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1.
Kumar M  Rathore DP  Singh AK 《Talanta》2000,51(6):1187-1196
A stable chelating resin matrix was synthesized by covalently linking o-aminophenol (o-AP) with the benzene ring of the polystyrene–divinylbenzene resin, Amberlite XAD-2, through a –N=N– group. Elemental analyses, thermogravimetric analysis (TGA) and infrared spectra have characterized the resulting chelating resin. It has been used to preconcentrate Cu2+, Cd2+, Co2+, Ni2+, Zn2+ and Pb2+, prior to their determination by flame atomic absorption spectrometry. The optimum pH values for quantitative sorption of Cu, Cd, Co, Ni, Zn and Pb are 6.2–7.4, 5.6–7.2, 5.6–9.0, 6.0–9.0, 5.7–7.0 and 5.0–6.0, respectively. These metals are desorbed (recovery 91–98%) with 4 mol dm−3 HNO3. The sorption capacity of the resin is 3.37, 3.42, 3.29, 3.24, 2.94 and 3.32 mg of metal g−1 of resin, respectively, for Cu, Cd, Co, Ni, Zn and Pb. The effect of NaF, NaCl, NaNO3, Na2SO4, and Na3PO4 on the sorption of these metal ions has been investigated. These electrolytes are tolerable up to 0.01 mol dm−3 in case of all the metal ions, except Cl which is tolerable even up to 0.1 mol dm−3 for Zn and 1.0 mol dm−3 for Pb. The preconcentration factor for Cu, Cd, Co, Ni, Zn and Pb are 50, 50, 100, 65, 40 and 40 (concentration level 10–25 μg dm−3) respectively. Simultaneous enrichment of the six metals is possible. The method has been applied to determine Cu, Cd, Co, Ni, Zn and Pb content in well water samples (RSD≤8%).  相似文献   

2.
Pyrocatechol is immobilized on cellulose via ---NH---CH2---CH2---NH---SO2---C6H4---N=N--- linker and the resulting macromolecular chelator characterized by IR, TGA, CPMAS 13C NMR and elemental analyses. It has been used for enrichment of Cu(II), Zn(II), Fe(III), Ni(II), Co(II), Cd(II) and Pb(II) prior to their determination by flame atomic absorption spectrometry (FAAS). The pH ranges for quantitative sorption (98.0–99.4%) are 4.0–7.0, 5.0–6.0, 3.0–4.0, 5.0–7.0, 5.0–8.0, 7.0–8.0 and 4.0–5.0, respectively. The desorption was found quantitative with 0.5 mol dm−3 HCl/HNO3 (for Pb). The sorption capacity of the matrix for the seven metal ions has been found in the range 85.3–186.2 μmol g−1. The optimum flow rate of metal ion solution for quantitative sorption of metal onto pyrocatechol functionalized cellulose as determined by column method, is 2–6 cm3 min−1, whereas for desorption it is 2–4 cm3 min−1. The tolerance limits for NaCl, NaBr, NaI, NaNO3, Na2SO4, Na3PO4, humic acid, EDTA, ascorbic acid, citric acid, sodium tartrate, Ca(II) and Mg(II) in the sorption of all the seven metal ions are reported. Ascorbic acid is tolerable up to 0.8 mmol dm−3 with Cu and Pb where as sodium tartrate does not interfere up to 0.6 mmol dm−3 with Pb. There is no interference of NaBr, NaCl and NaNO3 up to a concentration of 0.5 mol dm−3, in the sorption of Cu(II), Cd(II) and Fe(III) on to the chelating cellulose matrix The preconcentration factors are between 75 and 300 and t1/2 values ≤5 min for all the metal ions. Simultaneous sorption of Cu, Zn, Ni and Co is possible at pH 5.0 if their total concentration does not exceed lowest sorption capacity. The present matrix coupled with FAAS has been used to enrich and determine the seven metal ions in river and tap water samples (relative standard deviation (R.S.D.) 1.05–7.20%) and synthetic certified water sample SLRS-4 (NRC, Canada) with R.S.D. 2.03%. The cobalt present in pharmaceutical vitamin tablets was also preconcentrated on the modified cellulose and determined by FAAS (R.S.D. 1.87%).  相似文献   

