CN1103447C - Process for extracting alkyl nercury and phenyl mercury from coal and evaluating them - Google Patents
Process for extracting alkyl nercury and phenyl mercury from coal and evaluating them Download PDFInfo
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- CN1103447C CN1103447C CN 98119019 CN98119019A CN1103447C CN 1103447 C CN1103447 C CN 1103447C CN 98119019 CN98119019 CN 98119019 CN 98119019 A CN98119019 A CN 98119019A CN 1103447 C CN1103447 C CN 1103447C
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Abstract
The present invention relates to a technique for extracting and measuring alkyl nercury and phenyl mercury from coal, which controls the extraction quantity of alkyl mercury and phenyl mercury by regulating hydrochloric acidity and extraction time and temperature. Under an acid condition, the present invention uses potassium hypermanganate to oxidize organic mercury into inorganic mercury and then uses stannous chloride for reduction without using hypertoxic cadmium chloride. The method for investigating and monitoring alkyl mercury and phenyl mercury in coal has important application values for reducing environmental pollution and protecting ecological environment.
Description
One, technical field: the technology of extracting, measure alkyl mercury and phenyl mercury from coal is an analysis and testing technology.
Two, background technology: the existing technology of measuring organic mercury in fresh water, seawater, fish tissue, animal viscera, soil, the sediment (also have and claim alkyl mercury and phenyl mercury), but these technology are not suitable for the coal sample.Organomercurial technology in technology that connect most with the present invention, near prior art is methyl mercury in mensuration sediment and the soil and the mensuration fish tissue.Wherein the pretreatment technology of sediment and pedotheque pre-treatment and this application is approaching, and in the fish tissue in organic mercury determination technology and this application assay method be close.
Sample pre-treatments: take by weighing that 2-10 restrains air-dry sediment and pedotheque (60-80 order) adds 15-30 milliliter 1mol/L hydrochloric acid in centrifuge tube, stir evenly.Place a moment, after treating bubble collapse, add 1 milliliter of 1% copper-bath, fully stir, placed 10 minutes, centrifugal 10 minutes, clarified solution is transferred to beaker, be adjusted to pH=3 with 6mol/L NaOH and 1mol/L hydrochloric acid, placed about 10 minutes, if there is sediment to separate out, then use the fast qualitative filter paper filtering, filtrate is collected in 125 milliliters the separating funnel.The separating funnel lower end is connected with sulfhydryl cotton pipe with emulsion tube, makes solution pass through sulfhydryl cotton pipe with the flow velocity of 5-10 ml/min, treats that solution flows to end, and blows off moisture in the sulfhydryl cotton pipe with ear washing bulb.Take off sulfhydryl cotton pipe, its lower end is put into surveyed the mercury reaction bulb, be added in the sulfhydryl cotton pipe, allow it from Sulfhydryl Cotton, flow through naturally with 2 milliliters of branch secondaries of 2N hydrochloric acid.Purge raffinate with ear washing bulb at every turn.
Organomercurial mensuration: the reaction bulb that will contain the organic mercury eluent is put into frozen water and is cooled off, the water that adds 3 milliliters, add 1 milliliter of 0.1% cadmium chloride solution along the bottle wall successively, 6 milliliters of 6mol/L sodium hydroxide solutions, 1 milliliter 0.1% stannous chloride solution takes out reaction bulb from water-bath, at room temperature placed 10 minutes, the air that mercuryvapour is contained on reaction bulb top with the water filling degassing method pushes in the absorption tube of mercury vapor analyzer, reads the maximum absorbance value, checks in mercury content from typical curve.See " analysis of environmental pollution analytical approach first volume inorganics " P159-170 for details: Beijing Science Press, 1987.
Purpose of the present invention: alkyl mercury and phenyl mercury are the environmental contaminants with serious bio-toxicity.Methyl mercury in the alkyl mercury is the strongest to people and mammalian toxicity, and minamata disease is exactly a methylmercuric poisoning disease.Alkyl mercury in the coal and phenyl mercury can enter atmosphere, soil and water body by burning in the coal, and the mankind are worked the mischief.Extracting, measure alkyl mercury and phenyl mercury technology from coal provides the means of alkyl mercury and phenyl mercury in research and the monitoring coal, and for alleviating environmental pollution, the important use of having preserved the ecological environment is worth.This invention has been set up the new technology that is fit to extract, measure alkyl mercury and phenyl mercury from coal, simultaneously, shortcoming in existing organic mercury (containing alkyl mercury and the phenyl mercury) determination techniques is corrected.
