CN105973819A - Method for determining concentration of phosphate in high-concentration hydrogen sulfide hot liquid - Google Patents
Method for determining concentration of phosphate in high-concentration hydrogen sulfide hot liquid Download PDFInfo
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Abstract
The invention relates to a method for determining the concentration of phosphate in a high-concentration hydrogen sulfide hot liquid. The concentration of sulfur ions in a water sample of the hot liquid is determined by a sulfur ion selective electrode, and the sulfur ions are removed by a precipitation method. The method comprises the steps: firstly, preparing a sulfur ion-containing phosphate standard solution, adjusting the pH, making the pH of the phosphate-sulfur ion standard solution be 5.00-6.00, adding a precipitant zinc sulfate solution, making the sulfur ions form a zinc sulfide precipitate, aging for several hours, filtering, discarding the precipitate, and taking the filtrate for standby application; using a phosphomolybdenum blue spectrophotometric method, determining the absorbance of the filtrate at the wavelength of 880 nm, and drawing a phosphate-sulfur ion standard curve; and under the same conditions, measuring the absorbance of the water sample of the high-concentration hydrogen sulfide hot liquid, and calculating the concentration of phosphate in the water sample of the high-concentration hydrogen sulfide hot liquid from the phosphate-sulfur ion standard curve. The method is simple to operate, the determination trouble caused by easy oxidization of the sulfur ions can be avoided, the result is more accurate, and the reliability of analysis and determination of the content of phosphate in the hot liquid is improved.
Description
Technical field
The present invention is Marine Sciences nutritive salt analysis fields, relates to a kind of containing phosphoric acid in high-concentration hydrogen sulfide hydrothermal solution
The assay method of salinity.
Background technology
Nutritive salt is composition necessary to marine phytoplankton growth and breeding, is also primary productivity of marine ecosystem and food
The basis of chain, phosphatic content and distribution have important impact to marine biogeochemistry process.At present
Phosphate classics assay method the most commonly used in marine monitoring specification is P-Mo blue spectrophotography, and it is applicable to
The analysis of the general sea water not interfered with measures.At present, in ocean, hydrothermal vent is all over the world, studies hydrothermal solution
In nutritive salt particularly necessary, and phosphate is an important component part in nutritive salt.But hydrothermal solution contains
Having high concentration sulphion, the sulphion in hydrothermal solution water sample is easily oxidized again becomes sulfur simple substance, the sulfur list of precipitation
Matter will have a strong impact on the accuracy of P-Mo blue spectrophotography, therefore explores one and is suitable for high-concentration hydrogen sulfide hydrothermal solution
In water sample, phosphatic Accurate Determining analyzes method, and to Marine Sciences, worker has great importance.
The most relatively conventional method of the sulphion of higher concentration in sea water that removes has oxidizing process and acidization.Its
Middle oxidizing process is that in the sea water of acidifying after addition excess bromine water, sulphion is oxidized into sulfur simple substance, by sulfur list
Matter filters, and is passed through the bromine of air removing excess, but bromine is difficult to be divided, and the bromine not eliminated directly affects phosphorus
Chromogenic reaction in molybdenum blue spectrophotometric method, and the method operation complexity；Acidization be by sea water be acidified after,
Then passing to high pure nitrogen and remove hydrogen sulfide gas, the shortcoming of the method is to be completely removed by hydrogen sulfide.
The present invention is to use the sedimentation method to remove sulphion, it is provided that phosphatic in a kind of hydrothermal solution containing sulphion
Accurately analyze method, it is adaptable to measuring the sulfur-containing anion concentration hydrothermal solution in 50～700 μm ol/L, the method is compared
In conventional common phosphate determination method, capacity of resisting disturbance is strong, and its result is more accurate, improves in hydrothermal solution
The reliability that phosphate content measures.
Summary of the invention
Present invention aim at providing a kind of accuracy good, phosphoric acid in the hydrothermal solution of the high concentration sulphion that controllability is strong
The analysis method of salt.
