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1 Isobutyl alcohol IUPAC 2-methylpropan-1-ol Methyl-1-Propanol, Isobutanol CH 3 H 3 C OH CAS C 4 H 10 O log P ow ( C) ( C) (kpa) (g/l) ) ) 108 2) 1.2 2) 87 2) 0.8 2) ( ) 2) LD 50 : 3350 mg/kg EC 50 : 1250 mg/l/24 h 2) 1) kis-net 2) 1

2 1 (1) ODS GC/MS-SIM (2) Fluka -d 7 CDN Isotopes (2-methyl-d 3 -propyl-2,3,3,3,- d 4 -alcohol) μg/ml L(+)- Waters AC-2 ODS Waters C ml 5 ml (3) 21 3 L mg/l 100 mg 100 ml 2

3 (1000 µg/ml) (1000μg/mL) 1.00 μg/ml 100 μg/ml -d mg 100 ml (1000 µg/ml) -d 7 (1000 μg/ml) 50.0 μg/ml 4- (1000 μg/ml) 5.00 μg/ml 8 (3.00 ng/ml 5.00 ng/ml 10.0 ng/ml 30.0 ng/ml 50.0 ng/ml 100 ng/ml 300 ng/ml 500 ng/ml) -d ng/ml ng/ml 200 ml -d 7 (50.0 μg/ml) 5 μl (250 ng)c-18 1AC ml C-18 AC-2 10 ml 10 5 ml 1 ml 3 4- (5.00 μg/ml) 50 μl 3

4 GC/MS GC/MS GC QP2010 J&W DB-WAX (30 m 0.25 mm, 0.5 μm) 40 C (5 min) 5 C/min 80 C (0 min) 20 C/min 200 C(3 min) 200 C 1 min He 1.0 ml/min 2 μl 230 C EI SIM -d μl GC/MS -d 7 2 μl GC/MS -d 7 -d 7 -d 7 4- C (ng/l) C (ng/l) R Q / V 4

5 R Q (ng) V (L) IDL GC/MS IDL 15 1 IDL IDL (ng/ml) (L) (ml) IDL (ng/l) (MDL) (MQL) MDL MQL MDL MQL (L) (ml) MDL (ng/l) MQL (ng/l) C ml 20 ml 2 AC-2 20 ml 40 ml 3 4 m/z = 43 5

6 5 IDL IDL(3.00 ng/ml) 1 3 IDL (L) (ml) 5.0 (ng/ml) 3.00 (μl) (ng/ml) (ng/ml) (ng/ml) (ng/ml) (ng/ml) (ng/ml) (ng/ml) (ng/ml) 3.45 (ng/ml) (ng/ml) IDL (ng/ml)* 0.71 IDL (ng/l) 18 S/N 9.0 CV (%) 5.6 *:IDL = t (n-1, 0.05) σ n-1 2 6

7 m/z = 33 m/z = 74 -d 7 m/z = 50 m/z = m/z = 174 m/z = IDL (3.00 ng/ml) 7

8 6 MDL MQL MDL 2 4 MDL MQL (%) (L) (ml) 5.0 (ng) 50.0 (ng/l) 250 (ng/ml) 10.0 (μl) 2.0 (ng/l)* (ng/l)* (ng/l) (ng/l) (ng/l) (ng/L) (ng/L) (ng/l) (ng/l) (ng/l) (ng/l) (ng/l) MDL (ng/l)* 3 63 MQL (ng/l)* S/N 20 CV (%) *1: (n = 1) *2: MDL (n = 1) *3: MDL = t (n-1, 0.05) σ n-1 2 *4: MQL = σ n

9 m/z = 33 m/z = 74 -d 7 m/z = 50 m/z = m/z = 174 m/z = MDL 9

10 ml (200 mg) (-d7 250 ng) ODS () () 5 ml/min ODS 10 ml 5 ml 1 ml/min (4-250 ng) GC/MS-SIM 3 10

11 ( / ) 面積比 ( 対象物質 / 内標準物質 ) y = x R 2 = 濃度比 ( / ) ( 対象物質 / 内標準物質 ) (3) (5) (10) (30 ) (50) (ng/ml) ng/ml ng/ml ( / ) 面積比 ( 対象物質 / 内標準物質 ) y = x R 2 = 濃度比 ( 対象物質 / 内標準物質 ) ( / ) (30) (50) (100) (300 ) (500) (ng/ml) ng/ml ng/ml 11

12 5 / (min) (ng/ml) -d 7 % (m/z = 33) (m/z = 50) *50.0 ng/ml 6 / (min) (ng/ml) -d 7 % (m/z = 33) (m/z = 50) *50.0 ng/ml 12

13 6 7 -d

14 9 m/z = 33 m/z = 74 -d 7 m/z = 50 m/z = m/z = 174 m/z =

15 (%) (L) (ml) (ng) (μl) (ng/l) * (ng/l) * (ng/l) (ng/l) (ng/l) (ng/l) (ng/l) (ng/l) (ng/l) CV (%) *1: (n = 1) *2: (n = 1) 15

16 8 (%) (L) (ml) (ng) (μl) (ng/l) * (ng/l) * (ng/l) (ng/l) (ng/l) (ng/l) (ng/l) (ng/l) (ng/l) CV (%) *1: (n = 1) *2: (n = 1) 16

