Author John Entwisle LGC Queens Road Teddington Middlesex TW11 0LY, UK
Abstract
The quantitative determination of mercury in foodstuffs is presented using a 7500i ICP-MS. Microwave digests were prepared and then analyzed by ICP-MS. To avoid memory effects often experienced with mercury, gold was added offline to all standards/samples and wash solutions to act as a cleansing agent. The instrumental setup used a second vacuum pump, the integrated sample introduction system in the high sample throughput mode, and a micro- flow concentric nebulizer. This allowed the robust and rapid determination of mercury in the digests at the ppt range. Excellent agreement with the certified value was obtained for two certified reference materials and stabil- ity of the system was demonstrated over a 36-hour analytical run.
Introduction
The determination of sub-ppb concentrations of mercury has always been of special importance in the field of trace metal analysis. Even at trace levels, mercury is toxic and causes neurological damage, particularly in fetuses and young children. Anthropogenic sources of mercury in the environ-
Determination of Mercury in Microwave Digests of Foodstuffs by ICP-MS Application
ment include coal-fired power stations and chlor-alkali works. In the aquatic environment, bacteria convert elemental mercury Hg(0) to methylmercury which is accumulated and passed up the food chain. It has been reported that some whale meat contains 5000 times the Japanese legal limit of 0.4 µg/g. In addition, fish and shellfish are significant contributors to the human diet. Today mercury pollution is a global problem and exten- sive monitoring of foodstuffs is required. Therefore fast efficient and robust methods are needed. Mer- cury however is recognized as a problem element. It is known to adsorb onto the walls of storage con- tainers and volatilize as mercury vapor. Addition- ally, its high first ionization potential and numerous isotopes have limited its sensitivity in ICP-MS analysis. ICP-MS allows the rapid determi- nation of ultratrace levels of metals in food digests, however, extensive washout times have been required to reduce carryover for mercury analysis. Other workers have tried the addition of a number of chemical agents in the past. One of the most effective washout agents is gold chloride. To avoid memory effects and ensure stability, gold chloride (at the 5-ppm level) was added offline to all samples/standards and wash solutions. Extensive washout times were reduced by using by the inte- grated sample introduction system (ISIS). With the use of the high throughput pump, a large flush volume can be pumped through in a much shorter time. By summing the responses for multiple iso- topes (199, 200, 201, and 202) and with the help of a second interface vacuum pump and a micro-flow concentric nebulizer, detection levels of between 10 and 30 ppt were routinely achieved for the digests.