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1、9.2.40 AOAC Official Method 993.14 Trace Elements in Waters and Wastewaters Inductively Coupled PlasmaMass Spectrometric Method First Action 1993 (Applicabletodeterminationof20traceelements,atconcentrations of 0.8200 g/L, in finished drinking water, groundwater, and wastewaters.) Caution:The followi
2、ng reagents are highly toxic: antimony, ar- senic trioxide, beryllium sulfate, cadmium, chromium trioxide, lead nitrate, selenium dioxide, thallium nitrate, and uranium nitrate. Results of interlaboratory study: See Table 993.14A for interlaboratory study data. A. Principle Method describes multiele
3、ment determination of trace elements by inductively coupled plasmamass spectrometry (ICPMS). Ele- ments are digested in a nitrichydrochloric acid solution. Sample material in solution is introduced by pneumatic nebulization into radiofrequencyplasmawhereenergytransferprocessescausedesol- vation, ato
4、mization, and ionization. Ions are extracted from plasma through differentially pumped vacuum interface and are separated onthebasisofmass-to-chargeratiobyaquadrupolemassspectrom- eter having minimum resolution capability of 1 amu peak width at 5% peak height. Ions transmitted through quadrupole are
5、 detected by continuous dynode electron multiplier assembly, and ion infor- mation is processed by data handling system. B. Apparatus (a) Inductively coupled plasmamass spectrometer.(1) Instrument capable of scanning mass range 5250 amu with mini- mumresolutioncapabilityof1amupeakwidthat5%peakheight
6、and that may be fitted with conventional or extended dynamic range de- tection system. (2) Argon gas supply (high-purity grade, 99.99%). (3) Variable-speed peristaltic pump required for solution delivery to nebulizer. (4) Mass-flow controller on nebulizer gas supply may be required.Water-cooledspray
7、chamberbeneficialinreducinginterfer- ences.Operating conditions:Becauseofdiversityininstrumentation, manufacturer-provided operating conditions should be followed. (b) Glassware.Volumetric flasks, graduated cylinders, fun- nels, centrifuge tubes, and calibrated pipets. (c) Beakers.250mLconicalPhilli
8、pswith50mmwatchglasses and 250 mL Griffin with 75 mm watch glasses. (d) Storage bottles.125 and 250 mL, narrow mouth, Teflon FEP (fluorinated ethylene propylene), with Tefzel ETFE (ethylene tetrafluorethylene) screw caps. (e) Air displacement pipetter.Digital, capable of 102500 L range and disposabl
9、e pipet tips. (f) Analytical balance.Sensitivity 0.1 mg. (g) Hotplate.Withvariabletemperature,controllableto3C. (h) Centrifuge.Steel cabinet with guard bowl, electric timer, and brake, capable of 2000 g. (i) Drying oven.Gravity convection oven with thermostatic control capable of maintaining 105 5C.
10、 C. Reagents (a) Nitric acid (HNO3) solutions.(1) HNO3.Concentrated, specific gravity 1.41. (2) HNO3solution (1 + 1).Add 500 mL HNO3to 400 mL reagent water and dilute to 1 L. (3) HNO3solution (1 + 9).Add 100 mL HNO3to 400 mL reagent water and dilute to 1 L. (4) 1% (v/v) HNO3solution. (5) 2% (v/v) HN
11、O3solution. (b) Hydrochloric acid (HCl) solutions.(1) HCl.Concen- trated,specificgravity1.41.(2)HClsolution(1+1).Add500mL HCl to 400 mL reagent water and dilute to 1 L. (c) Ammonium hydroxide (NH4OH).Concentrated, specific gravity 0.902. (d) Tartaric acid. (e) Reagent water.ASTM type I water (ASTM D
12、1193) is required. Prepare water by distillation, polishing with mixed bed of ionexchangematerial,andfiltrationthrough0.2 mmembranefilter. (f) Standard solutions.Purchase or prepare from ultra high-puritychemicalsormetals(99.9999.999%pure).Picklemet- als (where indicated), to clean surfaces and redu
13、ce mass, by adding 20% excess of metal to acid; dry, weigh, and repeat process until desired weight is achieved. Dry salts 1 h at 105C, except where noted.Usereagentwater,(e),foralldilutionsunlessotherwisespec- ified.StorestocksolutionsinTeflonbottles,B(d).Accuratelyweigh all amounts to nearest 0.1