The assay method of phosphate concn in a kind of high-concentration hydrogen sulfide hydrothermal solution, step is as follows: utilize sulphion to select
The concentration of sulphion in selecting property determination of electrode high-concentration hydrogen sulfide to be measured hydrothermal solution water sample；Preparation phosphate-sulphion
Standard solution, makes the concentration of sulphion in standard solution essentially identical with detected water sample；The standard that regulation is prepared
The pH=5.00～6.00 of solution, adds 0.5～1.0mol/L zinc sulfate of standard solution volume 1/180～1/18mL
Solution, generates zinc sulfide precipitation, is aged 1～24h after reaction, the micropore using aperture to be 0.22～0.45 μm is fine
Dimension membrane filtration, discards precipitation, uses P-Mo blue spectrophotography, measures filtrate suction under 880nm wavelength
Luminosity, draws standard curve；Standard solution is replaced to high-concentration hydrogen sulfide hydrothermal solution water sample to be measured, uses above-mentioned side
Method measures the absorbance of water sample, obtains phosphatic concentration in high-concentration hydrogen sulfide hydrothermal solution according to standard curve.
In a kind of preferred implementation of said method, specifically comprise the following steps that
(1) take some high-concentration hydrogen sulfide hydrothermal solution water samples to be measured, use sulfide ionic selective electrode to determine water sample
The concentration of middle sulphion；
(2) take phosphate solution, add sodium sulfide solution, prepare phosphate-sulphion standard solution, make mark
In quasi-solution, the concentration of sulphion is basically identical with high-concentration hydrogen sulfide hydrothermal solution water sample to be measured；
(3) measuring the phosphate-sulphion standard solution two parts of 90mL same concentration respectively, a addition is extremely
In 100mL beaker A, in a addition to 100mL volumetric flask B；
(4) in beaker A, add between dilute sulfuric acid regulation pH to 5.00～6.00, record dilute sulfuric acid used
Consumption V1ML, then by V1Dilute sulfuric acid identical for mL adds in volumetric flask to regulate the pH of solution；
(5) solution of zinc sulfate of the 0.5～1.0mol/L of addition 0.5～5.0mL is in 100mL volumetric flask B,
Solution turned cloudy, is settled to 100mL with deionized water, shakes up, and is aged 1～24h；
(6) with solution in vacuum negative pressure filter filtration capacity bottle B, the micropore of 0.22～0.45 μm is used
Fibrous filter membrane, in filter process, filters in four times, and first three time takes 15～25mL solution respectively and filter,
Cleaning vacuum negative pressure filter with filtrate, after the 4th time has been filtered, discard precipitation, filtrate is stand-by；
(7) with P-Mo blue spectrophotometry filtrate absorbance under 880nm wavelength, standard is drawn bent
Line；
(8) standard solution is replaced to high-concentration hydrogen sulfide hydrothermal solution water sample to be measured, repeat (3) to (7) and survey
Determine the absorbance of water sample, obtain the phosphatic concentration in this water sample according to standard curve；
The method of the present invention is applicable to the hydrothermal solution water sample analyzing sulfur-containing anion concentration in 50～700 μm ol/L.
The Method And Principle of the present invention is under mildly acidic conditions, and sulphion and zinc ion generate zinc sulfide precipitation, warp
Ageing, filtration, with P-Mo blue spectrophotometry filtrate absorbance at 880nm.The present invention is carried
In the high-concentration hydrogen sulfide hydrothermal solution of confession, the method for phosphate determination has an advantage highlighted below: (1) (2) simple to operate
Reagent and consumptive material are conveniently easy to get high (4) good stability of (3) accuracy.
