CN202339293U - Device for detecting and pre-treating sulfide in water - Google Patents

Device for detecting and pre-treating sulfide in water Download PDF

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Publication number
CN202339293U
CN202339293U CN2011203931736U CN201120393173U CN202339293U CN 202339293 U CN202339293 U CN 202339293U CN 2011203931736 U CN2011203931736 U CN 2011203931736U CN 201120393173 U CN201120393173 U CN 201120393173U CN 202339293 U CN202339293 U CN 202339293U
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absorption bottle
main shaft
rotating mechanism
reaction bulb
fixed mount
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CN2011203931736U
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彭敬雪
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China Petroleum and Chemical Corp
Sinopec Fushun Research Institute of Petroleum and Petrochemicals
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China Petroleum and Chemical Corp
Sinopec Fushun Research Institute of Petroleum and Petrochemicals
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Abstract

The utility model discloses a device for detecting and pre-treating sulfide in water, and the device comprises absorption bottles, a reaction bottle, an absorption bottle fixing frame, a reaction bottle fixing frame, a gas path system, a main shaft, a rotating mechanism, a lifting mechanism and a constant-temperature water bath pot. The absorption bottle fixing frame and the reaction bottle fixing frame are fixed on the rotating mechanism; the main shaft is a hollow pipe which is vertically arranged on the middle part of the constant-temperature water bath pot; the rotating mechanism is rotatably sleeved on the main shaft; the lifting mechanism is provided with a lifting arm which moves up and down along the main shaft; and the lifting arm is supported at the bottom of the rotating mechanism. Compared with the prior art, two absorption bottles with different specifications can be put on the absorption bottle fixing frame, and the requirements of two standard methods (a methylene blue method and an iodometric method) for detecting the sulfide in water can be met. The device restricts the measuring ranges of both a main nitrogen intaking control valve and branch nitrogen intaking control valves and has the advantages of gas path stability, easiness for control over gas flow rate and high detection result accuracy.

