The complete decomposition of complex matrices containing molybdenum b
y potassium pyrosulphate and its subsequent spectrophotometric determi
nation using toluene 3,4-dithiol and thiocyanate was investigated. Res
ults given by intermethod comparison and linear regression analyses sh
ow that a very good positive correlation exists between the two method
s. The analytical results obtained from various international geochemi
cal certified samples (jasperiod, copper mill head, soil, manganese no
dule, shale, tropical soil molybdenum and tungsten ore) agreed well wi
th analytical values available in the literature. The procedure is ver
y simple, inexpensive, less labour-intensive and easily adaptable and
separation of molybdenum from tungsten is straight forward, hence stro
ngly recommended for a quality control programme and in the evaluation
of reference materials.