CN105973819B - The measuring method of phosphate concn in high-concentration hydrogen sulfide hydrothermal solution - Google Patents
The measuring method of phosphate concn in high-concentration hydrogen sulfide hydrothermal solution Download PDFInfo
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Abstract
The present invention relates to a kind of measuring methods of phosphate concn in high-concentration hydrogen sulfide hydrothermal solution.Using the concentration of sulphion in sulfide ionic selective electrode measurement hydrothermal solution water sample, sulphion is removed using the precipitation method.The phosphate standard solution for preparing sulfur-containing anion first, adjusts its pH, makes phosphate-sulphion standard solution pH=5.00~6.00, and precipitating reagent solution of zinc sulfate is added, and sulphion is made to generate zinc sulphide precipitating, is aged a few hours, and filtering discards precipitating, filtrate is stand-by.With P-Mo blue spectrophotometry, absorbance of the filtrate under 880nm wavelength is measured, phosphate-sulphion standard curve is drawn.The absorbance in high-concentration hydrogen sulfide hydrothermal solution water sample is measured under the same conditions, from phosphate-sulphion standard curve, finds out phosphatic concentration in high-concentration hydrogen sulfide hydrothermal solution water sample.This method is easy to operate, avoids the oxidizable bring measurement puzzlement of sulphion, and result is more accurate, improves the reliability of phosphate content analysis measurement in hydrothermal solution.
Description
Technical field
The present invention is Marine Sciences nutritive salt analysis field, is related to a kind of dense containing phosphate in high-concentration hydrogen sulfide hydrothermal solution
The measuring method of degree.
Background technique
Nutritive salt is ingredient necessary to marine phytoplankton growth and breeding and primary productivity of marine ecosystem and food chain
Basis, phosphatic content and distribution have important influence to marine biogeochemistry process.Marine monitoring specification at present
In the most commonly used phosphate classics measuring method be P-Mo blue spectrophotometry, the general seawater that it is suitable for not interfering with
Analysis measurement.Currently, hydrothermal vent is all over the world in ocean, the nutritive salt studied in hydrothermal solution is particularly necessary, and phosphate is
An important component in nutritive salt.However containing high concentration sulphion in hydrothermal solution, the sulphion in hydrothermal solution water sample is again very
Being oxidized easily becomes sulphur simple substance, and the sulphur simple substance of precipitating will seriously affect the accuracy of P-Mo blue spectrophotometry, therefore explore
Phosphatic Accurate Determining analysis method in a kind of suitable high-concentration hydrogen sulfide hydrothermal solution water sample has weight to Marine Sciences worker
The meaning wanted.
The method of the sulphion of higher concentration has oxidizing process and acidization in removing seawater relatively conventional at present.Wherein oxygen
Change method is after excessive bromine water is added in the seawater of acidification, and sulphion is oxidized into sulphur simple substance, and sulphur simple substance is filtered, and is passed through
Air removes excessive bromine, but bromine is difficult to be divided, and the bromine not eliminated directly affects the colour developing in P-Mo blue spectrophotometry
Reaction, and this method is complicated for operation；Acidization is to then pass to high pure nitrogen after being acidified seawater and remove hydrogen sulfide gas,
The disadvantages of the method are as follows hydrogen sulfide cannot be completely removed.
The present invention is to remove sulphion using the precipitation method, and it is phosphatic accurate in a kind of hydrothermal solution containing sulphion to provide
Analysis method, suitable for measuring sulfur-containing anion concentration in the hydrothermal solution of 50~700 μm of ol/L, this method is compared to common common phosphorus
Hydrochlorate measuring method, strong antijamming capability, result is more accurate, improves the reliability that phosphate content measures in hydrothermal solution.
Summary of the invention
It is good that it is an object of that present invention to provide a kind of accuracys, phosphatic in the hydrothermal solution of the strong high concentration sulphion of controllability
Analysis method.
The measuring method of phosphate concn in a kind of high-concentration hydrogen sulfide hydrothermal solution, steps are as follows: utilizing sulphion selectivity
The concentration of sulphion in determination of electrode high-concentration hydrogen sulfide hydrothermal solution water sample to be measured；With producing phosphate-sulphion standard solution, make to mark
The concentration with detected water sample of sulphion are essentially identical in quasi- solution；PH=5.00~6.00 of prepared standard solution are adjusted,
0.5~1.0mol/L solution of zinc sulfate of 1/180~1/18mL of standard solution volume is added, zinc sulphide precipitating is generated after reaction,
Ageing 1~for 24 hours, the microporous fibre membrane filtration for the use of aperture being 0.22~0.45 μm discards precipitating, with P-Mo blue spectrophotometric
Method measures absorbance of the filtrate under 880nm wavelength, draws standard curve；Standard solution is substituted for high concentration vulcanization to be measured
Hydrogen hydrothermal solution water sample measures the absorbance of water sample in aforementioned manners, finds out phosphoric acid in high-concentration hydrogen sulfide hydrothermal solution according to standard curve
The concentration of salt.