Description

A kind of water quality sulfide is measured pretreatment unit
Technical field
The utility model relates to a kind of environmental sample pretreatment unit, particularly relates to a kind of water quality sulfide working sample pretreatment unit.
Background technology
At present, the mensuration common method of sulfide is methylenum careuleum (GB/T16489-1996) and iodimetric titration (HJ/T60-2000) in the water quality, and two kinds of methods are applicable to the mensuration of low concentration and high concentration sulfide in the water sample respectively.The sulfide of surveying all refers to deliquescent inorganic sulphide and acid soluble metal sulfide in the water.
Above-mentioned sulfide not only produces stink, and corrosivity is strong, toxicity is big, so sulfide is an important indicator of water pollution, also is a big event of each daily water quality monitoring of environment monitoring department.If water sample exists suspension or turbidity height, when colourity is dark, must carries out acidifying-air blowing pre-service to water sample and could obtain to measure reliably the result.Therefore, sample pretreatment is a committed step measuring sulfide, should eliminate interference, the unlikely again loss that causes sulfide.Usually methylene blue method or iodimetric titration one cover sulfide pretreatment unit include: reaction bulb, absorption bottle, connecting pipe, spinner-type flowmeter, extension clamp, cross, titration platform, thermostat water bath (iodimetric titration) etc.Before sample carries out pre-service; Operating personnel need these test tools mades are put on the testing table; Just can make an experiment after connecting one by one by manual work again; The common pretreatment unit that connects of cover takies than large tracts of land, and once can only carry out pre-service to a sample, so complex operation, inefficiency.
CN201229272Y discloses a kind of water quality sulfide-acidifying air blowing absorption apparatus, this utility model absorption apparatus compact conformation, take up room little, once can handle 2-4 sample.Composition comprises: reaction bulb, absorption bottle and fixed mount separately; Main shaft; Air-channel system; Rotating mechanism; Elevating mechanism and thermostat water bath.But the absorption bottle fixed mount among the CN201229272Y can only be placed a kind of tubulose absorption bottle of specification, and can only be the absorption tubing of 2.5-3.0cm for diameter., utility model is not suitable for the sample pretreatment demand that iodimetric titration sulfide is measured so only being applicable to the first blue laws.Two kinds of used absorption bottle specifications of sulfide assay method of cause and profile differ bigger, and methylene blue method is the absorption tube of Φ 3cm, and iodimetric titration is the iodine flask of 150ml or 250ml.Employed absorption bottle volume and shape can not arbitrarily change in two kinds of assay methods of sulfide, because volume and shape all are the factors that influence the sample pretreatment effect.Influencing factor that sulfide measures also comprises and is blown into nitrogen time and nitrogen flow rate; And among the CN201229272Y control of the total air inflow of nitrogen and nitrogen are communicated to before the absorption bottle all measurement ranges of limiting control valve not of the nitrogen flow on each branch road; Therefore, this uses novel absorption apparatus in application, also to exist the nitrogen air inlet always to control valve and each branch road nitrogen operation valve measurement range is excessive, low precision and the gas circuit that causes is unstable, the wayward sulfide that makes of nitrogen flow rate is measured deficiencies such as result precision is low.
Summary of the invention
Deficiency to prior art; The utility model provides a kind of water quality sulfide to measure pretreatment unit; Can place on its absorption bottle fixed mount the absorption bottle of two kinds of different sizes, both can be used for sample pretreatment that methylene blue method sulfide measures, also can be used for the sample pretreatment that iodimetric titration sulfide measures and gas circuit is stable, nitrogen flow rate is prone to control, it is high that sample pretreatment is effective, sulfide is measured result precision.
The utility model water quality sulfide is measured pretreatment unit and is comprised six parts: absorption bottle, reaction bulb and fixed mount separately thereof, air-channel system, main shaft, rotating mechanism, elevating mechanism and thermostat water bath; Above-mentioned part connects fixing by existing mode; Like the described connected mode of CN201229272Y; Specifically comprise: the fixed mount of absorption bottle and reaction bulb fixed mount are fixed on the rotating mechanism, and main shaft is a hollow tube that is vertically installed in the thermostat water bath middle part, and the rotating mechanism rotary sleeve is located on the main shaft; Elevating mechanism has the lifting arm that moves up and down along main shaft, and this lifting arm support is in said rotating mechanism bottom.
Wherein: absorption bottle and fixed mount thereof are by the specification configuration of two kinds of standard methods of sulfide (iodimetric titration and methylene blue method) requirement; The absorption bottle fixed mount is fixed on the rotating mechanism; The absorption bottle fixed rack structure is " " type, and the lower end slightly is longer than in the upper end, and the upper end is fixed on the rotary system; On upper and lower two the plate faces of absorption bottle fixed mount 2 ~ 4 circular holes are set respectively, in order to place the absorption bottle of two kinds of standard methods; It is 15~16cm that the absorption bottle fixed mount is provided with length as required, wide 6.5~7.5cm, high 9~10cm; Circularhole diameter is 3.0~3.5cm, adjacent two pitch of holes 3-4cm; Steel plate thickness 0.5mm.