14、mg. (1) Aluminum stock solution (1000 mg Al/mL).Pickle Al metal in 7580C (1 + 1) HCl solution, (b)(2), to 0.100 g. Dis- solvemetalin10mLHCl,(b)(1),and2mLHNO3,(a)(1),byheat- ing ca 30 min at 7580C. Continue heating until solution has evaporated to 4 mL. Cool to room temperature and add 4 mL re- agent
15、water.Evaporateto2mLbyheating.Cooltoroomtempera- ture and dilute to 100 mL. (2) Antimony stock solution (1000 mg Sb/mL).Dissolve 0.100 g Sb powder in 2 mL (1 + 1) HNO3solution, (a)(2), and 0.5 mL HCl. Heat at 7580C to dissolve, cool to room temperature, and add 20 mL reagent water and 0.15 g tartari
16、c acid, (d). Warm solution to dissolve white precipitate. Cool and dilute to 100 mL. (3) Arsenic stock solution (1000g As/mL).Dissolve 0.1320 g As2O3in mixture of 50 mL reagent water and 1 mL NH4OH, (c), by heating at 7580C; cool to room temperature; and acidify with 2 mL HNO3. Dilute to 100 mL. (4)
17、 Barium stock solution (1000g Ba/mL).Dissolve 0.1437 g BaCO3in mixture of 10 mL reagent water and 2 mL HNO3by heat- ing while stiring. Dilute to 100 mL. (5) Beryllium stock solution (1000g Be/mL).Dissolve1.965g BeSO44H2O(donotdry)in50mLreagentwater.Add1mLHNO3. Dilute to 100 mL. (6) Bismuth stock sol
18、ution (1000g Bi/mL).Dissolve 0.1115 g Bi2O3in 5 mL HNO3by heating at 7580C, cool to room tempera- ture, and dilute to 100 mL. (7) Cadmium stock solution (1000g Cd/mL).Pickle Cd metal in(1+9)HNO3solution,(a)(3),to0.100g.Dissolvein5mL(1+1) HNO3solutionbyheatingat7580C,cooltoroomtemperature,and dilute
19、to 100 mL. (8) Chromium stock solution (1000 g Cr/mL).Dissolve 0.1923 g CrO3in mixture of 10 mL reagent water and 1 mL HNO3. Dilute to 100 mL. (9) Cobalt stock solution (1000g Co/mL).Pickle Co metal in (1+9)HNO3solutionto0.100g.Dissolvein5mL(1+1)HNO3so- lutionbyheatingat7580C,cooltoroomtemperature,a
20、nddiluteto 100 mL. 2000 AOAC INTERNATIONAL 2000 AOAC INTERNATIONAL Table 993.14A Interlaboratory study results for trace elements in water, inductively coupled plasmamass spectrometric method AnalyteAdded, g/LSpike recovery, g/LRecovery, %sRsrRSDR, %RSDr, % Reagent water Aluminum8.00 12.00 56.00 80.
21、00 160.00 200.00 10.01 10.98 59.13 82.59 158.95 200.89 125.13 91.50 105.59 103.24 99.34 100.45 2.33 5.16 5.55 4.92 11.82 8.61 1.74 4.19 8.90 23.28 46.99 9.39 5.96 7.44 4.29 16.58 5.91 4.95 Antimony2.80 4.00 20.00 28.00 80.00 100.00 2.75 4.22 19.76 27.48 82.52 98.06 98.21 105.50 98.80 98.14 103.15 98
22、.06 0.27 0.46 1.09 1.38 2.24 1.34 0.27 0.85 1.76 9.82 10.90 5.52 5.02 2.71 1.37 7.75 3.60 1.95 Arsenic8.00 12.00 56.00 80.00 160.00 200.00 8.64 12.58 55.44 85.15 161.80 201.52 108.00 104.83 99.00 106.44 101.13 100.76 3.01 3.18 4.64 2.54 11.15 10.81 3.02 3.51 3.96 34.84 25.28 8.37 2.98 6.89 5.36 28.4
23、6 4.99 2.18 Barium8.01 12.00 48.00 64.00 160.00 200.00 7.58 11.81 47.32 65.52 157.09 198.53 94.63 98.42 98.58 102.38 98.18 99.27 0.50 1.05 1.60 2.90 6.53 8.28 0.48 1.82 4.07 6.60 8.89 3.38 4.43 4.16 4.17 4.95 3.23 2.29 Beryllium2.80 4.00 20.00 28.00 80.00 100.00 3.31 4.45 22.38 30.02 84.18 102.88 11
24、8.21 111.25 111.90 107.21 105.23 102.88 0.81 0.73 2.76 2.86 4.79 5.90 0.26 1.00 4.02 24.47 16.40 12.33 9.53 5.69 5.73 6.70 3.82 4.30 Cadmium4.00 6.00 20.00 28.00 80.00 100.00 4.01 6.32 19.81 28.33 81.28 100.11 100.25 105.33 99.05 101.18 101.60 100.11 0.34 0.49 1.12 0.94 4.91 3.24 0.20 0.86 1.33 8.48
25、 7.75 5.65 3.32 6.04 3.24 3.87 3.57 1.47 Chromium8.00 12.00 56.00 80.00 160.00 200.00 8.27 13.88 57.86 84.73 157.66 197.43 103.38 115.67 103.32 105.91 98.54 98.72 0.32 3.10 4.03 2.65 13.62 9.47 1.54 2.68 6.97 3.87 22.33 6.97 3.13 8.64 4.80 13.91 3.76 3.93 Cobalt0.80 1.21 20.10 28.20 80.50 101.00 0.8
26、8 0.98 20.77 27.75 78.59 98.79 110.00 80.99 103.33 98.40 97.63 97.81 0.10 0.04 0.74 0.96 2.29 2.94 0.05 0.67 2.31 11.36 4.08 3.56 3.46 2.91 2.98 5.38 2.76 2.60 Copper4.00 6.00 20.00 28.00 80.00 100.00 3.88 6.14 20.07 27.97 79.80 99.57 97.00 102.33 100.35 99.89 99.75 99.57 0.73 1.00 1.08 1.94 3.22 4.
