CN104198415A - Method for testing total phosphorus in soil and sediments by virtue of microwave digestion ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) - Google Patents
Method for testing total phosphorus in soil and sediments by virtue of microwave digestion ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) Download PDFInfo
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Abstract
The invention provides a method for testing total phosphorus in soil and sediments by virtue of a microwave digestion ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry). According to the method, the recovery rate is 97.5%-106.2%, the relative standard deviation is 1.6%-3.4%, the detection limit is 5.74mg/kg (when the weighing dosage of a sample is 0.2500g and the volume of a digestion solution is set as 50ml); the correlation coefficient of a working curve is more than 0.9999 at 0-10.00mg/L, and the linearity is good; the method has no obvious difference from a national standard method on the testing result, and moreover the sample processing and testing processes are simple, convenient and rapid, so that the method has a preferable practical value.
Description
Technical field
The present invention relates to a kind of assay method of phosphorus content, relate in particular to a kind of method that micro-wave digestion ICP-AES method is measured total phosphorus in soils and sediments.
Background technology
Phosphorus is a kind of nonmetalloid comparatively widely that distributes on the earth, and occurring in nature mainly exists with various phosphatic forms, is biological metabolic indispensable element.Soil and stream sediment is as the important carrier of occurring in nature phosphorus, and to phosphorus, circulation plays vital effect.Under sluicing effect, the phosphorus in soil can enter water body, the too high algae excessive propagation that causes of the total phosphorus concentration, and then the eutrophication of initiation water body.
Assay method about P elements mainly contains spectrophotometric method, the chromatography of ions, atomic absorption spectrography (AAS), ICP-AES (ICP-AES) etc. at present.ICP-AES (ICP-AES), be to take the spectroscopic analysis methods that inductively coupled plasma square is excitation source, have that accuracy is high and precision is high, detection limit is low, mensuration is quick, the range of linearity is wide, can measure the advantages such as multiple element simultaneously.(Shandong is metallurgical for Zhang Li, the 1st phase in 2013, the phosphorus that 44-45) ICP-AES is measured in coke has been announced the content that a kind of ICP-AES of use method is measured phosphorus in coke, adopt ICP-AES to measure the phosphorus in coke, its accuracy and precision are good, measure the recovery of element at 98.7%-101.4%, method simple and fast, meets the requirement of analyzing and producing.CN 102564973 A are used ICP-AES method to measure the content of phosphorus, lead, zinc in iron dirt mud in industry.The ICP-AES that CN 103293144 A have announced foreign matter of phosphor content in a kind of iron and steel measures, and further illustrates accuracy and the precision of the method in phosphorus detection and more has superiority.
The pre-treating method of soils and sediments sample mainly contains NaOH fusion method, nitric acid-perchloric acid resolution method, potassium sulfate resolution method etc., its principle is under uniform temperature condition, highly basic or mixed strong acids are converted to the phosphorus of various forms in sample into solubility orthophosphate, then measure.NaOH fusion method sample decomposes completely, be the standard method of China's soil total phosphorus determination at present, but processing procedure is loaded down with trivial details, and labour intensity is large, and analysis time is long, is not suitable for the processing of batch samples, and the efficiency of whole analytical test is lower.It is also a kind of conventional Methods of Soil Digestion that electrical heating nitration mixture is cleared up, and decomposition efficiency has reached the requirement of analyzing total phosphorus, and operating performance is relatively simple, but due to the environment of clearing up of open type, and the sample preparation time is long is easily polluted, and energy consumption is larger.
Microwave digestion technology is a kind of quick sample pretreatment technology occurring in recent years, it combines the performance of high-pressure digestion and microwave heating two aspects, for the digestion process of sample provides an enclosed environment, have that solvent load is few, sample contamination is little, be easy to robotization control, favorable reproducibility, rapidly and efficiently, clear up the advantages such as ability is strong, environmental protection.CN 103558173 A have announced a kind of method that Microwave Digestion and FAAS is measured nickel content in soil, the sample that this method is processed have precision good, accurately and reliably, the recovery is high, advantage quickly and easily.A kind of water quality total phosphorus that CN 103267734 A announce is efficiently cleared up and the method for fast detecting, wherein reagent digestion procedure has solved the problem of process complexity that existing national standard detection method exists, time consumption and energy consumption, complex steps, meets the requirement of water quality total phosphorus field quick detection.
