Page:NIOSH Manual of Analytical Methods - 8310.pdf/5

 METALS in urine: METHOD 8310, Issue 2, dated 15 August 1994 - Page 5 of 5 TABLE 2. RECOVERY OF METALS FROM URINE [1,2]

Wavelength (nm)

Quantity Added, µg/50 mL sample

Precision, Sr (n = 4)

Precision, % Recovery

Accuracy ±%

Aluminum (Al)

308.2

20

0.088

100

17.2

Barium (Ba)

455.4

0.4

0.11

80

41.6 a

Cadmium (Cd)

226.5

1.0

0.12

100

23.5

Chromium (Cr)

205.6

1.0

0.078

100

15.3

Copper (Cu)

324.8

10

0.042

100

8.2

Iron (Fe)

259.9

40

0.059

100

11.6

Lead (Pb)

220.4

10

0.040

100

7.8

Manganese (Mn)

257.6

10

0.50

85

113 a

Molybdenum (Mo)

281.6

2.0

0.16

100

31.4 a

Nickel (Ni)

231.6

2.0

0.42

80

102 a

Platinum (Pt)

203.7

0.4

0.29

77

79.8 a

Silver (Ag)

328.3

2.0

0.12

100

23.5

Strontium (Sr)

421.5

4.0

0.25

100

49.0 a

Tin (Sn)

190.0

2.0

0.21

100

41.2 a

Titanium (Ti)

334.9

2.0

0.16

86

45.4 a

Zinc (Zn)

213.9

200

0.089

100

17.4

Element (Formula)

a

Does not meet the NIOSH criterion of ± 25% accuracy.

APPENDIX: POLYDITHIOCARBAMATE RESIN PREPARATION The procedure used for preparation of the polydithiocarbamate resin is that of Hackett and Siggia [5] as modified by Bary and Reilly [6]. 1. Dissolve 72 g polyethyleneimine, molecular weight 1800, in 1 L tetrahydrofuran and 28 g polymethylenepolyphenyl isocyanate in 1 L tetrahydrofuran. NOTE: Polyethyleneimine stored for one year would not dissolve in the solvent; however, fresh polyethyleneimine readily dissolved. 2. Pour these two solutions simultaneously into a large flask, allowing the two streams to mix before entering the flask. 3. Let the mixture stand at least 12 h with occasional mild agitation, then remove the solvent by filtration. 4. Wash the product twice with methanol and once with deionized water. 5. Add the product to 300 mL carbon disulfide, 100 mL ammonium hydroxide and 500 mL isopropyl alcohol; let stand 72 h. 6. Filter to remove the resin from the solvent mixture. Wash the resin three times with methanol and allow it to dry. 7. Grind and sieve the resin, saving the 60/80 mesh size for use.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94