Wherein: air-channel system comprises that valve is always controlled in air inlet pipeline, outlet pipe and nitrogen air inlet and nitrogen is communicated to the nitrogen flow operation valve on preceding each branch road of reaction bulb.Total control valve and branch road operation valve all adopt glass rotameter, and always controlling valve control nitrogen flow scope is 0.5 L/min~1.8 L/min, and branch road operation valve control nitrogen flow scope is 40 mL/min~400mL/min.Precision is respectively 50 mL/min and 10 mL/min.
Absorption bottle of the utility model and fixed mount thereof: absorption bottle is by the requirement specification configuration of two kinds of standard method of analyses of above-mentioned sulfide, and have two kinds of specifications: methylene blue method is the absorption tube of Φ 3cm; Iodimetric titration is the iodine flask of 150ml.Iodimetric titration is that secondary absorbs, so need a pair of absorption bottle.The absorption bottle fixed mount is fixed on the rotating mechanism.Absorption bottle fixed mount material is the stainless steel version, and structure is " " type, opening left, the lower end slightly is longer than in the upper end, the upper end is fixed on the rotary system.
Reaction bulb in the utility model and fixed mount thereof: reaction bulb is by the specification configuration of two kinds of standard method of analysis requirements of sulfide, and the reaction bulb fixed mount is fixed on the spring clamp of rotary system.
Main shaft in the utility model a: hollow tube that is vertically installed in the thermostat water bath middle part; From the nitrogen of steel cylinder from air inlet pipeline;, the air inlet overhead control passes the body of this main shaft after regulating; And form outlet pipe in the main shaft top, and be communicated on each preceding branch road of each reaction bulb at outlet pipe, be provided with the nitrogen flow operation valve.
Rotating mechanism in the utility model: rotary sleeve is located on the said main shaft; Said reaction bulb, absorption bottle and fixed mount separately thereof all are fixed on this rotating mechanism.
Thermostat water bath in the utility model: be used for carrying out sample water-bath heating, 0~100 ℃ of control temperature range.
The utility model water quality sulfide is measured in the pretreatment unit, said absorption bottle quantity be 2~4 (to), said reaction bulb quantity is corresponding with absorption bottle quantity.Reaction bulb and absorption bottle are along the rotating mechanism circle distribution.
The utility model water quality sulfide is measured in the pretreatment unit, has an elbow in the said outlet pipe, and this elbow inlet end is communicated to each reaction bulb with nitrogen air inlet pipeline end sealing and rotatable connection the, all the other each outlet sides through rubber tube.
The utility model water quality sulfide is measured in the pretreatment unit; Said elevating mechanism also comprises power wheel and leading screw; One end of leading screw is fixed in this power wheel axle center, and the other end is rotating to be placed in the fixed cover, and said lifting arm is through the sliding sleeve and the engagement of this leading screw of a tool internal thread.Said leading screw is provided with locating part in two ends up and down.
The utility model water quality sulfide is measured in the pretreatment unit, also is provided with supporting plate on the said rotating mechanism, and said reaction bulb seats on this supporting plate.The position that contacts with reaction bulb spheroid bottom on the said supporting plate is provided with rubber blanket.
The utility model water quality sulfide is measured pretreatment unit; Its absorption bottle fixed mount can be placed the absorption bottle of two kinds of different sizes; Both be applicable to the sample pretreatment demand that methylene blue method (GB/T16489-1996) sulfide is measured, and also be applicable to the sample pretreatment demand that iodimetric titration (HJ/T60-2000) sulfide is measured, it is stable also to have gas circuit; Nitrogen flow rate is prone to control, and sample pretreatment is effective, sulfide is measured the high advantage of result precision.
Description of drawings
Fig. 1 is that the utility model water quality sulfide is measured pretreatment unit (methylene blue method) structural representation;
Fig. 2 is that the utility model water quality sulfide is measured pretreatment unit (iodimetric titration) structural representation;
Fig. 3 is an absorption bottle fixed rack structure synoptic diagram.
Wherein:
1-absorption bottle fixed mount 2-absorption bottle 3-nitrogen flow branch road operation valve
4-air-out apparatus 5-reaction bulb 6-reaction bulb fixed mount
7-thermostat water bath 8-air inlet pipeline 9-power wheel
The 10-nitrogen flow is always controlled valve 11-main shaft 12-rotating mechanism
13-lifting arm 14-leading screw 15-elevating mechanism
16-nut body 17-fixed cover 18-upper limit spare
19-supporting plate 20-rubber blanket 21-condenser west tube.
Embodiment
Enforcement below in conjunction with Fig. 1, Fig. 2 and Fig. 3 measure pretreatment unit to the utility model water quality sulfide is set forth.
Like Fig. 1, Fig. 2 and shown in Figure 3; The utility model water quality sulfide is measured pretreatment unit and is comprised a thermostat water bath 7; It provides the water-bath heating for the sample in the reaction bulb 5; Because of with the sulfide in the iodometric determination water quality, sample needs under 60 ℃~70 ℃ temperature, carry out acidifying-air blowing-absorption pre-service.This thermostat water bath 7 is set to a rectangular shape, moves to make things convenient for manual work, and temperature range is 0 ℃~100 ℃.
Said main shaft 11 is a hollow tube, is vertically installed in thermostat water bath 7 middle parts, after the nitrogen that comes from steel cylinder is always controlled valve 10 via nitrogen, goes into nitrogen air inlet pipeline 8, and passes this body from the hollow tube bottom and form air-out apparatus 4 on its top.Air-out apparatus 4 has an elbow; The inlet end of this elbow and nitrogen air inlet pipeline end sealing; And can be around 8 rotations of nitrogen air inlet pipeline; This elbow is provided with the outlet side of respective amount according to the number of reaction bulb 5, and each outlet side is communicated to each reaction bulb 5 with rubber tube, is communicated at air-out apparatus 4 on each branch road of each reaction bulb and all is provided with nitrogen flow operation valve 3.