ICP-AES (ICP-AES) has been widely used in the mensuration of tens of kinds of elements in the samples such as environmental sample and rock, mineral, metal abroad, also fewer in the research aspect soil and sediment total phosphorus determination by microwave digestion technology processing sample.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method that micro-wave digestion ICP-AES method is measured total phosphorus content in soils and sediments, by micro-wave digestion rapidly and efficiently sample is carried out to pre-treatment, utilize accurately total phosphorus content in accurate measurement soils and sediments of ICP-AES method.
For achieving the above object, a kind of micro-wave digestion ICP-AES method is measured the method for total phosphorus content in soils and sediments, comprises the preparation of sample collection, typical curve and clearing up and mensuration of sample, and step comprises:
1, sample collection and processing
Sampling sample is removed the foreign material such as plant residue, stone after freeze drying, after being ground, sieves, and minute is filled to Polythene Bag and is placed in exsiccator and preserves.
2, the drafting of typical curve and working curve
With phosphorus solution, dilute the standard of preparation variable concentrations and use solution, with the deionized water using in testing, make blank, carry out the spectral intensity values of ICP-AES bioassay standard series solution.
3, Specimen eliminating and mensuration
By nitrate acid and hydrofluoric acid-hydrogen peroxide system, sample is cleared up.Accurately weigh a certain amount of sample and join in teflon digestion tube, each sample adds nitric acid dousing, clears up in advance soil is tentatively decomposed, then add hydrogen peroxide and hydrofluorite, adds a cover to be positioned in microwave system and clear up after question response is steady.Clear up complete cooling rear taking-up counteracting tank, digestion solution be transferred in teflon crucible, be placed on electric hot plate heating and catch up with acid, wait to no longer include white cigarette generate sample be thick till, cooling rear constant volume, after standing clarification, upper machine is measured.
Wherein, by the diagonal line method of layouting, gather topsoil soils, bed mud sample is used impact type column sediment sampler to gather.
The processing procedures such as wherein, mixing, pulverizing, grinding are used instrument all to use deionized water rinse 3 times.
Wherein, the top grade that nitric acid is preferably 65-70% is pure, and the top grade that hydrogen peroxide is preferably 30-40% is pure, and hydrofluorite is that 40-47% top grade is pure.
Wherein, take phosphorus concentration and spectral intensity as transverse and longitudinal coordinate drawing standard curve.
Wherein, the spectral intensity values of ICP-AES method working sample, and this spectral intensity values is contrasted with typical curve, obtain total phosphorus concentration.
Wherein, the reagent of standard phosphorus solution preparation is that orthophosphoric acid and/or its salt are selected from phosphoric acid, phosphate, hydrophosphate, dihydric phosphate, is preferably potassium dihydrogen phosphate.
Wherein, the condition of micro-wave digestion is, microwave power 600 ~ 1600W keeps 15 ~ 30 minutes after within 30 minutes, being warming up to 190 ~ 210 ℃.
Wherein, the condition of work of ICP-AES is: RF generator power 1180 ~ 1300W, cold gas 12 ~ 19L/min, flow rate of carrier gas 0.5 ~ 0.9L/min, plasma (orifice) gas 0.2 ~ 0.4L/min, observed altitude 14 ~ 16mm, sample introduction speed 1.0 ~ 1.8ml/min, according to actual conditions by instrument regulation to optimum Working.
Beneficial effect: a kind of micro-wave digestion ICP-AES method provided by the invention is measured the method for total phosphorus content in soils and sediments, micro-wave digestion ICP-AES method is measured total phosphorus in soil, the measurement result of soil national standard material and actual sample is comparatively desirable, the recovery is between 97.5%-106.2%, relative standard deviation is 1.6%-3.4%, detecting and being limited to the 5.74mg/kg(sample amount of taking is 0.2500g, and digestion solution is settled to 50ml).Working curve is greater than 0.9999 in 0-10.00mg/L related coefficient, linear good.(1) this method is with the measurement result of national standard method without significant difference, and sample preparation and mensuration are easier fast, have good practical value; (2) sample-pretreating method can be applicable to clearing up and extracting of common heavy metal simultaneously; (3) H
2o
2add and be particularly conducive to clearing up of organophosphorus in sample.
