Spectrophotometric study of Solvent extraction of Pb (II) and Cd (II) by aminooctyldiphosphonic acid

IKHOU Djamila; M'hamed Kaid; ZIANI Hanane; Didier Villemein

doi:10.12688/f1000research.54030.1

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Research Article

Spectrophotometric study of Solvent extraction of Pb (II) and Cd (II) by aminooctyldiphosphonic acid

[version 1; peer review: 1 approved with reservations, 1 not approved]

IKHOU Djamila¹, M'hamed Kaid ¹, ZIANI Hanane¹, Didier Villemein²

PUBLISHED 10 Nov 2021

Author details Author details

¹ Laboratoire d'études physico-chimique, Laboratoire d'études physico-chimique. University of Saida, Dr Moulay Tahar, 20000, Algeria
² EnsiCaen, LCMT, UMR CNRS 6507, INC3M,FR 338,Université de Caen, Caen, France, 14050, France

IKHOU Djamila
Roles: Software, Writing – Original Draft Preparation

M'hamed Kaid
Roles: Conceptualization, Methodology

ZIANI Hanane
Roles: Investigation, Writing – Original Draft Preparation

Didier Villemein
Roles: Conceptualization, Methodology

OPEN PEER REVIEW

REVIEWER STATUS

Abstract

This study has investigated the solvent extraction of cadmium and lead ions from an aqueous solution in nitrate medium using aminooctyldiphosphonic acid (AODPA) as extractant in chloroform. In order to establish spectrophotometrically the concentration of metal ion in the aqueous phase before and after extraction, the Arsenazo III method was used. The effects of several extraction parameters on the extraction of these metals ions including volume ratio between the aqueous and organic phases (1–5), extraction kinetic time (0–30 min), molar ratio Q (1–5), addition of HNO₃ (pH =2–6), addition of KNO₃ (0.01 – 1M), temperature (10–40°C) and the synergetic effect by adding TOPO (solvating agent) were evaluated. Thermodynamic parameters including the Gibbs free energy (ΔG⁰),enthalpy (ΔH⁰), and entropy (ΔS⁰) were calculated. Performed experiments showed that Pb (II) can be extracted till 73% when Cd (II) can be recovered completely after two cycles. The extraction of both metallic ions was spontaneous, endothermic and with a slight randomness. Positive synergetic effect was observed at a chelating agent/TOPO ratio of 3. It is a very encouraging result which can lead us to recover cadmium and lower the concentration of lead from wastewater.

Keywords

Aminooctylylphosphonic acid, solvent extraction, ion-exchange mechanism, Pb (II), Cd (II)

Corresponding author: M'hamed Kaid

Competing interests: No competing interests were disclosed.

Grant information: This work was supported by Dr Moulay Tahar University, Saida, Algeria and “PunchOrga” Network (Pole Universitaire Normand de Chimie Organique), the “Ministère de laRecherche et des Nouvelles Technologies,” CNRS (Centre National de laRecherche Scientifique).
The funders had no role in study design, data collection and analysis, decision to publish, or preparation of the manuscript.

Copyright: © 2021 Djamila I et al. This is an open access article distributed under the terms of the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

How to cite: Djamila I, Kaid M, Hanane Z and Villemein D. Spectrophotometric study of Solvent extraction of Pb (II) and Cd (II) by aminooctyldiphosphonic acid [version 1; peer review: 1 approved with reservations, 1 not approved]. F1000Research 2021, 10:1140 (https://doi.org/10.12688/f1000research.54030.1) First published: 10 Nov 2021, 10:1140 (https://doi.org/10.12688/f1000research.54030.1) Latest published: 10 Nov 2021, 10:1140 (https://doi.org/10.12688/f1000research.54030.1)

Introduction

The most rejected heavy metals are very polluting and dangerous. Lead and its inorganic derivatives are classified as category 2B (potentially carcinogenic to humans).¹ Lead modifies the cellular functioning by disrupting different physiological processes. It can thus cause blood anemia and renal effects (renal failure). Exposure to lead can affect the central nervous system (developmental delay, irritability, sleep disorders, loss of memory) and have long-term effects on fertility.² The effects of lead are generally amplified in the fetus and child (congenital abnormalities, persistent neurobehavioral deficits).^2,3 Cadmium, used in several industrial and agricultural processes as well as mining activities and designed carcinogenic by the United States (US) National Toxicology Program can increase the contamination of water and wastewaters around the world.⁴^,⁵ Cadmium can produce or increase the incidence of non-hereditary adverse effects in offspring.⁶ Inhalation, ingestion or skin penetration, even in very small quantities, can cause irritation in the stomach, leading to vomiting and diarrhea, renal insufficiency and, at high doses, chronic bronchitis, fibrosis, emphysema, damage to the bone system, kidney stones and increased blood pressure.^7–10

In order to eliminate or at least reduce the effects of these cations, many processes have been developed to face dangers towards human health and environment.

