Accuracy of calibrated-loop transfer

The accuracy of the 0.001-ml calibrated platinum loop was tested by two methods: visible absorption spectroscopy and weight determinations. By both methods it was demonstrated that the volume of the loop delivery is related to the angle at which the loop is withdrawn from the solution being sampled and the diameter of the container, provided that the volume in the container is adequate to cover the loop. Vertical sampling from small-diameter containers (less than or equal to 7-mm inside diameter) delivered approximately 50% of 0.001 ml, and sampling at a 45 degree angle from larger containers (greater than or equal to 22-mm inside diameter) gave a delivery volume of greater than 150% of 0.001 ml, resulting in a threefold difference in the amount delivered and an error rate of +/- 50%.