CN105413642A - Preparation and application method of nickel ion imprinted magnetic chitosan nanometer material - Google Patents

Preparation and application method of nickel ion imprinted magnetic chitosan nanometer material Download PDF

Info

Publication number
CN105413642A
CN105413642A CN201510755722.2A CN201510755722A CN105413642A CN 105413642 A CN105413642 A CN 105413642A CN 201510755722 A CN201510755722 A CN 201510755722A CN 105413642 A CN105413642 A CN 105413642A
Authority
CN
China
Prior art keywords
solution
nickel ion
chitosan
preparation
ion trace
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201510755722.2A
Other languages
Chinese (zh)
Inventor
马晓国
陈圆
彭俊标
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guangdong University of Technology
Original Assignee
Guangdong University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guangdong University of Technology filed Critical Guangdong University of Technology
Priority to CN201510755722.2A priority Critical patent/CN105413642A/en
Publication of CN105413642A publication Critical patent/CN105413642A/en
Pending legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/02—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor with moving adsorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28016—Particle form
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/405—Concentrating samples by adsorption or absorption

Abstract

The invention belongs to the technical field of analytical chemistry and relates to a preparation and application method of a nickel ion imprinted magnetic chitosan nanometer material. The nickel ion imprinted magnetic chitosan nanometer material is prepared by taking ferroferric oxide as a carrier, Ni2+ as a template and chitosan as a functional monomer and is prepared by steps: synthesizing ferroferric oxide chitosan according to a one-step method, adding Ni(NO3)2 aqueous solution to form a complex, adopting epoxy chloropropane and sodium tripolyphosphate for crosslinking by stirring ultrasonically at the temperature of 60 DEG C under the protection of N2, adopting EDTA-Na solution for oscillating elution of template ions, cleaning, drying and grinding. The preparation process is simple, quick and reliable, and the prepared material is not only specific in Ni2+ recognition but also has superparamagnetism. After the material is added into environmental water samples or other sample solutions containing Ni2+, Ni2+ can be enriched by stirring for 10min, and quickness in solid-liquid phase separation can be realized by the aid of an external magnetic field. The recovery rate is higher than 4% by adoption of the 5% EDTA-Na solution for elution of adsorbed Ni2+. The method is high in selectivity, and the material can be reused for 5-6 times.

