1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS I ISO 19730 KS I ISO 19730:2009 2009 12 18 http:/www.kats.go.krKS I ISO 19730:2009 : ( ) ( ) () ( ) : (ISO/TC190) () ( ) () : (http:/www.standard.go.kr) : :2009 12 18 2009-0831 : :(ISO/TC190) ( 02-509-7266) (http:/www.kats.go.kr). 10 5 , . KS I ISO 19730:
2、2009 i .1 1 1 2 1 3 1 4 2 5 2 6 3 6.1 3 6.2 .3 6.3 .3 6.4 (Phase separation) 3 6.5 .3 6.6 .3 7 3 8 .4 9 .5 A( ) 6 A.1 6 A.2 6 B( ) 7 C( ) , 9 C.1 9 C.2 .9 C.3 .9 10 KS I ISO 19730:2009 Soil quality Extraction of trace elements from soil using ammonium nitrate solution 2008 1 ISO 19730, Soil quality
3、Extraction of trace elements from soil using ammonium nitrate solution . 1 1 mol/L (NH4NO3) . A . 2 . . ( ) . KS I ISO 11464, KS I ISO 11465, ( ) KS M ISO 3696, 3 2 mm 1 mol/L 1: 2.5(m/V) (end-over-end shaker) (202) 120 . . 1 (Flame-AAS), (Hydride generation or electrothermal-AAS), (ICP-AES), (ICP-M
4、S) . 2 (solid-to-liquid ratio) . KS I ISO 19730:2009 2 4 . . 4.1 , KS M ISO 3696 2 0.1 ms/m(25 ), 0.01 M m(25 ) . 0.18 M m . 4.2 (NH4NO3), 1 mol/L ( 99 %, .) 80.04 g 1 L . 1 mol/L . 4.3 (HNO3), 65 %, 1.4 g/mL 4.4 , 5 % (4.3) 50 mL 1 L . 5 . 5.1 , (302) . 5.2 , . 5.3 , 2 mm( ), 5 mm 8 mm( ), . 5.4 ,
5、0.01 g . 5.5 (conical) , 50 mL ( , , , / ) . . , (4.4) 24 . 5.6 (End-over-end shaker), (202) (202) r/min . 5.7 , 1 0.45 m 1 . (4.4) . 0.2 m . . 5.8 1 , 10 mL 20 mL . KS I ISO 19730:2009 3 5.9 , (5.5) 1 000 g 3 000 g . 6 6.1 KS I ISO 11464 . 2 mm . , , (reductomorphic)- (gley soil) back water - 30 %
6、C . 6.2 KS I ISO 11465 . 6.3 1 mol/L NH4NO3 (202) 1: 2.5(m/V) . 50 mL (5.5) (100.01) g (6.1) 25 mL (4.2) . (5.6) (202) r/min (1205) . C . 6.4 (Phase separation) 1 000 g 10 . 1 mL . 10 mL 0.45 m 1 10 mL . . 6.5 1 % (4.3) (: 10 mL 0.1 mL ). ( ICP ). 50 mL (: 10 mL) 0.5 mL (4.3) 50 mL . . 6.6 . 7 KS I