3.
Goswami A  Singh AK  Venkataramani B 《Talanta》2003,60(6):1141-1154
The silica gel modified with (3-aminopropyl-triethoxysilane) was reacted with 5-formyl-8-hydroxyquinoline (FHOQx) to anchor 8-quinolinol ligand on the silica gel. It was characterised with cross polarisation magic angle spinning (CPMAS) NMR and diffuse reflectance infrared Fourier transformation (DRIFT) spectroscopy and used for the preconcentration of Cu(II), Pb(II), Ni(II), Fe(III), Cd(II), Zn(II) and Co(II) prior to their determination by flame atomic absorption spectrometry. The surface area of the modified silica gel has been found to be 227 m2 g−1 and the two pKa values as 3.8 and 8.0. The optimum pH ranges for quantitative sorption are 4.0–7.0, 4.5–7.0, 3.0–6.0, 5.0–8.0, 5.0–8.0, 5.0–8.0 and 4.0–7.0 for Cu, Pb, Fe, Zn, Co, Ni and Cd, respectively. All the metals can be desorbed with 2.5 mol l−1 HCl or HNO3. The sorption capacity for these metal ions is in range of 92–448.0 μmol g−1 and follows the order Cd3, NaCl, NaBr, Na2SO4 and Na3PO4, glycine, sodium citrate, EDTA, humic acid and cations Ca(II), Mg(II), Mn(II) and Cr(III) in the sorption of all the seven metal ions are reported. The preconcentration factors are 150, 250, 200, 300, 250, 300 and 200 for Cd, Co, Zn, Cu, Pb, Fe and Ni, respectively and t1/2 values <1 min except for Ni. The 95% extraction by batch method takes ≤25 min. The simultaneous enrichment and determination of all the metals are possible if the total load of the metal ions is less than sorption capacity. In river water samples all these metal ions were enriched with the present ligand anchored silica gel and determined with flame atomic absorption spectrometer (R.S.D.≤6.4%). Cobalt contents of pharmaceutical samples (vitamin tablet) were preconcentrated with the present chelating silica gel and estimated by flame AAS, with R.S.D.1.4%. The results are in the good agreement with the certified value, 1.99 μg g−1 of the tablets. Iron and copper in certified reference materials (synthetic) SLRS-4 and SLEW-3 have been enriched with the modified silica gel and estimated with R.S.D.<5%.  相似文献   

4.
A field oriented and economical method of coprecipitation of trace elements like Al, Au, Bi, Cd, Co, Cu, Fe, Mo, Ni, Pb, Pd, Ti, V, W, Zn and REE has been developed. A novel reductant D-glucose, reduces KMnO4 in solution to form a precipitate of MnO2. Two liters of clear natural water sample is adjusted to pH 3.5–4.0, and is treated with 10 ml of 1% KMnO4 and 20 ml of 0.1% D-glucose. The sample is heated at a temperature of 75–80 °C, MnO2 is formed which coprecipitates the above trace elements. The precipitate is separated by filtration, dissolved in 2 ml of 50% HCl and 2 ml of 30% H2O2 and diluted to 25 ml for analysis using AAS and ICP-AES. The recoveries were found to be 96–105%. The preconcentration factor is 80. Limits of determination by the proposed method in natural waters are 1 μg l−1 for Al, Cd, Mo, V, W, Ti and Zn, 5 μg l−1 for Au, Bi, Co, Cu, Fe, Ni, Pb and Pd and 8 μg l−1 for REE. The RSD of the present procedure (n=5) is 8% at 5 μg l−1 level. Twenty water samples can be analyzed by an analyst in an 8-h day.  相似文献   

5.
Narin I  Soylak M  Elçi L  Doğan M 《Talanta》2000,52(6):1041-1046
A simple preconcentration method is described for the determination of Cu, Mn, Co, Cd, Pb, Ni and Cr in water samples by flame AAS. Trace metal ions in water were sorbed as pyrocatechol violet complexes on activated carbon column at the pH range of 4–8, then eluted with 1 M HNO3 in acetone. The effect of major cations and anions of the natural water samples on the sorption of metal ions has been also investigated. The concentration of the metal ions detected after preconcentration was in agreement with the added amount. The present method was found to be applicable to the preconcentration of Cu, Mn, Co, Cd, Pb, Ni and Cr in natural water samples with good results such as R.S.D. from 3 to 8% (N=10) and detection limits under 70 ng l−1.  相似文献   

