1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS I 3224 KS I 3224:2009 2009 12 18 http:/www.kats.go.krKS I 3224:2009 : ( ) ( ) () ( ) : (ISO/TC147) ( ) () () KS I 3224:2009 : (http:/www.standard.go.kr) ： ：2004 9 30 ：2009 12 18 2009-0830 ： ： (ISO/TC147) ( 02-509-7266) (http:/www.kats.go.kr). 10 5 , . KS
2、I 3224:2009 Test method for ordorous compounds in water 1 (geosmin) 2-MIB . 1 2-MIB 2 . . ( ) . American Water Works Association(AWWA), Standarad Method 6040D, 1999 Guide to the Expression of Uncertainty in Measurement. ISO 3 SPME(solid-phase microextraction) pmole/mole . (headspace) . GC/MS (inject
3、ion port) . . GC/MS SIM . (mass SIM ions) . MIB, , IPMP, IBMP . SPME . (response factor) . OH OH 2-Me-isoborneol(MIB) KS I 3224:2009 2 2 SPME ( ) 4 250 mL , (headspace) . 3 10 mg/L . , . 5 5.1 . ： (251.0) ： (505) % 6 6.1 , (GC MS) . 6.2 SPME 6.3 , 65 , . 6.4 , 0.02 mg200 g . 6.5 , 15 mL SPME SPME SP
4、ME KS I 3224:2009 3 6.6 , 10 g/L . 3 SPME 7 7.1 SPME divinylbenzene-carboxen-polydimethylsiloxane (cross-link coating) . 7.2 100 mg/L , 2-MIB, , IBMP, IPMP 100 mg/L . 1 . 7.3 10 mg/L , 2-MIB, , IBMP, IPMP 100 mg/L 1： 10 10 mg/L . 30 . 7.4 45 g/L , 2-MIB, 45 g/L . 3 . 7.5 , 45 g/L 10 mL , . (plunger)
5、 (septum) (vial) KS I 3224:2009 4 4 SPME GC MS 2-MIB, 7.6 QC (Laboratory Control Standard, LCS) (Laboratory-Fortified Matrix standard, LFM) , QC 15 20 ng/L 2-MIB . 7.7 45 g/L IBMP (internal standard solution), 100 mg/L IBMP . 2-MIB . 10 ng/L IBMP . 7.8 45 g/L IPMP (surrogate standard solution), 10 m
6、g/L . ng/L 10 ng/L . IPMP SPME QC . 7.9 , 750 12 . 5 (IBMP) (IPMP) 8 8.1 SPME SPME 280 2 . 8.2 15 mL 3 g , N N N N OMe OMe 2-isobutyl-3-methoxypyrazine(IBMP) 2-isopropyl-3-methoxypyrazine(IPMP) KS I 3224:2009 5 . 1 65 . 8.3 SPME SPME . 30 . . 8.4 SPME SPME SPME GC GC . 10 SPME GC . 8.5 GC MS GC 5 %
7、(phenylmethyl silicon) , 1 . 1 GC MS (column) (oven temp.) (column flow) (split vent) (inlet temp.) MS (MS source temp.) (Mass range) MS (MS transfer line temp.) MS (MS ion source temp.) 5 % 60 m0.32 mm0.25 m 50 (2 ) 10 / 200 25 / 250 (2 ) 1.5 mL/ (splitless) 50 mL/ 1 250 200 33 amu350 amu(SIM ) 250
8、 200 MS SIM MS . 2-MIB： 95(1 ), 93, 107, 108, 135(2 ) ： 112(1 ), 126(2 ) IBMP： 124(1 ), 151, 94(2 ) IPMP： 137(1 ), 152, 124(2 ) 2 SPME SPME 2 cm 50/30 m DVB/Carboxen/PDMS 30 10 KS I 3224:2009 6 6 GC MS (SIM mode) 9 . y ax b bCCaAAixix CxreciixfCbAAa1 Cx ： (ng/L) Ci ： (ng/L) Ax ： Ai ： a ： b ： y frec
9、： 3 ng/L ng/L 2-MIB 8.96 12.86 2.28 4.42 Time IPMP 2-MIB IBMP KS I 3224:2009 7 7 ( ) 8 ( ) Time IPMP 2-MIB Time IPMP 2-MIB IBMP KS I 3224:2009 8 10 (Method Detection Limit, MDL) MDL 2 ng/L 10 . 2-MIB (10 ng/L) . MDL t(n 1, 1 a 0.99)S n： 4 2-MIB MDL ng/L MDL 2-MIB 2.20 0.32 2.20 0.19 11 SPME GC/MS .