In a kind of preferred implementation of the above method, the specific steps are as follows:
(1) several high-concentration hydrogen sulfide hydrothermal solution water samples to be measured are taken, using sulfide ionic selective electrode determine in water sample sulphur from
The concentration of son；
(2) phosphate solution is taken, sodium sulfide solution is added, matches producing phosphate-sulphion standard solution, makes in standard solution
The concentration of sulphion and high-concentration hydrogen sulfide hydrothermal solution water sample to be measured are almost the same；
(3) phosphate-two parts of sulphion standard solution of 90mL same concentration is measured respectively, and portion, which is added to 100mL, to be burnt
In cup A, portion is added into 100mL volumetric flask B；
(4) in beaker A, dilute sulfuric acid is added and adjusts between pH to 5.00~6.00, record the dosage of dilute sulfuric acid used
V1ML, then by V1The pH for adjusting solution is added in volumetric flask in the identical dilute sulfuric acid of mL；
(5) solution of zinc sulfate of 0.5~1.0mol/L of 0.5~5.0mL is added in 100mL volumetric flask B, solution becomes muddy
It is turbid, it is settled to 100mL with deionized water, is shaken up, ageing 1~for 24 hours；
(6) it with solution in vacuum negative pressure filter filtration capacity bottle B, is filtered using 0.22~0.45 μm of microporous fibre
Film in filter process, filters in four times, preceding to take 15~25mL solution to be filtered respectively three times, cleans negative pressure of vacuum with filtrate
Filter device discards precipitating, filtrate is stand-by after the completion of the 4th filtering；
(7) absorbance with P-Mo blue spectrophotometry measurement filtrate under 880nm wavelength, draws standard curve；
(8) standard solution is substituted for high-concentration hydrogen sulfide hydrothermal solution water sample to be measured, repeats the suction of (3) to (7) measurement water sample
Luminosity finds out the phosphatic concentration in the water sample according to standard curve；
Method of the invention is suitable for analyzing sulfur-containing anion concentration in the hydrothermal solution water sample of 50~700 μm of ol/L.
Method And Principle of the invention is that under mildly acidic conditions, sulphion and zinc ion generate zinc sulphide and precipitate, aged,
Filtering, with absorbance of the P-Mo blue spectrophotometry measurement filtrate at 880nm.High-concentration hydrogen sulfide heat provided by the present invention
The method of phosphate determination has the following prominent advantages: that (1) (2) reagent easy to operate and consumptive material are conveniently easy to get (3) accurately in liquid
It is good to spend high (4) stability.
Specific embodiment
Embodiment 1
(1) several high concentration hydrothermal solution water samples are taken, using sulfide ionic selective electrode measure in high concentration hydrothermal solution water sample sulphur from
Sub- concentration is 150 μM；
(2) phosphate solution is taken, sodium sulfide solution is added, matches producing phosphate-sulphion standard solution, makes in standard solution
The concentration of sulphion and water sample are almost the same；
(3) phosphate-two parts of sulphion standard solution of 90mL same concentration is measured respectively, and portion, which is added to 100mL, to be burnt
In cup A, portion is added into 100mL volumetric flask B；
(4) in beaker A, dilute sulfuric acid is added and adjusts pH to 5.00, record the amount V of dilute sulfuric acid used1ML, according to V1ML tune
The pH for saving solution in volumetric flask is 5.00；
(5) be added 1mL concentration be 1mol/L solution of zinc sulfate in 100mL volumetric flask B, solution becomes cloudy, spend from
Sub- water constant volume shakes up to 100mL, is aged 1h；
(6) edge for the microporous fibre filter membrane for being 0.22 μm with the antimagnetic type tweezer clamping aperture for being covered with polyethylene film, by
It opens ground to immerse straight down in the hydrochloric acid solution of 0.5mol/L, impregnates 12h, be washed with deionized water to neutrality, sealing is for use；With true
Solution in idling press filtering device filtration capacity bottle B uses aperture for 0.22 μm of microporous fibre filter membrane, in filter process,
It filters in four times, it is preceding to take 15mL solution to be filtered respectively three times, vacuum negative pressure filter, the 4th filtering are cleaned with filtrate
After the completion, precipitating is discarded, filtrate is stand-by；
(7) P-Mo blue spectrophotometry is used, absorbance of the filtrate under 880nm wavelength is measured, draws standard curve；
(8) absorbance for repeating (3) to (7) step measurement water sample, finds out high concentration hydrothermal solution water sample according to standard curve
Average phosphate concn is 1.91 μM, relative standard deviation 1.89%.
