CN204594870U - A kind of diffusion-absorption device being applicable to mensuration AVS and SEM - Google Patents
A kind of diffusion-absorption device being applicable to mensuration AVS and SEM Download PDFInfo
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- CN204594870U CN204594870U CN201520237113.3U CN201520237113U CN204594870U CN 204594870 U CN204594870 U CN 204594870U CN 201520237113 U CN201520237113 U CN 201520237113U CN 204594870 U CN204594870 U CN 204594870U
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Abstract
The utility model discloses a kind of diffusion-absorption device being applicable to measure AVS and SEM.It is characterized in that: pass into nitrogen testing fixture impermeability, get sediment sample afterwards and put into reaction bulb, hydrochloric acid is added by separating funnel, afterwards reaction bulb is placed on magnetic stirring apparatus, stir with constant speed, after fully reacting, again pass into nitrogen, then get the solution in absorption bottle, measure absorbance with spectrophotometric colo, obtain AVS and SEM value.This assay method combines the advantage of absorption process and diffusion method, catch is adopted to collect the hydrogen sulfide gas of diffusion, remaining a small amount of gas is blown into by nitrogen and is equipped with in the absorption bottle of alkali lye, bubble is made to increase in the shape of a spiral by arranging tandem annular catch, decrease the reaction time, improve the accuracy that AVS measures.
Description
Technical field
The utility model belongs to environmental monitoring technology field, particularly a kind of diffusion-absorption device being applicable to mensuration AVS and SEM.
Background technology
All the time, the ecological risk assessment of heavy metal in water is a difficult task, and one of the main reasons is wherein that heavy deposition tenor measures to waste time and energy, and can not ensure precision.In recent years, AVS-SEM model becomes the focus of heavy deposition Bioavailability of Metals.AVS (Acid Volatile Sulfide, acid volatile sulfide), being defined as can by the sulfide of the cold hydrochloric acid extraction of 1molL-1; SEM (Simultaneously Extracted Metals, synchronously extracts metal), is extracting the synchronous metal extracted in AVS process.AVS is the part of most activity in deposition sulfide, and SEM represents the part heavy deposition metal of most biological effectiveness (bio-toxicity).When AVS is greater than SEM, Heavy Metals in Sediments major part exists with the form of metal sulfide, greatly reduces its bio-toxicity, and therefore the relative value of SEM and AVS can be used as the important parameter characterizing Heavy Metals in Sediments biological effectiveness.USEPA (Environmental Protection Agency) thinks that AVS/SEM method is a kind of promising new method; there is huge development potentiality: " AVS/SEM method is based upon in solid theoretical foundation, uses equilibrium assignmen theory and movable metallic to predict the method for heavy deposition Bioavailability of Metals.This method becomes more easy than existing method the most at last and has more the method for accuracy " (USEPA, 1995).By related criteria, AVS/SEM method establishes concentration-bio-toxicity response relation between physicochemical data and biological data, thus has vital role to the formulation of sediment quality guidelines (SQC or SQGs); Require higher although AVS and SEM measures to operative technique, the time of measuring is shorter, and amount of work is less than heavy metal full dose and form (step by step arithmetic method) measures, and can make an appraisal to sample area heavy metal toxicity at short notice.
Usually two kinds of method test AVS and SEM:(1 are adopted at present) the cold Acid volatile sulfide of nitrogen carrier gas (the purge-and-trapmethod), is called for short " absorption process "; (2) hydrogen sulfide gas diffusion method (the diffusion method), is called for short " diffusion method ".These two kinds of methods respectively have relative merits, and the absorption process reaction time is shorter, but recall rate is on the low side; Diffusion method recall rate is a little more than absorption process, and operation is also relatively simple, but the reaction time is very long.Due to the test request of AVS higher (Sample storage not easily), the test job of a large amount of sample must be completed at short notice, so need to develop a kind of method both fast and sound.The utility model provides a kind of diffusion-absorption device and method measuring AVS and SEM, and the advantage of both set, avoids respective defect, can complete the test analysis work of a large amount of sample within the relatively short time preferably.
Prior art is compared, and the utility model tool has the following advantages and effect:
1, the utility model has the advantage of diffusion method and absorption process concurrently, avoids both defects, and have speed fast, the advantage that recall rate is high, can complete the test of a large amount of sample at short notice.
