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Abbreviation (ISO4): Prog Chem      Editor in chief: Jincai ZHAO

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Progress in Chemistry >

2024 , Vol. 36 >Issue 9: 1401 - 1411

DOI: https://doi.org/10.7536/PC240205

Review

Dissolved Aluminum Measurement Methods and Their Application in Atmospheric Aerosol Research

  • Tianyu Zhang 1, 2 ,
  • Zhenming Zhu 3 ,
  • Fu Wang 3 ,
  • Lanxiadi Chen 1, 2 ,
  • Rui Li , 4, * ,
  • Mingjin Tang , 1, *
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  • 1 State Key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640, China
  • 2 University of Chinese Academy of Sciences, Beijing 100049, China
  • 3 Longhua Center for Disease Control and Prevention of Shenzhen, Shenzhen 518109, China
  • 4 School of Public Health, Shanxi Medical University, Taiyuan 030600, China
*e-mail: (Rui Li);
(Mingjin Tang)

Received date: 2024-02-19

  Revised date: 2024-06-05

  Online published: 2024-08-30

Supported by

National Natural Science Foundation of China(42277088)

Guangdong Basic and Applied Basic Research Foundation(2022A1515110371)

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Abstract

Atmospheric deposition of desert dust aerosol is a major source of key nutrients for surface seawater In open oceans,significantly impacting marine biogeochemistry and primary productivity.As a tracer for desert dust aerosol,aluminum(Al)is widely used to estimate deposition fluxes of desert dust aerosol into the oceans,and dissolved Al concentrations in surface seawater and aerosol particles are key parameters for using this method to estimate desert dust deposition fluxes into the oceans.in this paper,we first review separation,extraction and detection methods used to measure dissolved Al in seawater and aerosol samples,and discuss their principles,advantages,limitations and applicability.After advances in aerosol Al solubility are systematically reviewed,we point out that the uncertainties in aerosol Al solubility are the bottleneck which currently limits accurate estimations of desert dust deposition fluxes into the oceans,and further analyze the sources of these uncertainties.in the final,we also outline research directions for dissolved Al analysis and aerosol Al solubility research。

Contents

1 Introduction

2 Pretreatment methods for dissolved aluminum

2.1 Filtration

2.2 Separation and preconcentration methods for seawater samples

2.3 Extraction methods for soil and aerosol samples

3 Detection methods for dissolved aluminum

3.1 UV-Visible spectrophotometry

3.2 Fluorescence spectrophotometry

3.3 Atomic spectrometry

3.4 Inductively coupled plasma mass spectrometry

4 Research progress of aerosol aluminum solubility

5 Conclusion and outlook

Key words： dissolved aluminum; surface seawater; atmospheric aerosol; separation and extraction; detection methods

Cite this article

Tianyu Zhang , Zhenming Zhu , Fu Wang , Lanxiadi Chen , Rui Li , Mingjin Tang . Dissolved Aluminum Measurement Methods and Their Application in Atmospheric Aerosol Research[J]. Progress in Chemistry, 2024 , 36(9) : 1401 -1411 . DOI: 10.7536/PC240205