10、MS . MIB . 12 . IPMP IBMP 130 % . 13 13.1 20 % . (LCS) 80 %120 % . . 13.2 (LCS) 20 1 SPME . SPME . 13.3 20 1 (LFM) 70 %130 %KS I 3224:2009 9 ( ). . 13.4 . 80 %120 % . 14 14.1 ISO Guide . 9 5 14.2 . linrecsisxixsisxixffAAAACCCC (1) linrecsrxrsisxixffAACCCC (2) Cx ： (ng/L) Cxi ： (IBMP) (ng/L) Cs ： (ng
11、/L) uiA B uc U , ci KS I 3224:2009 10 Csi ： (IBMP) (ng/L) Ax ： Axi ： (IBMP) As ： Asi ： (IBMP) frec ： flin ： Axr ： (IBMP) Asr ： (IBMP) 14.3 standard uncertainty, u(xi) , . 10 14.3.1 , u(Cs1), u(Cs2), u(Cs) 2 ng/L20 ng/L 3 . 1 . , 1 100 mg/L ( , ) . 2 1 , 10 mg/L , 3 2 45 g/L . . (V) (V) (Rs Rsi) (Rs
12、Rsi) (Cs) (Csi) (V) KS I 3224:2009 11 5 1 (100 mg/L 10 mg/L ) % % CpB 100 mg/L 1.10 mg/L 1.1 0.11 mg/L 86.1 , Vs1B 0.30 mL 0.210 3mL 0.1 12 0.01 mg/L 5.8 , Vr1B 3.00 mL 3.110 3mL 0.1 25 0.01 mg/L 8.1 u(Vr1) u(Vs1)(std solution) u(Vrel) (methanol) Crl10.0 mg/L 0.11 mg/L 1.1 211 676 6 3 (45 g/L 5 ng/L
13、 ) % % CpB 43.85 g/L 0.49 g/L 1.1 162 977 0.06 ng/L 86.2 u(Cp), u(Vs1), u(Vr1) VsB 11.810 3 mL 8.710 6 mL 0.1 12 0.00 mg/L 5.5 , VrB 100.8 mL 0.15 mL 0.2 49 0.01 mg/L 11.0 u(Vr) u(Vs)(std solution 4 ) u(VH)(H2O) Cs5.16 ng/L 0.06 ng/L 1.1 136 108 7 1 mg/L 2 g/L 3 ng/L 2-MIB 10.00.11 1.1 43.850.49 1.1
14、 5.160.06 1.1 10.00.14 1.4 43.850.60 1.4 5.160.07 1.4 IPMP 12.330.04 0.3 54.800.20 0.4 18.40.07 0.4 IBMP 12.240.11 0.9 54.890.48 0.9 18.10.16 0.9 14.3.2 (Asr, Axr) 10 mL n , n . KS I 3224:2009 12 8 RT(min) AsrAsrAsr SD RSD(%)2-MIB 12.59 0.386 0.311 0.329 0.342 0.040 0.023 11.6 15.81 0.275 0.238 0.28
15、6 0.266 0.025 0.014 9.3 9 ( A) RT(min) AxrAxrAxr SD RSD(%)2-MIB 12.59 0.565 0.553 0.523 0.547 0.022 0.012 4.0 15.81 0.121 0.125 0.112 0.119 0.007 0.004 5.8 10 ( B) RT(min) AxrAxrAxr SD RSD(%)2-MIB 12.59 0.820 0.696 0.681 0.733 0.076 0.044 10.4 15.81 0.210 0.189 0.227 0.209 0.019 0.011 9.1 14.3.3 (fr
