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A new method of hydride generation was used for the determination of lead at ng mL−1 levels by atomic absorption spectrometry (AAS). Lead hydride was generated at 65 °C using solid sodium borohydride and solid tartaric acid. The limit of detection was 4.5 ng mL−1 Pb. The calibration curve was linear from 50 to 1000 ng mL−1. The relative standard deviations of 10 replicate determinations of 500 ng mL−1 and 200 ng mL−1 Pb2+ were 2.05 and 4.00%, respectively. The effect of some transition metals on the determination of lead was also investigated. The reliability of the method was evaluated by determining the lead contents of different soil, earthenware, and synthetic samples. niques such as ultrasonication and microwave irradiation.