WO2020108030A1 - 一种同步测量土壤中胶体磷和纳米颗粒态磷的方法 - Google Patents

一种同步测量土壤中胶体磷和纳米颗粒态磷的方法 Download PDF

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WO2020108030A1
WO2020108030A1 PCT/CN2019/106538 CN2019106538W WO2020108030A1 WO 2020108030 A1 WO2020108030 A1 WO 2020108030A1 CN 2019106538 W CN2019106538 W CN 2019106538W WO 2020108030 A1 WO2020108030 A1 WO 2020108030A1
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phosphorus
soil
colloidal
supernatant
filtrate
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李发永
梁新强
何霜
金俊伟
刘枫
晋迎兵
王子琬
张楚旋
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Zhejiang University
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/24—Earth materials
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
    • G01N9/36—Analysing materials by measuring the density or specific gravity, e.g. determining quantity of moisture

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  • the invention belongs to the field of soil nutrient monitoring, and relates to a method for simultaneously measuring colloidal phosphorus and nanoparticulate phosphorus in soil by means of ultrafiltration.
  • Phosphorus is one of the important biogenic factors.
  • the soil phosphorus reservoir not only directly affects the soil fertility and agricultural production, but also causes frequent eutrophication of the water body due to the loss of soil phosphorus, which has caused widespread concern in the environmental field and society.
  • the phosphorus element in the soil has accumulated in large quantities. Studies have shown that the accumulation of phosphorus in the soil far exceeds the needs of crops.
  • the traditional view is that the loss of phosphorus in the soil is mainly due to the application of chemical fertilizers that causes the dissolved phosphorus in the soil to flow into the water body with rainwater and irrigation water.
  • Soil colloids are particles with a particle size between 1 nm and 1 ⁇ m, usually including inorganic colloids composed of minerals such as iron, aluminum oxide, clay minerals, organic colloids such as organic macromolecules, microorganisms, and organic-inorganic composites formed by the interaction of minerals and organic matter Colloids are widely present in the soil and water environment. Because of its small particle size, large specific surface area, strong reactivity, and other physical and chemical properties, it can be suspended in soil solution for a long time and has strong mobility. It is the main way for pollutants in soil systems to migrate to water bodies.
  • Soil colloidal phosphorus is a fine-grained phosphorus formed by the combination of soil phosphorus with inorganic mineral colloids such as iron/aluminum oxide, clay minerals, organic colloids such as organic macromolecules, microorganisms, and organic-inorganic composite colloids.
  • Colloid is an important carrier for the long-distance transport of nutrients such as phosphorus. Colloid-facilitated transport has been proved to be an important way for phosphorus transport in soil solutions, surface water bodies and agricultural non-point source pollution.
  • the analysis methods of colloidal phosphorus mainly include gravity centrifugal separation method and field flow separation method.
  • the gravity concentration separation method requires low-temperature centrifugation at 300 g of centrifugal force for 2 hours.
  • the entire step is cumbersome, and an expensive ultra-high-speed centrifuge is required, and consumables such as centrifuge tubes and other expensive materials are used. 4h, time-consuming and laborious.
  • Field flow separation is a technology for the separation of large molecules (biological macromolecules and synthetic polymers), colloids, nanoparticles, etc.
  • the basic principle is that macromolecules flow through the flat channel and are affected by the horizontal and vertical flow fields at the same time; molecules with relatively small sizes are subject to vertical forces and move toward the center of the flat channel; the size is relatively large Of the molecules, which are affected by the vertical force, are closer to the aggregation wall.
  • a dimension gradient is formed in the vertical direction.
  • the relatively small-sized component is detected by the rear-end detector first; the larger-sized component is subsequently detected. So as to achieve the purpose of separation.
  • the effect of the field-flow separation method is relatively good, it also requires an expensive field-flow separation instrument, whose price ranges from 500,000 to 1 million.
  • the purpose of the present invention is to solve the defects in the concentration and separation of colloidal phosphorus in the prior art, and to provide a method for simultaneously measuring colloidal phosphorus and nanoparticulate phosphorus in soil.