17 m/z = 33 m/z = 74 -d 7 m/z = 50 m/z = m/z = 174 m/z = L 250 ng 17

18 m/z = 33 m/z = 74 -d 7 m/z = 50 m/z = m/z = 174 m/z = L 250 ng 18

19 m/z = 33 m/z = 74 -d 7 m/z = 50 m/z = m/z = 174 m/z = L 19

20 m/z = 33 m/z = 74 -d 7 m/z = 50 m/z = m/z = 174 m/z = L 20

21 9 7 67% 9 (n = 2) ph 1 7 (%) (ng/l) (%) ) A B ph ph 7 ph 2 10 No.1 (n = 2) (%) (ng/l) 7 A 120 (ph 2) 59 (ph 7) 500 B 190 (ph 2) 74 (ph 5) 52 (ph 7) (ph 2) 140 (ph 5) 60 (ph 7) 21

22 ph No.2 (n = 2) (%) (ng/l) (ph 2) ph 2 L- 100 mg/l 12 54% 70% 12 No.3 (n = 2) (ng/l) L mg (100 mg/l) 20 mg (100 mg/l) (%) 7 54 (ph ) 70 (ph ) 200 (ph 2) L mg/l % 22

23 13 No.4 (n = 2) (%) (ng/l) L- ph ph 3.73 ph ) (n = 2) (%) (ng/l) ) (n = 2) (%) (ng/ml) 1 MDL

24 ODS (C-18) ODS 5 ml 0% ODS (AC-2) 1 ml 1 ml 100%0%14 回収率 100% 90% 80% 70% 60% 50% 40% 30% 20% 10% 0% 100% 0% 0% 0% 0% 0~1mL 1~2mL 2~3mL 3~4mL 4~5mL 14 24

25 2 3.0 ng/ml 50 ng/ml r 2 > IDL 18 ng/l MDL 63 ng/l 0.2 L n = ng 55 66% % 0.2 μg/l L , TEL FAX [email protected] 25

26 Isobutyl alcohol (2-Methyl-1-Propanol, Isobutanol) An analytical method has been developed for the determination of isobutyl alcohol in water by gas-chromatography mass spectrometry (GC/MS). Surrogate is added to a water sample containing ascorbic acid (1000 mg/l) and the sample is passed through an ODS cartridge column joined on the upper of an activated carbon (AC) cartridge column. The ODS column is removed from the AC column. The AC column is washed with 10 ml of purified water and then is sucked to dry, and eluted with 5 ml of acetone. The eluate is measured by GC/MS-SIM after adding an internal standard. The instrument detection limit (IDL) is 18 ng/l. The method detection limit (MDL) and the method quantification limit (MQL) is 63 ng/l and 170 ng/l, respectively. The average recoveries of environmental waters containing 250 ng of isobutyl alcohol were 59% in river water and 60% in seawater, respectively. Water sample Solid-Phase Extraction 200 ml ascorbic acids (200 mg) surrogate (Isobutyl alchole-d7 250 ng) ODS cartridge column (upper)+ activated carbon cartridge column (lower) 5 ml/min remove ODS column Wash purified water 10 ml Dehydration aspiration Elution acetone 5 ml 1 ml/min syringe spike (4-Bromofluorobenzene 250 ng) GC/MS-SIM 26

27 GC/MS-SIM ml (200 mg) (-d7 250 ng) ODS () () 5 ml/min (ng/l) 63 ODS 10 ml GC/MS: GC/MS-SIM QP ml 1 ml/min (4-250 ng) DB-WAX 30 m 0.25 mm, 0.5 μm 27

28 (VOC) GC/MS-SIM 50.0 ml -d 7 GC/MS-SIM Trap 5 ml GL AQUA Trap C 150 C 40 C 40 ml/min 8 min 40 ml/min 3 min 250 C 2 min 80 ml/min 250 C 18 min He (90 kpa) GC/MS GC/MS QP2010 GL AQUATIC (60 m 0.25 mm, 1.0 μm) GC 35 C (5 min) 6 C/min 90 C (0 min) 10 C/min 200 C (3 min) 150 C 200 C 200 C EI SIM -d

29 IDL GC/MS IDL 1 IDL (3.00 ng/ml) 1 1 IDL (L) (ng/ml) (ng/ml) (ng/ml) (ng/ml) (ng/ml) (ng/ml) (ng/ml) (ng/ml) (ng/ml) 3.1 (ng/ml) 3.01 (ng/ml) 0.07 IDL (ng/ml)* 0.25 IDL (μg/l) 0.25 S/N 10 CV (%) 2.2 *:IDL = t (n-1, 0.05) σ n-1 2 m/z = 33 m/z = 74 -d 7 m/z = 81 m/z = 50 1 IDL (3.00 ng/ml) 29

30 2 3 面積比 ( 対象物質 / 内標準物質 ) y = x R 2 = (3)(5)(10) (30 ) 濃度比 (50) ( 対象物質 / 内標準物質 (100) ) (ng/ml) ng/ml ng/ml 3 / (ng/ml) (min) % VOC GC GC GC IDL 0.25 μg/l 30

平成26年度化学物質分析法開発報告書

平成26年度化学物質分析法開発報告書 N,N- N,N-Dimethylacetamide Acethyldimethylamine CAS 127-19-5 C 4 H 9 NO 87.12 ~ 87.14 87.68413 163-165 C 1) - 18.59 C 2) 1 mg/l 25 C 3) 3.3 hpa 2 C 4) log P ow -.77 2).9429 2/4 C 1) 3.1 4) 1.31E - 8 atm-m