Radiocarbon dating of early Pre-Pottery Neolithic B (PPNB) deposits at the site of Motza, Israel, was achieved by first prescreening many charcoal and bone samples in order to identify those that are in the most suitable state of preservation for dating. For assessing bone preservation, we determined the collagen contents, and by infrared spectroscopy the collagen purity. The collagen samples of the best preserved bones were then further characterized by their C/N ratios and amino acid compositions. Prescreening of the charcoal samples involved monitoring the changes in infrared and Raman spectra during the acid-alkali-acid treatments. In some samples, we noted that the clay content increased with additional alkali treatments. These samples were rejected, as this could result in erroneous dates. No differences were observed in the 14C dates between charcoal and bone collagen samples. The dates range from 10,600–10,100 cal BP, which is consistent with dates for the early PPNB from other sites. This is of much interest in terms of better understanding where and when domestication of animals began in this period, and how agriculture spread throughout the Levant.