Said reaction bulb, absorption bottle and fixed mount separately thereof all are fixed on the said rotating mechanism 12; Rotating mechanism 12 is set on the outer wall of said main shaft 11; The bottom is seated on the lifting arm of elevating mechanism 15; Rotating mechanism 12 can rotate freely around main shaft 11, and each reaction bulb on it and absorption bottle are communicated with rubber tube and together rotate, and do not twine mutually.
Reaction bulb fixed mount 6 is provided with reaction bulb 5, and absorption bottle fixed mount 1 is provided with absorption bottle 2.In the utility model, said reaction bulb 5 quantity are 2~4, said absorption bottle 2 quantity be 2~4 (to).Reaction bulb 5 is along rotating mechanism 12 circumference uniform distributions, with handled easily with the arrangement of absorption bottle 2.Because reaction bulb 5 needs to immerse heating (iodimetric titration) in the thermostat water bath 7, thereby the position of reaction bulb 5 guarantees to be lower than absorption bottle 2.Absorption bottle 2 item next doors that can be positioned over reaction bulb 5 corresponding with reaction bulb 5.It is firm for reaction bulb 5 is placed; A supporting plate 19 is set on rotating mechanism 12; Reaction bulb 5 is placed between supporting plate 19 and the reaction bulb fixed mount 6, respectively reaction bulb 5 is imposed downwards and the power that makes progress by reaction bulb fixed mount 6 and supporting plate 19, with fixation reaction bottle 5.Position with the spheroid pig of reaction bulb 5 on the supporting plate 19 also is provided with the rubber blanket 20 with skidproof effect.
In the utility model; Also comprise an elevating mechanism 15; Its lifting arm 13 supports also can move up and down along main shaft 11 in the bottom of rotating mechanism 12, like this, rotating mechanism 12 are risen or decline; And then reaction bulb 5, absorption bottle 2 and corresponding fixed mount 6 and fixed mount 1 thereof are risen or descend, and reaction bulb 5 can descend as required to getting in the thermostat water bath 7 or rise and breaks away from thermostat water bath 7.
Above-mentioned elevating mechanism 15 comprises a power wheel 9; The axle center of this power wheel 9 wears a rhizoid thick stick 14; The other end of said leading screw 14 is rotating to be placed in the fixed cover 17; Leading screw is provided with the sliding sleeve with internal thread 16 that cooperates with it ingeniously, and said lifting arm 13 promptly is connected in this sliding sleeve 16.Said power wheel 9 can gain impetus from the outside, and for example, external motor rotates and can drive power wheel 9 rotations, and then leading screw 14 is rotated, and the sliding sleeve 16 that is engaged with driving rises or decline, and then lifting arm 13 is risen or decline.
Be provided with a upper limit spare 18 on leading screw top near the position of fixed cover 17; A lower limit part is set in the leading screw bottom; To guarantee in leading screw 14 rotation processes; The sliding sleeve that links to each other with lifting arm 13 21 is unlikely to be moved upward to and offsets with fixed cover 17 and stuck, or moves downward supporting plate 19 is contacted with the bottom of thermostat water bath 7.
In the utility model, partly go up to breaking away from thermostat water bath 7 fully, down to immersing thermostat water bath 7 fully for the spheroid of reaction bulb 5 between the motor area of said lifting arm 13.
The operation steps of brief description the utility model.
The first water level in 7 pots of inspection thermostat water baths during operation, opening power is set heating-up temperature again, and at this moment water-bath begins heating and keeps temperature constant state (only be used for iodimetric titration, methylene blue method need not heat).Several reaction bulbs 5 that testing sample is housed are placed on respectively on the reaction bulb fixed mount 6, some absorption bottles 2 that (iodimetric titration) or several (methylene blue method) is equipped with absorbing agent are placed on respectively on the absorption bottle fixed mount 1.After connecting air-channel system and inspection and not having gas leakage, open the nitrogen cylinder valve, use nitrogen always to control valve 5 and regulate nitrogen air inlet total flows, with each branch road operation valve 7 nitrogen flow is transferred to necessary requirement again.Regulate elevating mechanism 15, power wheel 9 drives leading screw 14 and rotates, and lifting arm 13 is moved down, and makes reaction bulb integral body reduce in the thermostat water bath 7 and heats, and blows simultaneously in the heating process.After sample preparation finishes, close the nitrogen cylinder valve, regulate rotating mechanism 12, it is taken off after making absorption bottle 2 be in the operator dead ahead.Regulate elevating mechanism 15, lifting arm 13 is moved up, each reaction bulb 5 is shifted out thermostat water bath 7.
The sample determination result relatively
Measure water quality sulfide-acidifying air blowing absorption apparatus device of pretreatment unit and CN201229272Y with the utility model water quality sulfide and respectively NEPA's standard model and actual water sample are measured, measure the result and see table 1 and table 2 respectively.
Table 1 standard model precision and accuracy determination result be (n=4) relatively.
Figure DEST_PATH_DEST_PATH_IMAGE001
Table 2 actual water sample accuracy determination result relatively.
Figure DEST_PATH_DEST_PATH_IMAGE002
Simultaneously, when CN201229272Y adopted iodimetric titration, because structure is unsuitable, operation is difficulty comparatively.