Accompanying drawing explanation
Fig. 1 is the total phosphorus working curve (typical curve) that the present invention prepares.
Embodiment
In conjunction with embodiment, the present invention is described in further detail.
1.1 instruments and reagent
Instrument: inductive coupling plasma emission spectrograph, microwave digestion system, electronic analytical balance; Freeze drier, visible spectrophotometer.
Reagent: hydrofluorite (top grade is pure), nitric acid (top grade is pure), 30% hydrogen peroxide (top grade is pure), potassium dihydrogen phosphate (analyzing pure), soil national standard material.
1.2 instrument conditions of work
ICP-AES condition of work: RF generator power: 1300W; Cold gas: 15.0L/min; Flow rate of carrier gas: 0.8L/min; Plasma (orifice) gas: 0.2L/min; Observed altitude: 15mm; Sample introduction speed: 1.5ml/min.
Micro-wave digestion condition: microwave power 1600W, keeps 15 minutes after being warming up to 190 ℃ in 30 minutes.
1.3 sample collection
Soil and bed mud sample are taken from section, suburbs, Ningbo City, Zhejiang Province and near farmland soil.Sample is removed the foreign material such as plant residue, stone after freeze drying, after being ground, sieves, and minute is filled to Polythene Bag and is placed in exsiccator and preserves.The processing procedures such as mixing, pulverizing, grinding are used instrument all to use deionized water rinse 3 times.By the diagonal line method of layouting, gather topsoil soils, bed mud sample is used impact type column sediment sampler to gather.
1.4 experimental technique
1.4.1 the preparation of typical curve
By the standard of 5 kinds of variable concentrations of potassium dihydrogen phosphate standard solution dilution preparation, use solution, to test with deionized water, make blank, the spectral intensity values according to 1.2 joint condition of work bioassay standard series solution, the results are shown in Table 1.
Response spectrum intensity and phosphorus concentration are carried out to linear fit and obtain working curve: Y=977.5X-24.3, R
2=0.99996, wherein Y-axis is spectral intensity, and X-axis is phosphorus concentration.It is fine that ICP-AES measures the working curve correlativity of total phosphorus as can be seen from Figure 1, and to compare the range of linearity wider with National Standard Method.
Molybdenum-antimony anti-spectrophotometric method in National Standard Method is used 30mm cuvette, and concentration absorbance when 1.5mg/L just reaches 0.9, and higher concentration sample need dilute rear mensuration.And concentration of the present invention while reaching 10mg/L also without dilution, there is good linearity, can directly measure.
1.4.2 sample clears up and mensuration
Adopt nitrate acid and hydrofluoric acid-hydrogen peroxide system to clear up sample.Accurately weigh sample 0.2500g and join in teflon digestion tube, each sample adds nitric acid dousing, clears up in advance soil is tentatively decomposed, and adds hydrogen peroxide and hydrofluorite, after adding a cover, is positioned in microwave system and clears up after question response is steady.Every batch sample is done blank and Duplicate Samples simultaneously.Clear up complete cooling rear taking-up counteracting tank, digestion solution is transferred in polytetrafluoro crucible, be placed into heating on electric hot plate and catch up with acid, wait to no longer include white cigarette generate sample be thick till, cooling rear constant volume, after standing clarification, measures examination with computer according to 1.2 joint instrument conditions of work.
2. result and discussion
2.1 method control tests
According to method and national standard method herein, respectively the phosphorus content of six actual samples of S1-S6 is measured, concrete outcome is as shown in table 2.Utilize t check to carry out significant difference analysis to above-mentioned two groups of data, calculate t=0.934, t0.05=2.571, t < t0.05, P=0.3932 > 0.05.Visible, the measurement result there was no significant difference of the micro-wave digestion ICP-AES law and state standard method that this experiment is used to this batch of soil.
2.2 method detection limits
Low concentration sample is carried out to 12 duplicate measurementss, and detection limit calculates divided by working curve slope by the standard deviation of 3 times of spectral intensity results, is 0.0287mg/L, is converted in solid sample and detects and be limited to 5.74mg/kg.