  • a method for simultaneously measuring colloidal phosphorus and nanoparticulate phosphorus in soil includes the following steps:
  • Soil colloidal phosphorus content (TP 1 -TP 2 ) ⁇ V 1 /m
  • Nano-particulate phosphorus content in soil (TP 3 -TP 4 ) ⁇ V 1 /m.
  • the size of the colloidal phosphorus particles separated by this method is 3KDa-1 ⁇ m, which basically matches the definition range of colloidal particles of 1nm-1 ⁇ m, and the colloidal size obtained by using a 1 ⁇ m filter membrane is relatively accurate.
  • the particles of 3KDa-1000KDa separated by ultrafiltration are in line with the nanoparticles, which basically matches the definition range of nanoparticles of 1nm-100nm. Therefore, the particle size measured above is really effective.
  • the soil sample is a soil sample that has not been ground and passed through an 8mm sieve.
  • step S1 the soil sample and deionized water are mixed at a soil-water ratio of 1:8, then moved to a shaker, and leached at 150-160 rpm for 16-24 hours.
  • the amount of primary filtrate discarded is 5 mL.
  • the concentrated size of colloidal phosphorus is 3KDa-1 ⁇ m.
  • the concentrated size of the nanoparticulate phosphorus is 3KDa-1000KDa.
  • the concentration and separation time of colloidal phosphorus has been reduced from the average gravity separation method of 4 hours per sample to 20 minutes per sample, eliminating the need for expensive ultra-high-speed centrifugal equipment.
  • This method can not only concentrate and separate colloidal phosphorus, but also separate nano-particulate phosphorus and accurately measure its content in soil.
  • the first ultrafiltration filtrate sample to be tested into the 3KDa, 4000g ultracentrifugation 40min, total phosphorus concentration in the supernatant was measured TP 2, the supernatant is removed true colloid component dissolved phosphorus component ,
  • the bottom of the ultrafiltration tube is water-diffusing colloidal phosphorus concentrate; put the second filtrate test sample into the ultrafiltration sample in a 1000KDa ultrafiltration tube, ultracentrifuge at 3000g for 20min, and take the supernatant to determine the total phosphorus Concentration TP 3 , the supernatant is a solution of the nanoparticle component that removes the colloidal component of large particles; then put the obtained supernatant into a 3KD ultrafiltration tube, ultracentrifuge at 4000g for 40min, and then take the supernatant
  • the total phosphorus concentration TP 4 is determined in the solution, the supernatant is the true dissolved component to remove the nano particles, and the bottom of the ultrafiltration tube is the nano particle
  • Table 1 is the comparison of colloidal phosphorus content measured by gravity separation method and the above ultrafiltration concentration separation method
  • the average content of the nanoparticulate phosphorus measured by this method is 2.58 mg/kg.
  • the error is only 0.05mg/kg. Since there is no mature method for determining nano-particulate phosphorus, this method cannot be compared with other methods.
  • the particles obtained by the processing method of this method basically match the definition range of nano-particle phosphorus in the range of 1 nm-100 nm. Therefore, in theory, the range of nano particles measured by this method is accurate and the precision is high.
  • the first ultrafiltration filtrate sample to be tested into the 3KDa, 4000g ultracentrifugation 40min, total phosphorus concentration in the supernatant was measured TP 2, the supernatant is removed true colloid component dissolved phosphorus component ,
  • the bottom of the ultrafiltration tube is water-diffusing colloidal phosphorus concentrate; put the second filtrate test sample into the ultrafiltration sample in a 1000KDa ultrafiltration tube, ultracentrifuge at 3000g for 20min, and take the supernatant to determine the total phosphorus Concentration TP 3 , the supernatant is a solution of nano-particle components to remove large-particle colloid components; then put the obtained supernatant into a 3KD ultrafiltration tube, ultracentrifuge at 4000g for 30min, and then take the supernatant
  • the total phosphorus concentration TP 4 is determined in the solution, the supernatant is the true dissolved component to remove the nano particles, and the bottom of the ultrafiltration tube is the nano particle state
  • Table 3 compares the colloidal phosphorus content measured by the gravity separation method and the above ultrafiltration concentration separation method
  • the colloidal phosphorus content measured by this method is very close to that measured by the traditional gravity separation method.