Three, summary of the invention:
Reagent preparation: 1. hydrochloric acid solution: get high purity hydrochloric acid, be mixed with the concentration that needs with redistilled water.
2.1% copper-bath: get the preparation of analytical pure sulfuric acid copper.
3.6mol/L NaOH: get the preparation of top grade pure cerium hydroxide sodium.
4.20% stannous chloride takes by weighing 20 gram top grade pure cerium hydroxide tin, is dissolved in 10 milliliters of hydrochloric acid,
Be diluted to 100ml, the logical nitrogen removal of mercury 30 minutes is standby.
5. Sulfhydryl Cotton: in 200 ml beakers, add 50 milliliters and analyze bright sulfurs for glycollic acid, 35 ml acetic anhydride, 16 milliliter of 36% acetate, 0.15 the milliliter concentrated sulphuric acid and 5 ml distilled waters, mixing, change over to after the cooling in the wide-necked bottle of 250 milliliters of tool grounds, put into 15 gram absorbent cotton in the bottle, cotton is all immersed in the solution, beyond the Great Wall bottle stopper, in 38 ℃ of-40 ℃ of baking ovens, place after 2-3 days, with distilled water cotton is washed till neutrality, removes moisture, spread on porcelain dish, put into 38 ℃ of-40 ℃ of baking ovens again and dry, it is standby to place brown port grinding bottle to preserve.
Instrument and equipment: mercury vapor analyzer, 125 milliliters of separating funnels, 150 milliliters of conical flasks.
Reaction bulb: capacity has scale for 30 milliliters or 100 milliliters, has the glass narrow-mouthed bottle of rubber stopper.
Sulfhydryl cotton pipe, internal diameter 6-8 millimeter, long 100-120 millimeter glass tube, one holds level with both hands together, and an end pulls into the sharp mouth of 2 millimeters of internal diameters, and sharp mouth portion is about 20 millimeters.Pack at every turn 0.10 the gram Sulfhydryl Cotton, above the filling a little absorbent cotton.
From coal, extract alkyl mercury and phenyl mercury:
Coal is levigate to the granularity of crossing 80 mesh sieves, accurately take by weighing 2-10 gram coal, put into conical flask, add hydrochloric acid and 1 milliliter of 1% copper-bath of 10-30 milliliter 6mol/L-12mol/L, shake up, bottleneck is put a little funnel, under 30 ℃ of-40 ℃ of constant temperature lixiviate 12-20 hour, use the fast quantification filter paper filtering, filtrate is collected in another conical flask, with the hydrochloric acid solution drip washing coal sample of 10 milliliters of 4mol/L, and soak coal conical flask funnel and filter paper with 1mol/L hydrochloric acid flushing.
The mensuration of alkyl mercury and phenyl mercury: regulate the pH=3.0-3.5 of filtrate with the sodium hydroxide solution of 4mol/L-10mol/L and the hydrochloric acid solution of 2mol/L-4mol/L, place a moment, generally there is precipitation to separate out, filter with the middling speed quantitative filter paper, filtrate is collected in the separating funnel, the separating funnel lower end is connected with sulfhydryl cotton pipe with emulsion tube, the 0.1 gram Sulfhydryl Cotton of packing in the pipe, allow solution with the flow velocity of 5-10 ml/min by sulfhydryl cotton pipe, after solution flows to end, take off sulfhydryl cotton pipe, with ear washing bulb remaining solution on the Sulfhydryl Cotton is blown to the greatest extent, reaction bulb is put in sulfydryl pipe lower end, 3 milliliters of the hydrochloric acid solutions of usefulness 2mol/L, divide and add for three times in the sulfhydryl cotton pipe, after treating under the hydrochloric acid spontaneous current, blow out residue hydrochloric acid at every turn, in eluent, add 1: 1 sulfuric acid with ear washing bulb, making in the reaction bulb final acidity is 1.8mol/L, adds 10-15 milliliter 4%KMnO
4Solution, placed under 30 ℃ of-40 ℃ of temperature 0.5 hour, and dripped 10% hydrochloric acid amine aqueous solution to potassium permanganate and take off red and excessive one, it is fixed molten to 50 milliliters or 15 milliliters (reaction bulb volume 1/2) to add water, add 2-4 milliliter 20% stannous chloride, jump a queue, vibrated 3-5 minute, placed 5-10 minute, extract gas in 10 milliliters of reaction bulbs with syringe, inject the mercury vapor analyzer absorption tube, read the maximum absorbance value, look into the calculation mercury content from typical curve.