2, by installing fan-shaped catch, extending the gas circuit of extracted hydrogen sulfide gas, soak time is extended, improve the absorption efficiency of gas.
3, adopt inverted absorption tube, tandem annular catch is set in absorption plant, makes bubble increase in the shape of a spiral, increase the absorption efficiency of gas.
Utility model content
The purpose of this utility model is, provides a kind of diffusion-absorption device measuring AVS and SEM, solves the deficiency of above-mentioned existing method and device existence.
Technical solutions of the utility model are as follows.
A kind of method being applicable to mensuration AVS and SEM, comprise the steps: to pass into nitrogen testing fixture impermeability, get sediment sample afterwards and put into reaction bulb, add hydrochloric acid by feed arrangement, then reaction bulb is placed on magnetic stirring apparatus, stir with constant speed, again nitrogen is passed into after fully reacting, and the solution got in absorption bottle, measure absorbance with spectrophotometric colo, obtain AVS and SEM value.
In said method, described in get sediment sample and refer to and get 1 ~ 3g bed mud, dry at 80 ~ 100 DEG C after weighing to water percentage be 20% ~ 25%; Described hydrochloric acid volume is 10 ~ 15mL, and concentration is 5 ~ 7mol/L.
In said method, magnetic stirring apparatus stirs 50 ~ 70min with the speed of 100 ~ 120r/min; Describedly pass into that to pass into nitrogen flow rate in nitrogen testing fixture impermeability step be 180 ~ 300cm
3/ min, the time is 3 ~ 10min; Describedly after abundant reaction, again pass in nitrogen steps that to pass into nitrogen flow rate be 180 ~ 300cm
3/ min, the reaction time is 3 ~ 10min.
In said method, described feed arrangement is separating funnel; Described spectrophotometer measures at 670nm or 665nm place.
In said method, concrete steps be:
(1) in reaction bulb, add deoxygenation deionized water, respectively add NaOH solution in the first absorption bottle and the first absorption bottle, device passes into N
2, testing fixture impermeability;
(2) get bed mud sample, join in reaction bulb, separately get the bed mud samples weighing post-drying of equal in quality, and calculate bed mud water cut;
(3) stop passing into nitrogen, in reaction bulb, add hydrochloric acid by feed arrangement, then valve-off, open magnetic stirring apparatus simultaneously, fully react;
(4) proceed in volumetric flask by the solution in absorption cell, the first absorption bottle and the first absorption bottle, add amino-xylene amine aqueous solution and ammonium ferric sulfate solution successively, at 670nm or 665nm place, spectrophotometric colo measures absorbance, obtains AVS value;
(5) reaction liquid in reaction bulb is got top turbid solution membrane filtration, measure filtrate content of beary metal with ICP, calculate adding and value of SEM.
Be applicable to the diffusion-absorption device measuring AVS and SEM, described diffusion-absorption device comprises nitrogen cylinder, the first Drexel bottle, the second Drexel bottle, reaction bulb, absorption cell, feed arrangement, the first absorption bottle and the first absorption bottle; Described nitrogen cylinder is connected in turn with the first Drexel bottle, the second Drexel bottle, reaction bulb, the first absorption bottle and the first absorption bottle; Described feed arrangement is arranged at reaction bulb bottle mouth position; Described absorption cell is arranged at reaction bulb inside; Described nitrogen cylinder, Drexel bottle, reaction bulb, absorption bottle is connected by wireway.
In said apparatus, described diffusion-absorption device also comprises flowmeter, magnetic stirring apparatus and magnetic rotor, and described flowmeter is arranged between Drexel bottle and nitrogen cylinder; Described magnetic rotor is arranged in reaction bulb; Described magnetic stirring apparatus is positioned over below reaction bulb.Described reaction bulb, by scribbling the rubber stopper seal of glass cement, rubber plug is equipped with feed arrangement and wireway.
In said apparatus, described feed arrangement is also communicated with reaction bulb by rubber tube, with holding device internal and external pressure balance, liquid is flowed into smoothly.
