CN105158054A - Method for determining total phosphorus concentration of seawater sediment by microwave digestion adopting small sample amount of potassium persulphate - Google Patents
Method for determining total phosphorus concentration of seawater sediment by microwave digestion adopting small sample amount of potassium persulphate Download PDFInfo
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- CN105158054A CN105158054A CN201510306888.6A CN201510306888A CN105158054A CN 105158054 A CN105158054 A CN 105158054A CN 201510306888 A CN201510306888 A CN 201510306888A CN 105158054 A CN105158054 A CN 105158054A
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Abstract
The invention discloses a method for determining a total phosphorus concentration of seawater sediment by microwave digestion adopting a small sample amount of potassium persulphate. The method comprises carrying out digestion pre-treatment on 0.006-0.04g of sample sediment by a digestion pipe, then carrying out dispersion and centrifugation, diluting a supernatant obtained by centrifugation, measuring an absorbance value and calculating a total phosphorus concentration of seawater sediment. The method for determining a total phosphorus concentration by small sample amount potassium persulphate digestion solves the problem that the method for determining a total phosphorus concentration by standard potassium persulphate digestion utilizes a large colorimetric pipe to digest a sample, has large sample consumption, has large time consumption and consumes a lot of an experiment reagent. The method provided by the invention has sensitivity, precision and recovery rate better than those of the national standard method, reduces use amounts of a sample and a reagent, has low time consumption, can produce the experiment result the same to that of the national standard method and solves the problems of the existing method for determining a total phosphorus concentration of seawater sediment.
Description
Technical field
The present invention relates to Method Measuring Total Quantity of Phosphorus in a kind of Marine Sediment, particularly relate to Method Measuring Total Quantity of Phosphorus in a kind of small sample quantities Marine Sediment and application.
Background technology
Aquaculture, urbanization and anthropogenic discharge cause river mouth and bay eutrophication and primary productivity to remain high.Eutrophication and thing followed red tide have been considered to the pollution problem that in nearly twenty or thirty year, coastal area of china is main.Phosphorus is the one of the chief elements causing body eutrophication, and total phosphorus is the important indicator that ambient water quality is evaluated.Method Measuring Total Quantity of Phosphorus in external conventional Marine Sediment, as document [AspilaK.I., AgemianH., ChauA.S.Y.Asemi-automatedmethodforthedeterminationofinor ganic, organicandtotalphosphateinsediments [J] .Analyst, 1976,101:187-197; RuttenbergK.C., Developmentofasequentialextractionmethodfordifferentform sofphosphorusinmarinesediments, Limnol.Oceanogr.1992,37:1460 – 1482.] described in, be first by after sample at room temperature drying in muffle furnace at 550 DEG C of ashing 2h, then at room temperature with 1mol.L-1 hydrochloric acid vibration lixiviate 16-18h, last P-Mo blue spectrophotometry.With abroad unlike, domesticly conventional be national standard method and improve one's methods, as document [GB17378.5-2007, marine monitoring specification Part V: sediment analysis; Cui Jiansheng, Zhang Yingxian, Huo Yuehui, Jiao Zhenxia. the research of determination of total phosphorus by potassium persulfate digestion with lower dosage. Hebei University of Science and Technology's journal, 2007,28 (2): 126-129.], described in, in 50ml or 25ml color comparison tube, namely add potassium persulfate be placed in pressure cooker and clear up sample, then use P-Mo blue spectrophotometry.Although internal method is more consuming time than foreign method short, this method consumes sediment sample and amount of reagent is still comparatively large, is unfavorable for making full use of and reagent saving of sediment sample.
Summary of the invention
The technical problem to be solved in the present invention overcomes existing defect, provides the investigation and application that a kind of small sample quantities potassium persulfate micro-wave digestion measures total phosphorus method in Marine Sediment.It adopts 12ml tool thread cap digestion tube pretreatment sample, consumption sample is little, decrease sample and reagent dosage, used time is shorter, and sensitivity, precision, the recovery are all better than national standard method, experimental result is consistent with national standard method, and it can make up the deficiency that in existing Marine Sediment, total phosphorus determination technology is above-mentioned.