27、42 0.59 0.92 1.91 18.81 16.29 5.38 6.94 4.04 4.44 11.78 3.83 2.13 Lead4.00 6.00 20.00 28.00 80.00 100.00 4.00 5.56 20.54 30.90 80.57 102.93 100.00 92.67 102.70 110.36 100.71 102.93 1.57 2.00 2.91 4.58 3.13 6.62 1.62 4.36 4.29 39.25 35.97 14.17 14.82 3.88 6.43 33.89 16.95 4.68 2000 AOAC INTERNATIONAL
28、 Table 993.14A (continued) AnalyteAdded, g/LSpike recovery, g/LRecovery, %sRsrRSDR, %RSDr, % Reagent water Manganese0.80 1.20 20.00 28.00 80.00 100.00 0.86 1.09 20.43 27.53 79.00 97.60 107.50 9.83 102.15 98.32 98.75 97.60 0.15 0.12 0.89 0.41 3.16 2.51 0.09 0.72 2.38 17.44 11.01 4.36 1.49 4.00 2.57 9
29、.23 3.00 2.70 Molybdenum2.80 4.00 20.00 28.00 80.00 100.00 2.63 3.85 19.75 27.87 83.07 100.08 93.93 96.25 98.75 99.54 103.84 100.08 0.32 0.31 0.64 1.07 3.07 4.32 0.16 0.64 1.78 12.17 8.05 3.24 3.84 3.70 4.32 4.94 2.69 1.94 Nickel4.00 6.00 20.00 28.00 80.00 100.00 4.02 6.36 19.93 28.02 79.29 100.87 1
30、00.50 106.00 99.65 100.07 99.11 100.87 0.41 0.91 1.30 1.25 2.95 7.20 0.50 0.63 2.55 10.20 14.31 6.52 4.46 3.72 7.14 9.63 2.63 2.83 Selenium32.00 40.00 80.00 96.00 160.00 200.00 33.54 41.03 81.40 98.34 165.58 214.30 104.81 102.58 101.75 102.33 102.24 107.15 4.63 6.04 5.86 8.57 15.69 10.57 1.57 5.44 9
31、.86 13.80 14.72 7.20 8.71 9.59 4.93 4.21 6.05 5.22 Silver0.80 1.20 48.00 64.00 160.00 200.00 0.93 1.51 49.39 63.54 136.42 153.74 116.25 125.83 102.90 99.28 85.26 76.87 0.09 0.23 3.25 2.75 48.31 57.34 0.14 1.81 12.19 9.68 15.23 6.58 4.33 35.41 37.30 11.48 3.21 8.40 Thallium2.80 4.00 20.00 28.00 80.00
32、 100.00 2.89 3.92 19.27 28.08 81.29 96.69 103.21 98.00 96.35 100.29 101.61 96.69 0.23 0.15 0.99 0.83 3.65 2.86 0.22 0.67 2.86 7.96 3.83 5.14 2.96 4.49 2.96 6.46 2.83 3.21 Thorium0.80 1.20 20.00 28.00 80.10 100.00 0.93 1.22 20.88 27.97 81.14 102.64 116.25 101.67 104.40 99.89 101.30 102.64 0.16 0.19 0
33、.90 1.11 2.99 3.39 0.09 0.71 2.14 17.20 15.57 4.31 3.97 3.68 3.30 8.37 2.91 2.33 Uranium0.80 1.20 20.10 28.10 80.30 100.00 0.86 1.10 21.38 28.36 82.47 103.49 107.50 91.67 106.37 100.93 102.70 103.49 0.05 0.11 0.99 1.10 4.03 5.24 0.08 0.82 2.16 5.81 10.00 4.63 3.88 4.89 5.06 8.16 3.30 2.32 Vanadium32
34、.00 40.00 80.00 96.00 160.00 200.00 31.02 38.54 79.14 93.47 162.43 208.20 96.94 96.35 98.93 97.36 101.52 104.10 2.68 2.94 4.94 3.85 5.67 2.65 2.19 4.29 3.30 8.64 7.63 6.24 4.12 3.49 1.27 6.30 4.97 1.78 Zinc8.00 12.00 56.00 80.00 160.00 200.00 8.33 15.49 56.07 85.53 165.17 207.27 104.13 129.08 100.13
