1,2,4-1,2,4-Trimethylbenzene Pseudocumene 1,3,5-1,3,5-Trimethylbenzene Mesitylene CH 3 CH 3 CH 3 CH 3 CH 3 CH 3 1,2,4-trimethylbenzene 1,3,5-trimethylbenzene CAS 95-63-6 CAS 108-67-8 C 9 H 12 C 9 H 12 mmhg mg/l LogPow 1,2,4 120.2 169171 2.262 57(25 ) 3.63 1,3,5 120.2 164.7 2.48 48.2(25 ) 3.93 The Merck Index Ver.12:2 2001 1,2,4- (Oncorhynchus mykiss) LC 50 9,220 μg/l (Primephales promelas) LC 50 7,720 μg/l (Daphnia magna) 48 h-ec 50 6,140 μg/l (Cancer magister) 96 h-lc 50 5,100 μg/l (Mysidopsis bahia) 96 h-lc 50 2,000 μg/l (Balanus amphitrite niveus) EC 50 9 μg/l
1,3,5- () LD 50 4,3008,642 mg/kg bw () 4 h-lc 50 24,000 mg/m 3 () (Scenedesmus subspicatus) 48 h-ec 50 25,000 μg/l (Carassius auratus) 96 h-lc 50 12,520 μg/l (Daphnia magna) 48 h-lc 50 6,000 μg/l (Balanus amphitrite niveus) LC 50 13 μg/l () (Daphnia magna) 21 d-noec400 μg/l 1,2,4-1,3,5-1 10 ml 1,2,4--d 12 1,3,5--d 12 -GC/MS-SIM 1 1,2,4-AccuStandard 0.2 mg/ml 1,3,5-AccuStandard 0.2 mg/ml 1,2,4--d 12 Medical Isotopes 98% 1,3,5--d 12 Medical Isotopes 98% 2 2 2
18 3 3 10 ml 3g 20 ml 4 1,2,4--d 12 1,3,5--d 12 0.01 mg/ml 1 μl [] 1,2,4-1,3,5-1 ml 10 ml 0.02 mg/ml [] 1 ml 10 ml 2 ng/μl 0.080.10.20.41 ng/μl 5 [] 1,2,4--d 12 1,3,5--d 12 50 mg 50 ml 1 mg/ml 1 ml 100 ml 0.01 mg/ml 5
GC/MS 6890N Agilent Technologies Rtx-624 RESTEK ( 0.25 mm 60 m 1.4 μm) 35 (2 min)10 /min100 5 /min200 (1 min) 150 He ( 1.0 ml/min) 230 EI 70 ev 150 SIM 1,2,4- m/z 120 () m/z 105 () 1,3,5- m/z 120 () m/z 105 () 1,2,4--d 12 m/z 132 1,3,5--d 12 m/z 132 G1888 Agilent Technologies oven 40 Loop 120 Tr.Line 150 GC Cycle Time 25.0 min Vial Eq.Time 15.0 min Pressurize Time 0.20 min Loop Fill Time 0.20 min Loop Eq.Time 0.05 min Injection Time 1.00 min Carrier 16.8 PSI Vial 9.6 PSI 3 g 20 ml 10 ml 10 μl 1 μl -GC/MS
10 ml -GCMS C(μg/L)R Q / V R Q(ng)() V(L) IDL GC/MS IDL 6 IDL IDL (g/ml) (ml) (ml) (g/ml) 1,2,4-0.025 10 10 0.025 1,3,5-0.021 10 10 0.021 MDLMQL 7 MDL MQL (ml) (ml) (μg/l) (μg/l) 1,2,4-10 10 0.031 0.080 1,3,5-10 10 0.044 0.112 1 2 3 3 4 30% 20 ml Agilent Technologies
5 6 IDL 18 3 1 IDL 0.04 ng/ml GCMS 1 (IDL) 1,2,4-1,3,5- (ml) 10 10 (ng/ml) 0.04 0.04 test1 0.0449 0.0442 test2 0.0391 0.0397 test3 0.0491 0.0454 (ng/ml) test4 0.0375 0.0414 test5 0.0398 0.0391 test6 0.0456 0.0316 test7 0.0294 0.0320 (ng/ml) 0.04075 0.03907 (ng/ml) 0.0065 0.0055 CV(%) 16 14 t(n-1,0.05) 1.94 1.94 S/N(0.04 ng/ml) 5.3 7.8 IDL(ng/mL) 0.025 0.021 IDL (ng/ml) 0.025 0.021 IDL=t(n-1,0.05) n-1 2
1 (IDL) SIM 0.04 ng/ml
( 7) MDLMQL 18 3 2 2 (MDL)(MQL) 1,2,4-1,3,5- (ml) 10 10 (ng) 2 2 (μg/l) 0.2 0.2 <0.031 μg/l <0.044 μg/l <0.031 μg/l <0.044 μg/l test1 0.196 0.192 test2 0.205 0.194 test3 0.197 0.225 (μg/l) test4 0.193 0.209 test5 0.208 0.202 test6 0.216 0.209 test7 0.204 0.200 (μg/l) 0.2027 0.2044 (μg/l) 0.0080 0.0112 CV(%) 3.9 5.5 t(n-1,0.05) 1.94 1.94 S/N 36 21 MDL(μg/L) 0.031 0.044 MQL(μg/L) 0.080 0.112 MDL=t(n-1,0.05) n-1 2 MQL= n-1 10 MDL