  • the average value of the colloidal phosphorus measured by the traditional method is 2.46 mg/kg, and the average value of the colloidal phosphorus measured by this method is also 2.46mg/kg.
  • the measurement error of this method is only 0.05mg/kg, which is much smaller than the traditional method of 0.23mg/kg. Therefore, this method has good detection stability and can effectively separate and quickly and accurately detect colloidal phosphorus in soil.
  • the average content of nanoparticulate phosphorus measured by this method is 0.87 mg/kg.
  • the error is only 0.06mg/kg. Since there is no mature method for determining nano-particulate phosphorus, this method cannot be compared with other methods.
  • the particles obtained by the processing method of this method basically match the definition range of nano-particle phosphorus in the range of 1 nm-100 nm. Therefore, in theory, the range of nano particles measured by this method is accurate and the precision is high.

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Abstract

一种同步测量土壤中胶体磷和纳米颗粒态磷的方法，该方法将土壤样品的浸提上清液预离心，然后用1μm微孔滤膜抽滤；抽滤所得样品中取出两份作为待测样品，第一份滤液待测样品放入3KDa的超滤管中，4000g下超速离心30～40min，取上清液测定总磷浓度TP 2；第二份滤液待测样品先放入超滤试样在1000KDa的超滤管中，3000g下超速离心20min，取上清液测定总磷浓度TP 3；然后再将获得的上清液放入3KD的超滤管中，4000g下超速离心40min，再取上清液测定总磷浓度TP 4，最后根据测定结果计算土壤中胶体磷和纳米颗粒态磷的含量。该方法对传统的重力分离和场流分离方法进行了改进，大大简化胶体磷测定分析步骤，缩短了测定时间，并且能有效的分离纳米颗粒态磷。

Description

一种同步测量土壤中胶体磷和纳米颗粒态磷的方法 技术领域
本发明属于土壤养分监测领域，涉及一种利用超滤的方式同步测量土壤中胶体磷和纳米颗粒态磷的方法。
背景技术
磷是重要的生源要素之一，土壤磷库不仅直接影响着土壤肥力及农业生产，还因土壤磷素流失导致水体富营养化问题频发而引起了环境领域及社会的广泛关注。近年来，随着化肥的大量投入，土壤中的磷元素大量累积，研究表明土壤磷的累积量远远超过了作物的需求。传统观点认为土壤中磷的流失主要是由于化肥施用导致了土壤中的溶解态磷随着雨水和灌溉水而流入水体。但是，近年来的研究表明，土壤磷素向水体的迁移实际上与土壤胶体磷颗粒密切相关。土壤胶体是粒径介于1nm至1μm之间的颗粒，通常包括铁、铝氧化物、粘土矿物等矿物组成的无机胶体，有机大分子、微生物等有机胶体以及矿物和有机质交互形成的有机无机复合胶体，广泛存在于土壤与水体环境中。由于土壤胶体粒径小，比表面积大，反应活性强等理化特性，能够在土壤溶液中长期悬浮，具有较强的移动性，是土壤系统中污染物向水体迁移的主要途径。土壤胶体磷即土壤磷与铁/铝氧化物、粘土矿物等无机矿物胶体，有机大分子、微生物等有机胶体以及有机-无机复合胶体结合形成的一种细颗粒态磷。胶体是磷等营养元素长距离运移的重要载体，胶体易化运移已被证实是土壤溶液、地表水体以及农业面源污染中磷素运移的重要途径