Description

A kind of preparations and applicatio method of nickel ion trace chitosan magnetic nano material
Technical field
The present invention relates to a kind of preparations and applicatio method of nickel ion trace chitosan magnetic nano material, be specifically related to a kind of to trace Ni 2+there is the preparation method of the nickel ion trace chitosan magnetic nano material of high selectivity fast separating concentration function, belong to technical field of analytical chemistry.
Background technology
Heavy metal serious harm health and ecological environment, receive the extensive concern of people.Wherein, nickel is listed in first kind environmental contaminants, and it can be entered in the organisms such as human body, animal, plant by number of ways, produces very large harm.Now, detect heavy metal element quickly and accurately and effectively administer the study hotspot that heavy metal pollution has become the fields such as environment, food, health.
In the samples such as environmental water sample, the content of nickel is usually in the trace even level of trace, and Modern Instrument Analytical Technique must be adopted to measure it.The detection method of nickel, mainly comprises AAS, atomic absorption spectrography (AAS), atomic emission spectrometry, ICP-MS, electrochemical process etc.Because nickel ion content is lower, and matrix composition is complicated, so, often need adopt separation and concentration technology, to improve the concentration of nickel ion and to eliminate interference matrix.Tradition method for separating and concentrating, as precipitation, complexing, extraction etc., exists that complex operation, poor reproducibility, enrichment times are low, the not high drawback of the rate of recovery.In recent years, a kind of new Sample Pretreatment Technique---SPE, high, easy and simple to handle with its enrichment times, can with the features such as various modern analytical instrument coupling, be used widely.But conventional SPE material selectivity is poor, spend slow, the easy blocking of post, operating time long (especially when sample volume is larger).Therefore, the SPE material of development of new, the selective and analysis speed improving SPE is the important development direction of solid phase extraction techniques.
Molecule (ion) engram technology is the effective means improving material selectivity.Ion blotting material obtains for template with specific object ion, can produce selective absorption effect to the object ion in sample solution.The chitin that shitosan is extensively existed by nature is through deacetylation, cheap and easy to get.Shitosan contains a large amount of amino, hydroxyl and amide groups, is a kind of excellent Biosorbent for heavy metals.Therefore, shitosan also can be used as the function monomer in heavy metal ion blotting process.Magnetic Nano material not only specific area is large, and owing to having paramagnetism, can realize solid-liquid phase be fast separated by externally-applied magnetic field.
Summary of the invention
The present invention is directed to prior art Problems existing, provide a kind of preparations and applicatio method of nickel ion trace chitosan magnetic nano material, the method take tri-iron tetroxide as carrier, Ni 2+for template, shitosan is function monomer, and epoxychloropropane and sodium phosphate trimer are crosslinking agent, prepares the nanoscale Ni with high selectivity and superparamagnetism 2+blotting chitosan material.Using this material as solid phase extraction adsorbents, achieve trace Ni in the sample such as environmental water sample, beverage 2+high selectivity fast separating concentration, substantially increase the efficiency of sample pre-treatments.
The technical solution adopted in the present invention is:
A preparation method for nickel ion trace chitosan magnetic nano material, comprises the steps:
(1) shitosan is dissolved in acetic acid solution, is mixed with 500mL1g/L shitosan acetic acid solution;
(2) by 0.25gFeCl 36H 2o, 0.25gFeSO 47H 2the mixed aqueous solution of O adds in above-mentioned shitosan acetic acid solution, constantly stirs, and drips 6.67mLNH rapidly 3h 2o, continues to stir 30min, obtains nano ferriferrous oxide chitosan solution;
(3) tri-iron tetroxide chitosan solution is added to containing 0.2gNi (NO 3) 26H 2in the aqueous solution of O, be settled to 150mL with ultra-pure water, be separated with magnet after 200rpm, the 15min that vibrates at 25 DEG C; The solid separated is washed 3 times, is added in 50mL5% sodium tripolyphosphate solution, at 60 DEG C of ultrasonic, N 2stir 10min under protection, then add the epoxychloropropane of 25mL2% through pre-open loop, continue to stir 30min, leave standstill 2h;
(4) with the Ni in 5%EDTA-Na solution oscillation cleaning above-mentioned material 2+, until there is no Ni 2+; The EDTA-Na using 0.1mol/LNaOH clean surface unnecessary again and the pH value of adjustment material, then replace cleaning 3 times with acetone and water;
(5) after being separated with magnet, material being put into drying box drying, then grind, cross 200 mesh sieves, obtain Powdered nickel ion trace chitosan magnetic nano material;
The chitosan solution that adds described in step (2) is at 80 DEG C of ultrasonic and N 2protection adds under stirring;
The pre-open loop of the epoxychloropropane described in step (3) is at alkali condition and 60 DEG C, through 500W microwave 5min;
Ni described in step (4) 2+detection method be atomic absorption spectrometry method;
Powdered nickel ion trace chitosan magnetic nano material average grain diameter described in step (5) is about 30nm, and saturation magnetization is 15.4emug -1, there is superparamagnetism.
