CN102353638A - Method and apparatus for rapid determination of water body sediment AVS and SEM - Google Patents
Method and apparatus for rapid determination of water body sediment AVS and SEM Download PDFInfo
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- CN102353638A CN102353638A CN2011101791459A CN201110179145A CN102353638A CN 102353638 A CN102353638 A CN 102353638A CN 2011101791459 A CN2011101791459 A CN 2011101791459A CN 201110179145 A CN201110179145 A CN 201110179145A CN 102353638 A CN102353638 A CN 102353638A
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Abstract
The invention discloses a method and an apparatus for rapid determination of water body sediments AVS and SEM. The apparatus comprises a nitrogen cylinder (1), gas-washing bottles (2), reaction bottles (6) and gas absorption bottles (11). A gas-washing bottle (2), a reaction bottle (6) and a gas absorption bottle (11) that are successively installed in series by a pipeline form a branch; a plurality of branches in parallel connection are connected to the nitrogen cylinder; a gas flowmeter (2) is arranged in front of each gas-washing bottle (2) in each branch, and a gas flowmeter (2) is arranged after the nitrogen cylinder in a main road; the reaction bottles are sealed by rubber plug (9) coated with glass cement, and the rubber plug are provided with acid inlet apparatuses. According to the method, hydrogen sulfide gas generated from the reaction is extracted by high purity nitrogen and absorbed by a lye; and the parallel connection accelerates a measure speed; and links of sample introduction, reaction and absorption are reinforced to increase speed and accuracy. On the premise of measure precision guarantee, the AVS determination method of the invention can as shortens time effectively and achieves good effects.
Description
Technical field
The invention belongs to field of measuring technique (environmental monitoring), method and the device of particularly a kind of fast measuring sediment AVS and SEM.
Background technology
The bio-toxicity problem of water body deposition heavy metal is one of the hot issue in current environment field, and core wherein and difficult point are the ecological hazard of deposition heavy metal is quantized, and then sets up correlation model conveniently to be applied to the environmental management practice.The AVS/SEM method is in this respect effective tool just.AVS is defined as can be by 1molL
-1The sulfide of cold hydrochloric acid extraction; SEM is meant the metal of simultaneous extraction in hydrochloric acid extraction AVS process.The theoretical foundation of AVS/SEM is the thiophilicity of heavy metal; The two is prone to form stable metal sulfide; Thereby reduce the part that the bio-toxicity of heavy metal: AVS represent in the sediment total sulfur (TS) tool reactivity, active in the SEM representative deposition heavy metal by force easily by part that biology utilized; As AVS>during SEM, the deposition heavy metal with reactivity exists with the form of metal sulfide, and this moment, water body weight metal bio-toxicity was very little.
The AVS/SEM method is a kind of new method of differentiating water body weight metal bio-toxicity, has many outstanding advantages.The AVS/SEM correlation theory has obtained the approval of academia and environmental management department at present, and has begun to be applied to real work.Developed countries such as the U.S., Holland and Britain have been considered as it setting up the major consideration on sediment quality basis.
The accurate mensuration of AVS is the condition precedent of all correlative studys, but the mensuration of AVS runs into a lot of difficulties in practical operation: whole process must keep anaerobic state, because its changeableness must be accomplished mensuration, 1molL at short notice
-1Cold hydrochloric acid (belonging to watery hydrochloric acid) and fully reaction of sediment, the hydrogen sulfide gas that its reaction produces fully absorption effectively detects or the like.So far lack measuring method fast and effectively for above-mentioned reasons.
At present, AVS measures has two kinds of methods: the one, and sulfide method, the 2nd, hydrogen sulfide gas diffusion method are dissolved in the cold acid of nitrogen carrier gas.
There are many problems in these two kinds of methods in practical operation; Mainly as follows: the one, be reaction time long (sample needs more than 2 hours); Because the preservation of AVS sample is difficulty (and the holding time can not surpass for 2 weeks in theory) very; Thereby can't measure large batch of sample, making AVS apply to large-scale ecological risk assessment almost becomes impossibility; The 2nd, lack effective input mode, influenced speed and accuracy, current methods is brought a large amount of air in the adition process of sediment sample and acid, make the AVS measured value be lower than actual value; The 3rd, lack good sealing means: influence the AVS measured value for preventing the sulphur in the rubber plug; Current methods adopts cork as the reactor air-tight manner; But cork is not so good as rubber plug on obturation effect; And operations such as cork is difficult to punch; Owing to will make a call to 3 holes at least on the reactor, in practical operation, be difficult to accomplish.