但关于土壤胶体结合磷的检测分析方法还很匮乏，目前，胶体磷的分析方法主要有重力离心分离法和场流分离法。其中，重力浓缩分离法，需要在300 000g的离心力下低温离心2h，整个步骤及其繁琐，需要用到价格昂贵的超高速离心机，且离心管等耗材及其昂贵，测定1个样品平均需要4h，费时费力。场流分离是一种针对大分子(生物大分子和合成高分子)，胶体，纳米颗粒等分离的技术。其基本原理是大分子流过扁平通道，同时受到水平和垂直方向的流场作用； 尺寸相对小的分子，受垂直方向的作用力较小，而向扁平通道中心平移扩散；而尺寸相对较大的分子，受垂直方向的作用力较大而更靠近聚集壁。从而在垂直方向形成尺寸梯度。而流体在扁平通道内，越靠近中心，流速越快，而越靠近边缘，流速越均匀，越缓慢。因此，尺寸相对较小的组分先被后端检测器检测到；而较大尺寸的组分随后被检测。从而达到分离的目的。虽然场流分离的方法效果也比较好，但是其也需用到价格昂贵的场流分离仪，其价格50-100万不等。
因此，如何降低土壤胶体磷和纳米颗粒态磷的检测分析成本以及耗时，是本发明亟待解决的技术问题。
发明内容
本发明的目的在于解决现有技术中胶体磷浓缩分离存在的缺陷，并提供一种同步测量土壤中胶体磷和纳米颗粒态磷的方法。
本发明所采用的具体技术方案如下：
一种同步测量土壤中胶体磷和纳米颗粒态磷的方法，其包括如下步骤：
S1：称取m克过筛的土样于锥形瓶中，加V 1毫升去离子水，浸提；
S2：浸提上清液在3000～3500g下预离心10～12min以去除大颗粒，取预离心后的上清液用1μm微孔滤膜抽滤，弃去初滤液后收集所有滤液；将收集的滤液混匀后，测定其总磷浓度TP 1(mg/L)；同时从混匀的滤液中取出两份作为待测样品；
S3：将第一份滤液待测样品放入3KDa的超滤管中，4000g下超速离心30～40min，取上清液测定总磷浓度TP 2(mg/L)，该上清液为去除胶体组分的真溶解态磷组分，超滤管底部为水扩散性胶体磷浓缩液；
S4：将第二份滤液待测样品先放入超滤试样在1000KDa的超滤管中，3000g下超速离心20min，取上清液测定总磷浓度TP 3(mg/L)，该上清液为去除大颗粒胶体组分的纳米颗粒态组分溶液；然后再将获得的上清液放入3KD的超滤管中，4000g下超速离心40min，再取上清液测定总磷浓度TP 4(mg/L)，该上清液为去除纳米颗粒的真溶解态组分，超滤管底部为纳米颗粒态磷浓缩液；
S5：计算土壤中胶体磷的含量(mg/kg)，计算公式为：
土壤胶体磷含量＝(TP 1-TP 2)×V 1/m
计算土壤中纳米颗粒态磷的含量(mg/kg)，计算公式为：
土壤中纳米颗粒态磷含量＝(TP 3-TP 4)×V 1/m。
本发明中，采用本方法分离获得的胶体磷颗粒的尺寸为3KDa-1μm，基本吻合1nm-1μm的胶体颗粒定义范围，利用1μm的滤膜获得的胶体尺寸相对比较精确。采用超滤方法分离获得的3KDa-1000KDa的颗粒符合纳米颗粒，基本吻合1nm-100nm的纳米颗粒态磷定义范围。因此，上述测定的颗粒尺寸真是有效。
作为优选，所述的土样为未经过研磨且过8mm筛的土样。
作为优选，步骤S1中，土样与去离子水以土水比1:8混合，然后移至摇床中，在150～160rpm下浸提16～24h。
作为优选，步骤S2中，初滤液的弃去量为5mL。
作为优选，胶体磷的浓缩尺寸为3KDa-1μm。
作为优选，纳米颗粒态磷的浓缩尺寸为3KDa-1000KDa。
该发明具有以下技术优势：