The nickel ion trace chitosan magnetic applications to nanostructures of preparation, concrete steps are: 50mg material is added to 200mL and contains finite concentration Ni 2+solution in, adjust ph is between 4-7, and vibrate 10min under 200rpm; Ni will have been adsorbed 2+material magnet separate, then add 1mL5%EDTA-Na solution, vibrate desorb 2min under 400rpm, totally 2 times, mixed by the eluent of 2 times, with Ni in Flame Atomic Absorption Spectrometry Determination eluent 2+content;
Described contains finite concentration Ni 2+solution refer to environmental water sample, drink sample or other water base sample;
Reusable 5-6 time of described nickel ion trace chitosan magnetic nano material.
The invention has the beneficial effects as follows:
(1) the nickel ion trace magnetic Nano material that prepared by the present invention take tri-iron tetroxide as carrier, Ni 2+for template, shitosan is function monomer, and preparation one step of tri-iron tetroxide shitosan completes, and preparation process is simple, quick, reliable;
(2) material prepared of the present invention is not only to Ni 2+there is specific recognition ability, and have the high surface area of superparamagnetism and nano material, utilize externally-applied magnetic field can to the Ni in matrix complicated solution 2+carry out fast separating concentration.Meanwhile, the material pH scope of application is wide, adsorption capacity is larger, selective good, repeatedly reusable;
(3) material prepared of the present invention is for Ni in solution 2+sPE, the rate of adsorption is fast, antijamming capability accelerates sample handling processes by force, greatly, efficiently concentrating Ni 2+, significantly improve instrument to Ni 2+the sensitivity detected.
Detailed description of the invention
Be described in further details the present invention below by embodiment, these embodiments are only used for the present invention is described, do not limit the scope of the invention.
Embodiment 1
(1) synthesis of chitosan magnetic nano particle: use acetic acid shitosan, is mixed with 500mL1g/L shitosan acetic acid solution, by 0.25gFeCl 36H 2o, 0.25gFeSO 47H 2the mixed aqueous solution of O, at 80 DEG C of ultrasonic and N 2protection adds in shitosan acetic acid solution under stirring, and drips 6.67mLNH rapidly 3h 2o, continues to stir 30min, obtains nano ferriferrous oxide chitosan solution;
(2) preparation of nickel ion trace chitosan magnetic nano material: tri-iron tetroxide chitosan solution is added to containing 0.2gNi (NO 3) 26H 2in the aqueous solution of O, be settled to 150mL with ultra-pure water; At 200rpm, vibrate at 25 DEG C 15min, is separated, the solid separated washed 3 times, is added in 50mL5% sodium tripolyphosphate solution, at 60 DEG C of ultrasonic, N with magnet 2stir 10min under protection, then add the epoxychloropropane of 25mL2% through pre-open loop (at alkali condition and 60 DEG C, 500W microwave 5min), continue to stir 30min, leave standstill 2h, with the Ni in 5%EDTA-Na solution oscillation cleaning material 2+, until there is no Ni 2+(detecting with Atomic Absorption Spectrometer), the EDTA-Na using 0.1mol/LNaOH clean surface unnecessary again and the pH value of adjustment material, then cleaning is replaced 3 times with acetone and pure water, after being separated with magnet, material is dry, grinding, crosses 200 mesh sieves, obtains Powdered nickel ion trace chitosan magnetic nano material.
Embodiment 2
Indices experiment is carried out to embodiment 1 resulting materials:
The 100mL that 50mg embodiment 1 resulting materials is added to different pH value is contained 1mg/LNi 2+solution in, investigate pH value to Ni 2+the impact of adsorption effect; Result shows, the rate of recovery is all close to 100% between 4-7 for pH, and therefore other adsorption experiment carries out all in neutral conditions.
The 100mL that 50mg embodiment 1 resulting materials is added to pH=7 is contained 1mg/LNi 2+solution in, investigate adsorption time to Ni 2+the impact of adsorption effect; After result shows 10min, reach adsorption equilibrium.
50mg embodiment 1 resulting materials is added to different initial Ni 2+in the solution of concentration, in constant temperature oscillator, adsorb 2h at 25 DEG C, the adsorbance of research material is with Ni 2+the change of initial concentration, by adsorption isotherm matching, calculates material to Ni 2+saturated extent of adsorption be 18.5mg/g.
Select Cu 2+, Pb 2+, Cd 2+for competing ions carries out adsorption test, research material is to Ni 2+adsorptive selectivity.Result shows, relative to Pb 2+, Cu 2+, Cd 2+, material is to Ni 2+trace coefficient be respectively 2.2,5.6,2.3, illustrate that imprinted material is to Ni 2+there is excellent Ion recognition character.
Test the change of externally-applied magnetic field to the impact of material magnetization intensity.Find that the intensity of magnetization strengthens with externally-applied magnetic field and increases, saturation magnetization is 15.4emug -1, and B-H loop crosses initial point, shows good superparamagnetism.
Embodiment 3
Embodiment 1 resulting materials is used for trace Ni in solution 2+the enrichment of magnetic Solid phase extraction separation:
50mg material is added to 200mL and contains finite concentration Ni 2+solution (environmental water sample, drink sample or other water base sample) in, adjust ph is 7, and vibrate 10min under 200rpm, will adsorb Ni with magnet 2+material separate from solution, then add 1mL5%EDTA-Na solution, vibrate desorb 2min under 400rpm, totally 2 times, mixed by the eluent of 2 times, with Ni in Flame Atomic Absorption Spectrometry Determination eluent 2+content, Ni 2+the rate of recovery between 94.4%-114.3%, the relative standard deviation between parallel determination (n=5) result is less than 3.2%;
The 5000 times of K coexisted in solution +, 2500 times of Na +, 4000 times of Ca 2+, 2500 times of Mg 2+, 800 times of Cd 2+, 2500 times of Al 3+, 800 times of Cu 2+, 600 times of Pb 2+, 200 times of Zn 2+, 1000 times of Fe 3+deng cation and 20000 times of NO 3 -, 12500 times of SO 4 2-, 25000 times of Cl -ni is not disturbed Deng anion 2+mensuration; Reusable 5-6 time of material.