1 2 10 ml 3g 1,2,4--d 12 1,3,5--d 12 10 ng 1 -GC/MS-SIM 1,2,4- トリメチルヘ ンセ ン 面積比 ( 対象物質 / サロゲート物質 ) 3 y = 1.2956x - 0.0062 2.5 R 2 = 0.9997 2 1.5 1 0.5 0 0 0.5 1 1.5 2 2.5 濃度比 ( 対象物質 / サロゲート物質 ) 面積比 ( 対象物質 / サロゲート物質 ) 1,3,5-トリメチルヘ ンセ ン 3 y = 1.35x - 0.0006 2.5 R 2 = 0.9994 2 1.5 1 0.5 0 0 0.5 1 1.5 2 2.5 濃度比 ( 対象物質 / サロゲート物質 ) 2 1.0 ng/ml 0.082 ng/ml
アバンダンス アバンダンス スキャン 4986 (22.311 min): H2008061904.D\data.ms 105 TIC: H2008061904.D\data.ms 6000 16000 14000 12000 5500 5000 4500 4000 10000 8000 6000 4000 3500 3000 2500 2000 1500 120 2000 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00 24.00 26.00 28.00 時間 --> 1000 77 91 500 44 51 115 58 65 0 35 40 45 50 55 60 65 70 75 80 85 90 95 100105110115120125 m/z--> 3 1,2,4 アバンダンスアバンダンス 18000 TIC: H2008061905.D\data.ms 6500 スキャン 4726 (21.308 min): H2008061905.D\data.ms 105 16000 6000 14000 5500 5000 12000 4500 10000 8000 6000 4000 4000 3500 3000 2500 2000 1500 120 時間 --> 2000 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00 24.00 26.00 28.00 1000 77 500 44 51 91 65 59 115 0 35 40 45 50 55 60 65 70 75 80 85 90 95 100105110115120125 m/z--> 4 1,3,5 5 1,2,4-d 12 6 1,3,5-d 12
() 3 3 1,2,4-1,3,5- (ml) 10 10 (ng) 20 20 (μg/l) 2.0 2.0 (ml) 10 10 (μg/l) <0.031 <0.044 (μg/l) <0.031 <0.044 test1 2.180 2.194 test2 2.172 2.079 (μg/l) test3 2.186 2.132 test4 2.113 2.078 test5 2.033 2.064 (μg/l) 2.137 2.109 (μg/l) 0.0649 0.0538 CV(%) 3.0 2.5 (%) 106-121 109-122 (%) 102-109 103-110 4 4 ph (μg/l) 1 (%) 5 (%) 1,2,4-2.0 103 112 104 5 1,3,5-2.0 109 118 108 1,2,4-2.0 94.3 93.6 98.1 7 1,3,5-2.0 99.4 96.7 103 1,2,4-2.0 101 93.4 102 9 1,3,5-2.0 104 93.3 105
MDL 7 SIM
8 2μg/L SIM
9 SIM
1,2,4-1,3,5-0.1 μg/l 206-0025 6-11-10 TEL042-372-6711 FAX042-372-6700 E-mailshimauchih@jfrl.or.jp 1,2,4-Trimethylbenzene 1,3,5-Trimethylbenzene This method provides the procedures for determining 1,2,4-trimethylbenzene and 1,3,5- trimethylbenzene in water samples employing headspace-gas chromatography/mass spectrometry with selected-ion monitoring (HS-GC/MS-SIM). A 10mL water sample is carefully poured into a 20 ml HS-glass vial already containing 3 g of NaCl. As a surrogate, 1,2,4-trimethylbenzene-d 12 and 1,3,5-trimethylbenzene-d 12 are placed in the glass vial. This vial is closed tightly with a cap and mixed well. The analytes are determined by HS-GC/MS-SIM as the monitoring ion of m/z 120 for the native substances and m/z 132 for the surrogates. The method detection limits (MDL) of 1,2,4-trimethylbenzene and 1,3,5-trimethylbenzene are 0.031μg/L and 0.044 μg/l, respectively. The recoveries of recovery tests using river water samples spiked with 1,2,4-trimethylbenzene and 1,3,5-trimethylbenzene at the concentrations of 2 μg/l were 102-109% and 103-110%, respectively. Water samples Curing salting HS-GC/MS-SIM 10 ml NaCl 3g Internal standards 1,2,4-trimethylbenzen-d 12 & 1,3,5-trimethylbenzen-d 12 ea.10 ng
[1]1,2,4- [2]1,3,5-10 ml 3g 1,2,4--d 12 1,3,5--d 12 10 ng GC/MS-SIM (μg/l) [1] 0.031 [2] 0.044 -GC/MS-SIM GCAgilent 6890 MSAgilent 5973MSD HSAgilent G1888 Rtx-624 60m0.25mm1.4 μm