Method for measuring contents of total nitrogen and total phosphorus contained in seawater substrate sludge by adopting combined digestion

A method of determination, a technology of phosphorus content, applied in the direction of material analysis by observing the influence of chemical indicators, and analysis by making materials undergo chemical reactions, etc., can solve the problems of no public literature reports, etc., and achieve accuracy High efficiency, improved work efficiency, easy and quick operation

Inactive Publication Date: 2011-09-07
CENT LAB TIANJIN ACADEMY OF AGRI SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The present invention designs the determination method of total nitrogen and total phosphorus in seawate

Method used

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  • Method for measuring contents of total nitrogen and total phosphorus contained in seawater substrate sludge by adopting combined digestion
  • Method for measuring contents of total nitrogen and total phosphorus contained in seawater substrate sludge by adopting combined digestion
  • Method for measuring contents of total nitrogen and total phosphorus contained in seawater substrate sludge by adopting combined digestion

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] (1) Preparation of sample solution: Weigh 1.0g of air-dried seabed sample that has passed through a Φ0.5mm sieve, add 8mL of sulfuric acid and 2mL of hydrogen peroxide, shake well and place overnight; slowly heat up the next day until the sulfuric acid emits smoke, remove it, and slightly After cooling, add a few drops of hydrogen peroxide and continue heating until the solution becomes colorless or off-white. Remove and cool slightly, add water to boil, remove and cool, transfer the digestion liquid to a volumetric flask without damage, add water to a constant volume, and let it stand Clarify or filter with non-phosphorus filter paper for use;

[0056] (2) Determination of total nitrogen: absorb 50mL of boiling liquid into the digestion tube, add 40mL sodium hydroxide solution (40%), the receiving solution is 25mL boric acid solution containing fixed nitrogen mixed indicator, heated and distilled, use 0.1mol / L hydrochloric acid standard solution titrate the distillate, t...

Embodiment 2

[0060] (1) Preparation of sample solution: Weigh 1.0g of air-dried sample that has passed through a Φ0.8mm sieve, add sulfuric acid and hydrogen peroxide, and shake it well overnight; the next day, slowly heat up until sulfuric acid emits smoke, remove it, and add it after cooling slightly A few drops of hydrogen peroxide, continue to heat until the solution becomes colorless or off-white, remove it and let it cool slightly, add water to boil, remove and cool, transfer the digestion liquid to a volumetric flask without damage, add water to a constant volume, set aside for clarification or use Filter with non-phosphorus filter paper for use; wherein the weight-volume ratio of sample: sulfuric acid: hydrogen peroxide is 1:6:2.

[0061] (2) Determination of total nitrogen: absorb 50mL of boiling liquid into the digestion tube, add 40mL sodium hydroxide solution (40%), the receiving solution is 25mL boric acid solution containing fixed nitrogen mixed indicator, heated and distilled, u...

Embodiment 3

[0065] Comparative Test:

[0066] (1) Determination by conventional method:

[0067] Sample; sea bottom mud sample

[0068] Determination of total nitrogen

[0069] Digestion: Weigh 0.5g of the air-dried seabed sample through a Φ0.5mm sieve, put it into a dry 50mL opener bottle, add 1.8g of mixed accelerator, add 2mL of water to make it moist, and then add 5mL of concentrated sulfuric acid. After shaking, cover the small funnel and place it on the electric stove. Start heating with a small fire. Take care to prevent the effect from being too strong, and then digest it slightly. When the digestion liquid is off-white, you can increase the temperature and wait until it becomes completely gray and slightly white. After green, continue to cook for 1 hour. The temperature during digestion should be such that the reflux height of sulfuric acid in the bottle is about 1 / 3 of the upper part of the bottleneck. Before the digestion is completed, carefully observe whether there are black carbo...

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Abstract

The invention relates to a method for measuring the contents of total nitrogen and total phosphorus contained in seawater substrate sludge by adopting combined digestion, comprising the following steps of: weighing 1.0 g of air-dried sample screened through a phi 0.5 mm sieve; adding 8 mL of sulfuric acid and 2 mL of hydrogen peroxide, carefully and uniformly shaking, and placing overnight; slowly increasing temperature till the sulfuric acid is smoky; slightly cooling, then adding a plurality of drops of hydrogen peroxide, and continuously heating till the solution is colourless or off-white; slightly cooling, adding water, and heating to boiling; taking down for cooling, nondestructively transferring a digested solution into a 100 mL volumetric flask, adding water, fixing volume, and standing for clarification or filtering by using phosphate-free filter paper; then sucking 10.0 mL of sample solution containing 0.05-1.0 mg of the phosphorus into a 50 mL volumetric flask, adding water to 20-30 mL, carrying out color development and color comparison with a standard solution series under same conditions, and reading absorbance; and carrying out a control experiment by respectively using standard substances, i.e. ammonium sulfate and monopotassium phosphate to measure the contents of the total nitrogen and the total phosphorus which are contained in the seawater substrate sludge. The measuring method has high accuracy and easiness, convenience and fastness for operation and is suitable for batched measurement, thereby enhancing the work efficiency.

Description

Technical field [0001] The invention belongs to the technical field of marine research and environmental protection. It involves the analysis method of total nitrogen and total phosphorus content in sea bottom mud. More specifically, it is a method that uses joint digestion to determine the total nitrogen and total phosphorus content of seabed mud. Background technique [0002] With the rapid development of the world economy, a large number of pollutants produced by humans are discharged into water bodies and gradually accumulate in the bottom sludge, causing the bottom sludge to be polluted to varying degrees. Among them, nitrogen and phosphorus are important elements of aquatic ecosystems. Excessive input can lead to eutrophication of water bodies and trigger red tides. A large part of the nutrients in nearshore water bodies comes from the exchange of materials between sediments and overlying water. The exchange and diffusion of nutrient elements at the material-water interfa...

Claims

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Application Information

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IPC IPC(8): G01N21/79
Inventor 刘烨潼陈秋生张强殷萍孟兆芳张玺
Owner CENT LAB TIANJIN ACADEMY OF AGRI SCI
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