In said apparatus, wherein said reaction bulb inwall is equipped with fan-shaped catch, be positioned at device 1/3 ~ 1/2 At The Height, and the height of fan-shaped catch is not higher than absorption cell, higher than liquid level in reaction bulb; When hydrogen sulfide gas is overflowed from solution, be subject to the stop of catch, diffuse near absorption cell, improve the absorption efficiency of gas.Described first absorption bottle and the first absorption bottle are inversion type conduit, and tandem annular catch is equipped with in inside, every gear sheet interval 10-12cm.Described absorption cell by support installing on reaction bulb inwall.
In said apparatus, in described first Drexel bottle and the second Drexel bottle, deionization deoxygenation high purity water is housed; In described feed arrangement, hydrochloric acid is housed; The alkaline acetic acid zinc solution that mass percent concentration is 2 ~ 4% is housed in described absorption cell; High purity water is filled in described reaction bulb; Described first absorption bottle and the first absorption bottle are equipped with NaOH solution.
Accompanying drawing explanation
AVS-SEM determinator schematic diagram in Fig. 1 the utility model
Fig. 2 reaction bulb detail drawing
Fig. 3 tandem annular catch detail drawing.
Embodiment
Do specifically to describe in detail further to the present invention below in conjunction with specific embodiment, but embodiments of the present invention are not limited thereto, for the technological parameter do not indicated especially, can refer to routine techniques and carry out.
Shown in Fig. 1-Fig. 3, described diffusion-absorption device comprises nitrogen cylinder 1, first Drexel bottle 3, second Drexel bottle 4, reaction bulb 5, absorption cell 6, feed arrangement 8, first absorption bottle 12 and the first absorption bottle 13; Described nitrogen cylinder 1 is connected in turn with the first Drexel bottle 3, second Drexel bottle 4, reaction bulb 5, first absorption bottle 12 and the first absorption bottle 13; Described feed arrangement 8 is arranged at reaction bulb 5 bottle mouth position; It is inner that described absorption cell 6 is arranged at reaction bulb 5; Described nitrogen cylinder 1, Drexel bottle 3, reaction bulb 4, absorption bottle 10 is connected by wireway 11.Described diffusion-absorption device also comprises flowmeter 2, magnetic stirring apparatus 10 and magnetic rotor 7, and described flowmeter 2 is arranged between Drexel bottle 3 and nitrogen cylinder 1; Described magnetic rotor 7 is arranged in reaction bulb 5; Described magnetic stirring apparatus 10 is positioned over below reaction bulb 5.Described feed arrangement 8 is also communicated with reaction bulb 5 by rubber tube 9.Wherein said reaction bulb 5 inwall is equipped with fan-shaped catch, is positioned at device 1/2 At The Height, and the height of fan-shaped catch is not higher than absorption cell 6, higher than liquid level in reaction bulb 5; Described first absorption bottle 12 and the first absorption bottle 13 are inversion type conduit, and tandem annular catch is equipped with in inside, every gear sheet interval 11cm.
Application the present invention and diffusion method, air blast, arrange three groups of control experiments respectively, refer to following embodiment.
Embodiment 1
The preparation method of typical curve: add 100mL high purity water in reaction bulb, adds the NaOH solution of 70mL 0.5mol/L in absorption bottle.Coupling arrangement, and pass into N to device
2, adjustment gas flow rate is to 250cm
3/ min, Continuous aeration 3min, also remove residual oxygen with testing fixture impermeability, prevent S
2-oxidized.Close nitrogenous source subsequently, in reaction bulb, add certain density normal concentration S respectively
2-solution (0,1,3,5,7,9,10mg/L).Added the HCl solution of 15mL 6mol/L by feed arrangement, generate H with reaction
2s gas, then with the S of alkali liquor absorption effusion
2-.
Then open magnetic stirring apparatus, stir 60min with the speed of 120r/min.
Use said apparatus to measure, after fully reacting, again pass into N
2(gas speed is 250cm to 10min
3/ min), the hydrogen sulfide gas of remnants is blown in absorption bottle, then solution in absorption bottle is proceeded to the volumetric flask of 100mL (with high purity water drip washing absorption cell, cleansing solution is proceeded in volumetric flask), the ammonium ferric sulfate solution of 2mL 0.25mol/L is added in volumetric flask, constant volume and leaving standstill after 30min, at 670nm place, spectrophotometric colo measures absorbance, records AVS value.Then the reaction liquid in reaction bulb got top turbid solution membrane filtration and number, filtrate measures content of beary metal with ICP, calculates SEM value.
