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ELEMENTS by ICP 7301 (Aqua Regia Ashing)

ELEMENTS by ICP 7301 . ( aqua Regia ashing ). MW: Table 1 CAS: Table 2 RTECS: Table 2. METHOD: 7301 , Issue 1 EVALUATION: PARTIAL Issue 1: 15 March 2003. OSHA : Table 2 PROPERTIES: Table 1. NIOSH: Table 2. ACGIH: Table 2. ELEMENTS : aluminum* calcium lead* phosphorus thallium zinc antimony* chromium* lithium potassium tin zirconium*. arsenic cobalt magnesium selenium titanium barium copper manganese silver tungsten*. beryllium iron* molybdenum strontium vanadium cadmium lanthanum nickel tellurium yttrium * Some compounds of those ELEMENTS require special sample treatment. SAMPLING MEASUREMENT. SAMPLER: FILTER TECHNIQUE: INDUCTIVELY COUPLED ARGON. ( m, cellulose ester membrane, or PLASMA, ATOMIC EMISSION. m, polyvinyl chloride membrane) SPECTROSCOPY (ICP-AES).

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition ELEMENTS by ICP 7301 (Aqua Regia Ashing) MW: Table 1 CAS: Table 2 RTECS: Table 2 METHOD: 7301, Issue 1 EVALUATION: PARTIAL Issue 1: 15 March 2003

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Transcription of ELEMENTS by ICP 7301 (Aqua Regia Ashing)

1 ELEMENTS by ICP 7301 . ( aqua Regia ashing ). MW: Table 1 CAS: Table 2 RTECS: Table 2. METHOD: 7301 , Issue 1 EVALUATION: PARTIAL Issue 1: 15 March 2003. OSHA : Table 2 PROPERTIES: Table 1. NIOSH: Table 2. ACGIH: Table 2. ELEMENTS : aluminum* calcium lead* phosphorus thallium zinc antimony* chromium* lithium potassium tin zirconium*. arsenic cobalt magnesium selenium titanium barium copper manganese silver tungsten*. beryllium iron* molybdenum strontium vanadium cadmium lanthanum nickel tellurium yttrium * Some compounds of those ELEMENTS require special sample treatment. SAMPLING MEASUREMENT. SAMPLER: FILTER TECHNIQUE: INDUCTIVELY COUPLED ARGON. ( m, cellulose ester membrane, or PLASMA, ATOMIC EMISSION. m, polyvinyl chloride membrane) SPECTROSCOPY (ICP-AES).

2 FLOW RATE: 1 to 4 L/min ANALYTE: ELEMENTS above VOL-MIN: Table 1 ashing . -MAX: Table 1 REAGENTS: aqua Regia (1 HNO3 : 3 HCl). SHIPMENT: Routine CONDITIONS: Room temperature, 30 min; 150 C to near dryness SAMPLE. STABILITY: Stable FINAL. SOLUTION: 5% aqua Regia , 25 mL. BLANKS: 2 to 10 field blanks per set WAVELENGTH: Depends upon element, Table 3. ACCURACY BACKGROUND. CORRECTION: Spectral wavelength shift RANGE STUDIED: Not determined CALIBRATION: ELEMENTS in 5% aqua Regia BIAS: Not determined RANGE: Varies with element [1]. OVERALL PRECISION ( r T ): Not determined ESTIMATED LOD: Tables 3 and 4. ACCURACY: Not determined PRECISION ( r ): Tables 3 and 4. APPLICABILITY: The working range of this method is to mg/m3 for each element in a 500-L air sample.

3 This is simultaneous elemental analysis, not compound specific. Verify that the types of compounds in the samples are soluble with the ashing procedure selected. This method does not digest PVC filters completely. INTERFERENCES: Spectral interferences are the primary interferences encountered in ICP-AES analysis. These are minimized by judicious wavelength selection, interelement correction factors and background correction [1-4]. OTHER METHODS: Flame atomic absorption spectroscopy ( , Methods 70XX) is an alternate analytical technique for many of these ELEMENTS . Graphite furnace AAS ( , 7102 for Be, 7105 for Pb) is more sensitive. NIOSH Methods 7300 &. 7302 are alternative digestion procedures. NIOSH Manual of Analytical Methods (NMAM), Fourth Edition ELEM ENT S by ICP (Aqu a Reg ia ashing ): MET HO D 730 1, Issue 1, dated 15 M arch 200 3 - Page 2 o f 8.

4 REAGENTS: EQUIPMENT: 1. Nitric acid (HNO 3), conc.*, ultra pure. 1. Sam pler: cellulose ester m em brane filter, 2. Hydrochloric acid (HCl), conc.*, ultra pure. m pore size; or polyvinyl chloride (PVC). 3. ashing acid ( aqua Regia ): 1:3 (v/v) HNO 3:HC l. m em brane, m pore size; 37-m m Mix 1 volume conc. HNO 3 with 3 volumes diam eter, in cassette filter holder. conc. HCl. 2. Personal sa m pling pum p, 1 to 4 L/m in, with 4. Ca libration s tock solutions, 1000 g/m L. flexible connecting tubing. Com mercially available, or prepared per 3. Inductively coupled plasma-atomic emission instrument manufacturer's recomm endation spectrometer, equipped as specified by the (see step 12 ). manufacturer for analysis of ELEMENTS of 5. Dilution acid, 1% HNO 3, 3% HCl.

