Contamination during lead analysis

S prevention of contamination during sampling and analysis has been inadequate leading... 

Having received the pre-weighed test item, preparation for its use in the field must be made. Ideally, water to be used in the dilution of the test item should be from mains water or a recognized source. The use of water from standing pools, rivers, etc., could potentially lead to problems with interference from contaminants during analysis of the crop samples. Depending on the formulation under test, the test item can be mixed in a variety of ways. First, the required water volume must be accurately measured. Approximately half of this amount can be poured into a clean bucket or similar mixing container. The temperature of the water should be noted at this point... 

Studies of the types described above must be re-evaluated to include control organisms which have body burdens of lead at natural levels (100-2000 times lower than present levels), which breathe air at natural levels, and which consume food and water containing lead at natural levels. Furthermore, since these studies would involve lead measurements at subnanogram levels, it is essential that they be carried out under ultra-clean conditions using the best clean-lab technology to avoid artifact contamination during sample handling and analysis. 

All of these techniques require an ultra-high vacuum chamber (10 to 10 Pa) to avoid contamination of the surface by undesired adsorption processes during the analysis. Vacuum conditions also limit the probability of accidental collisions between the emitted particles and gas molecules, which would lead to energy losses of the particles. 

Scarponi et al. [93] concluded that filtration of seawater through uncleaned membrane filters shows positive contamination by cadmium, lead, and copper. In the first filtrate fractions, the trace metal concentration maybe increased by a factor of two or three. During filtration, the soluble impurities are leached from the filter, which is progressively cleaned, and the metal concentration in the filtrate, after passage of 0.8 -11 of seawater, reaches a stable minimum value. Thus it is recommended that at least one litre of seawater at natural pH be passed through uncleaned filters before aliquots for analysis are taken... 

In solution, vitamin D (both D2 and D3) isomerizes to previtamin D and forms a temperature-dependent equilibrium mixture [520], which leads to quantification problems. Previtamin D is difficult to quantify because of interference from co-eluted contaminants. The reversibility of the isomerization is very slow, therefore the percentage of previtamin can be considered constant during the entire analysis. The quantification of the potential vitamin D can be performed using an external standard that has undergone saponification procedure as the sample [521]. Vitamin D2 and D3 can be used as an internal standard to quantify the other one. Indeed, the isomerization rates of vitamins D2 and D3 are virtually the same thereby the previtamin D/vitamin D ratio will be the same for both vitamers at any temperature. The isomerization problem can be resolved by... 

Usually, samples are presented for analysis as liquids. Thus, solid samples must be dissolved. Analytical or ultra-high-purity grade reagents must be used for dissolution to prevent contamination at trace levels. Certain volatile metals (e.g. cadmium, lead and zinc) may be lost when dry ashing, and volatile chlorides (e.g. arsenic and chromium) lost upon wet digestion. It is particularly easy to lose mercury during sample preparation. Appropriate steps must be taken in the choice of method of dissolution, acids and conditions (e.g. whether to use reflux conditions) to prevent such losses. 

A study of mercury in Lake Michigan found levels near 1.6 pM (1.6 X 10 12 M), which is two orders of magnitude below concentrations observed in many earlier studies.5 Previous investigators apparently unknowingly contaminated their samples. A study of handling techniques for the analysis of lead in rivers investigated variations in sample collection, sample containers, protection during transportation from the field to the lab, filtration techniques, chemical preservatives, and preconcentration procedures.6 Each individual step that deviated from best practice doubled the apparent concentration of lead in stream water. Clean rooms with filtered air supplies are essential in trace analysis. Even with the best precautions, the precision of trace analysis becomes poorer as the concentration of analyte decreases (Box 5-2). 

---