Summary of the invention
The object of the present invention is to provide a kind of sediment AVS and SEM assay method that quick and precisely is prone to row, to solve the problem that prior art exists.
The object of the invention is realized through following technical proposals: utilize high purity nitrogen will react the hydrogen sulfide gas that produces and extract, absorb with alkali lye, accelerate measuring speed through the mode of parallel connection; And to sample introduction, reaction, absorb each link and strengthen to improve accuracy.Adopt the mode (before each reactor all with the accurate pilot-gas flow of flowmeter) of a plurality of reactors parallel connection; Employing is got the mud device and is carried out sediment sampling and sample introduction (advancing reactor); Reactor has adopted effective seal mode and alr mode.
The device of a kind of fast measuring sediment AVS and SEM; Comprise nitrogen cylinder 1, Drexel bottle 2 reaction bulbs 6 and gas absorption bottle 11; Drexel bottle 2, reaction bulb 6 and gas absorption bottle 11 with the pipeline series connection constitutes a branch road successively; Be connected to nitrogen cylinder after some the branch road parallel connections; Before the Drexel bottle 2 of every branch road gas meter 2 is installed, gas meter 2 is installed behind the nitrogen cylinder of trunk roads; Said reaction bulb uses rubber plug 9 sealings that scribble glass cement, and into sour device is housed on the rubber plug.
Said to advance sour device be that sour device is advanced in separating funnel or special use, and it is the syringe that is with plastic tube on the sample introduction pipe that sour device is advanced in said special use.
Put into magnetic agitation 10 of 4.8cm in the said reaction bulb, again reaction bulb is put on the magnetic stirring apparatus 7.
The said Drexel bottle deionization deoxygenation high purity water of packing into, the NaOH that packs in the said gas absorption bottle, the reaction bulb deionization deoxygenation high purity water of packing into.
The method of application of described device specifically may further comprise the steps:
(1) water of packing in Bing Lian Drexel bottle and the reaction bulb, the NaOH solution of packing in the gas absorption bottle is opened nitrogen cylinder, feed nitrogen 4 ~ 6min after, stop logical nitrogen, get sediment sample, move into rapidly in the reaction bulb, logical again nitrogen 4 ~ 6min stops logical nitrogen; Get weigh back oven dry of sediment sample again from sampling just now, calculate its water percentage;
(2) add HC1 solution through advancing sour device, stir, earlier logical nitrogen 14 ~ 16min, gas speed is 80 ~ 100cm
3/ min stops logical nitrogen behind logical again nitrogen 4 ~ 6min, and gas speed is 240 ~ 260cm
3/ min;
(3) liquid in the gas absorption bottle is shifted out after, with water wash gas absorption bottle, detect cleansing solution and shift out the sulfide content in the liquid with methylene blue method, calculate the AVS value; Liquid in the reaction bulb is surveyed content of beary metal in the filtrating through membrane filtration with ICP, calculates SEM.
Said water is deionization deoxygenation high purity water.
The said sediment sample of getting preferably uses and gets the mud device.The said mud device of getting is the syringe that removes the sample introduction pipe.The sample introduction pipe connects the metal needle place for the syringe front end.
The gas speed of the said nitrogen of step (1) is 15L/h.
Said gas speed is the meter readings of every branch road.Said to advance sour device be that sour device is advanced in separating funnel or special use, and it is the syringe that is with plastic tube on the sample introduction pipe that sour device is advanced in said special use, and the rubber stopper of reaction bulb is installed with the hole, and the plastic tube long enough that sour device is advanced in special use can pass the hole and stretch in the reaction bulb.
The said Drexel bottle deionization deoxygenation high purity water of packing into is used to remove N
2Impurity, the NaOH that packs in the said gas absorption bottle is used for and H
2The S gas reaction.The reaction bulb deionization deoxygenation high purity water of packing into.The draft tube of Drexel bottle, reaction bulb and gas absorption bottle stretches into below the liquid level, and escape pipe is more than liquid level.
The said stirring of step (2) is to use the stirrer magnetic agitation of 4.8cm.The aperture of said filtering membrane is 0.45 μ m.
For realizing the present invention better:
In the above-mentioned steps (1), adopt the mode of a plurality of reactor parallel connections, can improve 2 ~ 4 times of finding speeds; For guaranteeing its degree of accuracy, need the testing fixture impermeability, most importantly:, gas meter also need be installed before each reactor to guarantee each reactor gas speed even one except in the trunk tracheae, installing the flowmeter.