1 Introduction

Aluminum is the most abundant metallic element in the earth's crust and occurs mainly as aluminosilicates in rocks and minerals[1]。 Under natural conditions,aluminum enters rivers,lakes and coastal oceans with the dissolution of weathering products of surface rocks and soils.acid rain and Acid wastewater caused by human activities have aggravated the problem of environmental acidification,and the dissolution of solid aluminum in soil has increased significantly,which has led to a significant increase in the concentration of soluble aluminum in groundwater and surrounding rivers in some areas[2]。 Excessive aluminum can limit the growth of plant roots,thus affecting the absorption of water and nutrients by plants[3⇓~5]; It can also interfere with the normal physiological activities of aquatic organisms,resulting in the decline of their vitality or even death[6,7]。 in the estuary,the mixing of fresh and saline water increases the salinity and pH,and the organic matter is flocculated and precipitated,resulting in the rapid removal of soluble aluminum.Therefore,the concentration of soluble aluminum in seawater(nmol/L level)is significantly lower than the common concentration in freshwater(μmol/L to mmol/L level),and it is not toxic to most marine organisms such as phytoplankton[8]。 Generally speaking,compared with iron,manganese and chromium,although the content of aluminum in various spheres of the earth system is very high,it has attracted less attention because it is neither a nutrient element nor a heavy metal element。
Since the 20th century,people have gradually realized the influence of atmospheric dust deposition on the distribution of trace elements in the pelagic waters[9,10]。 Dust carries a large number of minerals to the open ocean by long-distance transport,providing abundant nutrients for marine organisms,which affect marine primary productivity,marine carbon cycle and global climate change to varying degrees[8,11]。 in order to reveal the effects of dust aerosol on nutrient elements and biogeochemical cycling In the ocean,it is necessary to accurately estimate the ocean deposition flux of dust aerosol[12]。 aluminum is the main component of dust particles in arid and semi-arid areas,and its content is relatively uniform and stable;these dust particles are transported into the sea through the atmosphere and become the main source of soluble Aluminum in the surface water of the ocean;Aluminum has weak bioavailability and does not participate in complex redox reactions in the ocean.for These reasons,aluminum is considered to be a tracer element For dust transport from land to sea[13⇓⇓~16]。 Measures et al.Suggested that the concentration of soluble aluminum in the upper mixed layer of the ocean could be used to estimate the atmospheric dust deposition flux[11,12]; Using this method to calculate the dust deposition flux,two key parameters,the soluble aluminum concentration in marine water and the aluminum solubility in aerosol(the ratio of soluble aluminum concentration to total aluminum concentration),need to be defined[17]。
Due to the significant regional variation of atmospheric dust deposition flux,the concentration of soluble aluminum in the world's sea waters,especially in the open ocean,has a significant regional variation[13]。 Soluble Al concentrations in the global Ocean(excluding estuarine and coastal water regions)range from 0.05 nmol/L(Southern ocean)to 674 nmol/L(Arabian Sea),with a median value of 6.8 nmol/l[18]。 Due to the influence of Saharan dust,the concentration of soluble aluminum in the surface water of the Atlantic Ocean is generally higher than that of other oceans,with the highest average concentration of(19.8±15.8)nmol/L,while that of the Pacific Ocean is only(3.3±3.5)nmol/L[11,19]。 At present,the concentration distribution of soluble aluminum in the surface ocean has been comprehensively and deeply understood,but the scientific understanding of soluble aluminum in aerosols in different regions is still relatively preliminary[19⇓~21]。 on the one hand,there is no standard method for the extraction of aerosol soluble aluminum,so the measurement data of different laboratories are not comparable;On the other hand,the existing observation and research of aerosol aluminum solubility are still very limited,and mainly concentrated in a few sea areas of the Atlantic ocean and the Pacific Ocean,while the research On the Southern Ocean and the Southern Indian Ocean is relatively small.Therefore,there are still great uncertainties in our scientific understanding of the solubility of aerosol aluminum,which seriously limits the accurate estimation of the Ocean deposition flux of dust aerosol。
the premise of using aluminum as a tracer to estimate the ocean deposition flux of dust aerosol is to accurately obtain the concentration of soluble aluminum in seawater and aerosol,and the key foundation is to establish an accurate and efficient method for the analysis of soluble aluminum.in this paper,the pretreatment and analysis methods of soluble aluminum in seawater and aerosol are introduced,and the advantages and disadvantages of different methods are discussed;Then,the research progress of soluble aluminum in aerosols is summarized in detail,and the detection methods of soluble aluminum and the future development direction of aerosol soluble aluminum are briefly discussed。

2 Pretreatment method

the composition of environmental samples is complex,and direct analysis will interfere with the instrument signal,affecting the performance and reliability of the detection instrument.in addition,the concentration of soluble aluminum In natural water such as seawater is generally lower than the detection limit of conventional methods.Therefore,before analyzing the concentration of soluble aluminum,pretreatment methods such as filtration,separation and enrichment should be used to improve the accuracy of the method。

2.1 Filtration

soluble aluminum refers to the dissolved aluminum obtained from the solution by filtration through a filter membrane with a certain pore size(usually 0.2 or 0.4~0.45μm).Therefore,it is necessary to filter the sample before determining the concentration of soluble aluminum in the sample.in general,seawater filtration can be done in a ship-based laboratory,while filtration for aerosols,soils,and sediments is done in the laboratory after soluble extraction of the sample.for example,after collecting seawater samples,Sohrin et al.Filtered them with a polycarbonate filter with a pore size of 0.2μm on site,acidified them and stored them in low-density polyethylene bottles for subsequent analysis[22]。 Zhang et al.First collected atmospheric particulate matter samples and extracted them,filtered the extract with a 0.22μm needle filter,and then determined the content of soluble aluminum in the filtrate by ICP-MS(inductively coupled plasma mass spectrometry)[23]。 However,the needle filter is time-consuming and laborious,and is not easy to operate in the field.It is only suitable for filtering small volumes and limited numbers of samples in the laboratory.When large quantities of water need to be collected from the ocean,this method can not meet the filtration needs。

2.2 Separation and Enrichment of Soluble Aluminum in Seawater

separation and enrichment separates soluble aluminum from the complex matrix of seawater and concentrates it to increase the concentration of the analyte to ensure that it is detectable.Table 1 summarizes and compares the commonly used separation and enrichment methods of soluble aluminum in seawater,mainly including solid phase extraction,liquid phase extraction and chromatographic separation。
表1 Separation and Enrichment of Soluble Aluminum in Seawater

Table 1 Separation and preconcentration method for dissolved aluminum in seawaters

Methods Advantages Drawbacks
SPE High level of automation.
Low risk of contamination.		 High technical experience when combined with FIA
LLE Easy to operate. Long extraction time
Small extraction efficiency
Labor intensive
DLLME Short extraction time.
Extractant is easy to collect.		 Not robust enough to be completely automated.
CPE Less laboratory wastes. Mostly off-line
Labor intensive
HPLC High sensitivity.
Suitable for Al species separated.		 Mostly off-line
High instrument requirements