Measure:
In reaction bulb, add 100mL high purity water, in absorption bottle, add the NaOH solution of 70mL 0.5mol/L.Coupling arrangement, and pass into N to device
2, adjustment gas flow rate is to 250cm
3/ min, Continuous aeration 3min, also remove residual oxygen with testing fixture impermeability, prevent S
2-oxidized.Close nitrogenous source subsequently, get 3g bed mud with syringe, inject reaction bulb rapidly, separately get the bed mud of identical weight, dry in the baking oven of 100 DEG C after weighing, and calculate water percentage.Added the HCl solution of 15mL 6mol/L by feed arrangement, react with bed mud and generate H
2s gas, then with the S of alkali liquor absorption effusion
2-.
Then open magnetic stirring apparatus, stir 60min with the speed of 120r/min.
Use said apparatus to measure, after fully reacting, again pass into N
2(gas speed is 250cm to 10min
3/ min), the hydrogen sulfide gas of remnants is blown in absorption bottle, then solution in absorption bottle is proceeded to the volumetric flask of 100mL (with high purity water drip washing absorption cell, cleansing solution is proceeded in volumetric flask), the ammonium ferric sulfate solution of 2mL 0.25mol/L is added in volumetric flask, constant volume and leaving standstill after 30min, at 670nm place, spectrophotometric colo measures absorbance, records AVS value.Then the reaction liquid in reaction bulb got top turbid solution membrane filtration and number, filtrate measures content of beary metal with ICP, calculates SEM value.
Comparative example 1
Air blast: add 100mL high purity water in reaction bulb, adds the NaOH solution of 70mL 0.5mol/L in absorption bottle.N is passed into device
2(gas speed is 250cm to 10min
3/ min), testing fixture impermeability, gets 3g bed mud with syringe afterwards, injects reaction bulb rapidly, in other device, adds certain density normal concentration S respectively
2-solution (0,1,3,5,7,9,10mg/L), separately get the bed mud of identical weight, after weighing, take off oven dry 100, and calculate water percentage.Add the HCl solution of 15mL 6mol/L with separating funnel, then open magnetic stirring apparatus, stir 80minh with the speed of 120r/min.
Constantly N is passed in course of reaction
2(gas speed is 250cm
3/ min), the hydrogen sulfide gas extracted is blown in absorption bottle, then solution in absorption bottle is proceeded to the volumetric flask of 100mL (with high purity water drip washing absorption cell, cleansing solution is proceeded in volumetric flask), the ammonium ferric sulfate solution of 2mL 0.25mol/L is added in volumetric flask, constant volume and leaving standstill after 30min, measures absorbance and record at 670nm place with spectrophotometric colo.Then the reaction liquid in reaction bulb got top turbid solution membrane filtration and number, filtrate measures content of beary metal with ICP, calculates SEM value.
Comparative example 2
Diffusion method: add 100mL high purity water in reaction bulb, adds the NaOH solution of 70mL 0.5mol/L in absorption bottle.(gas speed is 250cm to pass into N210min to device
3/ min), testing fixture impermeability, gets 3g bed mud with syringe afterwards, injects reaction bulb rapidly, in other device, adds certain density normal concentration S respectively
2-solution (0,1,3,5,7,9,10mg/L), separately get the bed mud of identical weight, after weighing, take off oven dry 100, and calculate water percentage.Add the HCl solution of 15mL 6mol/L with separating funnel, then open magnetic stirring apparatus, stir 3h with the speed of 120r/min.
Without the need to logical N in course of reaction
2by the diffusion of gas in obturator, with the sulfuretted hydrogen that alkali liquor absorption extracts, then solution in absorption bottle is proceeded to the volumetric flask of 100mL (with high purity water drip washing absorption cell, cleansing solution is proceeded in volumetric flask), in volumetric flask, add the ammonium ferric sulfate solution of 2mL 0.25mol/L, constant volume and leaving standstill after 30min, measure absorbance and record at 670nm place with spectrophotometric colo.Then the reaction liquid in reaction bulb got top turbid solution membrane filtration and number, filtrate measures content of beary metal with ICP, calculates SEM value.
