Layered double hydroxides (LDHs) are a class of materials that may be readily synthesized in a laboratory environment. This work successfully conducted the synthesis of a new nanomaterial (ZnMnAl LDH). The characterization of this material was accomplished utilizing many analytical techniques, including FTIR, XRD, SEM-mapping, and FE-SEM. ZnMnAl LDH was employed to separate and enrich Cu(II) and Ni(II) from soil and water samples. The Cu and Ni ions were eluted from ZnMnAl LDH nanoparticles by using 2 mL of 0.1 mol L?1 of HNO3. The metal ions were quantified using flame atomic absorption spectrometry (FAAS). An investigation was conducted to examine the impact of many analytical factors on the efficiency of metal ions' extraction. These parameters include pH, sorbent amount, eluent volume, eluent concentration, sample volume, and possible interfering ions. The detection limits for Cu(II) and Ni(II) were found to be 0.74 and 0.52 μg kg?1, respectively. In addition, the relative standard deviation (RSD%) for Cu(II) is 3.8 and for Ni(II) is 1.9. The linear range for both analytes is 50–1000 μg L?1, and the preconcentration factor is 15 for both. The method’s validation was verified by the analysis of certified reference materials, namely BCR-505 estuarine water and GBW07429 (GSS-15) soil. For soil samples, Ni(II) and Cu(II) concentrations vary from 9.8 to 62.8 mg kg-1 and 9.9 to 73.5 mg kg-1, respectively. The technique described was used to quantify minute concentrations of copper (Cu) and nickel (Ni) in samples of both natural water and soil.