Object of the present invention carrys out specific implementation by the following technical programs:
A kind of small sample quantities potassium persulfate micro-wave digestion measures total phosphorus method in Marine Sediment, first with the sample deposition thing of digestion tube to 0.006-0.04g clear up, pre-service, again through dispersion and centrifuging, finally survey absorbance to after the supernatant dilution after centrifuging, total phosphorus concentration in Marine Sediment can be calculated.
Preferably, the quality of sample deposition thing is 0.03g.
Preferably, described in clear up, adopt alkaline chitinase digestion solution to carry out.
More preferably, described alkaline chitinase digestion solution is for containing 40g/lK
2s
2o
8, 3g/lNaOH mixed aqueous solution.
Further be preferably, described alkaline chitinase digestion solution consumption is 5ml.
Preferably, described in clear up, sample deposition thing and digestion solution are cleared up 15-30 point of kind at 122-165 DEG C.
Preferred further, when clearing up, heating and decompose in the microwave dissolver of test tube temperature control or the heating plate of band test tube jack.
Preferably, described digestion tube is 12ml tool thread cap digestion tube.
Preferably, described dispersion, disperses 10-20 minute in ultrasonic disperse instrument when adopting ultrasonic efficiency to be 50%.
Preferably, described separation is that digestion tube is placed in hydro-extractor, centrifugal separately 5-10 minute under 2000r/min rotating speed.
Preferably, pipette the supernatant of centrifuging gained and after diluting 5 times, under 882nm wavelength, measure absorbance by P-Mo blue spectrophotometric method, and calculating total phosphorus concentration according to typical curve.
Through test, in above-mentioned small sample quantities potassium persulfate micro-wave digestion mensuration Marine Sediment, total phosphorus method is as application process in oceanic sediment total phosphorus determination.RSD is not more than 2%, and average recovery rate is greater than 95%, highly sensitive, is better than national standard method [GB17378.5-2007], can applies in practice
Beneficial effect of the present invention:
The present invention is directed to standard alkaline potassium per-sulfate digestion mensuration total phosphorus to adopt large color comparison tube to clear up, consume large, the consuming time length of sample size and the problem of consumption great many of experiments reagent, provide a kind of method that small sample quantities potassium persulfate micro-wave digestion measures total phosphorus in Marine Sediment, sensitivity, precision, the recovery are all better than national standard method, and decrease sample and reagent dosage, used time is shorter, experimental result is consistent with national standard method, and it can make up the deficiency that in existing Marine Sediment, total phosphorus determination technology is above-mentioned.
Embodiment
Below the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein is only for instruction and explanation of the present invention, is not intended to limit the present invention.
Embodiment 1:
(1) key instrument adopted
DR5000 type ultraviolet-visible pectrophotometer (Hash company of the U.S.); DRB200 type counteract appearance (Hash company of the U.S.); 800 type hydro-extractors (Shanghai Jiang Xing Instrument Ltd.); KQ-100DE supersonic cleaning machine (Kunshan Ultrasonic Instruments Co., Ltd.).
(2) main agents adopted
Potassium persulfate, NaOH are pure for analyzing, and are produced by Aladdin reagent (Shanghai) Co., Ltd.; Potassium dihydrogen phosphate is that top grade is pure, and it is pure that other agent is analysis, produces by chemical reagents corporation of traditional Chinese medicines group.
1) 17% sulfuric acid solution: under constantly stirring, the 60mL concentrated sulphuric acid is slowly added in 300mL water, is stored in vial, for subsequent use.
2) potassium persulfate solution: 4g potassium persulfate adds 0.3g NaOH, is diluted with water to 100ml, for subsequent use.