The use of the extraction process was widely used thus occupying a special place (for analytical purposes, in the processing of nuclear raw materials and in industries related to the fuel cycle). Solvent extraction consists of treating aqueous industrial waste before it is released into the environment. This process is a very efficient way of upgrading or rendering industrial wastes inert, and to treat discharges contaminated with lead and cadmium, and is generally aimed at recovering these metals, in order to reuse them and thus reduce their eco-toxicological impact.^11-13

The aim of our work was to determine the optimal parameters, at which the extraction yield was maximum, of the solvent extraction of lead (II) and cadmium (II) from an aqueous solution in nitrate medium by a new chelating agent- aminooctyldiphosphonic acid (AAODMDP), dissolved in chloroform, synthesized under microwaves.¹⁴

Methods

Study design and setting

This study was conducted in April 2020 in our laboratory and LCMT Caen (France). The experimental procedure and metal cations analysis is detailed below. In brief after preparing aqueous and organic solutions, contact between the solutions was done. The two phases were separated gravimetrically, and 1 mL of aqueous solution was taken for UV/V analysis.

For synergetic effect, the organic phase was a mixture of our chelating agent (AODMDPA) and a solvating agent (tri octyl phosphine oxide) at different volume ratio.

Reagents and apparatus

The reagents used in this study (with supplier and catalogue number) were: Lead nitrate tetrahydrate Pb (NO₃)₂ 4H₂O (99%, Riedel De Haen, 10099-74-8), Cadmium nitrate tetrahydrate Cd (NO₃)₂ 4H₂O (99%, Riedel De Haen, 10022-68-1), Arsenazo III C₂₂H₁₈AS₂N₄O₁₄S₂ (99%, Aldrich, 216-788-6), Nitric acid (65%, Panreac, 7697 37 2), Acétic acid CH₃COOH (80%, prolabo, 64-19-7), Sodium Acétate CH₃COONa (98%, prolabo, 6131-90-4), Potassium nitrate KNO₃ (99%, Riedel De Haen, 7757-79-1),Chloroform CHCl₃ (99% Riedel De Haen, 67-66-3), Aminooctane C₈H₁₉N (Aldrich, 111-86-4), Phosphorus acid (H₃PO₃, Aldrich, 13598-36-2), Hydrochloric acid (HCl, Riedel de Haen, 7647-01-0) , Formaldehyde (HCHO, Aldrich, 50-00-0), Acetone (C₃H₆O, Aldrich, 67-64-1), Tri octyl phosphine oxide TOPO ((C₈H₁₇)₃PO, 78-50-2) and aminooctyldiphosphonic acid (AODPA).¹⁴ Microwave irradiations were performed using microwave oven Synthewave 402 (Prolabo) working at a frequency of 2450 MHz. Nuclear magnetic resonance (NMR) spectra were done on a Fourier Bruker AC multinuclear spectrometer. Ultraviolet–visible spectrophotometry (UV/Vis) spectra were obtained using the UV/Visdouble beam Optizen 3220UVspectrometer, a digital pH meter type Consort C863 to follow solution pH.

Synthesis and characterization of Aminooctyldimethylene diphosphonic acid¹⁴

A mixture of aminooctane (C₄H₁₁N) (4.96 mL, 30.0 mmol), phosphorus acid (H₃PO₃) (5.02 g, 60.0 mmol), water (3.0 mL) and hydrochloric acid (HCL) 37% (3.0 mL) was irradiated (in a microwave oven) in a glass cylinder reactor fitted with a cooler at 240 W for 2 min. After adding formaldehyde (HCHO) 37% (4.8 mL, 64.46 mmol) rapidly, the mixture was irradiated for 12 min at 240 W. After cooling and evaporation for 5 min, the precipitate was filtered and the white solid was washed with acetone and water.

The product had the following properties: Yield (92 %), mp > 240°C, Formula: C₁₀H₂₅NO₆P₂, ¹H NMR (D₂O, Na₂CO₃):1.07 (t, 3H, CH₃), 1.15 (m, 12H, CH₂), 3.2 (d, ²J_HP = 9,01 NCH₂-P), 3.46 (m, 2H, N-CH₂); ³¹P NMR (D₂O, Na₂CO₃): d/H₃PO₄ (ppm) s, 6.7; ¹³CNMR (D₂O, Na₂CO₃): 19 (s, C1), 25.4 (s, C2), 27.3(s, C3), 31.7 (s, C3), 51 (d, 2JCP = 137.7, NCH₂-P); IR (υ Cm⁻¹): 2925(νasCH), 1333 (Deformation of (CH₂)_n: n > 4) 1120 (νs P-OH), 1044 (νs P=O), 938 (νsCm υ P-O) (s:symetric, as: antisymetric); pKa: 2.75, 8.73, 9.35, (9.67). These values indicated that in the water–acetone media, the first proton was strong and the other protons were weak.

