Page:NIOSH Manual of Analytical Methods - 6017.pdf/4

 HYD RO GE N C YAN IDE: ME TH OD 6017, Issue 1, dated 1 5 Ma rch 2003 - Page 4 of 5

EVALUATION OF METHOD: Only the analytical procedure was evaluated for this method. The sampler, the soda lime tube, was evaluated for NIOS H m ethod 6010 by sam pling the test atmosph eres of H CN generated from a com pressed m ixture of HCN in nitrogen [1]. The range of HC N conc entra tion wa s eq uivalen t to 2 to 15 m g/m 3 for a 3-L air sample. Twenty-two samples collected at 0.2 L/min for 15 minutes indicated overall precision Ö rT of 0 .07 6 with nearly 100% recovery. Breakthrough occurred after 40 minutes of sampling at a flow rate of 0.2 L/min at an HCN concentration of 148 m g/m 3. Sample tubes spiked with solutions of KCN and analyzed after storage indicated that the samples of cyanide ions were stable on the tube for at leas t 2 week s. Analysis of 22 tubes which were spiked with KCN standard solutions in the range 10 to 50 µg indicated a recovery of nearly 100% with a pooled precision of 0.041. Desorption efficiency may be poor, below 10 µg CN ! [6]. This ion ch rom atog raph ic (IC) proc edu re for the determination CN- was developed by W isconsin Occupational He alth Labortory (W OH L) in 1997 [2]. Desorption, quantifiable limit, and linear range were investigated and found com para ble to m ethod 6010. W OH L also dem onstated that recovery below 10 :g was questionable.

REFERENCES: [1] W illiamson, George [1988]. Method Development Protocol and Backup Data Report on Hydrogen Cyan ide; Internal N IOS H/M RS B R epo rt. NIO SH (Un pub lished ). [2] Dobson L, Popp D, Reichmann L [1997]. Development of an Automated, Pyridine-Free Method for Aeroso l Cyanide Com pounds and Hydroge n Cyanide. Unpu blished paper. [3] NIOSH [1994]. Cyanides, aerosol and gas: Method 7904. In: Eller PM, Cassinelli ME, eds. NIOSH Ma nua l of Analytical Metho ds, 4 th ed. Cincinnati, OH: U.S. Department of Health and Human Services, Public Health Service, Centers for Disease Control and prevention, National Institute for Occupational Safety and Health, DHHS (NIOSH) Publication No. 94-113. [4] NIOSH [1994], Hydrogen Cyanide: Method 6010. In: Eller PM, Cassinelli ME, eds. NIOSH M anual of Analytical Metho ds, 4 th ed. Cincinnati, O H: U.S. De partm ent of He alth and H um an Servic es, Pu blic He alth Service, Cente rs for Diseas e Contro l and P reve ntion, N ationa l Institute fo r Occu pation al Safety and Health, DHHS (NIOSH) Publication No. 94-113. [5] DataC hem Laboratories [1990]. NIOS H Se quenc e #6837 -K, Unpub l. (Marc h 21, 1990). [6] W illiamson, George [1988]. Analysis of Air Samples on Project 166 (Firesmoke) on HCN; Sequence NIOS H/MR SB-636 6A. NIO SH.(U npublished). [7] NIOSH [1988]. NIOSH/OSHA Occupational Health Guidelines for Chemical Hazards [1981]. U.S. Department of Health and Human Services, Public Health Service, Centers for Disease Control and Prevention, National Institute for Occupational Safety and Health, DHHS (NIOSH) Publication No. 88119. [8] DataC hem Laboratories [1990]. User C heck, NIOSH Seque nce #68 37-J, (Marc h 19,Unp ublished ).

METHOD WRITTEN BY: LeR oy Do bso n, W isconsin Oc cup ationa l Hea lth Lab orato ry, Madison, W I.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition