CN100552427C - Sediment total nitrogen, total phosphorus simultaneous determination analytical approach - Google Patents
Sediment total nitrogen, total phosphorus simultaneous determination analytical approach Download PDFInfo
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- CN100552427C CN100552427C CNB200610085999XA CN200610085999A CN100552427C CN 100552427 C CN100552427 C CN 100552427C CN B200610085999X A CNB200610085999X A CN B200610085999XA CN 200610085999 A CN200610085999 A CN 200610085999A CN 100552427 C CN100552427 C CN 100552427C
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- total phosphorus
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 76
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 39
- 239000011574 phosphorus Substances 0.000 title claims abstract description 39
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 38
- 239000013049 sediment Substances 0.000 title claims abstract description 25
- 238000013459 approach Methods 0.000 title claims description 8
- 230000029087 digestion Effects 0.000 claims abstract description 36
- 230000001079 digestive effect Effects 0.000 claims abstract description 11
- 239000006228 supernatant Substances 0.000 claims abstract description 10
- 238000005303 weighing Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000002835 absorbance Methods 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000002360 preparation method Methods 0.000 claims description 6
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 4
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 10
- 239000002689 soil Substances 0.000 abstract description 7
- 238000004458 analytical method Methods 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 230000031700 light absorption Effects 0.000 abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 8
- 239000007788 liquid Substances 0.000 description 6
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 6
- 229960005070 ascorbic acid Drugs 0.000 description 4
- 235000010323 ascorbic acid Nutrition 0.000 description 4
- 239000011668 ascorbic acid Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000007696 Kjeldahl method Methods 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 238000012851 eutrophication Methods 0.000 description 3
- 229910001260 Pt alloy Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000003705 background correction Methods 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000004108 freeze drying Methods 0.000 description 2
- 239000011964 heteropoly acid Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 241001269238 Data Species 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 239000012916 chromogenic reagent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- CJGYQECZUAUFSN-UHFFFAOYSA-N oxygen(2-);tin(2+) Chemical compound [O-2].[Sn+2] CJGYQECZUAUFSN-UHFFFAOYSA-N 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- QHGNHLZPVBIIPX-UHFFFAOYSA-N tin(II) oxide Inorganic materials [Sn]=O QHGNHLZPVBIIPX-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a kind of sediment, soil total nitrogen total phosphorus determination and analysis method, at first with the fresh sample drying of gathering, pulverize, sieve, thoroughly mixing claims that a certain amount of digestion vessel that places is stand-by; In the digestion vessel of the good sample of weighing, add digestive pharmaceutical, mixing; The jam-pack grinding port plug wraps with gauze, places high pressure steam pot high temperature to clear up, and take out the cooling back; Draw the digestion supernatant and carry out 190～290nm length scanning, determine optimum absorb wavelength and background value; Measure light absorption value, obtain total nitrogen; Draw the digestion supernatant, add the colour developing of developer constant volume, 650～750nm length scanning is determined optimum absorb wavelength, measures absorbance, obtains total phosphorus.The disposable combined digestion of sample of the present invention, length scanning are determined the optimal absorption peak, fast, accurately measure sediment total nitrogen, total phosphorus.This method is specially adapted to the simultaneous determination of total nitrogen, total phosphorus in the sediment of water bottom such as river, lake, river, storehouse, sea and the soil.
Description
One, technical field
The present invention relates to the technical method that a kind of sediment, soil total nitrogen total phosphorus are measured, the disposable combined digestion of sample specifically, length scanning is determined the optimal absorption peak, the background correction value fast, is accurately measured the method for sediment total nitrogen, total phosphorus.
Two, background technology
Many research datas show, the eutrophication degree relation of being proportionate in the content of total nitrogen, total phosphorus and lake.And lake sediment is the aggregation of pollutant in the water environment, the polluter major part that enters in the water body in lake is deposited in the bottom mud in lake, therefore, lake sediment is that valley environment changes and human dossier to environmental impact the pollution history that can rebuild the lake by lake sediment.Nutritive salt in the synchronous deposits also is the internal loading of water body in lake eutrophication.Under the situation of external source minimizing or control external source, the sediment internal loading will stop or postpone the regulation effect of lake water quality in the time of a fixed length, therefore, want effectively to prevent and treat body eutrophication, it is just very necessary to measure total nitrogen in the water bottom sediments such as river, lake, river, storehouse, sea, total phosphorus.