The present invention has following advantage than prior art:
1. original technology use 2mol the hydrochloric acid of L cook leaching liquor because the coal quality is hard, tight, the carbon content height, original technology can only lixiviate goes out the alkyl mercury and the phenyl mercury of less than 10% (16 hours, 30 ℃), so be not suitable for the coal sample.Present technique then can lixiviate go out whole alkyl mercury of coal and phenyl mercury.See Fig. 1.
2. the prior art extraction time had only about 0.5 hour, and extraction time of the present invention is 12-20 hour, and the leaching amount of alkyl mercury and phenyl mercury obviously raises.See Fig. 2.
3. do not control temperature during the prior art lixiviate, thereby the lixiviate result understands temperature influence and produce fluctuation, the present invention controls extraction temperature, can obtain stable effect, make data have comparability.See Fig. 3, the highest 30-40 ℃ of leaching amount.
4. prior art under sodium hydroxide medium, is made catalyzer with caddy when measuring alkyl mercury and phenyl mercury total amount (title organic mercury), reduces organic mercury with stannous chloride, and wherein caddy is extremely toxic substance (can cause itai-itai).The present invention with reducing with stannous chloride behind the potassium permanganate oxidation organic mercury, has avoided the use caddy under acid condition.
Four, description of drawings: the relation of Fig. 1 alkyl mercury and phenyl mercury leaching amount and acidity,
The relation of Fig. 2 alkyl mercury and phenyl mercury leaching amount and extraction time,
The relation of Fig. 3 alkyl mercury and phenyl mercury and temperature
Five, embodiment:
1. from coal, extract alkyl mercury and phenyl mercury
Coal is levigate to crossing 80 mesh sieves, accurately take by weighing 10.00 gram coals, put into 150 milliliters of conical flasks, top grade pure hydrochloric acid and 1 milliliter of 1% copper-bath of adding 30 milliliters of 8mol/L shake all, and bottleneck is put a little funnel, lixiviate is 16 hours under 30 ℃ of temperature, use the fast quantification filter paper filtering, filtrate is collected in another conical flask, with the hydrochloric acid solution drip washing coal sample of 10 milliliters of 5mol/L, and with hydrochloric acid flushing conical flask, funnel and the filter paper of 1mol/L.
2. the mensuration of alkyl mercury and phenyl mercury: regulate the pH=3 of filtrate with the sodium hydroxide solution of 4mol/L and the hydrochloric acid solution of 2mol/L, place a moment, generally there is precipitation to separate out, filter with the middling speed quantitative filter paper, filtrate is collected in 125 milliliters of separating funnels, the separating funnel lower end is connected with sulfhydryl cotton pipe with emulsion tube, the 0.1 gram Sulfhydryl Cotton of packing in the pipe, allow solution with the flow velocity of 5 ml/min by sulfhydryl cotton pipe, after solution flows to end, take off sulfhydryl cotton pipe, with ear washing bulb remaining solution on the Sulfhydryl Cotton is blown to the greatest extent, the 100ml reaction bulb is put in the sulfhydryl cotton pipe lower end, 3 milliliters of the hydrochloric acid solutions of usefulness 2mol/L, divide and add for three times in the sulfhydryl cotton pipe, after treating under the hydrochloric acid spontaneous current, blow out residue hydrochloric acid at every turn, in eluent, add 1: 1 sulfuric acid with ear washing bulb, making in the reaction bulb final acidity is 1.8mol/L, adds 10 milliliters of 4%KMnO
4Solution, placed 0.5 hour under 30 ℃ of temperature, drip 10% oxammonium hydrochloride solution to potassium permanganate and take off red and excessive one, it is fixed molten to 50 milliliters to add water, add 2 milliliter of 20% stannous chloride, jump a queue, vibrated 3 minutes, placed 5 minutes, extract gas in 10 milliliters of reaction bulbs with syringe, inject the mercury vapor analyzer absorption tube, read the maximum absorbance value, look into the calculation mercury content from typical curve.