Claims (8)

1. a preparation method for nickel ion trace chitosan magnetic nano material, is characterized in that: comprise the steps:
(1) shitosan is dissolved in acetic acid solution, is mixed with 500mL1g/L shitosan acetic acid solution;
(2) by 0.25gFeCl 36H 2o, 0.25gFeSO 47H 2the mixed aqueous solution of O adds in above-mentioned shitosan acetic acid solution, constantly stirs, and drips 6.67mLNH rapidly 3h 2o, continues to stir 30min, obtains nano ferriferrous oxide chitosan solution;
(3) tri-iron tetroxide chitosan solution is added to containing 0.2gNi (NO 3) 26H 2in the aqueous solution of O, be settled to 150mL with ultra-pure water, be separated with magnet after 200rpm, the 15min that vibrates at 25 DEG C; The solid separated is washed 3 times, is added in 50mL5% sodium tripolyphosphate solution, at 60 DEG C of ultrasonic, N 2stir 10min under protection, then add the epoxychloropropane of 25mL2% through pre-open loop, continue to stir 30min, leave standstill 2h;
(4) with the Ni in 5%EDTA-Na solution oscillation cleaning above-mentioned material 2+, until there is no Ni 2+; The EDTA-Na using 0.1mol/LNaOH clean surface unnecessary again and the pH value of adjustment material, then replace cleaning 3 times with acetone and water;
(5) after being separated with magnet, material being put into drying box drying, then grind, cross 200 mesh sieves, obtain Powdered nickel ion trace chitosan magnetic nano material.
2. preparation method according to claim 1, is characterized in that: it is at 80 DEG C of ultrasonic and N that the mixed aqueous solution described in step (2) adds in chitosan solution 2protection adds under stirring.
3. preparation method according to claim 1, is characterized in that: the pre-open loop of the epoxychloropropane described in step (3) is at alkali condition and 60 DEG C, through 500W microwave 5min.
4. preparation method according to claim 1, is characterized in that: the Ni described in step (4) 2+detection method adopt atomic absorption spectrometry method.
5. preparation method according to claim 1, is characterized in that: the Powdered nickel ion trace chitosan magnetic nano material average grain diameter described in step (5) is about 30nm, and has superparamagnetism.
6. nickel ion trace chitosan magnetic applications to nanostructures method, is characterized in that: 50mg nickel ion trace chitosan magnetic nano material is added 200mL and contains finite concentration Ni 2+solution in, adjust ph is between 4-7, and vibrate 10min under 200rpm; Ni will have been adsorbed 2+imprinted magnetic material magnet separate, then add 1mL5%EDTA-Na solution, vibrate desorb 2min under 400rpm, totally 2 times, mixed by the eluent of 2 times, with Ni in Flame Atomic Absorption Spectrometry Determination eluent 2+content.
7. nickel ion trace chitosan magnetic applications to nanostructures method according to claim 6, is characterized in that: described finite concentration Ni 2+solution refer to environmental water sample, drink sample or other water base sample.
8. nickel ion trace chitosan magnetic applications to nanostructures method according to claim 6, is characterized in that: reusable 5-6 time of described nickel ion trace chitosan magnetic nano material.
CN201510755722.2A 2015-11-10 2015-11-10 Preparation and application method of nickel ion imprinted magnetic chitosan nanometer material Pending CN105413642A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510755722.2A CN105413642A (en) 2015-11-10 2015-11-10 Preparation and application method of nickel ion imprinted magnetic chitosan nanometer material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510755722.2A CN105413642A (en) 2015-11-10 2015-11-10 Preparation and application method of nickel ion imprinted magnetic chitosan nanometer material