In the last hundred years, mensuration sediment, soil total nitrogen are generally continued to use Kjeldahl method or do some improvement on the Kjeldahl method bases, but this method complex operation, digestion time is long, and power consumption is big, also needs to use a large amount of strong acid and strong bases.Measure total phosphorus and often use Na
2CO
3Dissolve method, this just needs to use platinum alloy crucible, but because of platinum alloy crucible costs an arm and a leg, after use NaOH instead and in silver-colored crucible, dissolve, it is normal at present that what adopt is to melt method in the acid that high temperature furnace carries out.These two mensuration all need high temperature, the high-pressure digestion step of a few hours.Because temperature, time, the reagent cleared up all have considerable influence to clearing up, and persulfate solution can not be put for a long time, measure ninety-nine times out of a hundred and all need production standard curve simultaneously, therefore time-consuming, the consumption power, loaded down with trivial details of mensuration respectively of total nitrogen and total phosphorus is felt very difficulty as the mensuration that a people bears these two project batch samples simultaneously.Total nitrogen, total phosphorus are extensively used in the persulfate oxidation method mensuration water, but this method is used to measure sediment total nitrogen, total phosphorus report is arranged also abroad in recent years, because the complicacy of sediment composition causes the absorption background of digestive juice to light, just different with water sample, if still being chosen in 220nm and 275nm two wavelength measures, the result is often very undesirable, must must carry out length scanning to its digestion solution, avoid the responsive uptake zone of digestion solution itself, determine optimum absorb wavelength, the background correction value just can obtain measurement result accurately.
Three, summary of the invention
Clear up the problems referred to above that measure to exist at current total nitrogen, total phosphorus, the objective of the invention is to change the traditional analysis method, provide a kind of fast, accurately, measure sediment, soil total nitrogen total phosphorus analytical approach.Utilize this method, can carry out the disposable combined digestion of sample total nitrogen total phosphorus, time saving and energy saving, bring convenience to operation.
The objective of the invention is to be achieved through the following technical solutions:
A kind of sediment total nitrogen, total phosphorus simultaneous determination analytical approach is characterized in that it may further comprise the steps:
(1) with the fresh sample drying of gathering, pulverize, sieve, thorough mixing, it is stand-by to take by weighing a certain amount of digestion vessel (color comparison tube) that places.Among the present invention, sample carries out freeze drying or natural air drying sample after gathering, and grinds the back and crosses 80～100 mesh sieves, clears up measured quantity and is less than the high limit of digestion weighing, and the high limit of digestion weighing is expressed from the next:
The high limit of digestion weighing=[the high limit of water sample (20 μ g/ml) ÷ C/N * digestive pharmaceutical consumption (ml)]/total nitrogen content (μ g/mg).
(2) the preparation digestive pharmaceutical adds digestive pharmaceutical, constant volume, mixing in the digestion vessel of the good sample of weighing.Digestive pharmaceutical generally adopts alkaline potassium persulfate (K
2S
2O
8), proportioning is every liter and contains K
2S
2O
820g and NaOH 3g.
(3) digestive juice in the digestion vessel is carried out high temperature and clear up, take out the cooling back.Digestion vessel is answered the jam-pack grinding port plug, wraps with gauze, places high pressure steam pot high temperature to clear up, and digestion condition is 120～124 ℃, about digestion time 30min.
(4) with the blank be contrast, draw the digestion supernatant and carry out the scanning of 190～290nm ultraviolet wavelength, determine optimum absorb wavelength and background value.Adopt supernatant to carry out 190～290nm length scanning, can avoid responsive uptake zone, choice criteria curve and sample all have and the level and smooth upcurve zone that obviously separates is an optimum absorb wavelength.
(5) typical curve of drafting nitrogen in optimum absorb wavelength place working sample absorbance, calculates the sample nitrogen pool according to the mark song, and optimum absorb wavelength is 210nm among the present invention.
(6) drawing the digestion supernatant, add the colour developing of developer constant volume, is contrast with the blank, and 650～750nm length scanning is measured optimum absorb wavelength.Developer is the mixed liquid of stannous oxide or ammonium molybdate-potassium antimony tartrate and ascorbic acid, colour temp between 20～40 ℃, colour developing 30～60min, all samples developing time is identical with typical curve, 650～750nm length scanning is determined optimum absorb wavelength.
