GOLD BELONGS TO THE GROUP OF ELEMENTS WHICH OCCUR ON THE EARTH IN VERY LOW NATURAL CONTENTS. THE CONCENTRATION OF GOLD IN NATURAL WATER IS EXTREMELY LOW [1], IN THE RANGE FROM 0.01 TO 10 NG L-1. IT IS WELL KNOWN THAT GOLD IS ONE OF THE MOST INTERESTING MICRO AMOUNT ELEMENTS DUE TO ITS SIGNIFICANT ROLE ON BIOLOGY, ENVIRONMENT AND INDUSTRY. IT COULD BE ALSO VERY TOXIC FOR HUMAN AND ANIMAL ORGANISM AND PLANTS AND ACCOUNT AS THE POLLUTANTBECAUSE OF ITS INHIBITING EFFECT UPON THE ACTIVITY OF MANY ENZYMES AND ITS PREVENTING EFFECT UPON THE DNA SEPARATION. [1].NUMEROUS METHODS FOR GOLD DETERMINATION ARE KNOWN: UV-VIS SPECTROPHOTOMETRY, ELECTROTHERMAL ATOMIC ABSORPTION SPECTROMETRY, INDUCTIVELY COUPLED PLASMA COMBINED WITH OPTICAL EMISSION SPECTROMETRY OR MASS SPECTROMETRY WAS APPLIED FOR A VARIETY OF SAMPLES IN THE ANALYSIS OF GOLD. FLAME ATOMIC ABSORPTION SPECTROMETRY (FAAS) IS ONE OF THE MOST WIDESPREAD TRADITIONAL ANALYTICAL TECHNIQUES FOR THE DETERMINATION OF TRACE ELEMENTS, BUT IT OFTEN SUFFERS FROM ITS LOW SENSITIVITY. THE DETERMINATION OF TRACE QUANTITY OF HEAVY METALS IN ENVIRONMENTAL SAMPLES LIKE NATURAL WATER AND OTHER REAL SAMPLES OF ENVIRONMENTAL INTEREST IN WHICH THEY ARE FOUND AT VERY LOW CONCENTRATIONS, REQUIRES THE USE OF PRECONCENTRATION METHODS COUPLED TO SPECTROSCOPIC METHODS, SUCH AS FAAS. TO OVERCOME THESE LIMITATIONS ON THE DETERMINATION OF GOLD BY FAAS, SEPARATION-ENRICHMENT IS NECESSARY. IN THE PRESENT WORK, WE REPORT AN IN SITU SOLID PHASE FORMATION EXTRACTION (ISSPFE). ISSPFE IS A NEW EXTRACTION METHOD THAT IS BASED ON USE OF SURFACTANTS [2]. IN THIS METHOD A CATIONIC SURFACTANT WITH A PROPER ALKYL GROUP CHAIN IS DISSOLVED IN THE AQUEOUS SAMPLE AND THEN A PROPERION-PAIRING AGENT IS ADDED. DUE TO INTERACTION BETWEEN SURFACTANT AND ION-PAIRING AGENT, VERY FINE SOLID PARTICLESARE FORMED. IN THIS RESEARCH, AU (III) IONS WERE COMPLEXED WITH 2-NITROSO-1-NAPHTHOLAND EXTRACTED WITH FINE SOLID PARTICLES THAT WERE FORMED INTO THE SOLUTION. AFTER EXTRACTION, THE CONCENTRATION OF GOLD WAS DETERMINED BY FLAME ATOMIC ABSORPTION SPECTROMETER. SEVERAL VARIABLES THAT AFFECT THE EXTRACTION EFFICIENCIES, INCLUDING PH, CONCENTRATION OF CHELATING AGENT, TYPE AND CONCENTRATION OF SURFACTANT, KCLO4 CONCENTRATION, EXTRACTION TIME AND SALT ADDITION, WERE INVESTIGATED AND OPTIMIZED. UNDER THE BEST EXPERIMENTAL CONDITIONS, THE CALIBRATION CURVE EXHIBITED LINEARITY OVER THE RANGE OF 5.0-800.0 NG ML-1 WITH A CORRELATION COEFFICIENT OF 0.998 AND DETECTION LIMIT BASED ON THREE TIMES THE STANDARD DEVIATION OF THE BLANK SIGNAL WAS 1.5 NG ML-1. EIGHT REPLICATE DETERMINATION OF 200.0 NG ML-1 GOLD GAVE A RSD OF ±2.1%. FINALLY, THE PROPOSED METHOD HAS BEEN SUCCESSFULLY APPLIED FOR THE DETERMINATION OF GOLD IN THE REAL WATER SAMPLES.