6.
Two new stable chelating resins have been synthesized incorporating the imidazolylazobenzene and 1,4-bis(imidazolylazo)benzene as functional group into Merrifield polymer through CN covalent bond and characterized by elemental analyses, IR and thermal study. A comparison of sorption capacity of newly formed resins towards the cations Ag(I), Cu(II), Zn(II), Cd(II), Hg(II) and Pb(II) as a function of pH has been studied. Kinetic studies show the time for the completeness of metal ion saturation with the resin phase. Cd(II) in trace quantities has been successfully separated and determined in different biological samples and Zn(II) in medicinal samples. It is also found that Cd(II) can be removed from water at usual pH of natural water. Both the resins can be employed for water purification as the resins reveal sorption ability towards toxic metal ions and exhibit no affinity to alkali or alkaline earth metal ions.  相似文献   

7.
在研究垃圾与污泥掺烧后焚烧飞灰中重金属浸出特征的基础上,重点研究了飞灰在1 000 ℃条件下高温处置过程中重金属(Cu、Zn 、Pb、Cd)随不同停留时间的挥发特性及添加剂(CaO、Al2O3、SiO2、高岭土、粉煤灰)对重金属转化与挥发特性的影响。研究结果表明,飞灰中重金属Zn、Pb、Mn含量较高,Ni的含量较低,而毒性较大的Cd达到29.4 mg/kg。浸出液中七种金属都满足危险废物鉴别标准(GB5085.3-1996),并且重金属的浸出浓度受浸取时间及浸取液pH值影响较大。在同样的高温处置条件下,焚烧飞灰中不同重金属的挥发特性有较大的差别。其中,Pb表现出易挥发的特性,其挥发率超过80%,而Cu挥发性较小,其挥发率小于30%。综合来看,飞灰中重金属的挥发性大小依次为Pb>Cd>Zn>Cu。飞灰中添加Al2O3和高岭土可以抑制Cd的挥发,添加Al2O3后Pb的挥发率有所减少,添加SiO2、CaO、高岭土、粉煤灰均使Zn的挥发率降低,而对Cu的挥发率没有抑制作用,这与飞灰中高Cl含量及各痕量元素化合物对固体添加剂活性位选择性的竞争吸附有关。  相似文献   

8.
Two novel azocalix[4]pyrrole Amberlite XAD-2 polymeric chelating resins were synthesized by covalently linking diazotized Amberlite XAD-2 with calix[4]pyrrole macrocycles. The chelating resins were used for extraction, preconcentration and sequential separation of metal ions such as Cu(II), Zn(II) and Cd(II) by column chromatography prior to their determination by UV/vis spectrophotometry or flame atomic absorption spectrophotometry (FAAS) or inductively coupled plasma atomic emission spectroscopy (ICP-AES). Various parameters such as effect of pH on absorption, concentration of eluting agents, flow rate, total sorption capacity, exchange kinetics, preconcentration factor, distribution coefficient, breakthrough capacity and resin stability, were optimized for effective separation and preconcentration. The resin showed good ability for the separation of metal ions from binary and ternary mixture on the basis of pH of absorption and concentration of eluting agents. The newly synthesized resins showed good potential for trace enrichment of Cu(II), Zn(II) and Cd(II) metal ions, especially for Cu(II), as compared to the earlier reported resins. The synthesized resins were recycled at least 8-10 times without much affecting column sorption capacity. The presented method was successfully applied for determination of Cu(II), Zn(II) and Cd(II) in natural and ground water samples.  相似文献   

9.
10.
Morlay C  Cromer M  Mouginot Y  Vittori O 《Talanta》1999,48(5):679-1166
The cadmium (II) or lead (II) complex formation with two poly(acrylic acids) of high molecular weight (Mw=2.5×105 and 3×106) was investigated in dilute aqueous solution (NaNO3 0.1 mol l−1; 25°C). Potentiometric titrations were carried out to determine the stability constants of the MA and MA2 complex species formed. Bjerrum’s method, modified by Gregor et al. (J. Phys. Chem. 59 (1955) 34–39), for the study of polymeric acids was used. The results were compared to those previously obtained in the same conditions with copper (II) and nickel (II) . It appeared that the two polymers under study present similar binding properties and that the stability constants of the complex species formed increased in the following order, depending on the metal ion: Ni(II)β102 was found to be close to 7.0) and allowed the formation of the predominant PbA2 species in a quite large pH domain. Finally, the greater stability of PAA complexes compared to those of their monomeric analogs, glutaric and acetic acids, was confirmed.  相似文献   