35、 106.91 103.23 103.64 2.56 4.18 2.91 5.81 7.78 14.61 1.78 2.47 9.87 30.73 26.99 5.19 6.79 4.71 7.05 14.95 3.49 5.30 2000 AOAC INTERNATIONAL Table 993.14A (continued) AnalyteAdded, g/LSpike recovery, g/LRecovery, %sRsrRSDR, %RSDr, % Drinking water Aluminum8.00 12.00 56.00 80.00 160.00 200.00 11.18 11
36、.02 56.97 82.73 159.89 189.98 139.75 91.83 101.73 103.41 99.93 94.99 9.02 3.02 7.14 8.01 11.94 12.97 6.34 6.18 10.59 80.68 27.40 12.53 9.68 7.47 6.83 57.12 8.85 6.05 Antimony2.80 4.00 20.00 28.00 80.00 100.00 2.73 4.10 19.17 26.48 83.43 97.19 97.50 102.50 95.85 94.57 104.29 97.19 0.29 0.47 1.37 1.72
37、 2.05 5.31 0.17 0.66 2.46 10.62 11.46 7.15 6.50 2.46 5.46 4.98 2.89 2.72 Arsenic8.00 12.00 56.00 80.00 160.00 200.00 9.00 11.37 53.77 87.72 157.56 197.99 112.50 94.75 96.02 109.65 98.48 99.00 3.13 1.77 4.12 4.14 4.83 10.66 1.96 4.07 6.30 34.78 15.57 7.66 4.72 3.07 5.38 19.24 5.75 3.54 Barium8.01 12.
38、00 48.00 64.00 160.00 200.00 8.21 12.56 49.13 65.30 155.25 196.52 102.50 104.67 102.35 102.03 97.03 98.26 1.21 1.79 3.72 4.16 7.82 5.70 1.11 3.77 5.67 14.74 14.25 7.57 6.37 5.04 2.90 10.69 6.59 3.22 Beryllium2.80 4.00 20.00 28.00 80.00 100.00 3.15 4.45 21.27 29.57 87.59 102.64 112.50 111.25 106.35 1
39、05.61 109.49 102.64 0.47 0.51 1.23 1.67 6.89 6.27 0.31 0.63 1.88 14.92 11.46 5.78 5.65 7.87 6.11 8.16 2.48 1.98 Cadmium4.00 6.00 20.00 28.00 80.00 100.00 4.11 5.87 19.57 27.68 80.62 98.15 102.75 97.83 97.85 98.86 100.78 98.15 0.88 0.58 1.45 1.27 4.45 3.60 0.71 1.26 2.02 21.41 9.88 7.41 4.59 5.52 3.6
40、7 14.23 5.33 2.26 Chromium8.00 12.00 56.00 80.00 160.00 200.00 9.46 13.10 56.04 84.38 158.24 196.72 118.25 109.17 100.07 105.48 98.90 98.36 2.34 2.39 2.24 3.18 5.12 7.47 2.08 1.29 3.16 24.74 18.24 4.00 3.77 3.24 3.80 18.44 1.84 1.78 Cobalt0.80 1.21 20.10 28.20 80.50 101.00 0.92 1.02 20.45 27.29 78.0
41、4 97.62 115.00 84.30 101.74 96.77 96.94 96.65 0.45 0.10 0.91 1.22 3.72 4.62 0.31 0.53 1.84 48.91 9.80 4.45 4.47 4.77 4.73 31.96 2.22 2.09 Copper4.00 6.00 20.00 28.00 80.00 100.00 3.33 5.95 18.90 27.21 76.64 96.17 83.25 99.17 94.50 97.18 95.80 96.17 0.85 1.78 1.64 2.76 5.30 5.64 0.99 1.51 3.42 25.53
42、29.92 8.68 10.14 6.92 5.86 21.34 6.55 3.96 Lead4.00 6.00 20.00 28.00 80.00 100.00 3.44 6.84 20.18 28.08 80.92 101.60 86.00 114.00 100.90 100.29 101.15 101.60 1.15 1.10 1.20 1.57 2.30 3.23 1.18 1.44 2.07 33.43 16.08 5.95 5.59 2.84 3.18 22.96 5.97 2.27 2000 AOAC INTERNATIONAL Table 993.14A (continued)