Detailed description of the invention
Embodiment 1
(1) taking some high concentration hydrothermal solution water samples, application sulfide ionic selective electrode records high concentration hydrothermal solution water sample
Middle sulphion concentration is 150 μMs；
(2) take phosphate solution, add sodium sulfide solution, prepare phosphate-sulphion standard solution, make mark
In quasi-solution, the concentration of sulphion is basically identical with water sample；
(3) measuring the phosphate-sulphion standard solution two parts of 90mL same concentration respectively, a addition is extremely
In 100mL beaker A, in a addition to 100mL volumetric flask B；
(4) in beaker A, dilute sulfuric acid regulation pH to 5.00, amount V of record dilute sulfuric acid used are added1ML,
According to V1In mL pondage bottle, the pH of solution is 5.00；
(5) add 1mL concentration be the solution of zinc sulfate of 1mol/L in 100mL volumetric flask B, solution
Become cloudy, with deionized water constant volume to 100mL, shake up, be aged 1h；
(6) limit of the microporous fibre filter membrane that aperture is 0.22 μm is clamped with the antimagnetic type tweezer being covered with polyethylene film
Edge, immerses in the hydrochloric acid solution of 0.5mol/L the most straight down, soak 12h, be washed with deionized water in
Property, seal stand-by；With the solution in vacuum negative pressure filter filtration capacity bottle B, using aperture is 0.22 μm
Microporous fibre filter membrane, in filter process, filter in four times, first three time takes 15mL solution respectively and filters,
Cleaning vacuum negative pressure filter with filtrate, after the 4th time has been filtered, discard precipitation, filtrate is stand-by；
(7) use P-Mo blue spectrophotography, measure filtrate absorbance under 880nm wavelength, draw standard
Curve；
(8) repetition (3) is to the absorbance of (7) step measurements water sample, obtains high concentration according to standard curve
The average phosphate concn of hydrothermal solution water sample is 1.91 μMs, and relative standard deviation is 1.89%.
Embodiment 2
(1) laboratory preparation simulation high-concentration hydrogen sulfide hydrothermal solution water sample, wherein sulphion concentration is 700 μMs,
Phosphate concn is 4.00 μMs；
(2) take phosphate solution, add sodium sulfide solution, prepare phosphate-sulphion standard solution, make mark
In quasi-solution, the concentration of sulphion is basically identical with water sample；
(3) measuring the phosphate-sulphion standard solution two parts of 90mL same concentration respectively, a addition is extremely
In 100mL beaker A, in a addition to 100mL volumetric flask B；
(4) in beaker A, dilute sulfuric acid regulation pH to 5.13, amount V of record dilute sulfuric acid used are added1ML,
According to V1In mL pondage bottle, the pH of solution is 5.13；
(5) add 5mL concentration be the solution of zinc sulfate of 1.0mol/L in 100mL volumetric flask B, solution
Become cloudy, with deionized water constant volume to 100mL, shake up, be aged 3h；
(6) limit of the microporous fibre filter membrane that aperture is 0.45 μm is clamped with the antimagnetic type tweezer being covered with polyethylene film
Edge, immerses in the hydrochloric acid solution of 0.5mol/L the most straight down, soak 12h, be washed with deionized water in
Property, seal stand-by；With the solution in vacuum negative pressure filter filtration capacity bottle B, using aperture is 0.45 μm
Microporous fibre filter membrane, in filter process, filter in four times, first three time takes 25mL solution respectively and filters,
Cleaning vacuum negative pressure filter with filtrate, after the 4th time has been filtered, discard precipitation, filtrate is stand-by；
(7) use P-Mo blue spectrophotography, measure filtrate absorbance under 880nm wavelength, draw standard
Curve；
(8) repetition (3) is to the absorbance of (7) step measurements simulated water sample, obtains water according to standard curve
The phosphate concn of sample is 2.74 μMs, and relative error is 8.67%.
