Abstract: The laboratory test and the onsite sample test confirmation were carried out to study the pretreatment and detection method for primary corrosion products pretreatment and detection method in PWR nuclear power plants. The effect of the sample pre-treatment and analysis method selection were considered in the whole process. The influence of different type of the acid（nitric acid and aqua regia, respectively） used in the pr-treatment process and the standing time for acidified samples（1 h, 4 h, 24 h） on the precision, accuracy and detection limit of analysis results were discussed. The detection methods considered in this paper include the flame atomic absorption, graphite furnace atomic absorption spectrometer, inductively coupled plasma-optical emission spectrometer, inductively coupled plasma emission mass spectrometer and ion chromatography. Based on the detection limit, the applicable objects and the PWR unit instrument configuration, the inductively coupled plasma-optical emission spectrometer was selected as the detection method and the graphite furnace atomic absorption spectrometer was supported verified. The study result shows that the corrosion product acidified with the nitric acid while the volume of nitric acid added controlled at 1%, and the acidified sample was analyzed in 24 hours after the acidified process. The inductively coupled plasma-optical emission spectrometer used as the nickel analysis method was proved to be a measurement method with lower detection limit（the detection limit below 1 μg/kg）, high precision（the relative standard deviation between 6.54% and 14.07%） and high accuracy（the recovery rate between 99.2% and 104.4%）.