3) potassium antimony tartrate: take 1.4g potassium antimony tartrate soluble in water, and be diluted to 1000mL, stores in polyethylene bottle, for subsequent use.
4) ascorbic acid solution: by soluble in water for 5.4g ascorbic acid solution and be diluted to 100mL, store in polyethylene bottle, less than 4 DEG C preservations, the term of validity 1 week.
5) ammonium molybdate solution: take 15.0g soluble in water and be diluted in 500mL polyethylene bottle, keep in Dark Place.
6) mix reagent: measure 100mL17% sulfuric acid solution successively, 40mL ammonium molybdate solution, 20mL potassium antimonyl tartrate solution, mixes, now with the current.
7) phosphate standard stock solution (1.6umol/ml): accurately take 0.2176g potassium dihydrogen phosphate (at 110 DEG C dry 2 hours), after a small amount of water-soluble solution, shift in 1000ml volumetric flask, namely constant volume obtains concentration is 1.6umol/ml phosphate standard stock solution.
8) phosphate standard stock solution (0.16umol/ml): accurately measuring 10ml concentration is 1.6umol/ml phosphate standard stock solution, shift in 100ml volumetric flask, namely constant volume obtains concentration is 0.16umol/ml phosphate standard stock solution.
(3) collection of sample
Gather Wai Luotou surrounding waters, main island, Zhoushan Marine Sediment surficial sediment, fill the polybag of people's cleaning respectively, air in venting bag, the same day transports laboratory back, through freeze drier drying 24 hours, pulverizes grinding, after crossing 80 mesh sieves, be placed in vial sealing and preserve, to be measured.
(4) test method
1) drafting of typical curve
Get in 6 12ml digestion tubes, add 0 respectively, 0.125,0.25,0.5,0.75,1ml concentration is 0.16umol/ml phosphate standard solution, then 5.0 are added successively, 4.875,4.75,4.50,4.25,4.0ml distilled water, adding 1ml mix reagent and 1ml ascorbic acid more respectively, after colour developing 10 ~ 15min, take distilled water as reference, under 882nm wavelength, measure its absorbance, then draw concentration-absorbance typical curve, obtain phosphorus concentration good in 0 ~ 0.032mmol/l scope internal linear.Y=0.6861x+0.0017, related coefficient is r
2=0.999, meet and measure requirement.
2) sedimental pre-service
Accurately take 0.03 ± 0.0002g sediment sample, put into 12ml digestion tube; Separately get a digestion tube, the silica sand (in the muffle furnace of 750 DEG C calcination 2h) adding 0.03 ± 0.0002g calcination makes sample blank.Pipette 5ml alkaline potassium per-sulfate digestion solution respectively, along clearing up tube wall, adhesion sample slowly being swept away, tightening cap stopper.Clear up 15 minutes at 122 DEG C after, take out and be cooled to room temperature.Under 50% ultrasonic efficiency, ultrasonic disperse is after 10 minutes, then under 2000r/min rotating speed in hydro-extractor centrifugal treating 5 minutes.Accurately pipette 1ml supernatant in clean digestion tube, with distilled water diluting to 5ml, add 1ml mix reagent and 1ml ascorbic acid respectively, develop the color measurement in 10 ~ 15 minutes, take distilled water as reference, under 882nm wavelength, measure its absorbance, deduction sample blank produces absorbance, then calculates its corresponding concentration value by typical curve.The concentration calculating Wai Luotou surrounding waters, main island, gathered Zhoushan Marine Sediment surficial sediment total phosphorus is 0.3654mg/g, and national standard method [GB17378.5-2007] data measured is 0.3565mg/g.
Method of the present invention, method RSD is not more than 2%, and average recovery rate is greater than 95%, highly sensitive, is better than national standard method [GB17378.5-2007], can applies in practice.