2.2.1 Solid phase extraction

Solid phase extraction(SPE)is based on the selective adsorption of the functional groups on the chelating resin to the analyte to achieve the classification and enrichment of the target element.the method is simple to operate and easy to automate,and can simultaneously separate and extract trace metal elements from a large volume of water sample.According to the functional groups of chelating resins,there are three main types of resins commonly used for soluble aluminum:8-hydroxyquinoline(8-HQ)type,iminooxalic acid(IDA)type,and ethylenediamine triacetic acid-iminodiacetic acid(EDTriA-IDA)complex type。
Resing et al.Synthesized 8-HQ chelating resin as a SPE material[24]。 When seawater flows through the resin column,the target metal ions are complexed and adsorbed,and then the target is eluted for detection.Although the interfering species in seawater are also partially retained on the resin column,aluminum can be effectively separated from the interfering species(especially iron)during leaching.Subsequently,Dierssen et al.Simplified the synthesis of the resin material,but the process was still cumbersome,time-consuming(>7 H),and unstable,which limited the practicality of the resin column[25]。
the development of commercial chelating resins has greatly contributed to the popularization of SPE technology.Among them,IDA type and EDTriA-IDA complex type are two commercial chelating resins commonly used for the separation and enrichment of soluble aluminum.Brown et al.Enriched the soluble aluminum in seawater on the IDA resin column,avoiding the resin column synthesis step[26]。 Under the selected experimental conditions,the resin column does not complex a large amount of alkali metals and alkaline earth metals in seawater,thereby effectively separating trace aluminum from a complex solution matrix[27]。 Moreover,the optimal pH range of IDA resin column for aluminum preconcentration is 5.0~7.4,which has more flexibility in the selection of eluent。
EDTriA-IDA composite resin has both ethylenediaminetriacetic acid and iminooxalic acid functional groups,and has good affinity for most transition metal elements and rare earth elements in a wide pH range,and has a low retention rate(~0.1%)for alkaline earth metals[28]。 Sohrin et al.Used this kind of resin column to enrich 9 metal elements such as aluminum from seawater at one time,which were eluted by nitric acid solution and determined by on-line ICP-MS[22]。 Moreover,the resin is very stable and can be thoroughly cleaned and repeatedly used,which is helpful to combine with online technologies such as continuous flow injection analysis(FIA)to analyze the concentration of soluble aluminum in the surface seawater of the ocean in situ or continuously,and to provide technical support for the study of the marine geochemical cycle of aluminum[27]。

2.2.2 Liquid phase extraction

(1)liquid-liquid extraction
soluble aluminum can not be directly extracted by organic solvents,so it is often necessary to add chelating agents to form hydrophobic metal chelates with metal ions,and then separate them from the matrix by extractants.Zhang et al.Used n-butanol to extract the chelate of Soluble aluminum and fluorescent gallium(LMG)reagent,and increased the detection signal by 20 times[29]; At the same time,masking agents such as phenanthroline are added to eliminate the interference of iron and other impurities in natural water.However,traditional liquid-liquid extraction(LLE)often uses a large amount of organic solution,which greatly affects the reagent blank.At present,liquid phase extraction technology has been developed towards solvent-free or solvent-less dispersive liquid-liquid microextraction,cloud point extraction and other new technologies。
(2)Dispersive liquid-liquid microextraction
Dispersive liquid-liquid microextraction(DLLME)is a miniaturized liquid-liquid extraction technique.the mixed solution of the extractant and the dispersant is injected into the analysis sample solution through an injector to form a three-phase suspension system of the extractant,the dispersant and the sample solution.the dispersant disperses the extractant into fine droplets and increases the contact area between the extractant and the analyte,thereby accelerating the distribution balance and completing the extraction quickly.Generally speaking,the extractant used in DLLME has a high density,and the organic extraction phase tends to deposit at the bottom after centrifugation,which is not easy to recover.Rezaee et al.Cooled the extractant suspended on the surface of the sample solution in an ice bath by suspending and solidifying DLLME,took it out after solidification,and performed ICP-OES(inductively coupled plasma atomic emission spectrometry)analysis after melting at room temperature[30]。 The detection limit of this method is 29.63 nmol/L,which can tolerate the interference of common coexisting ions such as Ca2+and Mg2+,and the use of ascorbic acid and other reagents can effectively mask the ions such as Cu2+and Fe3+in water samples.This method has been successfully applied to the determination of soluble aluminum in seawater and freshwater at concentrations from nmol/L toμmol/L 。
in order to further improve the technique,Su Suárez et al.Used DLLME In a syringe together with the flow technique,and selected n-hexanol with a density less than that of water to extract the complex of aluminum and LMG.After the extraction was completed,the extractant suspended on the surface of the sample solution was automatically collected and detected by fluorophotometry[31]。 the method realizes the automation of sample injection,reaction,phase separation and quantification,and can complete the detection within 4 min.the detection limit is 8.0 nmol/L,which can meet the requirements of the determination of soluble aluminum in coastal and surface seawater。
(3)cloud point extraction
cloud point extraction(CPE)is to change the experimental conditions to make the solution reach the Cloud point to initiate phase separation.Hydrophobic substances are extracted into the surfactant phase,while hydrophilic substances are retained in the aqueous phase to achieve the purpose of separation and enrichment[32,33]。 the method significantly reduces the consumption of organic solvent;Because the volume of the surfactant phase is much smaller than that of the water phase,this technology has a high enrichment and extraction rate。
Triton X-114 is the most commonly used surfactant in the extraction of trace metals by CPE[34⇓~36]。 Tabrizi compared the extraction ability of Triton X-114,Triton X-100 and PONPE-7.5,and the results showed that Triton X-114 had higher extraction efficiency,and the cloud point temperature of Triton X114 was 25℃,which was slightly higher than room temperature,which was convenient for subsequent operation[37]。 Santarossa et al.Mixed Triton X-114,CTAB and sodium cholate to extract and determine soluble aluminum in natural water[38]。 Compared with the single surfactant,the extraction sensitivity of the ternary mixed surfactant micelle system was improved by 2.5 times,and the detection limit was 10.41 nmol/L.the method also successfully reduces the cloud point temperature of the surfactant,shortens the time required for equilibration,and improves the simplicity of operation。
Some researchers also used PONPE 7.5,Tween-20 and Triton X-100 to extract aluminum chelates,and determined the trace aluminum content in natural water by spectrophotometry and atomic absorption spectrometry[39][40][41]。 the extract after CPE separation contains a certain amount of organic matter,which may have an impact on the subsequent detection results.However,some scholars believe that the methanol and surfactant used in CPE method will not affect the determination of atomic absorption spectrometry,but can reduce the droplet size,promote the dispersion of sample solution in the atomizer,and improve its atomization efficiency[42]。
Although the principle of liquid phase extraction is simple and widely used,its application in field analysis is limited due to the strict control of reaction conditions and the need for manual repeated operations.Based on this,this method is mainly applicable to the analysis of a limited number of samples in the laboratory,while the application of processing a large number of samples in the field long-term observation is relatively rare。

