to fritted glass disk bubbler, and the reaction bulb is placed on the liter On falling unit.
Preferably, the bottom surrounding of the detector uniformly installs four groups of rubber runners, the front panel of the detector It is upper that power switch, direction switch, thermometer is fixedly mounted, fuse base, electricity is fixedly mounted on the rear side panel of the detector Source line, service hatch, external ground wire and radiator fan, the detector are internally provided with water bath.
Preferably, it is fixedly connected with the needle-valve flowmeter on the experiment frame, bolt connection U-tube on the experiment frame Folder, the U-tube chuck are connected to the fritted glass disk bubbler.
Preferably, right angle setting plastics sieve plate in the fritted glass disk bubbler, the plastics sieve plate are provided with three groups, and The linearly equidistantly arrangement in the fritted glass disk bubbler.
Preferably, the lowering or hoisting gear includes stepper motor, and the stepper motor is fixedly mounted in the detector, institute The output shaft for stating stepper motor coordinates screw mandrel spiral shell in coaxially connected screw mandrel, the screw mandrel gap behind the top of the detector Mother, the feed screw nut are fixedly connected with lifting arm, and linear pattern through hole is provided with the experiment frame, and the lifting arm is straight through this The first limited block is fixedly connected with after line style through hole, the bottom of first limited block is fixedly connected with litter, and the litter passes through work Dynamic bolt is fixedly connected with sliding sleeve, and the bottom of the litter is fixedly connected with the second limited block, and the bottom of second limited block is fixed Connecting trays.
Preferably, the sliding sleeve on be evenly arranged with four groups of spring bolts, spring bolt described in four groups runs through the cunning Rear thread connection pressure ring is covered, the pressure ring is located at the surface of the reaction bulb, and its size and the top phase of the reaction bulb Matching.
Preferably, four groups of bottle holders are fixedly mounted on the pallet, are provided with the top of the bottle holder and the reaction bulb The groove that bottom matches, and bottle holder is symmetrically installed around the vertical central axis of the pallet described in four groups.
Compared with prior art, the beneficial effects of the invention are as follows:
1st, the present invention is compact-sized, easy to operate, and the reasonable cloth of unit detection means can be realized by detector and experiment frame Office, overall structure stability is strong, on the one hand reduces the floor space of device, on the other hand can operate four groups of unit detections simultaneously Device, accelerate detection procedure.
2nd, the present invention has the function of self-locking using screw rod transmission, passes through lowering or hoisting gear, it is possible to achieve pallet driving a reaction Bottle is sunk in water bath automatically, and moving process is steady, will not shake, and reduces manual operation, realizes that automation water-bath adds Heat, and the experiment maloperation for causing reaction bulb to be tumbled due to artificial taking and placing can be avoided completely.
3rd, the present invention substitutes conventional colour developing absorption tube by using fritted glass disk bubbler, can carry out short time sampling, Due to the barrier effect of sieve plate in fritted glass disk bubbler so that bubble declines, and increases the bubble containing gaseous hydrogen sulfide and is absorbed Chance and also extend soak time, so as to increase absorb developer absorption efficiency, increase precision of analysis.
4th, the present invention is made by the way that the needle-valve flowmeter in detector and fritted glass disk bubbler are installed on test stand Obtain in detector and keep fixed distance between various glass apparatus, installation area is small, is easy to arrange.
Brief description of the drawings
Fig. 1 is front view of the present invention;
Fig. 2 is rearview of the present invention;
Fig. 3 is unit structure of the detecting device schematic diagram in the present invention;
Fig. 4 is fritted glass disk bubbler structural representation in the present invention;
Fig. 5 is lifting device structure schematic diagram in the present invention;
Fig. 6 is pallet top view in the present invention;.
In figure:1 detector, 2 experiment frames, 201 U-tubes folder, 3 unit detection means, 301 nitrogen combs, 302 first rubbers Sebific duct, 303 needle-valve flowmeters, 304 second rubber tubes, 305 reaction bulbs, 306 dropping funels, 307 condenser west tubes, 308 the 3rd Rubber tube, 309 fritted glass disk bubblers, 310 plastics sieve plates, 4 lowering or hoisting gears, 401 stepper motors, 402 screw mandrels, 403 screw mandrel spiral shells Mother, 404 lifting arms, 405 first limited blocks, 406 litter, 407 sliding sleeves, 408 second limited blocks, 409 pallets, 410 spring bolts, 411 pressure rings, 412 bottle holders, 5 rubber runners, 6 rubber runners, 7 direction switches, 8 thermometers, 9 fuse bases, 10 power lines, 11 dimensions Repair hole, 12 external ground wires, 13 radiator fans, 14 water baths.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.It is based on Embodiment in the present invention, those of ordinary skill in the art are obtained every other under the premise of creative work is not made Embodiment, belong to the scope of protection of the invention.