Embodiment 2
(1) simulation high-concentration hydrogen sulfide hydrothermal solution water sample is prepared in laboratory, and wherein sulphion concentration is 700 μM, and phosphate is dense
Degree is 4.00 μM；
(2) phosphate solution is taken, sodium sulfide solution is added, matches producing phosphate-sulphion standard solution, makes in standard solution
The concentration of sulphion and water sample are almost the same；
(3) phosphate-two parts of sulphion standard solution of 90mL same concentration is measured respectively, and portion, which is added to 100mL, to be burnt
In cup A, portion is added into 100mL volumetric flask B；
(4) in beaker A, dilute sulfuric acid is added and adjusts pH to 5.13, record the amount V of dilute sulfuric acid used1ML, according to V1ML tune
The pH for saving solution in volumetric flask is 5.13；
(5) it is the solution of zinc sulfate of 1.0mol/L in 100mL volumetric flask B that 5mL concentration, which is added, and solution becomes cloudy, and spends
Ionized water constant volume shakes up to 100mL, is aged 3h；
(6) edge for the microporous fibre filter membrane for being 0.45 μm with the antimagnetic type tweezer clamping aperture for being covered with polyethylene film, by
It opens ground to immerse straight down in the hydrochloric acid solution of 0.5mol/L, impregnates 12h, be washed with deionized water to neutrality, sealing is for use；With true
Solution in idling press filtering device filtration capacity bottle B uses aperture for 0.45 μm of microporous fibre filter membrane, in filter process,
It filters in four times, it is preceding to take 25mL solution to be filtered respectively three times, vacuum negative pressure filter, the 4th filtering are cleaned with filtrate
After the completion, precipitating is discarded, filtrate is stand-by；
(7) P-Mo blue spectrophotometry is used, absorbance of the filtrate under 880nm wavelength is measured, draws standard curve；
(8) absorbance for repeating (3) to (7) step measurement simulated water sample, the phosphate of water sample is found out according to standard curve
Concentration is 2.74 μM, relative error 8.67%.
Embodiment 3
(1) simulation high-concentration hydrogen sulfide hydrothermal solution water sample is prepared in laboratory, and wherein sulphion concentration is 500 μM, and phosphate is dense
Degree is 4.00 μM；
(2) phosphate solution is taken, sodium sulfide solution is added, matches producing phosphate-sulphion standard solution, makes in standard solution
The concentration of sulphion and water sample are almost the same；
(3) phosphate-two parts of sulphion standard solution of 90mL same concentration is measured respectively, and portion, which is added to 100mL, to be burnt
In cup A, portion is added into 100mL volumetric flask B；
(4) in beaker A, dilute sulfuric acid is added and adjusts pH to 5.08, record the amount V of dilute sulfuric acid used1ML, according to V1ML tune
The pH for saving solution in volumetric flask is 5.08；
(5) it is the solution of zinc sulfate of 0.5mol/L in 100mL volumetric flask B that 2.0mL concentration, which is added, and solution becomes cloudy, and uses
Deionized water constant volume shakes up to 100mL, and ageing is for 24 hours；
(6) edge for the microporous fibre filter membrane for being 0.22 μm with the antimagnetic type tweezer clamping aperture for being covered with polyethylene film, by
It opens ground to immerse straight down in the hydrochloric acid solution of 1.0mol/L, impregnate for 24 hours, be washed with deionized water to neutrality, sealing is for use；With true
Solution in idling press filtering device filtration capacity bottle B uses aperture for 0.22 μm of microporous fibre filter membrane, in filter process,
It filters in four times, it is preceding to take 25mL solution to be filtered respectively three times, vacuum negative pressure filter, the 4th filtering are cleaned with filtrate
After the completion, precipitating is discarded, filtrate is stand-by；
(7) P-Mo blue spectrophotometry is used, absorbance of the filtrate under 880nm wavelength is measured, draws standard curve；
(8) absorbance for repeating (3) to (7) step measurement simulated water sample, the phosphate of water sample is found out according to standard curve
Concentration is 4.02 μM, relative error 0.50%.