2.2.3 Liquid chromatography

liquid chromatography is based on the continuous multiple exchange of solutes between the stationary phase and the mobile phase,and the separation is achieved by means of the difference in the interaction ability of different components between the two phases.Compared with solid phase extraction and classical liquid chromatography,high performance liquid chromatography(HPLC)has the characteristics of high pressure,high speed,high column efficiency and high sensitivity.Remenyi et al.Established reversed-phase high performance liquid chromatography,selected C18 column as the separation column,and reduced the interference of seawater background matrix by gradient elution[43]。 the detection limit was 0.56 nmol/L.in order to realize the shipboard determination of soluble aluminum in seawater,an automatic analysis system was further developed in this study,and the concentration of soluble aluminum in water samples from the vertical profile of the Antarctic polar zone was measured in the range of 0.1~1.0 nmol/L[44]。 It should be noted that although two distinct chromatographic peaks were observed in the chromatogram,the specific aluminum species corresponding to them were not identified in this study。
With the deepening of research work and the development of hyphenated techniques,the analysis of soluble aluminum has gradually evolved into the determination of individual aluminum species.The difference in retention time in the chromatography with high separation power can reflect the chemical behavior of different forms of aluminum,and the combined detection instrument can quantify the separated different forms of aluminum.Frankowski et al.Developed a HPLC-ICP-MS method to successfully measure the contents of free aluminum ions and aluminum fluoride AlFx(3−x)in soil and groundwater[45]。

2.3 Extraction of soluble aluminum from soil and aerosol

the research on the content and speciation of metals in soils and sediments has been carried out for a long time,and the sequential extraction method is the most widely used.Tessier et al.Extracted the metal elements in the samples in five steps,and divided the metal elements in the samples into exchangeable form,carbonate-bound form,iron-manganese oxide-bound form,organic-bound form and residual form[46]。 Based on Tessier's five-step extraction method and other research results,the European Commission for Reference Materials has developed the BCR extraction method,which divides the chemical forms of metals into acid exchangeable,reducible and oxidizable forms[47]。 The fractional extraction method defined by the experimental operation was also used for reference in the speciation analysis of aerosol aluminum.Fang Hongda et al.Used the BCR extraction method combined with ICP-MS to determine the content of different forms of metals in PM2.5and PM2.5~10,and the remaining residue was digested by aqua regia microwave.The analysis showed that the aluminum in atmospheric particulate matter was mainly in the residual form,with the content exceeding 85%[48]。
For the study of soluble elements in atmospheric aerosols,off-line samplers are generally used to collect the particles in the actual atmosphere onto the filter membrane,and then the soluble elements are extracted.in the analysis of aluminum,iron and other metal elements in aerosols,Whatman 41 cellulose filter is mostly used in the study,and its background value of metal elements is low[49⇓~51]。 When extracting soluble aluminum from atmospheric particulate matter,researchers from all over the world decide the extraction reagent,extraction method and extraction time according to the purpose of the experiment.In most laboratories,ultrapure water is used as the extractant to obtain soluble aluminum components by oscillation,ultrasound,continuous flow extraction,etc[23][50][52]。 However,some scholars believe that the buffer capacity of ultrapure water is limited,and the pH of the solution is greatly affected by particulate matter,so ammonium acetate buffer solution is used as the extractant to avoid the pH change of the dissolution medium[49]。 in order to better simulate the dissolution behavior of dust aerosol aluminum In the surface ocean,some researchers also used seawater as a solvent to leach particulate matter sampling film[12,53]。 However,there is no complete standard method for the extraction of soluble components of aerosols.Researchers adopt different extraction methods according to various needs,which reduces the comparability between data and limits people's understanding of the difference of aluminum solubility。

