**2.1 Enrichment by extraction**

Extraction is the process of passing a chemical compound from a liquid phase into another liquid which is not mixed there with. The extraction of trace element into the organic phase is based on the incorporation of the trace element into a neutral structure. Neutral structures used in such a reaction; chelate, ion pair and covalent structures. In order to accurately measure trace elements, it is very important to separate and enrich the matrix before the analysis. Specific and sensitive methods are required for this.

**69**

selectivity is ensured.

*New Methods in the Synthesis of (Meth)Acrylamides and Application Chelating Resin…*

The trace elements at various levels in natural waters, wastewater, surface water and ground water are converted into chelates at a suitable pH and extracted into a small volume organic phase according to the sample. These elements taken into the organic phase are concentrated back to the aqueous phase directly or again and are determined by various determination techniques. Extraction is used not only in liquid samples but in solid samples to recover from matrix. The first step is to dissolve the sample. In chelate extraction the sample in the first aqueous phase is the appropriate reagent selection depending on the elements it contains. The reagent should form chelates with the desired trace elements and not form chelates with undesirable components. In this regard, chelates are also preferred in the extraction of trace elements, in particular in the alkali and alkaline earth compounds, or in samples containing them. Because chelating ligands do not generally form with

Ion pair complexes can also be extracted into organic solvents because they are neutral structures. It is difficult to derive quantitative equivalents or formulas in the extraction of ion pair complexes. Because ion pairs occur in the presence of extremely strong electrolytes. At the same time, a number of different ion strands can be found. Most inorganic complexes are used in extraction from ion pairs. Ion pairs usually occur between the anionic complexes formed by inorganic ligands and the H+

‐ ]. In the extraction process, selectivity is achieved by utilizing variants such as pH, side reactions in the aqueous phase, ligand, solvent type and temperature. Extraction efficiency is defined as the size of the amount of material passing from the

D = Corganic/ Caqueous (1)

aqueous phase to the organic phase. The dispersion rate is determined by D.

When the balance is established, Corganic, total concentration of analyte in organic phase; Caqueous, denotes the total concentration of the analyte in the aqueous phase. To increase efficiency in extraction processes; synergistic effect, co-extrac-

The use of precipitation methods in the separation of elements is based on the different solubility of the compounds in aqueous solutions. Collectors are used in quantitative separation of trace elements in solution by the method of co-precipitation. A large-surface precipitate with inorganic or organic character is formed, so that the adsorbed surface is adsorbed. The mechanism of co-precipitation depends on the physical and chemical properties of the trace element and the carrier and on the experimental conditions. According to this; three mechanisms in the form of

The carrier should be added to the sample solution so that sufficient amount of precipitate is formed. In order to prevent the adsorption of ions that may interfere, the amount of carrier should be as low as possible. Precipitation methods are mostly used for the separation of trace elements into single press as well as separating the main component from trace components. By controlling the precipitation pH,

ion.

*DOI: http://dx.doi.org/10.5772/intechopen.88685*

*2.1.1 Chelation extraction of trace elements*

alkali and alkaline earth alkalis.

tion and salt effect processes are utilized.

confinement, mixed crystal formation or adsorption.

*2.1.3 Enrichment with co-precipitation*

*2.1.2 Ion pair extraction*

[H+

, MLn+1

*New Methods in the Synthesis of (Meth)Acrylamides and Application Chelating Resin… DOI: http://dx.doi.org/10.5772/intechopen.88685*

### *2.1.1 Chelation extraction of trace elements*

The trace elements at various levels in natural waters, wastewater, surface water and ground water are converted into chelates at a suitable pH and extracted into a small volume organic phase according to the sample. These elements taken into the organic phase are concentrated back to the aqueous phase directly or again and are determined by various determination techniques. Extraction is used not only in liquid samples but in solid samples to recover from matrix. The first step is to dissolve the sample. In chelate extraction the sample in the first aqueous phase is the appropriate reagent selection depending on the elements it contains. The reagent should form chelates with the desired trace elements and not form chelates with undesirable components. In this regard, chelates are also preferred in the extraction of trace elements, in particular in the alkali and alkaline earth compounds, or in samples containing them. Because chelating ligands do not generally form with alkali and alkaline earth alkalis.