(7) typical curve of drafting phosphorus is measured absorbance at the optimum absorb wavelength place, calculate the sample total phosphorus content according to the mark song.Optimum absorb wavelength is 710nm among the present invention.
The present invention adopts persulfate combined digestion method to measure sediment, soil total nitrogen, total phosphorus, not only can once clear up the mensuration that just can carry out total nitrogen, total phosphorus simultaneously, measurement result is accurate, and the whole operation process is simple, save chemical reagent, time saving and energy saving, in large batch of sample analysis, can increase work efficiency.
Four, Figure of description
Part treatments of the sample liquid 190～290nm length scanning figure among the present invention when Fig. 1 is the mensuration total nitrogen;
Part treatments of the sample liquid 650～750nm length scanning figure among the present invention when Fig. 2 is the mensuration total phosphorus.
Five, embodiment
The invention will be further described below in conjunction with embodiment.
Get 10 kinds of different samples (4 of sediments, 6 in soil) and carry out the mensuration of total nitrogen, total phosphorus, each sample do 3 parallel.To cross 80～100 mesh sieves after the fresh sample freeze drying of gathering, pulverizing, the grinding, thorough mixing, it is stand-by to take by weighing a certain amount of color comparison tube that places.
1, medicine preparation:
(1) mixed nitrogen, the bent liquid that uses of phosphorus mark are prepared, and every milliliter is used nitrogenous 10 μ g in the liquid, phosphorous 5 μ g;
(2) alkaline potassium persulfate solution preparation, 20g K
2S
2O
4With 3g NaOH, be dissolved in no ammoniacal liquor and be settled to 1000ml;
(3) chromogenic reagent solution preparation, ascorbic acid solution, the mensuration [GB11893-89] that GB water quality total phosphorus is seen in the molybdate solution preparation;
2, Specimen eliminating:
(1) in the 50ml color comparison tube, adds 0ml, 1ml, 2ml, 3ml, 4ml, 6ml and 8ml nitrogen, the mixed liquid of the bent use of phosphorus mark respectively;
(2) weighing 20mg testing sample is put into color comparison tube;
(3) add alkaline potassium persulfate solution 25mL in color comparison tube, no ammoniacal liquor is diluted to 50mL;
(4) grinding port plug of jam-pack color comparison tube is tightened pipe close with gauze and cotton cord, and color comparison tube is placed pressure cooker, 121 ℃ of heating 30min, and take out the cooling back;
3, sample determination:
(1) determination of total nitrogen content: drawing the digestion supernatant and put into the 1cm quartz colorimetric utensil, is reference with the blank, carries out the scanning of 190～290nm ultraviolet wavelength, obtains accompanying drawing 1.Selecting the smoother elevated areas intermediate point of 200～220nm 210nm is optimum absorb wavelength, almost not variation of absorption peak between 250～290nm, wavelength is a background value between the choosing compromise, determine optimum absorb wavelength 210nm and background value wavelength 275nm, measure light absorption value, draw calibration curve regression equation y=0.0111x+0.0119, coefficient R=0.9964, and draw total nitrogen content in the sample, see Table 1.
(2) total phosphorus determination: draw 10ml digestion supernatant and put into another color comparison tube, add 1ml ascorbic acid 2ml molybdate solution, be diluted to 25ml with no ammoniacal liquor, mixing, temperature are about 25 ℃, and 30min develops the color, draw above-mentioned solution and put into the 1cm glass cuvette, with the blank is reference, carries out 650～750nm length scanning, obtains accompanying drawing 2.In the total phosphorus determination, phosphato-molybdic heteropolyacid reduces with ascorbic acid, it is peak system that heteropoly acid has obviously wide at 690～730nm, peak-peak is determined optimum absorb wavelength 710nm at 710nm, measures light absorption value, draw the regression equation y=0.0044x+0.0006 of calibration curve, coefficient R=0.9992, and draw the content of total phosphorus in the sample, see Table 1.