5 Add 50 mL interest. ashing acid to 600 mL water; dilute to 1 L. 4. Regulator, two-stage, for argon. 6. Argon. 5. Beakers, Phillips, 125-mL, or Griffin, 50-mL, 7. Distilled,deionized water. with watch glass c overs .**. 6. Volum etric flasks , 10-, 25-,10 0-m L., and 1-L **. 7. Ass orted vo lum etric pipets as need ed.**. * See SPECIAL PRECAUTIONS. 8. Hotplate, surface temperature 150 C. ** Clean all glasswa re with conc. nitric acid and rinse thoroughly in distilled water before use. SPECIAL PRECAUTIONS: Conce ntrate d ac ids are po werful oxidizers, toxic, an d co rrosive liquids . W ear protective clothing and work in a fume hood. SAMPLING: 1. Calibrate each personal sampling pump with a representative sampler in line. 2. Sam ple at a n ac curately kn own flow ra te betwee n 1 and 4 L/m in for a total sam ple size of 200 to 2000 L.

6 (see Table 1) for TW A measurem ents. Do not exceed a filter loading of approximately 2 mg total dust. SAMPLE PREPARATION: 3. Open the cassette filter holders and transfer the samples and blanks to clean beakers. 4. Add 5 mL ashing acid. Cover with a watchglass. Let stand 30 min at room tem perature. NOTE: Start a reagent blank at this step. 5. Heat on hotplate (120 C) until ca. mL remains. NOT E 1: Reco very of lead from some paint matrices may require other digestion tech niqu es. See Method 7082 (Lead by Flame AA S) for an alternative hotplate digestion procedure or Method 730 2 for a m icrow ave diges tion pro ced ure. NOTE 2: So m e species of Al, Be , Co, C r, Li, Mo, S b, W , and Z r will not be com pletely solubilized by this procedure.

7 Alternative solubilization techniques for m ost of these ELEMENTS can be found elsewhe re [5-1 0]. 6. Add 2 m L ashing acid and repeat step 5. Rep eat this step until the solution is clear. NOT E: PVC filters will not completely dissolve after repeated additions of ashing acid. 7. Rem ove watchg lass and rinse into the beake r with distilled water. 8. Increase the tem perature to 150 C and take the s am ple to near dryness (ca. m L). 9. Dissolve the residue in 2 to 3 mL dilution acid. 10. Transfer the solutions quantitatively to 25-mL volumetric flasks. 11. Dilute to volume with dilution acid. NIOSH Manual of Analytical Methods (NMAM), Fourth Edition ELEM ENT S by ICP (Aqu a Reg ia ashing ): MET HO D 730 1, Issue 1, dated 15 M arch 200 3 - Page 3 o f 8.

8 CALIBRATION AND QUALITY CONTRO L: 12. Calibrate the spectrometer according to the manufacturer's recomm endations. NOTE: Typically, an acid blank and g/m L multielement working standards are used. The following multielement combinations are chemically compatible in 5% aqua Regia : a. Al, As, Ba, Be, Ca, Cd, Co, Cr, Cu, Fe, La, In, Na b. Ag, K, Li, Mg, Mn, Ni, P, Pb, Se, Sr, Tl, V, Y, Zn, Sc c. Mo, Sb, Sn, Te, Ti, W , Zr d. Acid blank 13. Analyze a standard for every ten samples. 14. Check recoveries with at least two spiked media blanks per ten samples. MEASUREMENT: 15. Set spec trome ter to conditions spe cified by manufac turer. 16. Analyze standards, samples, and blanks. NOTE: If the va lues for the sam ples are a bove the rang e of th e standa rds, dilute the solutions w ith dilution acid, reanalyze a nd apply the appropriate dilution fac tor in the calcula tions.

9 If more sensitivity is required, the final sample volume may be held to mL. CALCULATIONS: 17. Obtain the solution concentrations for the sample, C s ( g/m L), an d the average m edia blank , C b ( g/m L), from the ins trum ent. 18. Using the solution volum es o f sam ple, V s (m L), and m edia blank , V b (mL), calculate the concentration, C (m g/m 3), of each elem ent in the air volum e sam pled, V (L): NOT E: g/L / m g/m 3. EVALUATION OF METHOD: The precision and recovery data were determined at approximately 3x and 10x the instrumental detection limits on com m ercially prepared s pike d filters [12] using 25 .0 m L as the final sample volume. The precision and recovery data, instrumental detection lim its, and ana lytical wave lengths are listed in Ta bles 3 and 4.

10 In general, better recoveries were obtained from MCE filters than from PVC filters. The values in Tables 3 and 4 were determined with a Spectro Analytical Instruments model EOP opera ted according to m anufa cturer's instructions. REFERENCES: [1] Millson M, Andrews R [2002]. Backup data report, Method 7301 , unpublished report, NIOSH/DART. [2] Hull RD [1981]. Multielement Analysis of Industrial Hygiene Sam ples, NIO SH Internal Re port, presented at the American Industrial Hygiene Conference, Portland, Oregon. [3] NIOSH [1982]. NIOSH Manual of Analytical Methods, 2nd ed., V. 7, P&CAM 351 ( ELEMENTS by ICP), Department of Health and Human Services, Publ. (NIOSH) 82-100. [4] NIOSH [1994]. Elem ents by ICP : Method 7300. In: Eller PM, Cassinelli ME, eds.


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