#### *2.1.2 Ion pair extraction*

*Trace Metals in the Environment - New Approaches and Recent Advances*

sufficient. The second term is the enrichment coefficient.

With enrichment techniques;

increased.

ing process.

enrichment methods;

• Enrichment factor

• Contamination

• Sample size

• Number of samples

• Time for enrichment

**2.1 Enrichment by extraction**

methods are required for this.

• The complexity of the technique

• Price and laboratory conditions.

The first one is the recovery efficiency. However, it is not always possible to achieve a large recovery value. At low concentrations, 90 or 95% recovery efficiencies are

The enrichment methods in the work analysis undertake important functions.

2.Instead of the original media components (matrix), the new and the appropri-

especially with the enrichment process used in combination with the dissolv-

The following criteria should be taken into account when selecting trace element

Extraction is the process of passing a chemical compound from a liquid phase into another liquid which is not mixed there with. The extraction of trace element into the organic phase is based on the incorporation of the trace element into a neutral structure. Neutral structures used in such a reaction; chelate, ion pair and covalent structures. In order to accurately measure trace elements, it is very important to separate and enrich the matrix before the analysis. Specific and sensitive

1.The ratio of the amount of trace element to the amount of media is

3.In the new environment, the analyte shows homogeneous distribution,

ate technique for the determination technique is created.

4.The standard preparation for calibration is made easier.

• Minimum concentration limits of trace elements

• Number of desired trace elements

• Recovery value of the method

• The method of determination following the enrichment method

**68**

Ion pair complexes can also be extracted into organic solvents because they are neutral structures. It is difficult to derive quantitative equivalents or formulas in the extraction of ion pair complexes. Because ion pairs occur in the presence of extremely strong electrolytes. At the same time, a number of different ion strands can be found. Most inorganic complexes are used in extraction from ion pairs. Ion pairs usually occur between the anionic complexes formed by inorganic ligands and the H+ ion. [H+ , MLn+1 ‐ ]. In the extraction process, selectivity is achieved by utilizing variants such as pH, side reactions in the aqueous phase, ligand, solvent type and temperature. Extraction efficiency is defined as the size of the amount of material passing from the aqueous phase to the organic phase. The dispersion rate is determined by D.

$$\mathbf{D} = \mathbf{C}\_{\text{organic}} / \mathbf{C}\_{\text{aquous}} \tag{1}$$

When the balance is established, Corganic, total concentration of analyte in organic phase; Caqueous, denotes the total concentration of the analyte in the aqueous phase. To increase efficiency in extraction processes; synergistic effect, co-extraction and salt effect processes are utilized.

#### *2.1.3 Enrichment with co-precipitation*

The use of precipitation methods in the separation of elements is based on the different solubility of the compounds in aqueous solutions. Collectors are used in quantitative separation of trace elements in solution by the method of co-precipitation. A large-surface precipitate with inorganic or organic character is formed, so that the adsorbed surface is adsorbed. The mechanism of co-precipitation depends on the physical and chemical properties of the trace element and the carrier and on the experimental conditions. According to this; three mechanisms in the form of confinement, mixed crystal formation or adsorption.

The carrier should be added to the sample solution so that sufficient amount of precipitate is formed. In order to prevent the adsorption of ions that may interfere, the amount of carrier should be as low as possible. Precipitation methods are mostly used for the separation of trace elements into single press as well as separating the main component from trace components. By controlling the precipitation pH, selectivity is ensured.

The use of the precipitation process to separate the main component from the work component is not common. Because when the main component collapses, it can also drag and drop work components together. This leads to substance loss.

