Rapid direct determination of lead in evaporated milk by anodic stripping voltammetry without sample pretreatment.

The method presented describes the direct determination of lead in evaporated milk in which the milk ashing step prior to analysis is eliminated. Digital instrument readout units are microgram Pb/mL milk. Total analysis time after instrument calibration is less than 3 min per sample. Range of the method is 0.05-1.0 ppm lead in milk, and precision of the method expressed by relative standard deviation of duplicate pairs ranged from 30% at 0.1 micrograms/mL to 3% at 1.0 micrograms/mL of lead in milk. The method compares favorably with the AOAC official first action anodic stripping voltammetric method (25.074). In addition, the method appears to work equally well for skim evaporated milk, sweetened condensed milk, and nonfat powdered dry milk when the latter two are reconstituted with water according to product label instructions. Recovery and interference studies are presented.

Direct determination of lead in evaporated milk and apple juice by anodic stripping voltammetry: collaborative study.

A method for the direct determination of lead in evaporated milk and in fruit juice with no prior sample digestion was successfully collaborated by 13 laboratories. The anodic stripping voltammetric (ASV) method studied consisted of adding 0.2 mL aliquots of evaporated milk or 0.3 mL aliquots of fruit juice to 2.9 mL of a dechelating reagent, Metexchange. The reagent-sample mixture is then analyzed for lead by ASV with no further sample preparation. Each collaborator received 24 samples, 2 each at 5 different levels (0.07-0.70 ppm for spiked evaporated milk and 0.09-0.87 ppm for spiked apple juice) along with duplicate practice samples of labeled lead content at each of 2 levels for each sample type. All unknowns were coded with random numbers. Approximately 69% of the reporting laboratories had never analyzed either evaporated milk or fruit juice for lead. Average time between receipt of samples and reporting of results was 1.6 days for all laboratories. The pooled variations between duplicate determinations for apple juice and evaporated milk were 0.00059 and 0.00043, respectively. The method was adopted official first action for both fruit juice and evaporated milk.

Leak in evaporated milk by anodic stripping voltammetry and atomic absorption spectrophotometry: cooperative interlaboratory study.

The results of a cooperative study on the determination of lead in evaporated milk, using a double blind referee technique, are reported. This study was designed to determine the normal variability of methods currently used for lead analysis by canned food industry laboratories. Twenty-three laboratories participated in this study. Each laboratory was instructed to use atomic absorption spectrophotometry (AOAC 25.065), anodic stripping voltammetry, or carbon rod atomic absorption spectrophotometry. Overall, the results appear to be in close agreement with the spiking levels. The coefficient of variation for all laboratories was 36.0% at the 0.15 ppm lead level and 16.8% at the 0.40 ppm lead level.

Analysis of total arsenic in urine and blood by high speed anodic stripping voltammetry.

A method for the measurement of parts per billion levels of total arsenic in urine and blood is described. Samples are wet ashed with a mixture of HNO3, HCIO4, and H2SO4 acids. Ashed materials are subjected to a reductillationTM procedure to reduce As (V) to As (III) and to separate arsenic from the sample matrix. Collected arsenic is then quantitated by anodic stripping voltammetry (ASV) at a gold film electrode. ASV analysis time is only 2 minutes. By simultaneous reductillation of 4 samples, ppb arsenic determinations can be accomplished at a rate of about 12 per hour. The method is as accurate, precise and reliable at the nanogram level as the more universally accepted colorimetric techniques are at the microgram and milligram levels. For replicate analysis of real samples, method precision ranged from +/- 1.4 ppb at the 5 ppb level to +/- 0.96 ppb at the 25 ppb level. Accuracy is estimated at +/- 6% over the range 5 to 500 ppb arsenic.

Direct analysis of lead in fruit juice by anodic stripping voltammetry with no prior sample preparation.

A method is presented for determining lead in fruit juice in less than 3 min after instrument calibration. The range examined is 0.01 to 1.3 ppm lead. The method is compared with 3 other methods in general use. Standard error of estimates between the methods compared range from 0.023 to 0.051 ppm for a set of 50 samples and from 0.037 to 0.091 ppm for a set of 9 samples. Regression correlation coefficients between methods range from 0.968 to 0.995. Judged by the comparisons, the direct method is precise and accurate over greater than a 100-fold range of lead concentrations.