3 Analysis and detection method

for the determination of soluble aluminum in environmental samples,the field analysis is mostly based on the simple principle of molecular spectrometry,which includes ultraviolet-visible spectrophotometry and fluorescence spectrophotometry.Among them,fluorophotometry is more sensitive and is often used in combination with flow analysis techniques for continuous navigation analysis.Atomic emission spectrometry and inductively coupled plasma mass spectrometry are common methods for the determination of soluble aluminum in land-based laboratories,which have high analytical accuracy and good stability,and can realize the simultaneous analysis of multiple elements。

3.1 Ultraviolet-visible spectrophotometry

Soluble aluminum reacts with some reagents under certain conditions to form a complex with characteristic absorption at 200~700 nm.the key of this method is The selection of chromogenic reagents,which mainly include catechol violet(CV),chrome cyanine R(ECR),chrome azurol S(CAS),morin and quercetin。
Table 2 summarizes the relevant studies on the determination of soluble aluminum in natural water by UV-Vis spectrophotometry.It can be seen that this method has a high detection limit,which is mostly focused on the detection of fresh water with simple matrix and high concentration of soluble aluminum,and the detection limit can not meet the analysis needs of low concentration water samples and other complex environmental samples.in order to solve this problem,in addition to optimizing the experimental parameters of the original method,the establishment of a new pretreatment system can also successfully reduce the interference of coexisting components,reduce the detection limit,and expand the application field of this method.Zhou et al.Developed a SPE(IDA)-CAS spectrophotometric method by using solid phase extraction and continuous flow technology,which reduced the detection limit to 0.80 nmol/L,and the method showed good stability and reproducibility in the navigation monitoring of the Jiulong River Estuary[54]。 It should be pointed out that there is no application study on the spectrophotometry of soluble aluminum in surface and profile seawater and aerosol in the pelagic sea area。
表2 Application of Ultraviolet-Visible Spectrophotometry in Environment

Table 2 Method for determination of dissolved aluminum based on UV-Visible Spectrophotometry

Colour-forming system Detection limit/nmol/L Linear range/µmol/L Sample matrix Ref
Al-Aluminon 480 29.63~137.04 well and pond water 55
Al-CAS 0.8 0.001~0.25 seawater 54
Al-ECR 5.19 0.15~14.81 waste and tap water 56
Al-ECR 74 2.78~23.15 surface, drinking water, and tap water 57
Al-ECR 11.11 - soil extracts and ground waters 58
Al-Quercetin 50 0.1 ~ 80 river and stream water 59
Al-Quercetin 260 0.74~18.52 tap water 60
Al-Morin 160 0.1~0.8 - 61
Al-Morin - 0.37~185.19 natural water(e.g. river, pond and seawater) 62

3.2 Fluorophotometry

in the analysis of trace metals,fluorophotometry is widely Used in the determination of soluble aluminum because of its high sensitivity,good selectivity,very low detection limit and simple operation.aluminum itself does not emit fluorescence,and it needs to be added to the complex to form a complex with fluorescent effect.the commonly used fluorescent reagents for surface water analysis are LMG,salicyl fluorone,morin and 8-HQ.Hydes et Al.used LMG to analyze soluble aluminum in seawater,removed the interference of coexisting organic matter on Al-LMG ligand by ultraviolet digestion,and heated the mixture to accelerate the ligand complexation reaction[63]。 Dammsh Dammshäuser et al.Used this method to detect the concentration of soluble aluminum in the surface seawater of the Atlantic Ocean,with a detection limit of 0.1~0.3 nmol/L[64]。
flow injection analysis(FIA)can make the analytical process of spectrophotometry and fluorophotometry into a pipeline,and complete the on-line separation and determination of samples In a non-equilibrium state with the help of reagent flow.It only needs to control the same reaction conditions,does not need to reach chemical equilibrium,greatly reduces the analysis time,and can be well applied to low-stability reaction systems.in addition,the flow analysis reduces a large number of manual operations in the traditional chemical analysis method,reduces external pollution,and has good reproducibility.In addition,FIA can be assembled with other instruments to realize the automation of the whole process。
Fluorescence spectrophotometry combined with flow injection analysis is one of the common methods for the determination of trace aluminum.Resing and Measures combined FIA with Al-LMG method to establish an on-line enrichment flow injection analysis method[24]; the soluble aluminum in seawater was preconcentrated on the 8-HQ chelating resin column,and then the aluminum was eluted from the resin column with acidified seawater.the eluted aluminum reacted with LMG to form a complex,which was finally quantified by fluorescence spectrophotometry.the method has a cycle time of only 3 min and a detection limit of 0.15 nmol/L,and has become a classical analytical method for the determination of soluble aluminum concentration in the ocean by shipboard.in order to analyze the aluminum content in aerosols,Measures et al.Replaced the extraction column with a Teflon injection tube of a specific length,and accurately determined the concentration of soluble aluminum in aerosols,with a detection limit of 0.5 nmol/L[53]。
Brown et Al.Further optimized the experimental process to improve the field applicability of FIA-Al-LMG fluorophotometry,replaced the eluent from seawater to deionized water,reduced the purification steps of seawater,and reduced the reagent blank background[26]。 A wide range of soluble aluminum concentration(<1 nmol/L to>80 nmol/L)was obtained by changing the time of sample passing through the column.Artigue et al.Used an improved FIA-LMG fluorophotometry to analyze seawater samples collected in the subtropical North Atlantic region[65]。