Ten kinds of separate sources sample measurements of table 1 result
4, persulfate combined digestion method of the present invention and traditional analysis (Kjeldahl method surveys nitrogen and sour molten method is surveyed phosphorus) methods and results is relatively:
Above-mentioned 10 different samples (6 pedotheques of 4 lake sediments), each sample do 3 parallel, classic method is measured total nitrogen, total phosphorus, result and The above results of the present invention invest table 2 with equation of linear regression.
Table 2 persulfate combined digestion method and traditional analysis methods and results are relatively
| Measure item | The actual sample number that uses | Regression equation | Related coefficient |
| TN | 7 | y＝1.054x+0.0043 | R＝0.948 |
| TP | 8 | y＝1.032x+0.0051 | R＝0.934 |
The result shows that use persulfate combined digestion method of the present invention is measured sediment total nitrogen, total phosphorus conforms to substantially with traditional analysis method measurement result, thereby the present invention is feasible.
Claims (4)
1, a kind of sediment total nitrogen, total phosphorus simultaneous determination analytical approach is characterized in that it may further comprise the steps:
(1) with the fresh sample drying of gathering, pulverize, sieve, thorough mixing, it is stand-by to take by weighing a certain amount of digestion vessel that places;
(2) the preparation digestive pharmaceutical adds digestive pharmaceutical, constant volume, mixing in the digestion vessel of the good sample of weighing;
(3) digestive juice in the digestion vessel and sample are carried out high temperature and clear up, take out the cooling back;
(4) with the blank be contrast, draw the digestion supernatant and carry out the scanning of 190～290nm ultraviolet wavelength, determine optimum absorb wavelength and background value;
(5) typical curve of drafting nitrogen in optimum absorb wavelength place working sample absorbance, calculates the sample nitrogen pool according to the mark song;
(6) drawing the digestion supernatant, add the colour developing of developer constant volume, is contrast with the blank, and 650～750nm length scanning is determined optimum absorb wavelength;
(7) typical curve of drafting phosphorus is measured absorbance at the optimum absorb wavelength place, calculate the sample total phosphorus content according to the mark song.
2, sediment total nitrogen according to claim 1, total phosphorus simultaneous determination analytical approach, it is characterized in that: in the step (2), digestive pharmaceutical adopts alkaline potassium persulfate, and proportioning is every liter and contains K
2S
2O
820g and NaOH3g.
3, sediment total nitrogen according to claim 1, total phosphorus simultaneous determination analytical approach is characterized in that: in the step (3), answer the grinding port plug of jam-pack digestion vessel before clearing up, wrap with gauze, can place high pressure steam pot high temperature to clear up; Digestion condition is 120～124 ℃, digestion time 30min.
4, sediment total nitrogen according to claim 1, total phosphorus simultaneous determination analytical approach, it is characterized in that: in the step (4), supernatant carries out 190～290nm length scanning, avoid responsive uptake zone, choice criteria curve and sample all have and the level and smooth upcurve zone that obviously separates is optimum absorb wavelength.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610085999XA CN100552427C (en) | 2006-06-16 | 2006-06-16 | Sediment total nitrogen, total phosphorus simultaneous determination analytical approach |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610085999XA CN100552427C (en) | 2006-06-16 | 2006-06-16 | Sediment total nitrogen, total phosphorus simultaneous determination analytical approach |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1869656A CN1869656A (en) | 2006-11-29 |
| CN100552427C true CN100552427C (en) | 2009-10-21 |
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| CN2104447U (en) * | 1991-10-30 | 1992-05-13 | 中国科学院沈阳应用生态研究所 | Combined complete soil N-P-K dispeling instrument |
| DE19954783A1 (en) * | 1999-11-15 | 2001-05-17 | Gerhard Flick | Process for detecting presence of nitrogen and/or carbon from organic substances comprises determining nitrogen and/or carbon content of fraction, measuring using reflection and/or transmission spectroscopy and calibrating |
-
2006
- 2006-06-16 CN CNB200610085999XA patent/CN100552427C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2104447U (en) * | 1991-10-30 | 1992-05-13 | 中国科学院沈阳应用生态研究所 | Combined complete soil N-P-K dispeling instrument |
| DE19954783A1 (en) * | 1999-11-15 | 2001-05-17 | Gerhard Flick | Process for detecting presence of nitrogen and/or carbon from organic substances comprises determining nitrogen and/or carbon content of fraction, measuring using reflection and/or transmission spectroscopy and calibrating |
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