It is the total phosphorus content in Zhu Dao surrounding waters, the Zhoushan sediment recorded with the present invention in table 1.
Table 1: the total phosphorus content in the sediment of Zhu Dao surrounding waters, Zhoushan
Embodiment 2:
The present embodiment method is with embodiment 1, and difference is: the sample size added is 0.04g.Through surveying, RSD is not more than 2%, and average recovery rate is greater than 95%, highly sensitive, is better than national standard method [GB17378.5-2007], can applies in practice.
Embodiment 3:
The present embodiment method is with embodiment 1, and difference is: the sample size added is 0.006g, and sample, after centrifugal treating, accurately pipettes 5ml supernatant in clean digestion tube.Through surveying, RSD is not more than 2%, and average recovery rate is greater than 95%, highly sensitive, is better than national standard method [GB17378.5-2007], can applies in practice.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a small sample quantities potassium persulfate micro-wave digestion measures total phosphorus method in Marine Sediment, it is characterized in that: first clear up pre-service with the sample deposition thing of digestion tube to 0.006-0.04g, again through dispersion and centrifuging, finally survey absorbance to after the supernatant dilution after centrifuging, total phosphorus concentration in Marine Sediment can be calculated.
2. small sample quantities potassium persulfate micro-wave digestion according to claim 1 measures total phosphorus method in Marine Sediment, it is characterized in that: the quality of sample deposition thing is 0.03g.
3. small sample quantities potassium persulfate micro-wave digestion according to claim 1 and 2 measures total phosphorus method in Marine Sediment, it is characterized in that: described in clear up, adopt alkaline chitinase digestion solution to carry out.
4. small sample quantities potassium persulfate micro-wave digestion according to claim 3 measures total phosphorus method in Marine Sediment, it is characterized in that: described alkaline chitinase digestion solution is for containing 40g/lK
2s
2o
8, 3g/lNaOH mixed aqueous solution.
5. small sample quantities potassium persulfate micro-wave digestion according to claim 3 measures total phosphorus method in Marine Sediment, it is characterized in that: described alkaline chitinase digestion solution consumption is 5ml.
6. small sample quantities potassium persulfate micro-wave digestion according to claim 1 and 2 measures total phosphorus method in Marine Sediment, it is characterized in that: described in clear up, sample deposition thing and digestion solution are cleared up 15-30 point of kind at 122-165 DEG C.
7. small sample quantities potassium persulfate micro-wave digestion according to claim 6 measures total phosphorus method in Marine Sediment, it is characterized in that: when clearing up, heating and decompose in the microwave dissolver of test tube temperature control or the heating plate of band test tube jack.
8. small sample quantities potassium persulfate micro-wave digestion according to claim 1 and 2 measures total phosphorus method in Marine Sediment, it is characterized in that: described digestion tube is 12ml tool thread cap digestion tube.
9. small sample quantities potassium persulfate micro-wave digestion according to claim 1 and 2 measures total phosphorus method in Marine Sediment, it is characterized in that: described dispersion, disperses 10-20 minute when adopting ultrasonic efficiency to be 50% in ultrasonic disperse instrument; Described separation is that digestion tube is placed in hydro-extractor, centrifugal separately 5-10 minute under 2000r/min rotating speed.
10. small sample quantities potassium persulfate micro-wave digestion according to claim 1 and 2 measures total phosphorus method in Marine Sediment, it is characterized in that: pipette centrifuging gained supernatant and after diluting 5 times, under 882nm wavelength, measure absorbance by P-Mo blue spectrophotometric method, and calculate total phosphorus concentration according to typical curve.
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| CN111257252A (en) * | 2020-02-29 | 2020-06-09 | 武汉大学 | Method for detecting oxysulfate in water by heating separation integrated photometry |
| CN113916813A (en) * | 2021-10-09 | 2022-01-11 | 广东石油化工学院 | Method for measuring total phosphorus concentration in seawater |
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