3.3 Atomic spectrometry

atomic spectrometry for the determination of trace metal elements mainly includes atomic absorption spectrometry(AAS)and atomic emission spectrometry(AES).AAS has high selectivity and stability,and is widely used in qualitative and quantitative analysis of elements,especially for the analysis of micro and trace components.According to the different atomization methods,AAS is divided into flame atomic absorption spectrometry(FAAS)and electrothermal atomic absorption spectrometry(ETAAS)represented by graphite furnace atomic absorption spectroscopy(GFAAS).Compared with FAAS,ETAAS requires smaller sample volume,higher atomization efficiency and higher sensitivity。
When de Almeida Pereira et al.used ETAAS to determine the total aluminum concentration in drinking water,zirconium was Used as a permanent modifier to coat the graphite furnace tube to eliminate the reaction between aluminum and the graphite furnace tube wall during atomization and to prevent the formation of refractory carbides[66][67]。 the results show that the intensity of the target signal measured after zirconium coating is increased by as much as 2 times,and the service life of the graphite furnace tube is also increased.Salomon et al.Optimized the parameters of ETAAS method from two aspects of spectrum and electrothermal,and realized the direct detection of low concentration aluminum in high salinity basal seawater samples.However,when the sample concentration is close to the detection limit,the system error is large,which affects the accuracy of the determination results[68]。 Therefore,the study further used the Zeeman effect to correct the background absorption caused by fine structure and spectral interference,and the lower limit of detection was reduced to 1.11 nmo/L.Although AAS has the advantages of simple operation and relatively cheap instrument,it can not analyze multiple elements at the same time.If multiple elements need to be determined,the light source lamp must be replaced,which greatly reduces the working efficiency。
ICP-AES(also known as ICP-OES)uses a plasma torch as the excitation light source,which greatly improves the sensitivity of AES.Due to the strong excitation ability of ICP light source,a large number of atoms and ions in the sample matrix will be excited to produce abundant spectral lines.If the sample composition is complex or the instrument resolution is insufficient,it will produce certain spectral interference,which will make it difficult to distinguish the interference signal from the target analyte signal,thus making the detection limit worse[69,70]。 Therefore,the sample generally needs to be separated and enriched before entering the plasma to reduce the matrix interference[30]。 The most obvious advantage of ICP-AES is that it can determine multiple elements at the same time and the analysis speed is fast.Atomic spectrometry is mostly used to determine the concentration of soluble aluminum in seawater or aerosol samples in the laboratory.For example,Chance et al.extracted marine aerosol particles collected by a high-flow sampler with ammonium acetate,and then analyzed the soluble content of aluminum and other metals in the extract by ICP-AES.the detection limit of soluble aluminum was 1.3~8.6 nmol/L[71]。

3.4 Inductively coupled plasma mass spectrometry

Inductively coupled plasma mass spectrometry(ICP-MS)is one of the mainstream methods for the determination of trace metals,which has the characteristics of low detection limit,high sensitivity,wide linear response range,stable signal,high ionization efficiency,simple spectral line,and simultaneous determination of multiple elements[27]。 Chang Yan et al.Improved the microcirculation leaching technology to simulate the dissolution kinetics of various metals including aluminum in water and dilute hydrochloric acid in total suspended particulate matter in Shanghai atmosphere,and quantified the dissolution concentration of metals in the solution by high-resolution inductively coupled plasma mass spectrometry(HR-ICP-MS)[52]; The detection limit of soluble aluminum was 0.026 nmol/L。
Although the matrix interference of ICP-MS is not as serious as that of atomic spectrometry,the salt crystallization in seawater will block the nebulizer and interface,and the molecular ions formed by high salt matrix will interfere with the analysis of aluminum,which restricts the practical application[27]。 When detecting low concentration of soluble aluminum in seawater,it is necessary to optimize the ICP-MS detection process by using appropriate pretreatment methods to separate and concentrate trace elements from the substrate.On the basis of previous work,Minami et al.Improved the structure and performance of the solid phase extraction preconcentration system for quantitative recovery of nine trace metals such as aluminum[72][22]。 the results showed that the concentration of the main cation in the eluent obtained by the automated SPE system was 17%lower than that obtained by the previous manual operation,which could reduce the impact on the quantification of HR-ICP-MS.the method has a detection limit of 0.3 nmol/L and has been successfully applied to the determination of soluble metals in seawater from the western North Pacific Ocean[73]。 However,despite the high sensitivity and rapid detection of ICP-MS,the high cost of equipment and manpower maintenance limits its wide application,and it is difficult for small and medium-sized laboratories to use this method for the quantification of soluble aluminum。
it is worth noting that when quantifying the concentration of soluble aluminum in aerosols,It is generally necessary to detect the dissolved concentration of metals in the extraction solution after completing the extraction experiment of soluble metals in land-based laboratories.the pure chemical reagents such as ultrapure water or ammonium acetate needed in the extraction experiment are different from the actual seawater samples,which have fewer coexisting ions and less chemical interference;the extract can be tested on the computer after simple filtration.Because ICP-AES and ICP-MS can simultaneously determine a variety of metal elements and have high sensitivity,researchers often use these two methods to detect aluminum,iron and other target metal elements at one time when carrying out the study of soluble trace elements in aerosols。