Extraction procedure

After dissolving aminooctyldiphosphonic acid in chloroform, the obtained organic solutions were used for extraction studies. Aqueous metal solutions were prepared by dissolving Pb (NO₃)₂ 4H₂O and Cd (NO₃)₂ 4H₂O in distilled water. The first stage consisted of achieving curves of standardization of the absorbance according to the concentration of Pb²⁺ and Cd²⁺. The concentrations were in the range 10⁻⁶-10⁻³ mol. L⁻¹. Pb²⁺ and Cd ²⁺ analyses in the aqueous phase after extraction was performed by the Arsenazo III spectrophotometric method which consists of using this chromogenic reagent to form ion-arsenazo III complex. After separation of the organic from the aqueous phase, Arsenazo III was added to the later to form Arsenazo-Ion complex, which was placed in a quartz cuvette after adjusting the aqueous solution pH with buffer solution. The absorbance was learnt at λmax = 610 nm for Pb²⁺ (pH = 4)¹⁵ and λmax = 600 nm for Cd²⁺ (pH = 9.5),¹⁶ the second stage involved optimizing factors of extraction. The volume ratio Vaq/Vorg (the two phases: aqueous and organic; were mixed with different volumes) was carried out to establish the optimal yield of extraction and avoid emulsions, followed by the extraction kinetics (the two phases were stirred for different time). This was carried out to determine the necessary optimal time to reach the extraction equilibrium and for which the yield is maximal. The effect of different concentrations of the extractant (10⁻³M - 10⁻⁶M) on the extraction of the metallic ions was studied. The effect of the ionic strength (a salt (KNO₃) was added to the aqueous phase) and medium acidity (adding an acid (HNO₃) to the aqueous phase at a specific pH) were investigated adding salt or acids to aqueous solutions respectively. Synergetic effect was investigated by adding a solvating agent (Tri octyl phosphine oxide) to the chelating agent (AODPA) in the organic phase then determine the synergetic coefficient.

Results and discussion

In order to easily determine the different extraction factors, emulsions must be avoided. The distribution coefficient, D, and the extraction yield, Y, defined as follows,¹⁰ will be used to discuss the extraction results:

(1)

D = \frac{{Abs}_{org}}{{Abs}_{aq}} = \frac{{Abs}_{i} - {Abs}_{f}}{{Abs}_{f}}

(2)

Y % = \frac{{Abs}_{org}}{{Abs}_{aq}} = \frac{{Abs}_{i} - {Abs}_{f}}{{Abs}_{i}} \times 100

With the variables being as follows: Abi, Ab_f are the initial and final absorbance of aqueous solutions before and after extraction respectively.

Stirring speed effect

A parameter that appeared essential is the effect of the stirring speed. We noted that a medium stirring speed gave the highest extraction yield for both cations (Figure 1 and 2).²⁷ This can be explained by the fact that at the lowest speed, and taking into account the ionic radius of Pb²⁺ or Cd²⁺, the mass transfer is not favored. Also, at the highest stirring speed, the two cations seemed to be des-extracted which will help us in the des-extraction process.

Figure 1. Stirring speed effect on Lead extraction. [Pb²⁺] = 5 × 10⁻⁴ M, Vaq/Vorg = 1, T = 25°C.

rpm = rotations per minute.

Figure 2. Stirring speed effect on Cadmium extraction.

[Cd²⁺] = 5 × 10⁻⁴ M, Vaq/Vorg = 1, T = 25°C.

Aqueous to organic phase volume ratio

The effect of volume ratio on the extraction yield of Pb²⁺ or Cd²⁺ was investigated using lead and cadmium nitrate aqueous solutions of 5×10⁻⁴ M. A concentration of 10⁻³ M of the organic phase was prepared by dissolving aminooctyl diphosphonic acid in chloroform. The results are indicated in Figure 3.

Figure 3. Effect of volume ratio on extraction yield of Cd²⁺ and Pb²⁺.

Organic phase [AODMDPA] = M, [Cd²⁺] = [Pb²⁺] = M, 600 rpm, T = 25°C.

A volume ratio of 1 (which gave the maximum extraction yield) was used in the following experiences since the best-obtained yield of 40% and 25% were obtained, under this ratio, for Pb (II) and Cd (II) respectively. It is observed from Figure 3 that the higher the volume ratio, the lowest yield was, caused probably by a repulsion effect between the metal ions.

Extraction kinetics

The extraction kinetics results are shown in Figure 4. The variation of the stirring time between 0 and 30 minutes showed that the maximum yield of 32% was obtained for Pb²⁺ after 15 minutes, and 10 minutes was necessary for the Cd⁺². Thus, Pb²⁺ has greater resistance to mass transfer than Cd²⁺. This can be explained according to the atomic properties of the ionic radius of lead (1.2 A°) compared to that of cadmium (0.97 A°)

Figure 4. Kinetic of extraction of Lead and Cadmium, [AODMDPA] = M.

[Pb²⁺] = [Cd²⁺] = 5 × 10⁻⁴ M, (Vaq/Vorg) = 1, 600 rpm, T = 25°C.

Molar ratio effect

The molar ratio, Q, was used to investigate the extraction yield of the two metal ions. It is expressed as:

Q = \frac{n_{extractant}}{n_{metal ion}}

It can be seen in Figure 5, that the extraction of the two metal cations decreases with increasing AODMDPA concentration in the organic phase. The best extraction yields obtained were 55 % and 32% for Cd²⁺ and Pb²⁺ ions, respectively, at a molar ratio Q = 1.

Figure 5. Molar ratio effect on the extraction of Lead and Cadmium as function of Q.

[Pb²⁺] = [Cd²⁺] = 5 × 10⁻⁴ M, Vaq/Vorg = 1, 600rpm, T = 25°.

Ionic strength measures the electric field tension in a solution. To verify the influence of ionic strength on the output of extraction, we modified the aqueous phase by the addition of KNO₃ and HNO₃.