Publications (1)

Publication Number Publication Date
CN105413642A true CN105413642A (en) 2016-03-23

Family

ID=55492444

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510755722.2A Pending CN105413642A (en) 2015-11-10 2015-11-10 Preparation and application method of nickel ion imprinted magnetic chitosan nanometer material

Country Status (1)

Country Link
CN (1) CN105413642A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107570125A (en) * 2017-09-15 2018-01-12 哈尔滨工业大学深圳研究生院 A kind of EDTA Ni molecular engram materials and preparation method thereof and its application
CN108246262A (en) * 2018-03-12 2018-07-06 沈阳理工大学 A kind of trace Ceramic Balls for detaching and extracting for nickel ion and preparation method thereof
CN108445053A (en) * 2018-02-26 2018-08-24 江苏大学 A kind of ion blotting sensor and preparation method and application
CN108816204A (en) * 2018-07-09 2018-11-16 莆田学院 A kind of preparation method of copper ion imprinted crosslinked chitosan microballoon
CN111957301A (en) * 2020-08-12 2020-11-20 辽宁大学 Magnetic chitosan nickel ion molecular imprinting adsorbent and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101301604A (en) * 2008-06-04 2008-11-12 哈尔滨工程大学 Method for preparing magnetic powder heavy metal ion blotting chitosan compound adsorbing agent
CN104059167A (en) * 2013-03-20 2014-09-24 青岛科技大学 Preparation method of polyamine compound-modified magnetic chitosan and application thereof
CN104140530A (en) * 2014-07-22 2014-11-12 中国科学院烟台海岸带研究所 Mercury ion imprinted polymer and method and application thereof
US20150231598A1 (en) * 2012-09-19 2015-08-20 Tsinghua University MAGNETIC CORE COATED INORGANIC ION ADSORBENT FOR REMOVING Cs IONS IN RADIOACTIVE WASTEWATER AND PREPARATION METHOD THEREOF

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101301604A (en) * 2008-06-04 2008-11-12 哈尔滨工程大学 Method for preparing magnetic powder heavy metal ion blotting chitosan compound adsorbing agent
US20150231598A1 (en) * 2012-09-19 2015-08-20 Tsinghua University MAGNETIC CORE COATED INORGANIC ION ADSORBENT FOR REMOVING Cs IONS IN RADIOACTIVE WASTEWATER AND PREPARATION METHOD THEREOF
CN104059167A (en) * 2013-03-20 2014-09-24 青岛科技大学 Preparation method of polyamine compound-modified magnetic chitosan and application thereof
CN104140530A (en) * 2014-07-22 2014-11-12 中国科学院烟台海岸带研究所 Mercury ion imprinted polymer and method and application thereof

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
D. HARIKISHORE KUMAR REDDY，ET AL: "Application of magnetic chitosan composites for the removal of toxic metal and dyes from aqueous solutions", 《ADVANCES IN COLLOID AND INTERFACE SCIENCE》 *
SU HAIJIA，ET AL: "Biosorption of Ni2+ by the surface molecular imprinting adsorbent", 《PROCESS BIOCHEMISTRY》 *
任月明: "铜离子印迹磁性生物吸附材料的制备及性能研究", 《中国博士学位论文全文数据库 工程科技I辑》 *
肖玲，等: "表面印迹纳米磁性壳聚糖的制备及对Cu(II) 的吸附研究", 《离子交换与吸附》 *
黎厚斌，等: "《包装应用化学》", 31 January 2004, 印刷工业出版社 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107570125A (en) * 2017-09-15 2018-01-12 哈尔滨工业大学深圳研究生院 A kind of EDTA Ni molecular engram materials and preparation method thereof and its application
CN108445053A (en) * 2018-02-26 2018-08-24 江苏大学 A kind of ion blotting sensor and preparation method and application
CN108246262A (en) * 2018-03-12 2018-07-06 沈阳理工大学 A kind of trace Ceramic Balls for detaching and extracting for nickel ion and preparation method thereof
CN108816204A (en) * 2018-07-09 2018-11-16 莆田学院 A kind of preparation method of copper ion imprinted crosslinked chitosan microballoon
CN111957301A (en) * 2020-08-12 2020-11-20 辽宁大学 Magnetic chitosan nickel ion molecular imprinting adsorbent and preparation method and application thereof

