CN102841174A - Method for analyzing reductive inorganic sulfur in deposit sediment - Google Patents
Method for analyzing reductive inorganic sulfur in deposit sediment Download PDFInfo
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- CN102841174A CN102841174A CN 201110174338 CN201110174338A CN102841174A CN 102841174 A CN102841174 A CN 102841174A CN 201110174338 CN201110174338 CN 201110174338 CN 201110174338 A CN201110174338 A CN 201110174338A CN 102841174 A CN102841174 A CN 102841174A
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Abstract
The invention discloses a method for analyzing reductive inorganic sulfur in deposit sediment. The method comprises the steps of: placing alkaline zinc acetate in a small opened container I, and then placing the small opened container I in a large opened container; placing the deposit sediment in the large container; adding hydrogen chloride and ascorbic acid for reaction for 18-24 hours; taking out the small opened container I to test sulfur content; placing the alkaline zinc acetate in a small opened container II, and then placing the small opened container II in the large container; adding a Cr II solution for reaction for 48-54 hours; taking out the small opened container II to test sulfur content; further placing the alkaline zinc acetate in a small opened container III, and then placing the small opened container III in the large container; and adding N,N-dimethylformamide, the Cr II solution and the hydrogen chloride solution for reaction for 24-36 hours; taking out the small opened container III to test sulfur content. According to the method for analyzing reductive inorganic sulfur in deposit sediment provided by the invention, the reductive inorganic sulfur in deposit sediment can be quickly and continuously analyzed effectively, so that the method is simple and the data is accurate.
Description
Technical field
The present invention relates to a kind of analytical approach of sulphur, relate in particular to the analytical approach of reducing inorganic sulphur in a kind of sediment.
Background technology
Sulphur is one of most widespread element in the earth's crust.Occurring in nature sulphur exist form varied, migration between the sulphur of various forms transforms, and is very sensitive to environmental baseline, the circulation of sulphur biomass geochemistry has vital role to global environmental change.Sulphur is again one of main chemical composition of seawater, and the biogeochemical reaction of sulphur in the oceanic sediment diagenetic process and circulation have caused the Historical Evolution of the redox environment of earth surface, have directly influenced the marine biogeochemistry circulation.Sea, the land effect of estuary coast area is strong, is the important response and the indication area of global environmental change and regional environment problem.Therefore, the circulation of the biomass geochemistry of the sulphur in the coastal zone ecosystem always is the focus that people pay close attention to.
The mesolittoral zone is the exchange area between ocean and land, between conversion and ocean and the land, has formed sediment-water, multiple interface such as sediment-atmosphere.The distinctive redox environment in mesolittoral zone has formed the special transform mode of sediment, and simultaneously, in effect such as rainwash, morning and evening tides down, the migration of intertidalite conversion is different from soil and river, marine bottom sediment.
At present, the research of sulphur is main with reducing inorganic sulphur (being called for short RIS) mostly in the sediment, and reducing inorganic sulphur mainly is divided three classes: sour volatile sulfide (being called for short AVS), chromium reduced sulphur (being called for short CRS) and elementary sulfur (being called for short ES).The reducing inorganic sulphur of these three kinds of forms is most active parts of sulphur in the sediment, and the geochemical behavior of the iron in the sediment, phosphorus and heavy metal is played control action.
Sediment in the DIFFERENT DEPOSITIONAL ENVIRONMENTS and follow the sulfide that buries, their relative abundance and reallocation are the decision flat key factors of atmosphere oxygenated water in the past.Therefore the analytical approach to reducing inorganic sulphur in the sediment just seems extremely important.
Summary of the invention
Technical matters to be solved by this invention provides the analytical approach of reducing inorganic sulphur in a kind of sediment.
The present invention seeks to realize through following technical scheme:
The analytical approach of reducing inorganic sulphur in a kind of sediment, form by following step:
(1) alkaline zinc acetate solution is placed a little open containers; Should place a bulk container by little open containers again; Get sediment sample and place this bulk container; In this bulk container, add hydrogen chloride solution and ascorbic acid solution; Reaction is 18-24 hour under the room temperature; From bulk container, take out this little open containers of alkaline zinc acetate solution is housed,, be the content of sour volatile sulfide in the deposit with the content of sulphur in the little open containers of iodometric determination;
(2) alkaline zinc acetate solution is placed another little open containers; Again this another little open containers is placed this bulk container; Add Cr II solution; Reaction is 48-54 hour under the room temperature; From bulk container, take out this another little open containers of alkaline zinc acetate solution is housed; With the content of sulphur in the little open containers of iodometric determination this another, be the content of chromium reduced sulphur in the deposit;
(3) alkaline zinc acetate solution is placed a little open containers again; Again with this a littler open containers place this bulk container; Add N; Dinethylformamide, Cr II solution and hydrogen chloride solution; Reaction is 24-36 hour under the room temperature; From bulk container, take out this little open containers again of alkaline zinc acetate solution is housed,, be the content of elementary sulfur in the deposit with this content of sulphur in little open containers again of iodometric determination;
Above-mentioned each step is all accomplished in airtight protective cover under nitrogen carrier gas condition.
The analytical approach of reducing inorganic sulphur in the sediment of the present invention can in extremely rapid succession effectively be analyzed sour volatile sulphur, chromium reduced sulphur and elementary sulfur in the sediment, and method is simple, and test data is accurate.
Embodiment
Below in conjunction with embodiment the present invention is further described.
In the laboratory; The freezing sediment sample of part is thawed under room temperature; Dry being lower than under 40 ℃ of conditions then, grind evenly, the sample segment usefulness of sealing bag of packing in order to sreen analysis with quartzy mortar; Remaining sample is crossed 100 orders (0.154mm) nylon mesh screen, and the sample after sieving is packed in the sealing bag in order to analyzing.