7、ISO 11465 g/kg (wx) . (1) KS I ISO 19730:2009 4 (2) . : 100)100(0OHBx2+=mwVFw (1) : +=100OHOHdBx22wmVFw (2) (%): 100dd0OH2=mmmw (3) wx: (x) (g/kg) B: (g/L) V : (L)(0.025 L) F : (Vend/Vi): Vi NH4NO3 , Vend m0: (kg) md: KS I ISO 11465 (kg) OH2w : KS I ISO 11465 OH2 : KS I ISO 11465 (M, g/dm3) (4) . M
8、wx d (4) d: (kg/dm3) 8 g/kg g/dm3 . wPb 20.3 g/kg wCd 1.3 g/kg . . B . KS I ISO 19730:2009 5 9 . a) b) c) KS I ISO 19730:2009 6 A ( ) A.1 A.1 . A.1 1 mol/L g/L g/kg 10 25 1 2.5 2 5 4 10 20 50 100 250 8 20 2 000 5 000 0.4 1 10 25 100 250 1 2.5 10 25 100 250 A.2 1 mo/L g/L . KS I ISO 11047 KS I ISO 20
9、280 (AAS), ISO 22036 (ICP-AES) KS I ISO 17294 2 (ICP-MS) . (matrix modifier) 300 . ICP-AES . . . KS I ISO 19730:2009 7 B ( ) B.1 . 2007 . 14 . 2 1 mol/L BAM . . A: INRA( ) , (HF) : Zn 3 960 mg/kg, Pb 970 mg/kg, Cd20 mg/kg B: VDLUFA( ) C: UKZUZ, NRL( ) , : As 13 mg/kg, Hg 0.8 mg/kg, Ni57 mg/kg, Cr 51
10、 mg/kg D: UKZUZ, NRL( ) , : As 8.5 mg/kg, Hg 0.6 mg/kg, Ni30 mg/kg, Cr 51 mg/kg (BAM) 1 mm 80 g . (ICP-MASS), Agilent 7500cs, , He/H2, Babington nebuliser Scott (chamber), 2 , 15 L/min , Pt . 1 mol/L (80 g/L) ICP-MS . 1 % 10 GE Ho(10 g/L) . 1.0 mL 100 g/L 8.9 mL (1 %) . A B Zn Pb 1: 100 1: 1 000 . 1
11、0 . . A, B, D . KS I ISO 19730:2009 8 B.1 KS I ISO 19730 l n x g/kg SRg/kg Srg/kg CV(R)% CV(r) % R g/kg r g/kgA Sb 12 24 18.57 0.569 0.195 3.07 1.05 1.58 0.54 B Sb 12 24 11.75 0.491 0.099 4.18 0.84 1.36 0.28 C Sb 13 26 9.15 1.15 0.117 12.57 1.28 3.19 0.32 D Sb 11 22 13.19 0.912 0.174 6.91 1.32 2.53
12、0.48 A As 13 26 3.99 0.438 0.112 10.99 2.81 1.21 0.31 B As 13 26 62.56 4.584 0.44 7.33 0.70 12.70 1.22 C As 14 28 18.05 0.948 0.185 5.25 1.02 2.63 0.51 D As 13 26 26.49 1.189 1.061 4.49 4.01 3.29 2.94 A Cd 13 26 5 605.15 222.38 67.629 3.97 1.21 615.99 187.33B Cd 11 22 138.76 7.562 0.878 5.45 0.63 20
13、.95 2.43 C Cd 11 22 75.39 4.423 0.639 5.87 0.85 12.25 1.77 D Cd 10 20 16.08 0.929 0.235 5.78 1.46 2.57 0.65 A Co 14 28 175.82 9.013 3.75 5.13 2.13 24.97 10.39B Co 13 26 44.29 2.011 0.405 4.54 0.92 5.57 1.12 C Co 13 26 45.62 1.19 0.47 2.61 1.03 3.30 1.30 D Co 13 26 13.89 0.914 0.615 6.58 4.42 2.53 1.