Above-mentioned steps (2) adopts special use to advance sour device or separating funnel sample introduction, and reactor adopts rubber stopper seal (to keep good sealing effectiveness), influences measurement result for preventing the Determination of Trace Sulfur in the rubber plug, with glass cement coat with rubber plug surface.Special use is advanced sour device and is comprised syringe and plastic casing two parts; Utilize scale is arranged on the syringe; Before using the syringe part is separated with sleeve pipe; Port stretches under the liquid level; Slowly extract 20ml hydrochloric acid and (note not bringing into bubble; Operation skill is to extract excessive a little acid, depresses piston to 20ml scale place (with a small amount of bubble of forcing outbound port to exist) then gently, then sleeve pipe is connected with the syringe sampling pipe again.During reaction, depress piston, hydrochloric acid is from the sleeve opening injecting reactor.
Above-mentioned steps (3) adopts special use to get the mud device, to guarantee to accomplish at short notice sampling and sample introduction, avoids sediment to contact with air to greatest extent.To get mud device port and slowly insert in the sediment sample, pulling piston while inserting.Pull out gently then and get the mud device, hold port with plastic plate rapidly,, depress piston the sediment injecting reactor with port parallel with the reactor bottleneck (avoiding sediment to be bonded at a bottle wall).
Above-mentioned steps (4) adopts separating funnel or special use to advance sour device, avoids in advancing the HCl process, bringing O into
2
Above-mentioned steps (4) adopts lengthening magnetic agitation to stir, to shorten the reaction time; Suitable low in beginning stage of reaction gas speed, react and add atmosphere speed after more than half.
With high purity water wash-bottle wall, cleansing solution also changes volumetric flask in the above-mentioned steps (5), all changes volumetric flask over to guarantee the sulfide in the absorption liquid.
All mud mixtures should be filtered in the above-mentioned steps (6), when filtering, can not add high purity water or acid is washed.
Compared with prior art, the present invention has following beneficial effect:
(1) under the prerequisite that guarantees measuring accuracy, can effectively shorten the time, the Mean Time Measurement of single sample can shorten 3 ~ 4 times, makes the AVS and the SEM that accurately measure a large amount of sediment samples at short notice become possibility;
(2) in addition because at sediment and HCl sample introduction; Overall processes such as reactor sealing means, reaction alr mode, gas speed control system, absorption liquid and mud mixture processing have been taked a series of improvement; Make that the measurement operation of sediment AVS and SEM is more convenient, for its operation in enormous quantities continuously provides possibility.
Description of drawings
Fig. 1 AVS-SEM rapid measurement device figure (two reactor parallel connections, separating funnel advances HCl);
Fig. 2 AVS-SEM rapid measurement device figure (two reactor parallel connections, special use is advanced sour device and advanced HCl);
The mud device is got in Fig. 3 special use;
Fig. 4 reactor (separating funnel advances HCl);
Fig. 5 AVS-SEM rapid measurement device figure (four reactor parallel connections, special use is advanced sour device and advanced HCl);
Fig. 6 AVS-SEM rapid measurement device figure (four reactor parallel connections, separating funnel advances HCl);
Fig. 7 reactor (special use is advanced sour device and advanced HCl);
Sour device is advanced in Fig. 8 special use;
Wherein, 1. nitrogen cylinder 2. gas meters 4. Drexel bottles (interior dress high purity water) 6. reaction bulb 7. magnetic stirring apparatuss 8. advance sour device 9. rubber plugs 10. magnetic agitation 11. gas absorption bottles (interior dress 2%NaOH).
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is done further concrete description, but embodiment of the present invention is not limited thereto.
Like Fig. 1 and 2; The device of a kind of fast measuring sediment AVS and SEM; Comprise nitrogen cylinder 1, Drexel bottle 2 reaction bulbs 6 and gas absorption bottle 11; Drexel bottle 2, reaction bulb 6 and gas absorption bottle 11 with the pipeline series connection constitutes a branch road successively; Be connected to nitrogen cylinder after some the branch road parallel connections; Before the Drexel bottle 2 of every branch road gas meter 2 is installed, gas meter 2 is installed behind the nitrogen cylinder of trunk roads; Said reaction bulb uses rubber plug 9 sealings that scribble glass cement, and into sour device is housed on the rubber plug.
Said to advance sour device be that sour device is advanced in separating funnel or special use, and it is the syringe that is with plastic tube on the sample introduction pipe that sour device is advanced in said special use, so that the port of syringe stretches in the reaction bulb.