### *2.1.4 Electrolytic enrichment*

The electrolysis method is used to separate trace amounts of heavy metals from various solutions. The composition of the electrolyte and sample, the type and shape of the electrode, the electrolysis cell and other experimental variables greatly affect the electrolytic deposition of an element. Potentially controlled electrolysis, as well as stripping methods, are widely used in the enrichment of trace elements.

#### *2.1.5 Ion exchange*

Ion exchange technique is a method of enrichment of trace elements. The ion exchange method can be practiced in three ways. The first is the rinsing technique that the solution and the ion exchanger interact in the same container. The second is the filtration technique in which the sample solution is held by ion-exchanging paper or membrane filter and the trace elements are kept. The third technique is the column technique which is the most commonly used technique in the application. In the rinsing technique, the solution containing the trace element ion is rinsed with resin. It is expected to establish a balance of time distribution. The resin is separated from the solution by filtration. The resin can be reacted with suitable solutions and trace elements can be determined by solution techniques or directly by solid analysis techniques. In the filtration technique, the sample solution is passed through an ion exchanger paper or membrane filter. Filter elements are determined by direct or degradation. In the column technique, large-volume solutions containing trace elements from the filled column with ion-exchange resin are passed to selectively hold them. These trace elements are attached with a smaller volume of eluent. This final volume can be further reduced by evaporation. Selectivity of the functional groups in the selection of ion exchangers, changing capacity, exchange rate, regeneration of the ion exchanger and use of the appropriate eluent are the considerations.

#### *2.1.6 Enrichment with evaporation*

It is a very convenient method for some elements that can be converted to volatile or easily volatile components. In fly enrichment, the volatility difference between the matrix and the trace element must be large. The separation by blowing can be done in two ways by blowing both the matrix and the trace element. However, in inorganic analysis, it is not common to enrich the trace elements by flying.

#### *2.1.7 Adsorption-enrichment*

The change in the concentration of a solid or a liquid on the boundary surface is called adsorption. This phenomenon arises from the accumulation of molecules or ions of the solute from the gas, liquid or any solution by adhering to the surface of a solid substance. The increase in concentration is called positive adsorption. The decrease in concentration is also called negative adsorption. Physical and chemical properties of adsorbent substances are the most important factors affecting the adsorption process. Solids, metals and plastics have more or less adsorption power. Some natural solids with high adsorption power; coals, clays, zeolites and various

**71**

**Figure 1.**

*Column technique processing steps.*

*New Methods in the Synthesis of (Meth)Acrylamides and Application Chelating Resin…*

metal sprouts, and artificial solids are activated charcoal, silica gel and special polymers. The amount of adsorbed substance in the solids having high adsorption

The solid phase extraction method is applied in three ways: rinsing technique, semi-permeable retaining disc filtration technique and column technique [30–35].

Solid phase extraction method is widely used in the column technique. Columns of different sizes can be used. This technique consists of four process steps: These

As column filler natural and artificial polymers, silica gel, alumina, florusil, octadecyl (C18); octyl (C8), ethyl (c2), cyano, phenyl, cyclohexyl, amino, diol,

quaternary amine, aromatic sulfonic acid, carboxylic acid can be used.

**3. Functional methacrylates from α-chloro-N-arylacetamides**

Synthesis of α-chloro-N-arylacetamide is as follows: potassium carbonate (K2CO3) (0.1 mol) and arylamine (1 mol) and are dissolved in 30 mL of anhydrous benzene. The reaction mixture is taken in a three-neck round bottom flask equipped with a magnetic stirrer, thermometer, and cooled to 0°C. After then chloroacetyl chloride (1.1 mol) are added dropwise to the solution and stirred at room temperature for 16 h. The organic layer is washed several times with diethyl ether and separation phase is filtered and dried over MgSO4. α-Chloro-N-arylacetamide is crystallized

from methanol. Yield: 80%. The synthesis reaction path is given in **Figure 2.**

The structure of the compoundα-chloro-N-arylacetamide is identified by the

): 3340 (NH); 3100–2800 (C─H); 1680 (>C═O);

**3.1 Synthesis of α-chloro-N-arylacetamide**

FT-IR techniques. FT-IR (cm<sup>−</sup><sup>1</sup>

1580 (aromatic, C═C) [36, 37].

power varies depending on the surface size and porous structure.