Influence of the addition of potassium nitrate (KNO₃)

The concentrations of KNO₃ were taken equal to 0.01 M, 0.1 M and 1 M. The obtained results are shown in Figures 6 and 7. According to the results, we found that there was an increase in the extraction yield of Pb²⁺ ions whatever the quantity of KNO₃ added to the system. A higher extraction percentage of lead ions in the presence of potassium nitrate can be attributed to the formation of stable complexes of Pb²⁺ in the aqueous phase in the presence of the latter salt.¹⁷ However, Additions of KNO₃ reduce the extraction yield in the case of Cd⁺². This may be due to the competition between Cd²⁺ and K⁺ ions, which is in accordance with the literature.¹⁸

Figure 6. Evolution of the extraction yield of Lead according to Q with the addition of potassium nitrate KNO₃.

[Pb²⁺] = 5×10⁻⁴ M, Vaq/Vorg = 1, T = 25°C.

Figure 7. Evolution of the extraction yield of Cadmium according to Q with the addition of potassium nitrate KNO₃.

[Cd²⁺] = 5 × 10⁻⁴ M, Vaq/Vorg = 1, T = 25°C.

Influence of the addition of nitric acid (HNO₃)

The effect of nitric acid addition to the aqueous phase before extraction was investigated, in the range of pH 2 – 3, on the extraction of 5×10⁻⁴ M of metallic cations. The results are shown in Figures 8 and 9. It was noted that the acidic medium disadvantages the lead ions extraction whereas, that of cadmium ions was seen to be favoured. Similar results were obtained in previous papers.^19,20

Figure 8. Evolution of the extraction yield of Lead according to Q with the addition of HNO₃.

[Pb²⁺] = 5 × 10⁻⁴ M, Vaq/Vorg = 1, T = 25°C.

Figure 9.

Evolution of the extraction yield of Cadmium according to Q with the addition of HNO₃ - [Cd²⁺] = 5 × 10⁻⁴ M, Vaq/Vorg = 1, T = 25°C.

Second extraction step

Another important variable affecting lead and cadmium recovery was studied. In Figures 10, 11, other extraction steps were realized. It was noted that Cd²⁺ can be recovered completely when Pb²⁺ reached 73% after two steps.

Figure 10. Evolution of the yield according to the second cycle of Lead by AODMDPA.

[Pb²⁺] = 5×10⁻⁴ M, Vaq/Vorg = 1, T = 25°C.

Figure 11. Evolution of the yield according to the second cycle of Cadmium by AODMDPA.

[Cd²⁺] = 5 × 10⁻⁴ M, Vaq/Vorg = 1, T = 25°C.

Temperature effect

The extraction yield was studied in the range of 10 to 40 ± 1°C. The results are given in Figure 12.

Figure 12.

Effect of temperature of the extraction yield of Lead and Cadmium, [AODMDPA] = 10⁻³M [Pb²⁺] = [Cd²⁺] = 5 × 10⁻⁴ M, (Vaq/Vorg) = 1.

From Figure 8, it noticed that an increase in the temperature from 10°C to 40°C favoured extraction yield. It allows us to predict the Pb²⁺ and Cd²⁺ des-extraction at high temperatures. This may be associated with the increase in the release of water molecules upon dehydration of ions during extraction. This is in good agreement with the results found in the literature.^21,22

Thermodynamic parameters calculation

Plots of the ln K values as a function of the inverse temperature [1/T (K)] in the range 283–313 K gave a straight line (Figure 13). The thermodynamic parameters can be determined by the following expressions²³:

Figure 13.

Variation in Ln Kin function 1/T for Lead and Cadmium extraction with AODMDPA.

(1)

Δ G^{o} = - RT \ln K

(2)

Δ G^{o} = Δ H^{o} - T Δ S^{o}

From these equations (1) and (2) we pull the following equation (3) to calculate ∆H° and ∆S° while drawing the curve LnK according to the temperature.

(3)

Ln K = Δ S^{o} / R - Δ H^{o} / RT

The numerical values of ΔH⁰, ΔS⁰ are computed from the slope.²⁴ The negative value of Gibbs free energy as shown in Table 1 indicates the spontaneous nature of extraction, while positive value of ΔH⁰ reflects the endothermic extraction behavior. The positive value of ΔS⁰ may be due to the increase in randomness around the chelating function.²⁵

Table 1. Thermodynamic parameters of the lead and cadmium at 298 K.

Cation	ΔG° (Kcal/mol)	ΔH° (Kcal/mol)	ΔS° (Cal/mol.K)
Pb²⁺	− 0.526	+ 17.30	+ 59.82
Cd²⁺	− 0.091	+ 15.80	+ 53.34

Synergetic effect

In order to study the synergetic effect, Tri octyl phosphine oxide TOPO (solvating agent) was added to our extractant (chelating agent) at 298 K. The synergetic coefficients were obtained as described by M. Taube and al.²⁶

Different phosphonic/TOPO volume ratios were tested presenting negative coefficients maybe because of steric and competition phenomena in the organic phase. The best synergetic coefficient was obtained at a phosphonic acid/TOPO volume ratio of 3 (Figures 14 and 15). The synergistic enhancement is attributed to the formation of complexes with the two extractants. Different positive synergetic coefficients are gathered in Table 2 showing that whatever the molar ratio, a positive synergetic coefficient was obtained.