4 Research Progress of Aluminum Solubility in Aerosol

Table 3 summarizes the data of soluble aluminum in aerosols in some regions of the world.It can be seen that the research on soluble aluminum in aerosols is mainly focused on the Atlantic Ocean,the Pacific Ocean and their coastal areas,while the research on the Southern Ocean,the Indian Ocean and other vast sea areas,as well as inland cities,is still blank.in these studies,the observed values of aerosol aluminum solubility vary widely,and different extraction schemes are also important reasons for the differences,in addition to the mineral properties of aerosols themselves and their influence in the transport process。
表3 Observations of aluminium solubility in aerosols over parts of the globe

Table 3 Distribution of Al solubility in atmospheric aerosols in global distinct regions

Location Leaching solution Leaching technique Contact time Detection method Sample Al solubility
Pacific Ocean (Hawaii) [53] Seawater Batch (shaking) 5 min FIA TSP 0.087%~14.3%
Pacific Ocean[88] Deionized water Flow-through Instant HR-ICP-MS TSP 0.2%~15.9%
North Atlantic Ocean[89] Deionized water Flow-through Instant HR-ICP-MS TSP 4%~50%
North Atlantic Ocean[75] Deionized water Flow-through Instant ICP-MS TSP 0.34%~28%
Acetic acid Batch (soaking) 10 min 4.1%~100%
North East Atlantic Ocean[49] Ammonium acetate Batch (shaking) 60~120 min ICP-OES and ICP-MS dp>1.09 μm 0.43%~2.03%
dp<1.09 μm 4.53%~10.31%
South East Atlantic Ocean[71] Ammonium acetate Batch (shaking) 60 min ICP-OES TSP 3%~78%
PM1 7%~79%
East China Sea
(Huaniao Island) [82]		 Deionized water Batch (sonication) 40 min ICP-OES TSP 0.1%~23%
East China Sea[81] Deionized water Batch (shaking) 60 min ICP-OES TSP 5.1% ± 2.8%
(non-dust period)
1.1 %± 1.8%
(dust period)
Qingdao, China[90] Deionized water Batch (shaking) 30 min ICP-MS TSP 2.8% ± 3.9%
Hiroshima, Japan[50] Deionized water Batch (shaking) 30 min ICP-MS TSP 1.46%~7.39%
dp>1.3 μm 3.25% ± 3.41%
dp<1.3 μm 8.82% ± 6.48%
Hsieh et al.Extracted soluble aluminum with three different media:pure water,ammonium acetate,and acetate-hydroxylamine hydrochloride,and the results were quite different[74]。 According to Shelley et al.,the lower limit of solubility is obtained by using pure water as extract,while the upper limit of solubility is obtained by using acetic acid-hydroxylamine hydrochloride,that is,the potential maximum soluble part of elements[75]; the combination of the two methods can provide a dynamic range of element solubility.Ammonium acetate,as a weak buffer solution(pH=4.7),can avoid the pH change caused by the dissolution of aerosol components during the extraction process,allowing the comparison of different aerosol measurement results.Seawater is also a common extraction solution,but due to its higher ionic strength and pH,the resulting aluminum solubility is often lower than that in ultrapure water[76]。 However,the complex dynamics,physicochemical forms,and microbial communities of seawater vary widely from region to region and season to season,making it difficult to produce reproducible results.Therefore,it is necessary to take into account the differences in extraction methods when calculating the distribution of soluble aluminum in aerosols in different regions of the world.For better comparability of the data,some scholars have proposed that pure water or ammonium acetate should be preferred as the extract[77]。
aluminum in aerosols mainly comes from dust particles produced by wind erosion in arid and semi-arid areas,and its initial solubility is very low.Aghnatios et al.Collected carbonate minerals from the source area of the desert and found that the solubility of Aluminum in pure water was less than 0.2%[78]。 Shi et al.Selected two types of representative soils in the Sahara source area,used a resuspension device to resuspend dust particles,and collected aerosol samples of different particle sizes on a filter membrane through a staged sampler[79]; It was Found that the solubility of aluminum increased with the decrease of particle size,but even in the smallest particles(0.18~0.32μm),the solubility(1.42%)was significantly lower than that of the actual atmospheric particles.Baker et al.found that the solubility of aluminum in aerosols collected in the Atlantic Ocean was 1.9%~86%,which varied significantly with the source of air mass[17]。 Among them,the aluminum solubility of aerosols from the Saharan dust source area(median value of 3.0%)is significantly lower than that of aerosols from other sources(median value of 9.0%).One of the reasons may be that the initial source or composition of aluminum in different air masses is different,and some studies suggest that aluminum in anthropogenic combustion aerosols is more soluble[49]。 For example,Li et al.'s Research shows that the aluminum solubility in MSWI fly ash is 5.7%,which is much higher than that in dust particles and coal fly ash(0.8%±0.4%and 0.4%±0.6%)[80]。 in addition,due to the different sources of aerosols,there are obvious seasonal differences In the solubility of aluminum[81,82]。 Guo et al.Observed in Huaniao Island in the East China Sea that the total aluminum mass concentration in particulate matter was higher in spring,but the aluminum solubility(1.2%~1.5%)was significantly lower than that in summer and autumn(2.9%~3.3%),which was related to the frequent Asian dust activity in spring[82]。
Some studies based on field observations have found an inverse relationship between aluminum solubility and dust concentration[17,49,83]。 Previous studies have suggested that physical settlement is the main cause of this phenomenon.In the process of aerosol transport,due to the different settling velocities produced by gravity,the larger particles are preferentially removed,the concentration and average particle size of particles gradually decrease,the specific surface area of dust particles increases,and more trace elements are close to the surface of particles,which are easy to be extracted and dissolved.However,the change of concentration and particle size is not the only reason for this inverse relationship.Shi et al.Compared the laboratory simulated values with the observed values,and found that the simulated values obtained by only considering the gravity settlement were only slightly larger than their initial aluminum solubility(an increase of<2%),but were generally 1 to 2 orders of magnitude lower than the Atlantic field observations[79]。 This study suggests that the main mechanism of the change of aluminum solubility is not physical gravity sedimentation,but the result of physical action,chemical reaction and transport mixing process。
Laboratory studies have shown that the pH of the medium can affect the dissolution of aluminum in aerosols,resulting in changes in the solubility of aluminum.Researchers have studied the dissolution kinetics of clay minerals such as illite and montmorillonite in acidic solutions with different pH values,and found that with the increase of acidity of the solution,the dissolution rate of aluminum is accelerated and the amount of dissolution is increased[84⇓~86]。 Spokes et al.Collected aerosols from Sahara and urban areas,and simulated the periodic pH changes experienced by particulate matter in the cloud process by repeatedly adjusting the pH of the solution[87]。 the experimental results show that aerosol aluminum has higher solubility in low pH environment.the solubility of urban aerosol in pure water is only 3.1%,and the solubility can reach 27%when The pH value of the solution is reduced(2)。
Some field observations have shown that acidification reactions occurring in the atmosphere can increase the solubility of aluminum in aerosols.Measures et al.Found that the content of soluble aluminum in Hawaii aerosol in the Pacific Ocean increased with the increase of the content of secondary anions(non-sea salt sulfate and nitrate)[53]。 Baker et al.Observed that fine particles showed high aluminum solubility,because sulfate mainly existed in fine particles and nitrate mainly existed in coarse particles[49]; This study suggests that the heterogeneous reaction between mineral aerosols and SO2adsorbed on their surfaces during transport promotes the dissolution of aluminum.Sakata et al.Also observed that there was a good correlation between aluminum solubility and non-sea salt sulfate(no correlation with nitrate)in fine particulate matter,thus inferring that aluminum solubility was mainly controlled by SO2acidification reaction[50]。 However,there is no direct microscopic evidence that atmospheric acids react with aerosol aluminum,and the specific reaction mechanism is still uncertain。
In a word,there are many factors affecting the solubility of aerosol aluminum,and these factors are interrelated.For example,gravity sedimentation leads to the decrease of dust particle size,the increase of specific surface area and the sink of acidification reaction,which indicates that physical processes can promote acidification reaction and lead to the increase of aluminum solubility[81]。 In general,when predicting the change of aluminum solubility,regional and seasonal factors should be considered comprehensively,and the influence of various factors on aerosol aluminum solubility should be weighed,so as to accurately quantify the flux of aluminum solubility and dust deposition。