Claims (1)
1. from coal, extract, measure the technology of alkyl mercury and phenyl mercury, it is characterized in that extraction time and temperature are controlled the leaching amount of alkyl mercury and phenyl mercury by regulating the acidity of hydrochloric acid,
A. from coal, extract alkyl mercury and phenyl mercury:
Coal is levigate to the granularity of crossing 80 mesh sieves, accurately take by weighing 2-10 gram coal, put into conical flask, add hydrochloric acid and 1 milliliter of 1% copper-bath of 10-30 milliliter 6mol/L-12mol/L, shake up, bottleneck is put a little funnel, under 30 ℃ of-40 ℃ of constant temperature lixiviate 12-20 hour, use the fast quantification filter paper filtering,, and soak coal conical flask, funnel and filter paper with the flushing of the hydrochloric acid of 1mol/L with 10 milliliters of 4mol/L hydrochloric acid solution drip washing coal samples;
B. the mensuration of alkyl mercury and phenyl mercury total amount: regulate the pH=3.0-3.5 of filtrate with the sodium hydroxide solution of 4mol/L-10mol/L and the hydrochloric acid solution of 2mol/L-4mol/L, place a moment, generally there is precipitation to separate out, filter with the middling speed quantitative filter paper, filtrate is collected in the separating funnel, the separating funnel lower end is connected with sulfhydryl cotton pipe with emulsion tube, pack in the pipe 0.1 the gram Sulfhydryl Cotton, allow solution pass through sulfhydryl cotton pipe with the flow velocity of 5-10 ml/min, after solution flows to end, take off sulfhydryl cotton pipe, with ear washing bulb remaining solution on the Sulfhydryl Cotton is blown to the greatest extent, reaction bulb is put in sulfydryl pipe lower end, 3 milliliters of the hydrochloric acid solutions of usefulness 2mol/L, divide and add for three times in the sulfhydryl cotton pipe, after treating under the hydrochloric acid spontaneous current, blow out residue hydrochloric acid at every turn, in eluent, add 1: 1 sulfuric acid with ear washing bulb, making in the reaction bulb final acidity is 1.8mol/L, adds 10-15 milliliter 4%KMnO
4Solution, placed under 30 ℃ of-40 ℃ of temperature 0.5 hour, and dripped 10% oxammonium hydrochloride solution to potassium permanganate and take off red and excessive one, it is fixed molten to 50 milliliters or 15 milliliters (reaction bulb volume 1/2) to add water, add 2-4 milliliter 20% stannous chloride, jump a queue, vibrated 3-5 minute, placed 5-10 minute, extract gas in 10 milliliters of reaction bulbs with syringe, inject the mercury vapor analyzer absorption tube, read the maximum absorbance value, look into the calculation mercury content from typical curve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 98119019 CN1103447C (en) | 1998-09-25 | 1998-09-25 | Process for extracting alkyl nercury and phenyl mercury from coal and evaluating them |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 98119019 CN1103447C (en) | 1998-09-25 | 1998-09-25 | Process for extracting alkyl nercury and phenyl mercury from coal and evaluating them |
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| CN1249429A CN1249429A (en) | 2000-04-05 |
| CN1103447C true CN1103447C (en) | 2003-03-19 |
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| CN101839900B (en) * | 2010-05-19 | 2011-05-04 | 重庆大学 | Detection method of mercury content in burning coal |
| CN112326569A (en) * | 2020-10-21 | 2021-02-05 | 内蒙古国城实业有限公司 | Method for rapidly detecting molybdenum oxide minerals in molybdenum ore |
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