Embodiment 3
(1) laboratory preparation simulation high-concentration hydrogen sulfide hydrothermal solution water sample, wherein sulphion concentration is 500 μMs,
Phosphate concn is 4.00 μMs；
(2) take phosphate solution, add sodium sulfide solution, prepare phosphate-sulphion standard solution, make mark
In quasi-solution, the concentration of sulphion is basically identical with water sample；
(3) measuring the phosphate-sulphion standard solution two parts of 90mL same concentration respectively, a addition is extremely
In 100mL beaker A, in a addition to 100mL volumetric flask B；
(4) in beaker A, dilute sulfuric acid regulation pH to 5.08, amount V of record dilute sulfuric acid used are added1ML,
According to V1In mL pondage bottle, the pH of solution is 5.08；
(5) add 2.0mL concentration be the solution of zinc sulfate of 0.5mol/L in 100mL volumetric flask B, molten
Liquid becomes cloudy, and with deionized water constant volume to 100mL, shakes up, and is aged 24h；
(6) limit of the microporous fibre filter membrane that aperture is 0.22 μm is clamped with the antimagnetic type tweezer being covered with polyethylene film
Edge, immerses in the hydrochloric acid solution of 1.0mol/L the most straight down, soak 24h, be washed with deionized water in
Property, seal stand-by；With the solution in vacuum negative pressure filter filtration capacity bottle B, using aperture is 0.22 μm
Microporous fibre filter membrane, in filter process, filter in four times, first three time takes 25mL solution respectively and filters,
Cleaning vacuum negative pressure filter with filtrate, after the 4th time has been filtered, discard precipitation, filtrate is stand-by；
(7) use P-Mo blue spectrophotography, measure filtrate absorbance under 880nm wavelength, draw standard
Curve；
(8) repetition (3) is to the absorbance of (7) step measurements simulated water sample, obtains water according to standard curve
The phosphate concn of sample is 4.02 μMs, and relative error is 0.50%.
Embodiment 4
(1) laboratory preparation simulation high-concentration hydrogen sulfide hydrothermal solution water sample, wherein sulphion concentration is 50 μMs,
Phosphate concn is 1.00 μMs；
(2) take phosphate solution, add sodium sulfide solution, prepare phosphate-sulphion standard solution, make mark
In quasi-solution, the concentration of sulphion is basically identical with water sample；
(3) measuring the phosphate-sulphion standard solution two parts of 90mL same concentration respectively, a addition is extremely
In 100mL beaker A, in a addition to 100mL volumetric flask B；
(4) in beaker A, dilute sulfuric acid regulation pH to 6.00, amount V of record dilute sulfuric acid used are added1ML,
According to V1In mL pondage bottle, the pH of solution is 6.00；
(5) add 0.5mL concentration be the solution of zinc sulfate of 0.5mol/L in 100mL volumetric flask B, molten
Liquid becomes cloudy, and with deionized water constant volume to 100mL, shakes up, and is aged 24h；
(6) limit of the microporous fibre filter membrane that aperture is 0.45 μm is clamped with the antimagnetic type tweezer being covered with polyethylene film
Edge, immerses in the hydrochloric acid solution of 3.0mol/L the most straight down, soak 24h, be washed with deionized water in
Property, seal stand-by；With the solution in vacuum negative pressure filter filtration capacity bottle B, using aperture is 0.45 μm
Microporous fibre filter membrane, in filter process, filter in four times, first three time takes 25mL solution respectively and filters,
Cleaning vacuum negative pressure filter with filtrate, after the 4th time has been filtered, discard precipitation, filtrate is stand-by；
(7) use P-Mo blue spectrophotography, measure filtrate absorbance under 880nm wavelength, draw standard
Curve；
(8) repetition (4) is to the absorbance of (7) step measurements simulated water sample, obtains water according to standard curve
The phosphate concn of sample is 0.85 μM, and relative error is 15.0%.
