Page:NIOSH Manual of Analytical Methods - 8308.pdf/2

 FLUORIDE in urine: METHOD 8308, Issue 2, dated 15 August 1994 - Page 2 of 4 REAGENTS: 1. 2. 3. 4. 5. 6. 7. 8.

9.

EQUIPMENT:

Distilled or deionized water. Sodium citrate (Na 3C6H3O 7·2H 2O). Ethylene dinitrilotetracetic acid (EDTA), disodium salt. Acetic acid, glacial. Sodium chloride. Sodium hydroxide, 5 M. Dissolve 20 g NaOH in distilled water; dilute to 100 mL. Sodium fluoride. Calibration stock solution, 100 µg F /mL. Dissolve 0.2211 g dry sodium fluoride in distilled water. Make 1000 mL solution. Total ionic strength activity buffer (TISAB), pH 5. Add 57 mL glacial acetic acid, 58 g sodium chloride, and 0.30 g sodium citrate to a 1-L beaker containing 500 mL distilled water. Stir to dissolve. Place beaker in waterbath for cooling. Slowly add 5 M sodium hydroxide until the pH is between 5.0 and 5.5. Cool to room temperature; dilute to 1 L with distilled water.

1. Polyethylene bottles, 125-mL, wide-mouth. 2. Fluoride ion specific electrode (ISE), with reference electrode. 3. pH/millivolt meter, reading to ± 0.5 mV. 4. Stirrer, magnetic. 5. Stirring bars, PTFE-coated. 6. Beakers, plastic, 50-mL. 7. pH electrode. 8. Pipets, appropriate sizes for standards. 9. Volumetric flasks for standards. 10. Waterbath.

SPECIAL PRECAUTIONS: Samples of urine collected from humans pose a real health risk to laboratory workers who collect and handle these samples. These risks are primarily due to personal contact with infective biological samples and can have serious health consequences, such as infectious hepatitis, and other diseases. There is also some risk from the chemical content of these samples, but this is much less. Those who handle urine specimens should wear protective gloves, and avoid aerosolization of the samples. Mouth pipetting, of course, must be avoided.

SAMPLING: 1. 2.

Collect pre- and post-shift spot urine samples in polyethylene bottles containing 0.2 g EDTA. Ship samples in insulated container at about 4 °C using bagged refrigerant.

SAMPLE PREPARATION: 3.

Perform a creatinine determination on an aliquot of the urine (e.g., [5]).

CALIBRATION AND QUALITY CONTROL: 4. 5.

6. 7.

Prepare at least five working standards in the range 0.1 to 100 µg F /mL by appropriate dilutions of the calibration stock solution with distilled water. Analyze a set of working standards together with the samples and blanks (steps 9 through 12) starting with the lowest concentration. NOTE: Working standards, samples, and blanks must be analyzed under the same conditions, including temperature, for accurate results. Prepare a calibration graph on three-cycle semi-log paper plotting millivolts on the linear scale and fluoride concentration, µg/mL, on the log scale. Maintain standardization by running a standard with every 10 specimens. NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94