Fig. 1-6 are referred to, the present invention provides a kind of technical scheme:Sulfide in a kind of mud sample with efficient absorption function Detection means, including detector 1, experiment frame 2, unit detection means 3 and lowering or hoisting gear 4, the top of detector 1 are fixedly mounted in fact Frame 2 is tested, unit detection means 3 includes nitrogen comb 301, and nitrogen comb 301 connects outside nitrogen by the first rubber tube 302 Tank.The port of export of nitrogen comb 301 is fixedly connected with the entrance point of needle-valve flowmeter 303, and needle-valve flowmeter 303 adjusts four respectively Nitrogen flow in reaction bulb 305, the port of export of needle-valve flowmeter 303 are socketed with the second rubber tube 304, the second 304 sets of rubber tube It is connected to a side bottleneck of reaction bulb 305.Reaction bulb 305 is three-necked flask, and its another side bottleneck ground dropping funel 306, the top bottleneck ground connection condenser west tube 307 of reaction bulb 305, condenser west tube 307 is socketed with the 3rd rubber tube 308, the 3rd rubber tube 308 is socketed with fritted glass disk bubbler 309.Right angle setting plastics sieve plate in fritted glass disk bubbler 309 310, plastics sieve plate 309 is provided with three groups, and linearly equidistantly arrangement reaction bulb 305 is put in fritted glass disk bubbler 309 Put on lowering or hoisting gear 4.
Lowering or hoisting gear 4 includes stepper motor 401, and stepper motor 401 is fixedly mounted on 1 in detector, stepper motor 401 Output shaft coaxially connected screw mandrel 402 behind the top of detector 1, the gap of screw mandrel 402 coordinate feed screw nut 403, feed screw nut 403 are fixedly connected with lifting arm 404.Linear pattern through hole is provided with experiment frame 2, lifting arm 404 runs through after the linear pattern through hole admittedly Surely the first limited block 405 is connected, the bottom of the first limited block 405 is fixedly connected with litter 406, and litter 406 is consolidated by movable bolt Surely sliding sleeve 407 is connected, is evenly arranged with four groups of spring bolts 410 on sliding sleeve 407, four groups of spring bolts 410 run through sliding sleeve 407 Rear thread connects pressure ring 411.Pressure ring 411 is located at the surface of reaction bulb 305, and its size and the top phase of reaction bulb 305 Match somebody with somebody.The bottom of litter 406 is fixedly connected with the second limited block 408, and the bottom of the second limited block 408 is fixedly connected with pallet 409, pallet Four groups of bottle holders 412 are fixedly mounted on 409, the top of bottle holder 412 is provided with the groove to match with the bottom of reaction bulb 305, and And four groups of bottle holders 412 are symmetrically installed around the vertical central axis of pallet 409.
The bottom surrounding of detector 1 uniformly installs four groups of rubber runners 5, and electricity is fixedly mounted on the front panel of detector 1 Source switch 6, direction switch 7, thermometer 8, fuse base 9, power line 10, maintenance are fixedly mounted on the rear side panel of detector 1 Hole 11, external ground wire 12 and radiator fan 13, detector 1 are internally provided with water bath 14.Needle-valve is fixedly connected with experiment frame 2 Flowmeter 303,2 bolt connection U-tubes folder 201 on experiment frame, U-tube folder 201 are socketed with fritted glass disk bubbler 309.
Operation principle:After mud sample is detected using sub-methyl blue spectrum analysis, hydrogen sulfide is generated in reaction bulb 305 Gas, under the protection and promotion of nitrogen, pushed to from condenser west tube 307 in fritted glass disk bubbler 309, and by porous Colour developing absorbent in plate absorption tube 309 absorbs, and unabsorbed hydrogen sulfide gas is formed in the absorbent that develops the color contains gaseous sulfur Change the minute bubbles of hydrogen, under Effects of Density, minute bubbles float collided with sieve plate 310 upwards, because the stop of sieve plate 310 is made With so that minute bubbles are broken or decline, the chance that increase gaseous hydrogen sulfide minute bubbles are absorbed by absorption developer and extension Soak time, so as to increase the absorption efficiency for absorbing developer, increase precision of analysis.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding And modification, the scope of the present invention is defined by the appended.