Figure 14. Synergetic effect of the extraction yield of Cadmium according to Q.

[Cd²⁺] = 5 × 10⁻⁴ M, (Vaq/Vorg) = 1; (AODMDPA: TOPO = 3: 1), T = 25°C.

Figure 15. Synergetic effect of the extraction yield of Lead according to Q.

[Pb²⁺] = 5 × 10⁻⁴ M, (Vaq/Vorg) = 1;(AODMDPA: TOPO = 3: 1), T = 25°C.

Table 2. Different synergetic coefficients of Tri octyl phosphine oxide and phosphonic Acid (TOPO/AODMDPA) according to molar ratio Q.

Q: molar ratio Q₁: Q = 1, Q2: Q = 2, Q3: Q = 3, Q4: Q = 4, Q5: Q = 5.

D₁: Distribution factor using TOPO alone. D₂: Distribution factor using AODMDPA alone.

S: Synergetic factor $S = log \frac{D_{1 + 2}}{D_{1} + D_{2}}$ .

Cation	Molar ratio Q	Q1	Q2	Q3	Q4	Q5
Pb (II)	D₁ TOPO	0.096	0.108	0.116	0.056	0.047
	D₂ AODMDPA	0.44	0.377	0.375	0.383	0.381
	D₁₊₂ (AODMDPA +TOPO)	0.879	0.989	1.031	1.063	0.969
S₁ > 0 (positive synergy)		0.214	0.309	0.322	0.384	0.354
Cd (II)	D₁ TOPO	0.115	0.131	0.140	0.143	0.148
	D₂ AODMDPA	1.882	1.164	0.885	0.699	0.614
	D₁₊₂ (AODMDPA +TOPO)	2.130	2.363	1.461	1.220	1.017
S₂ > 0 (positive synergy)		0.028	0.26	0.166	0.161	0.125

Conclusion

A new phosphonic acid extractant named aminooctylphosphonic acid easily synthesized under microwave using low-cost chemicals. Complete achievement of Cd²⁺ can be reached when Pb²⁺ extraction reaches 73% after two cycles. A positive synergetic effect was observed at an AODMDPA/TOPO ratio of 3. It is a very encouraging result that can lead us to recover Cd²⁺ and lower the concentration of Pb²⁺ from wastewater.

Data availability

Open Science Framework: Spectrophotometric study of Solvent extraction of Pb (II) and Cd (II) by aminooctyldiphosphonic acid. https://doi.org/10.17605/OSF.IO/FMHT4.²⁷

This project contains the following underlying data:

- NMR Spectra
- Raw tables

Data are available under the terms of the Creative Commons Zero “No rights reserved” data waiver (CC0 1.0 Public domain dedication).

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Author details Author details

¹ Laboratoire d'études physico-chimique, Laboratoire d'études physico-chimique. University of Saida, Dr Moulay Tahar, 20000, Algeria
² EnsiCaen, LCMT, UMR CNRS 6507, INC3M,FR 338,Université de Caen, Caen, France, 14050, France

IKHOU Djamila
Roles: Software, Writing – Original Draft Preparation

M'hamed Kaid
Roles: Conceptualization, Methodology

ZIANI Hanane
Roles: Investigation, Writing – Original Draft Preparation

Didier Villemein
Roles: Conceptualization, Methodology

Competing interests

No competing interests were disclosed.

Grant information

This work was supported by Dr Moulay Tahar University, Saida, Algeria and “PunchOrga” Network (Pole Universitaire Normand de Chimie Organique), the “Ministère de laRecherche et des Nouvelles Technologies,” CNRS (Centre National de laRecherche Scientifique).
The funders had no role in study design, data collection and analysis, decision to publish, or preparation of the manuscript.

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Djamila I, Kaid M, Hanane Z and Villemein D. Spectrophotometric study of Solvent extraction of Pb (II) and Cd (II) by aminooctyldiphosphonic acid [version 1; peer review: 1 approved with reservations, 1 not approved]. F1000Research 2021, 10:1140 (https://doi.org/10.12688/f1000research.54030.1)

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Reviewer Report 19 Dec 2022

Yehezkiel Steven Kurniawan, Department of Chemistry, Universitas Gadjah Mada, Yogyakarta, Indonesia

Not Approved

https://doi.org/10.5256/f1000research.57474.r158212

1) The authors describe the harmful effects of lead(II) and cadmium(II) ions in the introduction but no explanation of why the authors use aminooctyldiphosponic acid structure as the extraction agent.

2) As a new compound, the HRMS ... Continue reading

1) The authors describe the harmful effects of lead(II) and cadmium(II) ions in the introduction but no explanation of why the authors use aminooctyldiphosponic acid structure as the extraction agent.

2) As a new compound, the HRMS measurement of aminooctyldiphosponic acid shall be reported.

3) Statistical error bars were reported in Figure 2 but other Figures do not show any error bars. Please revise the other Figures with error bars.

4) The authors give a small portion of the discussion of the experimental results and focus on reporting the experimental data without enough explanation/description.

5) How to recover the extraction reagent? Did the authors do the stripping experiment?

Is the work clearly and accurately presented and does it cite the current literature?