2.3 accuracy and precision
Accurately take soil national standard material and clear up, and replication 7 times, the results are shown in Table 4.Actual sample S-2 and S-6 be replication 7 times also, and relative standard deviation is 2.1%-3.4%; Method precision is good.Standard soil test mean value is respectively 3.7% and 1.0% with the relative deviation of demarcating true value, and relative deviation calculates divided by demarcating true value according to both differences; Actual sample is carried out to mark-on recovery test, to S1-S6 sample, add a certain amount of standard solution, according to 1.2 joint conditions of work, clear up and measure, calculate the recovery of standard substance, the results are shown in Table 5.Can see, the recovery of standard addition of sample is between 97.5%-106.2%, and the method has good accuracy.
3. conclusion
Micro-wave digestion ICP-AES method is measured total phosphorus in soil, the measurement result of soil national standard material and actual sample is comparatively desirable, the recovery is between 97.5%-106.2%, relative standard deviation is 1.6%-3.4%, detect and be limited to the 5.74mg/kg(sample amount of taking at 0.2500g, digestion solution is settled to 50ml).Working curve is greater than 0.9999 in 0-10.00mg/L related coefficient, linear good.This method is with the measurement result of national standard method without significant difference, and sample preparation and mensuration are easier fast, have good practical value.
Above specific embodiments of the invention be have been described in detail, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and alternative also all among category of the present invention.Therefore, equalization conversion and the modification done without departing from the spirit and scope of the invention, all should contain within the scope of the invention.
Claims (9)
1. micro-wave digestion ICP-AES method is measured a method for total phosphorus in soil and/or sediment, it is characterized in that, step comprises:
A. sample collection and processing: wherein, remove after sampling after foreign material are ground and sieve;
B. Specification Curve of Increasing: wherein, take phosphorus concentration and spectral intensity as transverse and longitudinal coordinate drawing standard curve;
C. Specimen eliminating: wherein, by nitrate acid and hydrofluoric acid-hydrogen peroxide system, sample is cleared up in advance, then cleared up in microwave system;
The spectral intensity values of d.ICP-AES method working sample, and this spectral intensity values is contrasted with typical curve, total phosphorus concentration obtained; Wherein, described Specification Curve of Increasing method is: with the standard serial solution of orthophosphoric acid and/or its salt preparation different phosphate concentration, with deionized water, make blank, carry out the spectral intensity values of ICP-AES bioassay standard series solution.
2. method according to claim 1, it is characterized in that, ICP-AES condition of work is: RF generator power 1180 ~ 1300W, cold gas 12 ~ 19L/min, flow rate of carrier gas 0.5 ~ 0.9L/min, plasma (orifice) gas 0.2 ~ 0.4L/min, observed altitude 14 ~ 16mm, sample introduction speed 1.0 ~ 1.8ml/min, according to actual conditions by instrument regulation to optimum Working.
3. method according to claim 1, is characterized in that, the condition of micro-wave digestion is: microwave power 600 ~ 1600W, keeps 15 ~ 30 minutes after within 30 minutes, being warming up to 190 ~ 210 ℃.
4. method according to claim 1, is characterized in that, the described step of clearing up is in advance: accurately weigh sample and join in teflon digestion tube, add nitric acid dousing and clear up in advance, then carry out micro-wave digestion after adding hydrogen peroxide and hydrofluorite stable reaction.
5. according to the method described in claim 1 or 4, it is characterized in that, the concentration of nitric acid is 65-70%, and the concentration of hydrofluorite is 40-47%, and the concentration of hydrogen peroxide is 30-40%.
6. method according to claim 1, is characterized in that, clear up complete sample cooling after, digestion solution is transferred in teflon crucible, in electric hot plate heating, catch up with acid, wait to no longer include white cigarette generate sample be thick till, cooling rear constant volume.
7. method according to claim 1, is characterized in that, described orthophosphoric acid and/or its salt are selected from phosphoric acid, phosphate, hydrophosphate, dihydric phosphate.
8. method according to claim 7, is characterized in that, with potassium dihydrogen phosphate, prepares described standard serial solution.