Said reaction bulb uses rubber plug 9 sealings that scribble glass cement.
Put into magnetic agitation 10 of 4.8cm in the said reaction bulb, again reaction bulb is put on the magnetic stirring apparatus 7.
The said Drexel bottle deionization deoxygenation high purity water of packing into is used to remove N
2Impurity, the NaOH that packs in the said gas absorption bottle is used for and H
2The S gas reaction.The reaction bulb deionization deoxygenation high purity water of packing into.The draft tube of Drexel bottle, reaction bulb and gas absorption bottle stretches into below the liquid level, and escape pipe is more than liquid level.
Assay method: connect experimental provision and check gas-tight property; Reactor partly adopts the mode of two branch road parallel connections; Add high purity water 100mL (institute's water is deionization deoxygenation high purity water in the measuring process) in the reaction bulb; Respectively add 70mL 2%NaOH solution in two gas absorption bottles, (gas speed is 250cm for 15L/h to the logical high purity nitrogen 5min of device
3/ min, following indication gas speed is the meter readings before the reactor).Getting the mud device is the syringe (like Fig. 3) that removes the sample introduction pipe.Get wet deposition matter sample 2 ~ 3g with getting the mud device, rapidly sample is moved in the reactor (like Fig. 4), logical nitrogen 5min (gas speed is 15L/h).Get 5 ~ 10g sediment (from the position of taking a sample just now) with getting the mud device in addition, its water percentage is calculated in the back oven dry of weighing.Stop the supple of gas or steam,, close the separating funnel piston rapidly with the HC1 solution of 20 milliliters of 6mol/L of separating funnel adding.Under the situation of magnetic agitation, (use the stirrer of 4.8cm, earlier with 6L/h (100cm
3/ min) the logical nitrogen 15min of speed is again with 15L/h (250cm
3/ min) the logical nitrogen 5min of speed.Stop the supple of gas or steam; Liquid in two gas absorption bottles is changed in the 100mL volumetric flask (with high purity water drip washing absorption bottle; Cleansing solution also changes in the volumetric flask), use GB methylene blue method (GB/T 16489-1996) to detect sulfide content wherein then, calculate the AVS value.Whole liquid in the reaction bulb are surveyed content of beary metal in the filtrating with 0.45 μ m membrane filtration with ICP, calculate SEM.
As illustrated in Figures 5 and 6, connect experimental provision and check gas-tight property, reactor partly adopts the mode of four branch road parallel connections, with the gas meter Control Flow.Add high purity water 100mL (institute's water is deionization deoxygenation high purity water in the test) in the reaction bulb, respectively add 70mL 2%NaOH solution in two gas absorption bottles, the logical high purity nitrogen 6min (gas speed is 15L/h) of device.Get wet deposition matter sample 2 ~ 3g with the special-purpose mud device of getting as shown in Figure 3, getting the mud device is the syringe that removes the sample introduction pipe, rapidly sample is moved in the reaction bulb among Fig. 7, logical nitrogen 6min (gas speed is 15L/h).Use plastics bale-out 2 ~ 3g sediment (from the position of taking a sample just now) in addition, its water percentage is calculated in the back oven dry of weighing.Stop the supple of gas or steam, advance HC1 solution that sour device (like Fig. 8) adds 20 milliliters of 6mol/L to reaction bulb (like Fig. 7) with special use.It is the syringe that is with plastic tube on the sample introduction pipe that sour device is advanced in said special use, so that the port of syringe stretches in the reaction bulb.Under the situation of magnetic agitation, (use the stirrer of 4.8cm), earlier with 6L/h (100cm
3/ min) the logical nitrogen 16min of speed is again with the logical nitrogen 6min of the speed of 15L/h.Stop the supple of gas or steam; Liquid in two gas absorption bottles is changed in the 100mL volumetric flask (with high purity water drip washing absorption bottle; Cleansing solution also changes in the volumetric flask), use GB methylene blue method (GB/T 16489-1996) to detect sulfide content wherein then, calculate the AVS value.Whole liquid in the reaction bulb are surveyed content of beary metal in the filtrating with 0.45 μ m membrane filtration with ICP, calculate SEM.
Claims (9)
1. the device of fast measuring sediment AVS and SEM; It is characterized in that; Comprise nitrogen cylinder (1), Drexel bottle (2) reaction bulb (6) and gas absorption bottle (11); Drexel bottle (2), reaction bulb (6) and gas absorption bottle (11) with the pipeline series connection constitutes a branch road successively; Be connected to nitrogen cylinder after some the branch road parallel connections; The preceding gas meter (2) that is equipped with of the Drexel bottle of every branch road (2) is equipped with gas meter (2) behind the nitrogen cylinder of trunk roads; Said reaction bulb uses rubber plug (9) sealing that scribbles glass cement, and into sour device is housed on the rubber plug.