Claims (7)

1. sulfide detection means in a kind of mud sample with efficient absorption function, including detector(1), experiment frame(2), unit Detection means(3)And lowering or hoisting gear(4), it is characterised in that:The detector(1)Top be fixedly mounted experiment frame(2), it is described Unit detection means(3)Including nitrogen comb(301), the nitrogen comb(301)Pass through the first rubber tube(302)Connection is outside Nitrogen pot, the nitrogen comb(301)The port of export be fixedly connected with needle-valve flowmeter(303)Entrance point, the needle-valve flow Meter(303)The port of export be socketed with the second rubber tube(304), second rubber tube(304)It is socketed with reaction bulb(305)One Side bottleneck, the reaction bulb(305)For three-necked flask, and its another side bottleneck ground dropping funel(306), the reaction Bottle(305)Top bottleneck ground connection condenser west tube(307), the condenser west tube(307)It is socketed with the 3rd rubber tube (308), the 3rd rubber tube(308)It is socketed with fritted glass disk bubbler(309), the reaction bulb(305)It is placed on described Lowering or hoisting gear(4)On.
2. sulfide detection means in a kind of mud sample with efficient absorption function according to claim 1, its feature exist In:The detector(1)Bottom surrounding uniformly installation four groups of rubber runners(5), the detector(1)Front panel on it is solid Dingan County fills power switch(6), direction switch(7), thermometer(8), the detector(1)Rear side panel on be fixedly mounted insurance Base(9), power line(10), service hatch(11), external ground wire(12)And radiator fan(13), the detector(1)Inside It is provided with water bath(14).
3. sulfide detection means in a kind of mud sample with efficient absorption function according to claim 1, its feature exist In:The experiment frame(2)On be fixedly connected with the needle-valve flowmeter(303), on the experiment frame(2)Bolt connection U-tube is pressed from both sides (201), the U-tube folder(201)It is socketed with the fritted glass disk bubbler(309).
4. sulfide detection means in a kind of mud sample with efficient absorption function according to claim 1, its feature exist In:The fritted glass disk bubbler(309)Middle right angle setting plastics sieve plate(310), the plastics sieve plate(310)It is provided with three Group, and in the fritted glass disk bubbler(309)In linearly equidistantly arrangement.
5. sulfide detection means in a kind of mud sample with efficient absorption function according to claim 1, its feature exist In:The lowering or hoisting gear(4)Including stepper motor(401), the stepper motor(401)It is fixedly mounted in the detector (1), the stepper motor(401)Output shaft run through the detector(1)Top after coaxially connected screw mandrel(402), it is described Screw mandrel(402)Gap coordinates feed screw nut(403), the feed screw nut(403)It is fixedly connected with lifting arm(404), the experiment Frame(2)On be provided with linear pattern through hole, the lifting arm(404)The first limited block is fixedly connected with after the linear pattern through hole (405), first limited block(405)Bottom be fixedly connected with litter(406), the litter(406)Consolidated by movable bolt Surely sliding sleeve is connected(407), the litter(406)Bottom be fixedly connected with the second limited block(408), second limited block (408)Bottom be fixedly connected with pallet(409).
6. sulfide detection means in a kind of mud sample with efficient absorption function according to claim 1 or 5, its feature It is:The sliding sleeve(407)On be evenly arranged with four groups of spring bolts(410), spring bolt described in four groups(410)Through institute State sliding sleeve(407)Rear thread connects pressure ring(411), the pressure ring(411)Positioned at the reaction bulb(305)Surface, and its Size and the reaction bulb(305)Top match.
7. sulfide detection means in a kind of mud sample with efficient absorption function according to claim 1 or 5, its feature It is:The pallet(409)Four groups of bottle holders of upper fixed installation(412), the bottle holder(412)Top be provided with and the reaction Bottle(305)The groove that matches of bottom, and bottle holder described in four groups(412)Around the pallet(409)Vertical central axis pair Claim installation.
CN201711089769.5A 2017-11-08 2017-11-08 Sulphide detection device in mud appearance with high-efficient absorption function Active CN107860768B (en)

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Cited By (1)

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