Partly
Is the study design appropriate and is the work technically sound?

No
Are sufficient details of methods and analysis provided to allow replication by others?

Yes
If applicable, is the statistical analysis and its interpretation appropriate?

Partly
Are all the source data underlying the results available to ensure full reproducibility?

Yes
Are the conclusions drawn adequately supported by the results?

Partly

Competing Interests: No competing interests were disclosed.

Reviewer Expertise: Solvent extraction, Metal separation, Separation engineering, Metal-organic framework, Heterocyclic compounds

I confirm that I have read this submission and believe that I have an appropriate level of expertise to state that I do not consider it to be of an acceptable scientific standard, for reasons outlined above.

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Reviewer Report 20 Sep 2022

Mohamed Abdelkrim Hasnaoui, Laboratoire de Chimie des Matériaux-LCM, Université Oran, Oran, Algeria

Approved with Reservations

https://doi.org/10.5256/f1000research.57474.r148149

Page 3 : Extraction procedure:

Authors should give the definition of Q the “molar ratio”and why it’s fixed to 1, 2, 3 , 4 and 5. It’s mentioned that different concentrations of the extractant (10^-3M to 10^-6 M)

Page 3 : Extraction procedure:

Authors should give the definition of Q the “molar ratio”and why it’s fixed to 1, 2, 3 , 4 and 5. It’s mentioned that different concentrations of the extractant (10^-3M to 10^-6 M) have been studied. These values are not compatible with the Q ratios given on figures 1 and 2, when [M²⁺]= 5.10^-4M) (M= Pb²⁺ or Cd²⁺). If the concentration of the cation is fixed, the concentration of the extractant should vary from 5.10^-4 to 25 10^-4.

Page 4 : Results and discussion

It’s more convenient to start with stirring time (Kinetic) in order to get the optimal time of extraction.
The parameter time has not been mentioned anywhere. Once this parameter is fixed, the volume ratio must be investigated followed by volume ration and molar ratio.
The investigation of the volume ratio (figure 3), has the molar ratio is close to 2 (see concentration of M2+ and organic phase). This parameter “volume ratio” should be investigated again at Q=1 for a convenient comparative study.
The comparison of the maximum %yield obtained, it can be seen a substantial difference. The maximum %yield of Cd2+ extraction reached 83 % (figure 2) when only 55% (figure 5) was obtained at ( 600rpm; Va/Vorg=1, and Q=1 fixed). (see table below). It can also be seen that the maximum of %yield of cadmium obtained after 10 mn is close to 31 % (figure 4), while 83% was obtained when stirring speed was investigated (figure 2). This Result needs more interpretation. See table: https://f1000researchdata.s3.amazonaws.com/linked/452329.Table.png

Effect of KNO3 addition:

On figure 6, it’s mentioned that the max %Yield obtained for free-KNO3 solution ( initial Pb2+) when, Va/Vorg=1, 600rpm and Q=1, is lower than mentioned on figure 1 ( 32 %).
On page 7 ”..can be attributed to the formation of stable complexes of Pb2+ in the aqueous phase in the presence of the latter salt..” : the authors tried to explain the augmentation of the yield of Pb²⁺ by the stability of the complex in the presence of KNO3. The authors are invited to explain why only for weak concentration 0,01M, the complex is stable?
Likewise, for better comparison the study should be investigated even at molar ratio Q=1. Because, it can be shown, that for the free-KNO3 solution, %Yield of cadmium is close to 65 %, while it reached 81 % when molar ratio Q=1 (figure 1). This lead to suppose that probably higher yield than 92% will be obtained at Q=1.

Influence of temperature:

On page 8: “..It allows us to predict the Pb2+ and Cd2+ des-extraction at high temperatures..” . There is no extremum for the two curves to predict the des-extraction by extrapolation, the study should be extended to others temperature higher than 40°.
The procedure to keep the temperature constant should be given in experimental section.

Conclusion

Rephrase the conclusion in a way that covers all the results obtained.

Is the work clearly and accurately presented and does it cite the current literature?

Partly
Is the study design appropriate and is the work technically sound?

Yes
Are sufficient details of methods and analysis provided to allow replication by others?

No
If applicable, is the statistical analysis and its interpretation appropriate?

I cannot comment. A qualified statistician is required.
Are all the source data underlying the results available to ensure full reproducibility?

Yes
Are the conclusions drawn adequately supported by the results?

Partly

Competing Interests: No competing interests were disclosed.

I confirm that I have read this submission and believe that I have an appropriate level of expertise to confirm that it is of an acceptable scientific standard, however I have significant reservations, as outlined above.

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Version 1

VERSION 1 PUBLISHED 10 Nov 2021

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Version 1 10 Nov 21	read	read

Mohamed Abdelkrim Hasnaoui, Université Oran, Oran, Algeria
Yehezkiel Steven Kurniawan, Universitas Gadjah Mada, Yogyakarta, Indonesia

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Reviewer Report

9 Views

19 Dec 2022 | for Version 1

Yehezkiel Steven Kurniawan, Department of Chemistry, Universitas Gadjah Mada, Yogyakarta, Indonesia

9 Views Cite this report Responses(0)

Not Approved

1) The authors describe the harmful effects of lead(II) and cadmium(II) ions in the introduction but no explanation of why the authors use aminooctyldiphosponic acid structure as the extraction agent.