16、ec) . 11 5 ng/L diff. % frec% 2-MIB 4.82 4.55 94.4 % 5.6 2.8 4.82 4.38 90.8 % 9.2 4.5 12 10 ng/L diff. % frec% 2-MIB 9.92 10.20 102.8 % 2.8 1.4 9.92 9.57 96.4 % 3.6 1.8 14.3.4 (flin) . 13 diff. % flin% 2-MIB 0.56 0.57 0.9 0.4 0.28 0.31 10.2 1.5 KS I 3224:2009 13 14.4 Combined uncertainty, uc(Cx) . 0
17、.59 ng/L 6.6 %( 3) . , (IBMP) 48.8 % . 2/12122/1221)()()(iNiiiNiicxucxuxfyu ci： 14 % % CxiB 17.56 ng/L 0.16 ng/L 0.9 52 052 0.46 0.07 ng/L 6.5 CsB 5.16 ng/L 0.06 ng/L 1.1 136 108 1.55 0.09 ng/L 8.3 CsiB 18.12 ng/L 0.16 ng/L 0.9 52 770 0.44 0.07 ng/L 6.5 AxrA 0.547 0.012 2.3 2 14.61 0.18 ng/L 16.7 As
18、rA 0.342 0.023 6.7 2 23.35 0.53 ng/L 48.8 frecA 1 0.014 1.4 34 7.99 0.11 ng/L 10.1 flinA 1 0.004 0.4 19 7.99 0.03 ng/L 3.0 Cx8.96 ng/L 0.59 ng/L 6.6 3 14.5 (Expanded uncertainty, U) kt (95 %) . U(Cx) kuc(Cx) k： (95 % ) (veff) iiiceffvucyuv44)()(KS I 3224:2009 14 15 U(Cx) ng/L uc(Cx) ng/L k95%veffU(C
19、x) ng/L uc(Cx) ng/L k95%veff2-MIB 2.54 0.59 4.3 3 2.86 1.03 2.78 4 0.42 0.18 2.3 9 0.86 0.37 2.31 8 16 ng/L ng/L % ng/L ng/L % 2-MIB 8.96 2.54 28.4 12.86 2.86 22.3 2.28 0.42 18.5 4.42 0.86 19.3 17 Q R2* MDL* ng/L % % * % 2-MIB 95,93,107,108,135 0.998 7 0.32 0.9 8.9 94 103 6.7 112,126 0.999 6 0.19 0.
20、5 3.6 91 96 5.4 * 2 ng/L (n 9) * ： 2 ng/L20 ng/L * SPME GC MS (n 3) 15 , , , , , . GC , . 15.1 15.2 15.3 ( ) ( , ) 15.4 15.5 ( ) KS I 3224:2009 15 15.6 (CRM) ( , CRM , ) 15.7 ( ) 15.8 15.9 15.10 15.11 KS I 3224:2009 16 1 R. McCallum, P. Pendleton, R. Schumann and M.U. Trinh, “Determination of geosmi
21、n an d2-methylisoborneal in water using SPME GC MS CI/EI ionization-ion-trap MS”, The Analyst, v. 123, no. 10(1998), pp. 2155 2160 153787 1 92 3(13) (02)26240114 (02)262401489 http:/ KS I 3224:2009 KSKSKS SKSKS KSKS SKS KS SKS KSKS SKSKS KSKSKS Test method for ordorous compounds in water ICS 13.060 Korean Agency for Technology and Standards http:/www.kats.go.kr