14、70 C Cr 14 28 11.68 2.925 1.529 25.03 13.09 8.10 4.24 A Cu 12 24 250.18 25.969 3.543 10.38 1.42 71.94 9.82 B Cu 13 26 287.03 25.556 2.713 8.90 0.95 70.79 7.52 C Cu 13 26 384.41 45.203 6.095 11.76 1.59 125.21 16.88D Cu 13 26 587.75 48.057 23.773 8.18 4.04 133.12 65.85A Ni 13 26 905.7 40.74 16.18 4.50
15、 1.79 112.85 44.82B Ni 14 28 211.0 16.08 2.11 7.62 1.00 44.55 5.85 C Ni 13 26 999.2 45.66 7.52 4.57 0.75 126.47 20.83D Ni 13 26 141.6 9.49 6.091 6.70 4.30 26.29 16.87A Pb 14 28 13 302.4 665.702 205.771 5.00 1.551 1 844.00 569.99B Pb 14 28 74.14 16.667 6.454 22.48 8.70 46.17 17.88A Se 14 28 1.80 0.10
16、 0.086 5.82 4.78 0.29 0.24 B Se 14 28 4.16 0.21 0.105 5.02 2.54 0.58 0.29 C Se 14 28 6.21 0.42 0.204 6.81 3.29 1.17 0.57 D Se 14 28 4.79 0.41 0.081 8.59 1.69 1.14 0.22 l : n : x : , g/kg Sr: , g/kg CV(r) : , % SR: , g/kg CV(R) : , % R : (2.77) r : (2.77) KS I ISO 19730:2009 9 C ( ) , C.1 2 mm, 5 mm
17、8 mm . 2 mm . (: 100 g 250 mL ). . C.2 . . (: 40 g 100 mL ). (20 g, 3 mm .) . . C.3 . . KS I ISO 19730:2009 10 1 KS A ISO 5725 1, ( ) 1: 2 KS A ISO 5725 2, ( ) 2: 3 KS A ISO 5725 3, ( ) 3: 4 KS A ISO 5725 4, ( ) 4: 5 KS A ISO 5725 5, ( ) 5: 6 KS A ISO 5725 6, ( ) 6: 7 KS I ISO 11047, , , , , , , 8 K
18、S I ISO 17294 2, (ICP MS) 2: 62 9 KS I ISO 20280, , , 10 ISO 22036, Soil quality Determination of trace elements in extracts of soil by inductively coupled plasma atomic emission spectrometry(ICP AES) 11 LEITERER, M., BREUER, J., FEUCHT, G., JANSSEN, E. Untersuchungen zur Przision der Spurenelementa
19、nalytik in Ammoniumnitrat Bodenextrakten Studies of the precision of trace element analysis in ammonium nitrate soil extracts. VDLUFA publication series, No. 43, VDLUFA, Darmstadt, 1996 12 PRESS, A. Vorsorgewerte und Prfwerte fr mobile und mobilisierbare, potentiell kotoxische Spurenelemente in Bden
20、 Precautionary values and test values for mobile and mobilizable, potentially ecotoxic trace elements in soil. Verlag Ulrich E. Grauer, Wendlingen, 1992, 145 p. 13 PRESS, A., TURIAN, G., SCHWEIKLE, V. Ableitung kritischer Gehalte an NH4NO3-extrahierbaren kotoxikologisch relevanten Spurenelementen in
21、 Bden SW Deutschlands Derivation of critical contents of NH4NO3-extractable ecotoxically relevant trace elements in soil encountered in Southwest Germany. Mitteilungen Dtsch. Bodenkundl. Gesellsch. 1991, 66 (1), pp. 385 388 14 SYMEONIDES, C., MCRAE, S.G. The assessment of plant available cadmium in
22、soils. J. Environm. Qual. 1977, 6, pp. 120 123 15 ZEIEN, H., BRMMER, G.W. Analysenvorschrift zur Extraktion der “mobilen” und der “leicht nachlieferbaren” Schwermetalle Analytical procedure for extracting “mobile” and “easily replenishable” heavy metals. Institut fr Bodenkunde der Rheinischen Friedr
23、ich WilhelmsUniversitt Bonn, Bonn 16 ZEIEN, H., BRMMER, G.W. Chemische Extraktionen zur Bestimmung von Schwermetallbindungsformen in Bden. Chemical extractions for the determination of heavy metals in soil. Mitteilungen. Dtsch. Bodenkundl. Gesellsch., 1989, 59 (1), pp. 505 510 17 ZEIEN, H., BRMMER,
24、G.W. Ermittlung der Mobilitt und Bindungsformen in Bden mittels sequentieller Extraktionen Determining the mobility and bonding forms in soil by means of sequential extractions. Mitteilungen. Dtsch. Bodenkundl. Gesellsch. 1991, 66 (1), pp. 439 442 153787 1 92 3(13) (02)26240114 (02)262401489 http:/ Korean Agency for Technology and Standards http:/www.kats.go.kr KS I ISO 19730:2009KSKSKS SKSKS KSKS SKS KS SKS KSKS SKSKS KSKSKS Soil quality Extraction of trace elements from soil using ammonium nitrate solution ICS 13.080