2) As a new compound, the HRMS measurement of aminooctyldiphosponic acid shall be reported.

3) Statistical error bars were reported in Figure 2 but other Figures do not show any error bars. Please revise the other Figures with error bars.

4) The authors give a small portion of the discussion of the experimental results and focus on reporting the experimental data without enough explanation/description.

5) How to recover the extraction reagent? Did the authors do the stripping experiment?

Is the work clearly and accurately presented and does it cite the current literature?

Partly
Is the study design appropriate and is the work technically sound?

No
Are sufficient details of methods and analysis provided to allow replication by others?

Yes
If applicable, is the statistical analysis and its interpretation appropriate?

Partly
Are all the source data underlying the results available to ensure full reproducibility?

Yes
Are the conclusions drawn adequately supported by the results?

Partly

Competing Interests

No competing interests were disclosed.

Reviewer Expertise

Solvent extraction, Metal separation, Separation engineering, Metal-organic framework, Heterocyclic compounds

I confirm that I have read this submission and believe that I have an appropriate level of expertise to state that I do not consider it to be of an acceptable scientific standard, for reasons outlined above.

Respond to this report

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Back to all reports

Reviewer Report

9 Views

20 Sep 2022 | for Version 1

Mohamed Abdelkrim Hasnaoui, Laboratoire de Chimie des Matériaux-LCM, Université Oran, Oran, Algeria

9 Views Cite this report Responses(0)

Approved With Reservations

Page 3 : Extraction procedure:

Authors should give the definition of Q the “molar ratio”and why it’s fixed to 1, 2, 3 , 4 and 5. It’s mentioned that different concentrations of the extractant (10^-3M to 10^-6 M) have been studied. These values are not compatible with the Q ratios given on figures 1 and 2, when [M²⁺]= 5.10^-4M) (M= Pb²⁺ or Cd²⁺). If the concentration of the cation is fixed, the concentration of the extractant should vary from 5.10^-4 to 25 10^-4.

Page 4 : Results and discussion

It’s more convenient to start with stirring time (Kinetic) in order to get the optimal time of extraction.
The parameter time has not been mentioned anywhere. Once this parameter is fixed, the volume ratio must be investigated followed by volume ration and molar ratio.
The investigation of the volume ratio (figure 3), has the molar ratio is close to 2 (see concentration of M2+ and organic phase). This parameter “volume ratio” should be investigated again at Q=1 for a convenient comparative study.
The comparison of the maximum %yield obtained, it can be seen a substantial difference. The maximum %yield of Cd2+ extraction reached 83 % (figure 2) when only 55% (figure 5) was obtained at ( 600rpm; Va/Vorg=1, and Q=1 fixed). (see table below). It can also be seen that the maximum of %yield of cadmium obtained after 10 mn is close to 31 % (figure 4), while 83% was obtained when stirring speed was investigated (figure 2). This Result needs more interpretation. See table: https://f1000researchdata.s3.amazonaws.com/linked/452329.Table.png

Effect of KNO3 addition:

On figure 6, it’s mentioned that the max %Yield obtained for free-KNO3 solution ( initial Pb2+) when, Va/Vorg=1, 600rpm and Q=1, is lower than mentioned on figure 1 ( 32 %).
On page 7 ”..can be attributed to the formation of stable complexes of Pb2+ in the aqueous phase in the presence of the latter salt..” : the authors tried to explain the augmentation of the yield of Pb²⁺ by the stability of the complex in the presence of KNO3. The authors are invited to explain why only for weak concentration 0,01M, the complex is stable?
Likewise, for better comparison the study should be investigated even at molar ratio Q=1. Because, it can be shown, that for the free-KNO3 solution, %Yield of cadmium is close to 65 %, while it reached 81 % when molar ratio Q=1 (figure 1). This lead to suppose that probably higher yield than 92% will be obtained at Q=1.

Influence of temperature:

On page 8: “..It allows us to predict the Pb2+ and Cd2+ des-extraction at high temperatures..” . There is no extremum for the two curves to predict the des-extraction by extrapolation, the study should be extended to others temperature higher than 40°.
The procedure to keep the temperature constant should be given in experimental section.

Conclusion

Rephrase the conclusion in a way that covers all the results obtained.

Is the work clearly and accurately presented and does it cite the current literature?

Partly
Is the study design appropriate and is the work technically sound?

Yes
Are sufficient details of methods and analysis provided to allow replication by others?

No
If applicable, is the statistical analysis and its interpretation appropriate?

I cannot comment. A qualified statistician is required.
Are all the source data underlying the results available to ensure full reproducibility?

Yes
Are the conclusions drawn adequately supported by the results?

Partly

Competing Interests

No competing interests were disclosed.

I confirm that I have read this submission and believe that I have an appropriate level of expertise to confirm that it is of an acceptable scientific standard, however I have significant reservations, as outlined above.