11.
Factors affecting the efficiency of electrochemical recovery of EDTA and Pb(II) from their chelated solutions were systematically examined using a cation exchange membrane Neosepta CM-1. The catholyte contained an equimolar amount of Pb(II) and EDTA, and the anolyte contained 0.1 M NaNO3. The iridium oxide coated on titanium (IrO2/Ti) and stainless steel were used as anode and cathode, respectively. Experiments were carried out at different current densities (46.3–185 A/m2), initial catholyte pH values (1.47–6.02) and Pb(II) concentrations (0.005–0.03 M). An economically feasible current efficiency and recovery percentages of Pb(II) and EDTA could be achieved if the concentration of the chelated Pb(II) was sufficiently high.  相似文献   

12.
Migration of radioactive radium, 226Ra, in soil is an environmental concern, especially in areas adjacent to uranium processing facilities. Barium(II), as Ba2+, was used as a Ra analog and reacted with a Na-montmorillonite to obtain mechanistic insights into the interaction of Ra with soil matrices. The majority of sorbed Ba is associated with the permanently charged surface sites on the montmorillonite basal surface. This is indicated by the facts that (1) sorption of Ba(II) on montmorillonite is not highly sensitive to solution pH, although an increase of sorption was observed at higher pH values; and (2) displacement of sorbed Ba increased with increased NaNO3 concentration. As demonstrated by EXAFS, a small fraction of Ba also adsorbed on the montmorillonite edge, forming an inner-sphere surface complex through sharing of oxygen atom(s) from deprotonated –OH group of the Al octahedral layer. The EXAFS measured distances between Ba and O at the first shell, and Ba and Al of the second shell are 2.7–2.8 and 3.7–3.9 Å, respectively, consistent with the results from geometry of a inner-sphere complex at the edge site. Results from bulk experiments and spectroscopic analysis suggest a co-existence of outer- and inner-sphere surface complexes for Ba sorbed to the montmorillonite surface.  相似文献   

13.
Jain VK  Sait SS  Shrivastav P  Agrawal YK 《Talanta》1997,45(2):397-404
A very stable chelating resin matrix was synthesized by covalently linking o-vanillinthiosemicarbazone (oVTSC) with the benzene ring of the polystyrene-divinylbenzene resin Amberlite XAD-2 through a -NN- group. The resin was used successfully for the separation and preconcentration of copper(II), zinc(II) and lead(II) prior to their determination by atomic absorption spectrophotometry. The total sorption capacity of the resin was 850, 1500 and 2000 mug g(-1) of the resin for Cu(II), Zn(II) and Pb(II), respectively. For the quantitative sorption and recovery of Cu(II), Zn(II) and Pb(II), the optimum pH and eluants were pH 2.5-4.0 and 4 M HCl or 2 M HNO(3) for Cu(II), pH 5.5-6.5 and 1.0-2.0 M HCl for Zn(II) and pH 6.0-7.5 and 3 M HCl or 1 M HNO(3) for Pb(II). Both, the uptake and stripping of these metal ions were fairly rapid, indicating a better accessibility of the chelating sites. The t (1 2 ) values for Cu(II), Zn(II) and Pb(II) were also determined. Limit of tolerance of some electrolytes like NaCl, NaF, NaNO(3), Na(2)SO(4) and Na(3)PO(4) have been reported. The preconcentration factor for Cu(II), Zn(II) and Pb(II) was 90, 140 and 100 respectively. The method was applied for the determination of Cu(II), Zn(II) and Pb(II) in the water samples collected from Sabarmati river, Ahmedabad, India.  相似文献   