The AVS value result of three groups of control experiment gained is as shown in the table:
As seen from the above table, in device, add the normal concentration S of equivalent
2-solution, within the identical reaction time, the average recall rate that the inventive method records is higher than air blast and diffusion method.This illustrates that the present invention fully can extract the sulfide in sediment, more truly records Heavy Metals in Sediments content, for judging that heavy metal toxicity and biological effectiveness provide foundation further.
To add the standard solution of 3 μm of ol/g, when recall rate close to, compare the reaction time of three kinds of methods.
Recall rate of the present invention a little more than other two kinds of methods, the shortest time needed for sufficient reacting.Can reach a conclusion: when reaction conditions is consistent, fan-shaped catch in the present invention and tandem catch, by extending the gas circuit of gas, improve the absorption efficiency of gas, and under the prerequisite ensureing high recall rate, highly shortened the reaction time, this is of great significance detecting AVS-SEM tool fast.
The above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.All any amendments done within the spirit and principles in the present invention, equivalent to replace and improvement etc., within the protection domain that all should be included in the claims in the present invention.
Claims (4)
1. one kind is applicable to the diffusion-absorption device measuring AVS and SEM, it is characterized in that, described diffusion-absorption device comprises nitrogen cylinder (1), the first Drexel bottle (3), the second Drexel bottle (4), reaction bulb (5), absorption cell (6), feed arrangement (8), the first absorption bottle (12) and the first absorption bottle (13); Described nitrogen cylinder (1) is connected in turn with the first Drexel bottle (3), the second Drexel bottle (4), reaction bulb (5), the first absorption bottle (12) and the first absorption bottle (13); Described feed arrangement (8) is arranged at reaction bulb (5) bottle mouth position; It is inner that described absorption cell (6) is arranged at reaction bulb (5); Described nitrogen cylinder (1), Drexel bottle (3), reaction bulb (4), absorption bottle (10) is connected by wireway (11).
2. be applicable to the diffusion-absorption device measuring AVS and SEM according to claim 1, it is characterized in that, described diffusion-absorption device also comprises flowmeter (2), magnetic stirring apparatus (10) and magnetic rotor (7), and described flowmeter (2) is arranged between Drexel bottle (3) and nitrogen cylinder (1); Described magnetic rotor (7) is arranged in reaction bulb (5); Described magnetic stirring apparatus (10) is positioned over reaction bulb (5) below.
3. be applicable to the diffusion-absorption device measuring AVS and SEM according to claim 1, it is characterized in that, described feed arrangement (8) is also communicated with reaction bulb (5) by rubber tube (9).
4. be applicable to the diffusion-absorption device measuring AVS and SEM according to claim 1, it is characterized in that, wherein said reaction bulb (5) inwall is equipped with fan-shaped catch, be positioned at device 1/3 ~ 1/2 At The Height, and the height of fan-shaped catch is not higher than absorption cell (6), higher than liquid level in reaction bulb (5); Described first absorption bottle (12) and the first absorption bottle (13) are inversion type conduit, and tandem annular catch is equipped with in inside, every gear sheet interval 10-12cm.
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| CN201520237113.3U CN204594870U (en) | 2015-04-17 | 2015-04-17 | A kind of diffusion-absorption device being applicable to mensuration AVS and SEM |
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| CN201520237113.3U CN204594870U (en) | 2015-04-17 | 2015-04-17 | A kind of diffusion-absorption device being applicable to mensuration AVS and SEM |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104807763A (en) * | 2015-04-17 | 2015-07-29 | 华南理工大学 | Diffusion-absorption device and method suitable for measuring AVS (Acid Volatile Sulfide) and SEM (Simultaneously Extracted Metals) |
-
2015
- 2015-04-17 CN CN201520237113.3U patent/CN204594870U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104807763A (en) * | 2015-04-17 | 2015-07-29 | 华南理工大学 | Diffusion-absorption device and method suitable for measuring AVS (Acid Volatile Sulfide) and SEM (Simultaneously Extracted Metals) |
| CN104807763B (en) * | 2015-04-17 | 2018-01-02 | 华南理工大学 | A kind of diffusion absorption device and method for being applied to measure AVS and SEM |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150826 |
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