Similar Documents

Publication Publication Date Title
CN105413642A (en) Preparation and application method of nickel ion imprinted magnetic chitosan nanometer material
Huang et al. Speciation of inorganic tellurium from seawater by ICP‐MS following magnetic SPE separation and preconcentration
Gao et al. Chemically modified activated carbon with 1-acylthiosemicarbazide for selective solid-phase extraction and preconcentration of trace Cu (II), Hg (II) and Pb (II) from water samples
Wang et al. Preparation of a functionalized magnetic metal–organic framework sorbent for the extraction of lead prior to electrothermal atomic absorption spectrometer analysis
Huang et al. Magnetic immobilization of amine-functionalized magnetite microspheres in a knotted reactor for on-line solid-phase extraction coupled with ICP-MS for speciation analysis of trace chromium
Chen et al. Speciation analysis of inorganic arsenic in natural water by carbon nanofibers separation and inductively coupled plasma mass spectrometry determination
Ye et al. Preparation and characterization of magnetic nanoparticles for the on-line determination of gold, palladium, and platinum in mine samples based on flow injection micro-column preconcentration coupled with graphite furnace atomic absorption spectrometry
Wang et al. Determination of trace amounts of Se (IV) by hydride generation atomic fluorescence spectrometry after solid-phase extraction using magnetic multi-walled carbon nanotubes
CN104275155B (en) A kind of preparation method of novel cadmium ion trace magnetic mesoporous silica gel solid phase extracting agent and application
CN104226262A (en) Preparing method and application thereof of functional magnetic MOFs (Metal-Organic Frameworks) material
Jia et al. Development of a novel, fast, sensitive method for chromium speciation in wastewater based on an organic polymer as solid phase extraction material combined with HPLC–ICP-MS
Li et al. Extraction of imide fungicides in water and juice samples using magnetic graphene nanoparticles as adsorbent followed by their determination with gas chromatography and electron capture detection
Abbaszadeh et al. Speciation analysis of inorganic arsenic in food and water samples by electrothermal atomic absorption spectrometry after magnetic solid phase extraction by a novel MOF-199/modified magnetite nanoparticle composite
Zhang Preparation, characterization and application of thiosemicarbazide grafted multiwalled carbon nanotubes for solid-phase extraction of Cd (II), Cu (II) and Pb (II) in environmental samples
Guo et al. Dual dispersive extraction combined with electrothermal vaporization inductively coupled plasma mass spectrometry for determination of trace REEs in water and sediment samples
Kaykhaii et al. Magnetic molecularly imprinted polymer nanoparticles for selective extraction of copper from aqueous solutions prior to its flame atomic absorption determination
CN103028351B (en) Benzene sulfonic acid modified magnetic microsphere and preparation method and application thereof
Wu et al. Speciation of chromium in water using crosslinked chitosan-bound FeC nanoparticles as solid-phase extractant, and determination by flame atomic absorption spectrometry
Zhang et al. Preparation, characterization and application of Saussurea tridactyla Sch-Bip as green adsorbents for preconcentration of rare earth elements in environmental water samples
CN104568787B (en) Method for detecting metal ions by combining nanosilver and magnetic nano material
CN101811032B (en) Preparation and application methods of Cd (II) imprinted magnetic material
Zhang et al. Selective solid-phase extraction of trace thallium with nano-Al 2 O 3 from environmental samples
Soylak et al. Solid-phase extraction of heavy metal ions on bucky tubes disc in natural water and herbal plant samples
Habila et al. 1-nitroso-2-naphthol impregnated multiwalled carbon nanotubes (NNMWCNTs) for the separation-enrichment and flame atomic absorption spectrometric detection of copper and lead in hair, water, and food samples
Shih et al. Online coupling of ultraviolet titanium dioxide film reactor with poly (methyl methacrylate) solid phase extraction–inductively coupled plasma mass spectrometry for speciation of trace heavy metals in freshwater

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20160323

RJ01 Rejection of invention patent application after publication