The analysis of reduction inorganic sulfur in the sediment:
Get freezing sediment sample, adopt cold three step of diffusion extraction method to measure wherein sour volatile sulphur, chromium reduced sulphur and elementary sulfur, adopt iodometric determination sulphur, whole leaching process is operation completion in airtight protective cover under nitrogen carrier gas condition, and concrete steps are:
(1) prepares: get fresh sediment sample 5-10g, put into the 250ml glass flask, put into the small beaker that 15ml alkalescence zinc acetate solution (logical nitrogen deoxidation) is housed simultaneously, cover the logical nitrogen deoxidation 30s of bottle stopper; For preventing S2-, in sediment, add 1mol/L ascorbic acid solution 2ml by the Fe3+ oxidation;
(2) sour volatilizable sulphur (AVS) separates: with stopcock injection 6mol/L anaerobic hydrogen chloride 15ml and the 1mol/L ascorbic acid solution 2ml of 20ml syringe by mouth of pipe B, reactor flask placed under the room temperature react 18h; The beaker of Alkaline Zinc solution is equipped with in taking-up, and with the iodometric determination content of sulphur wherein, the sulphur that records is AVS, puts into the small beaker that another contains 15ml Alkaline Zinc solution fast simultaneously, and bottle stopper is towards nitrogen 30s beyond the Great Wall;
(3) chromium reduced sulphur (CRS) separates: inhale 15mlCr (II) solution in reaction bulb, react 48h under the room temperature; The beaker of Alkaline Zinc solution is equipped with in taking-up, and with the iodometric determination content of sulphur wherein, the sulphur that records is CRS;
(4) elementary sulfur (ES) separates: pour 20mlN in the reaction bulb into, dinethylformamide (being called for short DMF) is put into Alkaline Zinc solution bottle, towards nitrogen 30s, injects 5mlCr (II) solution and 5ml concentrated hydrochloric acid, reacts 24h under the room temperature; The beaker of Alkaline Zinc solution is equipped with in taking-up, and with the iodometric determination content of sulphur wherein, the sulphur that records is ES.
Wherein, said Cr (II) solution can adopt following method to prepare: add 104gCrCl
36H
2O and 60gZn (Hg) arrive 200mL0.2N HCl, the 500mL conical flask of packing into, and the diplopore rubber plug leads to nitrogen 10min beyond the Great Wall, shuts cock and slightly shakes 3 hours, can make.
The analytical approach of reducing inorganic sulphur in the sediment of the present invention can in extremely rapid succession effectively be analyzed sour volatile sulphur, chromium reduced sulphur and elementary sulfur in the sediment, and method is simple, and test data is accurate.
The present invention is to the separation and Extraction of the sulphur of the sour volatile sulfide, chromium reduced sulphur and these the three kinds of forms of elementary sulfur that exist in the sediment; It mainly is difference according to its physicochemical property; Utilize different chemical reagent respectively different sulfur chemistries to be extracted mutually or change into the sulfuretted hydrogen form, reach the purpose of separating or extracting.
Major advantage of the present invention mainly can be summarized as following 3 points:
1) needed experimental apparatus and equipment are simple and easy to, and experimental implementation is also simpler and easy, particularly when handling a large amount of sample;
2) after AVS is extracted, CRS diffusion extraction method will only can be extracted the FeS2 in the sediment, and selectivity is strong;
3) ES can directly spread extraction in the step in the end and not need extra dissolution extraction process.
Claims (1)
1. the analytical approach of reducing inorganic sulphur in the sediment is characterized in that, is made up of following step:
(1) alkaline zinc acetate solution is placed a little open containers; Should place a bulk container by little open containers again; Get sediment sample and place this bulk container; In this bulk container, add hydrogen chloride solution and ascorbic acid solution; Reaction is 18-24 hour under the room temperature; From bulk container, take out this little open containers of alkaline zinc acetate solution is housed,, be the content of sour volatile sulfide in the deposit with the content of sulphur in the little open containers of iodometric determination;
(2) alkaline zinc acetate solution is placed another little open containers; Again this another little open containers is placed this bulk container; Add CrII solution; Reaction is 48-54 hour under the room temperature; From bulk container, take out this another little open containers of alkaline zinc acetate solution is housed; With the content of sulphur in the little open containers of iodometric determination this another, be the content of chromium reduced sulphur in the deposit;
(3) alkaline zinc acetate solution is placed a little open containers again; Again with this a littler open containers place this bulk container; Add N; Dinethylformamide, Cr II solution and hydrogen chloride solution; Reaction is 24-36 hour under the room temperature; From bulk container, take out this little open containers again of alkaline zinc acetate solution is housed,, be the content of elementary sulfur in the deposit with this content of sulphur in little open containers again of iodometric determination;
Above-mentioned each step is all accomplished in airtight protective cover under nitrogen carrier gas condition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110174338 CN102841174A (en) | 2011-06-24 | 2011-06-24 | Method for analyzing reductive inorganic sulfur in deposit sediment |
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| CN 201110174338 CN102841174A (en) | 2011-06-24 | 2011-06-24 | Method for analyzing reductive inorganic sulfur in deposit sediment |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113219126A (en) * | 2021-04-20 | 2021-08-06 | 华南理工大学 | Separation and extraction method and application of sulfur in metal sulfide |
-
2011
- 2011-06-24 CN CN 201110174338 patent/CN102841174A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113219126A (en) * | 2021-04-20 | 2021-08-06 | 华南理工大学 | Separation and extraction method and application of sulfur in metal sulfide |
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Application publication date: 20121226 |