14.
Prabhakaran D  Subramanian MS 《Talanta》2003,59(6):1227-1236
A new chelating polymeric sorbent was developed by functionalizing Amberlite XAD-16 with 1,3-dimethyl-3-aminopropan-1-ol via a simple condensation mechanism. The newly developed chelating matrix offered a high resin capacity and faster sorption kinetics for the metal ions such as Mn(II), Pb(II), Ni(II), Co(II), Cu(II), Cd(II) and Zn(II). Various physio-chemical parameters like pH-effect, kinetics, eluant volume and flow rate, sample breakthrough volume, matrix interference effect on the metal ion sorption have been studied. The optimum pH range for the sorption of the above mentioned metal ions were 6.0–7.5, 6.0–7.0, 8.0–8.5, 7.0–7.5, 6.5–7.5, 7.5–8.5 and 6.5–7.0, respectively. The resin capacities for Mn(II), Pb(II), Ni(II), Co(II), Cu(II), Cd(II) and Zn(II) were found to be 0.62, 0.23, 0.55, 0.27, 0.46, 0.21 and 0.25 mmol g−1 of the resin, respectively. The lower limit of detection was 10 ng ml−1 for Cd(II), 40 ng ml−1 for Mn(II) and Zn(II), 32 ng ml−1 for Ni(II), 25 ng ml−1 for Cu(II) and Co(II) and 20 ng ml−1 for Pb(II). A high preconcentration value of 300 in the case of Mn(II), Co(II), Ni(II), Cu(II),Cd(II) and a value of 500 and 250 for Pb(II) and Zn(II), respectively, were achieved. A recovery of >98% was obtained for all the metal ions with 4 M HCl as eluting agent except in the case of Cu(II) where in 6 M HCl was necessary. The chelating polymer showed low sorption behavior to alkali and alkaline earth metals and also to various inorganic anionic species present in saline matrix. The method was applied for metal ion determination from water samples like seawater, well water and tap water and also from green leafy vegetable, from certified multivitamin tablets and steel samples.  相似文献   

15.
Morin was successful as a chemical modifier to improve the reactivity of the nanometer SiO2 surface in terms of selective binding and extraction of heavy metal ions. This new functionalized nanometer SiO2 (nanometer SiO2-morin) was used as an effective sorbent for the solid-phase extraction (SPE) of Cd(II), Cu(II), Ni(II), Pb(II), Zn(II) in solutions prior to its determination by inductively coupled plasma atomic emission spectrometry (ICP-AES). Experimental conditions for effective adsorption of trace levels of metal ions were optimized with respect to different experimental parameters using static and dynamic procedures in detail. The pH 4.0 was chosen as the optimum pH value for the separation of metal ions on the newly sorbent. Complete elution of the adsorbed metal ions from the nanometer SiO2-morin was carried out using 2.0 mL of 0.5 mol L−1 of HCl. Common coexisting ions did not interfere with the separation and determination at pH 4.0. The maximum static adsorption capacity of the sorbent at optimum conditions was found to be 22.36, 36.8, 40.37, 33.21 and 25.99 mg metal/g SiO2-morin for Cd(II), Cu(II), Ni(II), Pb(II) and Zn(II), respectively. The time for 95% sorption for Cu(II) and Ni(II) and 70% sorption for Cd(II), Pb(II) and Zn(II) was less than 2 min. The relative standard deviation (RSD) of the method under optimum conditions was lower than 5.0% (n = 11). The procedure was validated by analyzing the certified reference river sediment material (GBW 08301, China), the results obtained were in good agreement with standard values. The nanometer SiO2-morin was successfully employed in the separation and preconcentration of trace Cd(II), Cu(II), Ni(II), Pb(II) and Zn(II) from the biological and natural water samples yielding 75-folds concentration factor.  相似文献   

16.
Amberlite XAD-2 has been functionalized by coupling it, through the ---N=N--- group, with Pyrocatechol Violet (PV), and the resulting resin has been characterized by elemental analysis, thermogravimetric analysis (TGA) and IR spectra. The resin has been used for preconcentrating Zn(II), Cd(II), Pb(II) and Ni(II) ions prior to their determination by flame atomic absorption spectrometry. The optimum pH values for quantitative sorption are 5, 5–7, 4, and 3 for Zn, Cd, Pb and Ni, respectively. The four metals can be desorbed (recovery ˜98%) with 4 M HNO3; also, 4 M HCl is equally suitable except for Zn. The sorption capacity of the resin is 1410, 1270, 620 and 1360 μg g−1 resin for Zn, Cd, Ni and Pb, respectively. The effect of F, Cl, NO3, SO42− and PO43− on the sorption of these four metal ions has been investigated. They are tolerable in the range 0.01–0.20 M, for Pb. In the sorption of Zn(II) and Ni(II), the tolerance limits of all these ions are upto 0.01 M, whereas for Cd(II), F, NO3, and PO43− have been found to be tolerable upto 0.50, 0.10 and 0.10 M, respectively. The preconcentration factors are 60, 50, 23 and 18 for Zn, Cd, Pb and Ni, respectively. Simultaneous collection and determination of the four metals are possible. Cations commonly present in drinking water do not affect the sorption of either metal ion if present at a concentration level similar to that of water. The method has been applied to determine Zn, Ni and Pb content of well-water samples (RSD ≤9%).  相似文献   