9. method according to claim 1, is characterized in that, by the diagonal line method of layouting, gathers topsoil soils, and bed mud sample is used impact type column sediment sampler to gather.
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| CN105092496A (en) * | 2015-08-14 | 2015-11-25 | 武钢集团昆明钢铁股份有限公司 | Method for detecting content of phosphorus in nitrification intensifier |
| CN105158054A (en) * | 2015-06-05 | 2015-12-16 | 浙江海洋学院 | Method for determining total phosphorus concentration of seawater sediment by microwave digestion adopting small sample amount of potassium persulphate |
| CN106092720A (en) * | 2016-08-19 | 2016-11-09 | 上海应用技术学院 | A kind of Soil K+adsorption measures the micro-wave digestion pre-treating method of total sodium potassium calcium content |
| CN106248772A (en) * | 2015-06-05 | 2016-12-21 | 天津市农业质量标准与检测技术研究所 | A kind of use combined digestion to measure the method for harmful heavy metal content in edible fungus culturing substrate simultaneously |
| CN106569246A (en) * | 2016-10-28 | 2017-04-19 | 南京理工大学 | Method for analyzing radioactive activity based on heavy metal content in sludge |
| CN107192683A (en) * | 2017-07-25 | 2017-09-22 | 福建海峡环保集团股份有限公司 | A kind of method of total phosphorus in measure sludge |
| CN107462690A (en) * | 2016-06-06 | 2017-12-12 | 杭州中检测研究院有限公司 | A kind of Soil K+adsorption method and its application |
| CN108267358A (en) * | 2018-01-17 | 2018-07-10 | 睿科仪器（厦门）有限公司 | A kind of automatic capping takes the Specimen eliminating instrument of lid |
| CN109883810A (en) * | 2019-03-26 | 2019-06-14 | 攀钢集团攀枝花钢铁研究院有限公司 | The digestion procedure and detection method of titanium slag or vanadium slag |
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| CN117990772A (en) * | 2024-04-07 | 2024-05-07 | 中国科学院生态环境研究中心 | Method for determining phosphorus element in plant by utilizing ICP-MS |
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Cited By (13)
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| CN105158054A (en) * | 2015-06-05 | 2015-12-16 | 浙江海洋学院 | Method for determining total phosphorus concentration of seawater sediment by microwave digestion adopting small sample amount of potassium persulphate |
| CN106248772A (en) * | 2015-06-05 | 2016-12-21 | 天津市农业质量标准与检测技术研究所 | A kind of use combined digestion to measure the method for harmful heavy metal content in edible fungus culturing substrate simultaneously |
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| CN107462690A (en) * | 2016-06-06 | 2017-12-12 | 杭州中检测研究院有限公司 | A kind of Soil K+adsorption method and its application |
| CN107462690B (en) * | 2016-06-06 | 2019-12-10 | 杭州中一检测研究院有限公司 | Soil detection method and application thereof |
| CN106092720A (en) * | 2016-08-19 | 2016-11-09 | 上海应用技术学院 | A kind of Soil K+adsorption measures the micro-wave digestion pre-treating method of total sodium potassium calcium content |
| CN106569246A (en) * | 2016-10-28 | 2017-04-19 | 南京理工大学 | Method for analyzing radioactive activity based on heavy metal content in sludge |
| CN107192683A (en) * | 2017-07-25 | 2017-09-22 | 福建海峡环保集团股份有限公司 | A kind of method of total phosphorus in measure sludge |
| CN108267358A (en) * | 2018-01-17 | 2018-07-10 | 睿科仪器（厦门）有限公司 | A kind of automatic capping takes the Specimen eliminating instrument of lid |
| CN109883810A (en) * | 2019-03-26 | 2019-06-14 | 攀钢集团攀枝花钢铁研究院有限公司 | The digestion procedure and detection method of titanium slag or vanadium slag |
| CN112834685A (en) * | 2020-12-31 | 2021-05-25 | 中国环境监测总站 | Method for measuring total phosphorus concentration in surface water |
| CN117990772A (en) * | 2024-04-07 | 2024-05-07 | 中国科学院生态环境研究中心 | Method for determining phosphorus element in plant by utilizing ICP-MS |
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