*DOI: http://dx.doi.org/10.5772/intechopen.88685*

*2.1.8 Solid phase extraction*

*2.1.8.1 Column technique*

process steps is given in **Figure 1**.

*New Methods in the Synthesis of (Meth)Acrylamides and Application Chelating Resin… DOI: http://dx.doi.org/10.5772/intechopen.88685*

metal sprouts, and artificial solids are activated charcoal, silica gel and special polymers. The amount of adsorbed substance in the solids having high adsorption power varies depending on the surface size and porous structure.

### *2.1.8 Solid phase extraction*

*Trace Metals in the Environment - New Approaches and Recent Advances*

*2.1.4 Electrolytic enrichment*

*2.1.6 Enrichment with evaporation*

*2.1.7 Adsorption-enrichment*

*2.1.5 Ion exchange*

The use of the precipitation process to separate the main component from the work component is not common. Because when the main component collapses, it can also drag and drop work components together. This leads to substance loss.

The electrolysis method is used to separate trace amounts of heavy metals from various solutions. The composition of the electrolyte and sample, the type and shape of the electrode, the electrolysis cell and other experimental variables greatly affect the electrolytic deposition of an element. Potentially controlled electrolysis, as well as stripping methods, are widely used in the enrichment of trace elements.

Ion exchange technique is a method of enrichment of trace elements. The ion exchange method can be practiced in three ways. The first is the rinsing technique that the solution and the ion exchanger interact in the same container. The second is the filtration technique in which the sample solution is held by ion-exchanging paper or membrane filter and the trace elements are kept. The third technique is the column technique which is the most commonly used technique in the application. In the rinsing technique, the solution containing the trace element ion is rinsed with resin. It is expected to establish a balance of time distribution. The resin is separated from the solution by filtration. The resin can be reacted with suitable solutions and trace elements can be determined by solution techniques or directly by solid analysis techniques. In the filtration technique, the sample solution is passed through an ion exchanger paper or membrane filter. Filter elements are determined by direct or degradation. In the column technique, large-volume solutions containing trace elements from the filled column with ion-exchange resin are passed to selectively hold them. These trace elements are attached with a smaller volume of eluent. This final volume can be further reduced by evaporation. Selectivity of the functional groups in the selection of ion exchangers, changing capacity, exchange rate, regeneration of the ion exchanger and use of the appropriate eluent are the considerations.

It is a very convenient method for some elements that can be converted to volatile or easily volatile components. In fly enrichment, the volatility difference between the matrix and the trace element must be large. The separation by blowing can be done in two ways by blowing both the matrix and the trace element. However, in inorganic analysis, it is not common to enrich the trace elements by

The change in the concentration of a solid or a liquid on the boundary surface is called adsorption. This phenomenon arises from the accumulation of molecules or ions of the solute from the gas, liquid or any solution by adhering to the surface of a solid substance. The increase in concentration is called positive adsorption. The decrease in concentration is also called negative adsorption. Physical and chemical properties of adsorbent substances are the most important factors affecting the adsorption process. Solids, metals and plastics have more or less adsorption power. Some natural solids with high adsorption power; coals, clays, zeolites and various

**70**

flying.

The solid phase extraction method is applied in three ways: rinsing technique, semi-permeable retaining disc filtration technique and column technique [30–35].

### *2.1.8.1 Column technique*

Solid phase extraction method is widely used in the column technique. Columns of different sizes can be used. This technique consists of four process steps: These process steps is given in **Figure 1**.

As column filler natural and artificial polymers, silica gel, alumina, florusil, octadecyl (C18); octyl (C8), ethyl (c2), cyano, phenyl, cyclohexyl, amino, diol, quaternary amine, aromatic sulfonic acid, carboxylic acid can be used.

**Figure 1.**

*Column technique processing steps.*