Embodiment 4
(1) simulation high-concentration hydrogen sulfide hydrothermal solution water sample is prepared in laboratory, and wherein sulphion concentration is 50 μM, phosphate concn
It is 1.00 μM；
(2) phosphate solution is taken, sodium sulfide solution is added, matches producing phosphate-sulphion standard solution, makes in standard solution
The concentration of sulphion and water sample are almost the same；
(3) phosphate-two parts of sulphion standard solution of 90mL same concentration is measured respectively, and portion, which is added to 100mL, to be burnt
In cup A, portion is added into 100mL volumetric flask B；
(4) in beaker A, dilute sulfuric acid is added and adjusts pH to 6.00, record the amount V of dilute sulfuric acid used1ML, according to V1ML tune
The pH for saving solution in volumetric flask is 6.00；
(5) it is the solution of zinc sulfate of 0.5mol/L in 100mL volumetric flask B that 0.5mL concentration, which is added, and solution becomes cloudy, and uses
Deionized water constant volume shakes up to 100mL, and ageing is for 24 hours；
(6) edge for the microporous fibre filter membrane for being 0.45 μm with the antimagnetic type tweezer clamping aperture for being covered with polyethylene film, by
It opens ground to immerse straight down in the hydrochloric acid solution of 3.0mol/L, impregnate for 24 hours, be washed with deionized water to neutrality, sealing is for use；With true
Solution in idling press filtering device filtration capacity bottle B uses aperture for 0.45 μm of microporous fibre filter membrane, in filter process,
It filters in four times, it is preceding to take 25mL solution to be filtered respectively three times, vacuum negative pressure filter, the 4th filtering are cleaned with filtrate
After the completion, precipitating is discarded, filtrate is stand-by；
(7) P-Mo blue spectrophotometry is used, absorbance of the filtrate under 880nm wavelength is measured, draws standard curve；
(8) absorbance for repeating (4) to (7) step measurement simulated water sample, the phosphate of water sample is found out according to standard curve
Concentration is 0.85 μM, relative error 15.0%.
Claims (1)
1. the measuring method of phosphate concn in a kind of high-concentration hydrogen sulfide hydrothermal solution, the sulphion concentration in hydrothermal solution water sample is 50 ~
700μmol/L；It is characterized by the following steps: measuring high-concentration hydrogen sulfide hydrothermal solution water sample to be measured using sulfide ionic selective electrode
The concentration of middle sulphion；With producing phosphate-sulphion standard solution, make the concentration of sulphion and detected water sample base in standard solution
This is identical；Adjust pH=5.00 ~ 6.00 of prepared standard solution, be added 1/180 ~ 1/18mL of standard solution volume 0.5 ~
1.0mol/L solution of zinc sulfate generates zinc sulphide and precipitates after reaction, and ageing 1 ~ for 24 hours, the micropore for the use of aperture being 0.22 ~ 0.45 μm
Fibrous filter membrane filtering, discards precipitating, with P-Mo blue spectrophotometry, measures absorbance of the filtrate under 880nm wavelength, draws mark
Directrix curve；Standard solution is substituted for high-concentration hydrogen sulfide hydrothermal solution water sample to be measured, measures the absorbance of water sample, root in aforementioned manners
Phosphatic concentration in high-concentration hydrogen sulfide hydrothermal solution is found out according to standard curve；
Specific step is as follows for method:
1) several high-concentration hydrogen sulfide hydrothermal solution water samples to be measured are taken, the dense of sulphion in water sample is determined using sulfide ionic selective electrode
Degree；
2) take phosphate solution, sodium sulfide solution be added, match producing phosphate-sulphion standard solution, make in standard solution sulphur from
The concentration and high-concentration hydrogen sulfide hydrothermal solution water sample to be measured of son are almost the same；
3) phosphate-two parts of sulphion standard solution of 90mL same concentration is measured respectively, portion is added into 100mL beaker A,
Portion is added into 100mL volumetric flask B；
4) in beaker A, dilute sulfuric acid is added and adjusts between pH to 5.00 ~ 6.00, record the dosage V of dilute sulfuric acid used1ML, then will
V1The pH for adjusting solution is added in volumetric flask B in the identical dilute sulfuric acid of mL；
5) solution of zinc sulfate of 0.5 ~ 1.0mol/L of 0.5 ~ 5.0mL is added in 100mL volumetric flask B, solution becomes cloudy, and spends
Ionized water is settled to 100mL, shakes up, and ageing 1 ~ for 24 hours；
6) it is filtered with solution in vacuum negative pressure filter filtration capacity bottle B using 0.22 ~ 0.45 μm of microporous fibre filter membrane
In the process, it filters in four times, it is preceding to take 15 ~ 25mL solution to be filtered respectively three times, vacuum negative pressure filter is cleaned with filtrate,
After the completion of 4th filtering, precipitating is discarded, filtrate is stand-by；
7) absorbance with P-Mo blue spectrophotometry measurement filtrate under 880nm wavelength, draws standard curve；
8) standard solution is substituted for high-concentration hydrogen sulfide hydrothermal solution water sample to be measured, repeated 3) to the absorbance for 7) measuring water sample, root
The phosphatic concentration in the water sample is found out according to standard curve.
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Citations (3)
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|---|---|---|---|---|
| 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 (1)
| Title |
|---|
| 海水中活性磷酸盐的萃取比色测定研究;暨卫东;《海洋海沼通报》;19891231(第4期);第2-5节及摘要 |
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