胶体磷的浓缩分离时间由原来重力分离方法的平均每个样品4h降低到了每个样品20min，不再需要昂贵的超高速离心设备。本方法不但可以浓缩分离胶体磷，而且可以分离纳米颗粒态磷，并对其在土壤中的含量进行准确测量。
具体实施方式
下面结合具体实施方式对本发明做进一步阐述和说明。本发明中各个实施方式的技术特征在没有相互冲突的前提下，均可进行相应组合。
为了使本领域的技术人员能够更好的理解本发明的具体测定方法，下面结合具体实施案例对本发明进一步说明，但所举案例不作为本发明的限定。
实施例1：
从浙江省桐庐县采集0-20cm土壤3份，带回实验室后，将土壤自然风干，称取10g待测未经研磨土样，过8mm筛，放入250mL锥形瓶中，加去离子水80mL，土水比1:8，移至摇床中，在160rpm下浸提24h。浸提上清液在3000g下预离心12min以去除大颗粒，取预离心后的上清液用1μm微孔滤膜抽滤，弃去5mL初滤液后收集所有滤液，测量收集滤液体积约75mL；将收集的滤液混匀后，测定其总磷浓度TP1；同时从混匀的滤液中取出两份作为待测样品；
将第一份滤液待测样品放入3KDa的超滤管中，4000g下超速离心40min，取上清液测定总磷浓度TP 2，该上清液为去除胶体组分的真溶解态磷组分，超滤 管底部为水扩散性胶体磷浓缩液；将第二份滤液待测样品先放入超滤试样在1000KDa的超滤管中，3000g下超速离心20min，取上清液测定总磷浓度TP 3，该上清液为去除大颗粒胶体组分的纳米颗粒态组分溶液；然后再将获得的上清液放入3KD的超滤管中，4000g下超速离心40min，再取上清液测定总磷浓度TP 4，该上清液为去除纳米颗粒的真溶解态组分，超滤管底部为纳米颗粒态磷浓缩液；土壤胶体磷含量(mg/kg)＝(TP 1-TP 2)×80mL/10g，土壤中纳米颗粒态磷含量(mg/kg)＝(TP 3-TP 4)×80mL/10g。本实施例中胶体磷的测定结果如表1所示，纳米颗粒态磷的测定结果如表2所示。
表1为重力分离方法和上述超滤浓缩分离方法测定的胶体磷含量的对比
Figure PCTCN2019106538-appb-000001
由表1可知，本方法测定的胶体磷含量和传统的重力分离方法测定的胶体磷含量值非常接近，传统方法的胶体磷平均值为7.55mg/kg，本方法测定的胶体磷平均值为7.73mg/kg。且本方法测定的误差只有0.06mg/kg，远小于传统方法的0.30mg/kg。因此，本方法具良好的检测稳定性，可以有效分离和快速准确的检测土壤中的胶体磷。
表2超滤浓缩分离方法测定的纳米颗粒态磷含量
Figure PCTCN2019106538-appb-000002
由表2可知，本方法测定的纳米颗粒态磷的平均含量为2.58mg/kg。误差只有0.05mg/kg。由于目前还没有成熟的纳米颗粒态磷测定方法，为此，本方法不能与其他方法进行比较。但本方法的处理过程得到的颗粒基本吻合1nm-100nm的纳米颗粒态磷定义范围，因此理论上本方法测定的纳米颗粒范围准确，精度较高。
实施例2：
从浙江开化县采集茶园土壤，采集0-20cm土层土壤3份，带回实验室后，将土壤自然风干，称取5g待测未经研磨土样，过8mm筛，放入250mL锥形瓶中，加去离子水40mL，土水比1:8，移至摇床中，在150rpm下浸提16h。浸提上清液在3500g下预离心10min以去除大颗粒，取预离心后的上清液用1μm微孔滤膜抽滤，弃去5毫升初滤液后收集所有滤液，测量收集滤液体积约35mL；将收集的滤液混匀后，测定其总磷浓度TP 1；同时从混匀的滤液中取出两份作为待测样品；
将第一份滤液待测样品放入3KDa的超滤管中，4000g下超速离心40min，取上清液测定总磷浓度TP 2，该上清液为去除胶体组分的真溶解态磷组分，超滤管底部为水扩散性胶体磷浓缩液；将第二份滤液待测样品先放入超滤试样在1000KDa的超滤管中，3000g下超速离心20min，取上清液测定总磷浓度TP 3，该上清液为去除大颗粒胶体组分的纳米颗粒态组分溶液；然后再将获得的上清液放入3KD的超滤管中，4000g下超速离心30min，再取上清液测定总磷浓度TP 4，该上清液为去除纳米颗粒的真溶解态组分，超滤管底部为纳米颗粒态磷浓缩液；土壤胶体磷含量(mg/kg)＝(TP 1-TP 2)×40mL/5g，土壤中纳米颗粒态磷含量(mg/kg)＝(TP 3-TP 4)×40mL/5g。本实施例中胶体磷的测定结果如表3所示，纳米颗粒态磷的测定结果如表3所示。