Claims (10)

1. a water quality sulfide is measured pretreatment unit, comprises six parts: absorption bottle, reaction bulb and fixed mount separately thereof, air-channel system, main shaft, rotating mechanism, elevating mechanism and thermostat water bath; The fixed mount of absorption bottle and reaction bulb fixed mount are fixed on the rotating mechanism; Main shaft is a hollow tube that is vertically installed in the thermostat water bath middle part; The rotating mechanism rotary sleeve is located on the main shaft; Elevating mechanism has the lifting arm that moves up and down along main shaft, and this lifting arm support is in said rotating mechanism bottom; It is characterized in that: absorption bottle and fixed mount thereof are by the specification configuration of two kinds of standard method requirements of sulfide, and the absorption bottle fixed mount is fixed on the rotating mechanism, and the absorption bottle fixed rack structure is " " type, and the lower end slightly is longer than in the upper end, and the upper end is fixed on the rotary system; On upper and lower two the plate faces of absorption bottle fixed mount 2 ~ 4 circular holes are set respectively, in order to place the absorption bottle of two kinds of standard methods.
2. device according to claim 1 is characterized in that: it is 15~16cm that the absorption bottle fixed mount is provided with length, wide 6.5~7.5cm, high 9~10cm; Circularhole diameter is 3.0~3.5cm, adjacent two pitch of holes 3-4cm.
3. device according to claim 1 is characterized in that: air-channel system comprises that valve is always controlled in air inlet pipeline, outlet pipe and nitrogen air inlet and nitrogen is communicated to the nitrogen flow operation valve on preceding each branch road of reaction bulb.
4. device according to claim 3; It is characterized in that: always control valve and the branch road operation valve all adopts glass rotameter; Total control valve control nitrogen flow scope is 0.5 L/min~1.8 L/min, and branch road operation valve control nitrogen flow scope is 40 mL/min~400 mL/min.
5. device according to claim 1; It is characterized in that: main shaft is a hollow tube that is vertically installed in the thermostat water bath middle part; From air inlet pipeline, after the air inlet overhead control is regulated, pass the body of this main shaft from the nitrogen of steel cylinder, and form outlet pipe in the main shaft top; And be communicated on each preceding branch road of each reaction bulb at outlet pipe, be provided with the nitrogen flow operation valve.
6. device according to claim 1 is characterized in that: 0~100 ℃ of thermostat water bath control temperature range.
7. device according to claim 1 is characterized in that: absorption bottle quantity is 2~4, and reaction bulb quantity is corresponding with absorption bottle quantity, and reaction bulb and absorption bottle are along the rotating mechanism circle distribution.
8. device according to claim 3 is characterized in that: have an elbow in the outlet pipe, this elbow inlet end is communicated to each reaction bulb with nitrogen air inlet pipeline end sealing and rotatable connection the, all the other each outlet sides through rubber tube.
9. device according to claim 1; It is characterized in that: elevating mechanism comprises power wheel and leading screw; One end of leading screw is fixed in this power wheel axle center; The other end is rotating to be placed in the fixed cover, and lifting arm is through the sliding sleeve and the engagement of this leading screw of a tool internal thread, and leading screw is provided with locating part in two ends up and down.
10. device according to claim 1, it is characterized in that: rotating mechanism is provided with supporting plate, and reaction bulb seats on this supporting plate.
CN2011203931736U 2011-10-17 2011-10-17 Device for detecting and pre-treating sulfide in water Expired - Lifetime CN202339293U (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107860768A (en) * 2017-11-08 2018-03-30 浙江省海洋水产研究所 Sulfide detection means in a kind of mud sample with efficient absorption function
CN108088973A (en) * 2017-11-08 2018-05-29 浙江省海洋水产研究所 The device and assay method that water body sulfide content measures
CN110927146A (en) * 2019-08-29 2020-03-27 上海王奇实业有限公司 Quality of water sulphide pretreatment device
CN111141573A (en) * 2020-03-04 2020-05-12 广东石油化工学院 Device and method capable of extracting volatile sulfide of sediment acid in batches

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107860768A (en) * 2017-11-08 2018-03-30 浙江省海洋水产研究所 Sulfide detection means in a kind of mud sample with efficient absorption function
CN108088973A (en) * 2017-11-08 2018-05-29 浙江省海洋水产研究所 The device and assay method that water body sulfide content measures
CN108088973B (en) * 2017-11-08 2020-08-14 浙江省海洋水产研究所 Device and method for measuring sulfide content in water body
CN110927146A (en) * 2019-08-29 2020-03-27 上海王奇实业有限公司 Quality of water sulphide pretreatment device
CN111141573A (en) * 2020-03-04 2020-05-12 广东石油化工学院 Device and method capable of extracting volatile sulfide of sediment acid in batches

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