5 Conclusion and prospect

the establishment of an efficient analytical method for soluble aluminum in seawater and aerosols is essential to accurately grasp the concentration distribution of soluble aluminum in the ocean and aerosols,and can provide technical support for the accurate calculation of dust deposition flux in the ocean,thus deepening our understanding of the impact of aerosol deposition on marine biogeochemical cycles.in recent years,with the development of sampling and determination technology,the analysis and detection methods of soluble aluminum in environmental samples have made considerable progress,and the quantity and quality of data have been greatly improved.However,there are still some problems to be solved。
(1)the form of soluble aluminum in the environment is complex and changes with the change of environmental pH.the different chemical forms directly affect the chemical reaction activity and biological effect of aluminum.the existing sampling,pretreatment and analysis methods often change the pH of the experimental medium,so that the soluble aluminum no longer maintains its original compound form.to develop in-situ and in-situ analytical methods for seawater and aerosol samples To observe different species and provide a reference for further study of the dissolution mechanism of aluminum in ocean and particulate matter。
(2)different sample extraction schemes make the extraction results of soluble aluminum in aerosols different,so It is difficult to compare the solubility of aluminum in aerosols in different regions horizontally,and it is impossible to evaluate the precision between laboratories.it is urgent to establish standard sampling and extraction methods for aerosol soluble components,strengthen the quality control of the whole process of analysis methods,and provide technical support for the study of natural differences in aerosol aluminum solubility in different regions。
(3)At present,there are few field observations of aerosol aluminum,the coverage area is limited,and few studies have explored the trend of aerosol aluminum solubility with particle size.Compared with coarse particulate matter,fine particulate matter has a longer atmospheric life,a longer transport distance and a greater degree of aging,which may better reflect the enhancement of aluminum solubility by atmospheric chemical reactions.Therefore,long-term field observation of aerosol aluminum in typical areas and further exploration of particle size differences in aerosol aluminum solubility are helpful to clarify the spatial and temporal distribution of aerosol aluminum solubility and its key controlling factors。

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