2. device according to claim 1 is characterized in that, said to advance sour device be that sour device is advanced in separating funnel or special use, and it is the syringe that is with plastic tube on the sample introduction pipe that sour device is advanced in said special use.
3. device according to claim 1 and 2 is characterized in that, puts into magnetic agitation (10) of 4.8cm in the said reaction bulb, reaction bulb is put on the magnetic stirring apparatus (7) again.
4. device according to claim 3 is characterized in that, the said Drexel bottle deionization deoxygenation high purity water of packing into, the NaOH that packs in the said gas absorption bottle, the reaction bulb deionization deoxygenation high purity water of packing into.
5. the method for application of the described device of claim 2 specifically may further comprise the steps:
(1) water of packing in Bing Lian Drexel bottle and the reaction bulb, the NaOH solution of packing in the gas absorption bottle is opened nitrogen cylinder, feed nitrogen 4 ~ 6min after, stop logical nitrogen, get sediment sample, move into rapidly in the reaction bulb, logical again nitrogen 4 ~ 6min stops logical nitrogen; Get weigh back oven dry of sediment sample again from sampling just now, calculate its water percentage;
(2) add HC1 solution through advancing sour device, stir, earlier logical nitrogen 14 ~ 16min, gas speed is 80 ~ 100cm
3/ min stops logical nitrogen behind logical again nitrogen 4 ~ 6min, and gas speed is 240 ~ 260cm
3/ min;
(3) liquid in the gas absorption bottle is shifted out after, with water wash gas absorption bottle, detect cleansing solution and shift out the sulfide content in the liquid with methylene blue method, calculate the AVS value; Liquid in the reaction bulb is surveyed content of beary metal in the filtrating through membrane filtration with ICP, calculates SEM.
6. method according to claim 5 is characterized in that, said water is deionization deoxygenation high purity water.
7. method according to claim 6 is characterized in that, the gas speed of the said nitrogen of step (1) is 15L/h.
8. method according to claim 7 is characterized in that said gas speed is the meter readings of every branch road.
9. method according to claim 8 is characterized in that, the said sediment sample of getting uses and to get the mud device.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103335874A (en) * | 2013-06-14 | 2013-10-02 | 宁波大学 | Constant-pressure inner loop acidification blowing absorption device |
| CN103454233A (en) * | 2013-09-11 | 2013-12-18 | 浙江中一检测研究院股份有限公司 | Method for measuring sulfide in environment |
| CN104749002A (en) * | 2013-12-30 | 2015-07-01 | 中国科学院烟台海岸带研究所 | Device for extraction of volatile substances in water body and sediments |
| 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) |
| CN105486569A (en) * | 2015-12-09 | 2016-04-13 | 华东师范大学 | Experimental apparatus for continuous extraction of various forms of sulfur in sediment sample |
| CN110208062A (en) * | 2019-06-26 | 2019-09-06 | 核工业北京地质研究院 | Multichannel extraction element and method for pyritic sulfur in rock, pedotheque |
| 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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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103335874A (en) * | 2013-06-14 | 2013-10-02 | 宁波大学 | Constant-pressure inner loop acidification blowing absorption device |
| CN103335874B (en) * | 2013-06-14 | 2015-06-17 | 宁波大学 | Constant-pressure inner loop acidification blowing absorption device |
| CN103454233A (en) * | 2013-09-11 | 2013-12-18 | 浙江中一检测研究院股份有限公司 | Method for measuring sulfide in environment |
| CN104749002A (en) * | 2013-12-30 | 2015-07-01 | 中国科学院烟台海岸带研究所 | Device for extraction of volatile substances in water body and sediments |
| 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 |
| CN105486569A (en) * | 2015-12-09 | 2016-04-13 | 华东师范大学 | Experimental apparatus for continuous extraction of various forms of sulfur in sediment sample |
| CN110208062A (en) * | 2019-06-26 | 2019-09-06 | 核工业北京地质研究院 | Multichannel extraction element and method for pyritic sulfur in rock, pedotheque |
| CN110208062B (en) * | 2019-06-26 | 2024-07-16 | 核工业北京地质研究院 | Multichannel extraction device and method for pyrite sulfur in rock and soil samples |
| 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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Application publication date: 20120215 |