Respond to this report

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[2] 2. Mason, Lisa H, Jordan P, et al.: Pb neurotoxicity: neuropsychological effects of lead toxicity. BioMed Res Int. 2014; 8.ID 840547

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[11] 11. Seubert A, Klingenberg A: Sulfoacylated macroporous polystyrene-divinylbenzene: a new type of cation exchanger for the analysis of multivalent metal cations. J. Chromatogr. 1997; A 782,2: 149–157. Publisher Full Text

[12] 12. Didi MA, Kaid M, Villemin D: Dodecylhydroxydiphosphonic acid for solvent extraction. Solvent Extr Ion Exch. 2008; 26(2): 113–127. Publisher Full Text

[13] 13. M’hamed K, Mohamed AD, Didier V: Poly (aminomethylenephosphonic) acid for solvent extraction of metal ions. Chemistry & Chemical Engineering, Biotechnology, Food Industry. 2011; 12,269–280.

[14] 14. Boulenouar I, Kaid M’h, Abbes O, et al.: Solvent Extraction of Lanthanum (III) and Europium (III) from Nitrate Media by Aminooctyldimethylene Diphosphonic Acid. Solvent Extraction Res Devel., Japan . 2016; 23(1): 51–61. Publisher Full Text

[15] 15. Michalova V, Kuleva N: Arsenazo III as a spectrophotometric reagent for deter mination of lead. Talanta . 1979; 27: 63–66. Publisher Full Text

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[17] 17. Soltani H, Yaftian MR, Zamani A, et al.: Selective Liquid-Liquid Extraction of Lead Ions Using Newly Synthesized Extractant 2-(Dibutylcarbamoyl) benzoic Acid. Anal. Bioanal. Chem. Res. 2015; 2(2): 91–98. Publisher Full Text

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[19] 19. Konczyk J, Kozlowski C, Walkowiak W: Lead (II) removal from aqueous solutions by solvent extraction with tetracarboxylresorcin[4]arene. Physicochem. Probl. Miner. Process. 2013; 49(1): 213–222. Publisher Full Text

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[21] 21. Huang C: Rare earth coordination chemistry: fundamentals and applications. Singapore: John Wiley & Sons (Asia) Pte Ltd.; 2010. p. 1–39.

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[23] 23. Yaftian MR, Hassanzadeh L, Eshraghi ME, et al.: Solvent extraction of thorium (IV) and europium (III) ions by diphenyl-N,N-dimethylcarbamoylmethylphosphine oxide from aqueous nitrate media. Sep Purif Technol. 2003; 31: 261–268. Publisher Full Text

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[27] 27. Mhamed K, Djamila I, Hanane Z, et al.: Spectrophotometric study of Solvent extraction of Pb (II) and Cd (II) by aminooctyldiphosphonic acid.2021, August 12. Publisher Full Text

Spectrophotometric study of Solvent extraction of Pb (II) and Cd (II) by aminooctyldiphosphonic acid

Abstract

Keywords

Introduction

Methods

Study design and setting

Reagents and apparatus

Synthesis and characterization of Aminooctyldimethylene diphosphonic acid14

Extraction procedure

Results and discussion

(1)

(2)

Stirring speed effect

Figure 1. Stirring speed effect on Lead extraction. [Pb2+] = 5 × 10−4 M, Vaq/Vorg = 1, T = 25°C.

Figure 2. Stirring speed effect on Cadmium extraction.

Aqueous to organic phase volume ratio

Figure 3. Effect of volume ratio on extraction yield of Cd2+ and Pb2+.

Extraction kinetics

Figure 4. Kinetic of extraction of Lead and Cadmium, [AODMDPA] = M.

Molar ratio effect

Figure 5. Molar ratio effect on the extraction of Lead and Cadmium as function of Q.

Figure 6. Evolution of the extraction yield of Lead according to Q with the addition of potassium nitrate KNO3.

Figure 7. Evolution of the extraction yield of Cadmium according to Q with the addition of potassium nitrate KNO3.

Figure 8. Evolution of the extraction yield of Lead according to Q with the addition of HNO3.

Figure 9.

Second extraction step

Figure 10. Evolution of the yield according to the second cycle of Lead by AODMDPA.

Figure 11. Evolution of the yield according to the second cycle of Cadmium by AODMDPA.

Temperature effect

Figure 12.

Thermodynamic parameters calculation

Figure 13.

(1)

(2)

(3)

Table 1. Thermodynamic parameters of the lead and cadmium at 298 K.

Synergetic effect

Figure 14. Synergetic effect of the extraction yield of Cadmium according to Q.

Figure 15. Synergetic effect of the extraction yield of Lead according to Q.

Table 2. Different synergetic coefficients of Tri octyl phosphine oxide and phosphonic Acid (TOPO/AODMDPA) according to molar ratio Q.

Conclusion

Data availability

References

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Synthesis and characterization of Aminooctyldimethylene diphosphonic acid¹⁴

Figure 1. Stirring speed effect on Lead extraction. [Pb²⁺] = 5 × 10⁻⁴ M, Vaq/Vorg = 1, T = 25°C.

Figure 3. Effect of volume ratio on extraction yield of Cd²⁺ and Pb²⁺.

Figure 6. Evolution of the extraction yield of Lead according to Q with the addition of potassium nitrate KNO₃.

Figure 7. Evolution of the extraction yield of Cadmium according to Q with the addition of potassium nitrate KNO₃.

Figure 8. Evolution of the extraction yield of Lead according to Q with the addition of HNO₃.