表3为重力分离方法和上述超滤浓缩分离方法测定的胶体磷含量的对比
Figure PCTCN2019106538-appb-000003
由表3可知，本方法测定的胶体磷含量和传统的重力分离方法测定的胶体磷含量数值非常接近，传统方法的胶体磷平均值为2.46mg/kg，本方法测定的胶体磷平均值也为2.46mg/kg。且本方法测定的误差只有0.05mg/kg，远小于传统方法的0.23mg/kg。因此，本方法具良好的检测稳定性，可以有效分离和快速准确的检测土壤中的胶体磷。
表4超滤浓缩分离方法测定的纳米颗粒态磷含量
Figure PCTCN2019106538-appb-000004
由表4可知，本方法测定的纳米颗粒态磷的平均含量为0.87mg/kg。误差只有0.06mg/kg。由于目前还没有成熟的纳米颗粒态磷测定方法，为此，本方法不能与其他方法进行比较。但本方法的处理过程得到的颗粒基本吻合1nm-100nm的纳米颗粒态磷定义范围，因此理论上本方法测定的纳米颗粒范围准确，精度较高。
以上所述的实施例只是本发明的一种较佳的方案，然其并非用以限制本发明。有关技术领域的普通技术人员，在不脱离本发明的精神和范围的情况下，还可以做出各种变化和变型。因此凡采取等同替换或等效变换的方式所获得的技术方案，均落在本发明的保护范围内。

Claims (5)

  1. 一种同步测量土壤中胶体磷和纳米颗粒态磷的方法，其特征在于，包括如下步骤：
    S1：称取m克过筛的土样于锥形瓶中，加V 1毫升去离子水，浸提；
    S2：浸提上清液在3000～3500g下预离心10～12min以去除大颗粒，取预离心后的上清液用1μm微孔滤膜抽滤，弃去初滤液后收集所有滤液；将收集的滤液混匀后，测定其总磷浓度TP 1；同时从混匀的滤液中取出两份作为待测样品；
    S3：将第一份滤液待测样品放入3KDa的超滤管中，4000g下超速离心30～40min，取上清液测定总磷浓度TP 2，该上清液为去除胶体组分的真溶解态磷组分，超滤管底部为水扩散性胶体磷浓缩液；
    S4：将第二份滤液待测样品先放入超滤试样在1000KDa的超滤管中，3000g下超速离心20min，取上清液测定总磷浓度TP 3，该上清液为去除大颗粒胶体组分的纳米颗粒态组分溶液；然后再将获得的上清液放入3KD的超滤管中，4000g下超速离心40min，再取上清液测定总磷浓度TP 4，该上清液为去除纳米颗粒的真溶解态组分，超滤管底部为纳米颗粒态磷浓缩液；
    S5：计算土壤中胶体磷的含量，计算公式为：
    土壤胶体磷含量＝(TP 1-TP 2)×V 1/m
    计算土壤中纳米颗粒态磷的含量，计算公式为：土壤中纳米颗粒态磷含量＝(TP 3-TP 4)×V 1/m。
  2. 根据权利要求1的同步测量土壤中胶体磷和纳米颗粒态磷的方法，其特征在于，所述的土样为未经过研磨且过8mm筛的土样。
  3. 根据权利要求1的同步测量土壤中胶体磷和纳米颗粒态磷的方法，其特征在于，步骤S1中，土样与去离子水以土水比1:8混合，然后移至摇床中，在150～160rpm下浸提16～24h。
  4. 根据权利要求1的同步测量土壤中胶体磷和纳米颗粒态磷的方法，其特征在于，步骤S2中，初滤液的弃去量为5mL。
  5. 根据权利要求1的同步测量土壤中胶体磷和纳米颗粒态磷的方法，其特征在于，胶体磷的浓缩尺寸为3KDa-1μm，而纳米颗粒态磷的浓缩尺寸为3KDa -1000KDa。
PCT/CN2019/106538 2018-11-27 2019-09-18 一种同步测量土壤中胶体磷和纳米颗粒态磷的方法 Ceased WO2020108030A1 (zh)

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