Claims (3)
1. the assay method of phosphate concn in a high-concentration hydrogen sulfide hydrothermal solution, it is characterised in that step is as follows:
Sulfide ionic selective electrode is utilized to measure the concentration of sulphion in high-concentration hydrogen sulfide hydrothermal solution water sample to be measured；Preparation phosphorus
Hydrochlorate-sulphion standard solution, makes the concentration of sulphion in standard solution essentially identical with detected water sample；Regulation
The pH=5.00～6.00 of the standard solution prepared, adds standard solution volume 1/180～1/18mL
0.5～1.0mol/L solution of zinc sulfate, generates zinc sulfide precipitation after reaction, be aged 1～24h, and use aperture is
The microporous fibre membrane filtration of 0.22～0.45 μm, discards precipitation, uses P-Mo blue spectrophotography, measures filtrate
Absorbance under 880nm wavelength, draws standard curve；Standard solution is replaced to high concentration to be measured sulfuration
Hydrogen hydrothermal solution water sample, measures the absorbance of water sample in aforementioned manners, obtains high-concentration hydrogen sulfide heat according to standard curve
Phosphatic concentration in liquid.
Method the most according to claim 1, it is characterised in that specifically comprising the following steps that of method
1) take some high-concentration hydrogen sulfide hydrothermal solution water samples to be measured, use sulfide ionic selective electrode to determine in water sample
The concentration of sulphion；
2) take phosphate solution, add sodium sulfide solution, prepare phosphate-sulphion standard solution, make standard
In solution, the concentration of sulphion is basically identical with high-concentration hydrogen sulfide hydrothermal solution water sample to be measured；
3) measuring the phosphate-sulphion standard solution two parts of 90mL same concentration respectively, a addition is extremely
In 100mL beaker A, in a addition to 100mL volumetric flask B；
4) in beaker A, add between dilute sulfuric acid regulation pH to 5.00～6.00, record dilute sulfuric acid used
Consumption V1ML, then by V1Dilute sulfuric acid identical for mL adds in volumetric flask to regulate the pH of solution；
5) solution of zinc sulfate of the 0.5～1.0mol/L of addition 0.5～5.0mL is in 100mL volumetric flask B, molten
Liquid becomes cloudy, and is settled to 100mL with deionized water, shakes up, and is aged 1～24h；
6) with solution in vacuum negative pressure filter filtration capacity bottle B, the micropore using 0.22～0.45 μm is fine
Dimension filter membrane, in filter process, filters in four times, and first three time takes 15～25mL solution respectively and filter, and uses
Filtrate cleans vacuum negative pressure filter, after the 4th time has been filtered, discards precipitation, and filtrate is stand-by；
7) with P-Mo blue spectrophotometry filtrate absorbance under 880nm wavelength, standard curve is drawn；
8) standard solution is replaced to high-concentration hydrogen sulfide hydrothermal solution water sample to be measured, repeat (3) to (7) and measure
The absorbance of water sample, obtains the phosphatic concentration in this water sample according to standard curve.
3. the purposes of a method as claimed in claim 1, it is characterised in that be applicable to analyze sulfur-containing anion
Concentration is at the hydrothermal solution water sample of 50～700 μm ol/L.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3796265A (en) * | 1972-06-07 | 1974-03-12 | J Eickmeier | Method for producing high hydrogen sulfide content gas wells |
| CN104122219A (en) * | 2014-07-31 | 2014-10-29 | 攀钢集团江油长城特殊钢有限公司 | Method for determining content of phosphorus in ferroniobium |
| CN105424628A (en) * | 2015-12-10 | 2016-03-23 | 苏州国环环境检测有限公司 | Determination method for total phosphorus in water |
-
2016
- 2016-04-28 CN CN201610278569.3A patent/CN105973819B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3796265A (en) * | 1972-06-07 | 1974-03-12 | J Eickmeier | Method for producing high hydrogen sulfide content gas wells |
| CN104122219A (en) * | 2014-07-31 | 2014-10-29 | 攀钢集团江油长城特殊钢有限公司 | Method for determining content of phosphorus in ferroniobium |
| CN105424628A (en) * | 2015-12-10 | 2016-03-23 | 苏州国环环境检测有限公司 | Determination method for total phosphorus in water |
Non-Patent Citations (2)
| Title |
|---|
| 暨卫东: "海水中活性磷酸盐的萃取比色测定研究", 《海洋海沼通报》 * |
| 福建水产学校主编: "《海水化学》", 31 May 1983, 农业出版社 * |
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