43、 AnalyteAdded, g/LSpike recovery, g/LRecovery, %sRsrRSDR, %RSDr, % Drinking water Manganese0.80 1.20 20.00 28.00 80.00 100.00 0.96 1.13 21.06 27.60 79.57 97.97 120.00 94.17 105.30 98.57 99.46 97.97 0.32 0.38 1.32 1.47 4.18 4.10 0.42 0.96 2.01 33.33 33.63 6.27 5.33 5.25 4.18 40.19 3.95 2.26 Molybdenu
44、m2.80 4.00 20.00 28.00 80.00 100.00 2.80 3.95 19.78 27.87 85.65 99.06 100.00 98.75 98.90 99.54 107.06 99.06 0.20 0.47 0.60 1.51 3.50 2.89 0.32 1.16 3.07 7.14 11.90 3.03 5.42 4.09 2.92 9.48 4.87 3.32 Nickel4.00 6.00 20.00 28.00 80.00 100.00 3.66 5.44 18.42 27.09 75.84 95.83 91.50 90.67 92.10 96.75 94
45、.80 95.83 0.53 1.32 0.87 1.68 4.40 4.41 1.03 1.11 3.94 14.48 24.26 4.72 6.20 5.80 4.60 22.64 4.88 4.59 Selenium32.00 40.00 80.00 96.10 160.00 200.00 32.57 42.18 79.97 94.94 163.48 212.19 101.78 105.45 99.96 98.79 102.18 106.10 4.37 3.71 6.66 7.90 9.17 16.49 3.65 5.28 10.06 13.42 8.80 8.33 8.32 5.61
46、7.77 9.77 6.04 5.36 Silver0.80 1.20 48.00 64.00 160.00 200.00 0.70 1.37 45.43 60.35 119.06 172.15 87.50 114.17 94.65 94.30 74.41 86.08 0.34 0.33 6.78 2.22 55.28 31.92 0.34 5.15 36.34 48.57 24.09 14.92 3.68 46.43 18.54 32.85 9.74 24.96 Thallium2.80 4.00 20.00 28.00 80.00 100.00 2.88 3.96 19.77 27.61
47、85.32 100.07 102.86 99.00 98.85 98.61 106.65 100.07 0.40 0.21 1.13 1.24 4.08 4.33 0.16 0.83 4.05 13.89 5.30 5.72 4.49 4.78 4.33 4.68 3.50 4.37 Thorium0.80 1.20 20.00 28.00 80.10 100.00 0.78 1.09 21.66 28.09 79.99 100.50 97.50 90.83 108.30 100.32 99.86 100.50 0.13 0.19 0.94 0.83 2.03 4.56 0.07 0.54 2
48、.60 16.67 17.43 4.34 2.95 2.54 4.54 7.49 2.17 2.88 Uranium0.80 1.20 20.10 28.10 80.30 100.00 0.85 1.05 22.30 28.89 80.31 100.70 106.25 87.50 110.95 102.81 100.01 100.70 0.15 0.13 1.40 1.47 2.00 5.30 0.09 0.46 2.71 17.65 12.38 6.28 5.09 2.49 5.26 9.47 1.80 2.99 Vanadium32.00 40.00 80.00 96.00 160.00
49、200.00 33.15 40.20 77.83 96.32 161.89 214.91 103.59 100.50 97.29 100.33 101.18 107.46 2.51 1.88 4.18 1.34 7.63 5.89 2.28 2.75 6.56 7.57 4.68 5.37 1.39 4.71 2.74 6.22 3.16 3.48 Zinc8.00 12.00 56.00 80.00 160.00 200.00 11.60 10.21 56.83 82.88 156.69 191.59 145.00 85.08 101.48 103.60 97.93 95.80 6.18 4.96 7.66 8.34 17.01 17.21 5.72 4.56 9.48 53.28 48.58 13.48 10.06 10.86 8.98 52.45 6.53 5.44 2000 AOAC INTERNATIONAL Table 993.14A (continued) AnalyteAdded, g/LSpike recovery, g/LRecovery, %sRsrRSDR, %RSDr