17.
Micro volume changes due to Pb(II) and Cu(II) sorption on amorphous Fe(III) hydroxide (AFH) were determined by a dilatometer at pH 4.50. Volume change is attributed to change in hydration status of dissolved and/or suspended substances. The volume of the system increased due to Pb(II) and Cu(II) sorption, suggesting that water molecules hydrated around Pb(II) or Cu(II) ions and AFH were released during sorption. Volume increases due to Pb(II) and Cu(II) sorption were smaller than those due to bulk precipitation of Pb and Cu hydroxides. Precipitation of Pb(II) and Cu(II) was not likely to occur at pH 4.50 in the presence of AFH. In conclusion, Pb(II) and Cu(II) formed an inner-sphere complex on AFH at pH 4.50, keeping hydrated water on the adsorbed species. Adsorbed Cu(II) kept more hydrated water than adsorbed Pb(II) on AFH.  相似文献   

18.
Filho NL  Polito WL  Gushikem Y 《Talanta》1995,42(8):1031-1036
2-Mercaptobenzothiazole loaded on previously treated clay was prepared, characterized and used for sorption and preconcentration of Hg(II), Pb(II), Zn(II), Cd(II), Cu(II) and Mn(II) from an aqueous solution. The support used was a natural clay previously treated with sulphuric acid solution. Adsorption isotherms of metal ions from aqueous solutions as function of pH were studied at 298 K. Conditions for quantitative retention and elution were established for each metal by batch and column methods. The chemically treated clay was very selective to Hg(II) in solution in which Zn(II), Cd(II), Pb(II), Cu(II) and Mn(II) were also present.  相似文献   

19.
20.
A new polychelatogen, AXAD-16-1,2-diphenylethanolamine, was developed by chemically modifying Amberlite XAD-16 with 1,2-diphenylethanolamine to produce an effective metal-chelating functionality for the preconcentration of Mn(II), Ni(II), Cu(II), Zn(II), Cd(II), and Pb(II) and their determination by flame atomic absorption spectrometry. Various physiochemical parameters that influence the quantitative preconcentration and recovery of metal were optimized by both static and dynamic techniques. The resin showed superior extraction efficiency with high-metal loading capacity values of 0.73, 0.80, 0.77, 0.87, 0.74, and 0.81 mmol/g for Mn(II), Ni(II), Cu(II), Zn(II), Cd(II), and Pb(II), respectively. The system also showed rapid metal-ion extraction and stripping, with complete saturation in the sorbent phase within 15 min for all the metal ions. The optimum condition for effective metal-ion extraction was found to be a neutral pH, which is a great advantage in the preconcentration of trace metal ions from natural water samples without any chemical pretreatment of the sample. The resin also demonstrated exclusive ion selectivity toward targeted metal ions by showing greater resistivity to various complexing species and more common metal ions during analyte concentration, which ultimately led to high preconcentration factors of 700 for Cu(II); 600 for Mn(II), Ni(II), and Zn(II); and 500 for Cd(II) and Pb(II), arising from a larger sample breakthrough volume. The lower limits of metal-ion detection were 7 ng/mL for Mn(II) and Ni(II); 5 ng/mL for Cu(II), Zn(II), and Cd(II), and 10 ng/mL for Pb(II). The developed resin was successful in preconcentrating metal ions from synthetic and real water samples, multivitamin-multimineral tablets, and curry leaves (Murraya koenigii) with relative standard deviations of < or = 3.0% for all analytical measurements, which demonstrated its practical utility.  相似文献   

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