Chinese Journal of Chromatography ›› 2024, Vol. 42 ›› Issue (1): 92-98.DOI: 10.3724/SP.J.1123.2023.10027
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LEI Jiacheng1, ZHENG Huangrong1, LIU Lu2, LI Weixia1,*()
Received:
2023-10-25
Online:
2024-01-08
Published:
2024-01-10
Supported by:
CLC Number:
LEI Jiacheng, ZHENG Huangrong, LIU Lu, LI Weixia. Simultaneous determination of six nitroaromatic compounds and three anions in environmental matrices using a liquid chromatography-ion chromatography coupled system[J]. Chinese Journal of Chromatography, 2024, 42(1): 92-98.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2023.10027
Stage in | Operation process | Time/min | Left six-way valve | Right six-way valve |
---|---|---|---|---|
A | sample loading to quantitative ring | - | loading | injection |
B | separation of nitroaromatic compounds and anions in C18 column | 0-1.5 | injection | injection |
C | anions enrichment in AG20 column | 1.5-3.0 | injection | loading |
D | determination of nitroaromatic compounds and anions by HPLC and | 3.0-20 | injection | injection |
IC, respectively |
Table 1 Switching status of the two six-way valves in the HPLC-IC system
Stage in | Operation process | Time/min | Left six-way valve | Right six-way valve |
---|---|---|---|---|
A | sample loading to quantitative ring | - | loading | injection |
B | separation of nitroaromatic compounds and anions in C18 column | 0-1.5 | injection | injection |
C | anions enrichment in AG20 column | 1.5-3.0 | injection | loading |
D | determination of nitroaromatic compounds and anions by HPLC and | 3.0-20 | injection | injection |
IC, respectively |
Analyte | Linear range/ (mg/L) | Correlation coefficient (r2) | LOD/ (mg/L) | LOQ/ (mg/L) | RSDs/%(n=5) | |
---|---|---|---|---|---|---|
Retention time | Peak area | |||||
HMX | 0.49-50 | 0.9973 | 0.150 | 0.49 | 0.17 | 4.2 |
RDX | 0.35-50 | 0.9999 | 0.112 | 0.35 | 0.14 | 4.2 |
TNB | 0.31-10 | 0.9931 | 0.089 | 0.31 | 0.15 | 5.0 |
1,3-Dinitrobenzene | 0.29-50 | 0.9996 | 0.085 | 0.29 | 0.14 | 4.2 |
TNT | 0.18-10 | 0.9997 | 0.057 | 0.18 | 0.13 | 4.5 |
2,4-Dinitrotoluene | 0.13-50 | 0.9978 | 0.043 | 0.13 | 0.04 | 3.6 |
Cl- | 0.016-25 | 0.9991 | 0.005 | 0.016 | 0.28 | 5.0 |
N | 0.049-40 | 0.9991 | 0.016 | 0.049 | 0.28 | 3.5 |
N | 0.059-40 | 0.9993 | 0.020 | 0.059 | 0.25 | 1.6 |
Table 2 Linear parameters, limits of detection (LODs), limits of quantification (LOQs), and repeatabilities
Analyte | Linear range/ (mg/L) | Correlation coefficient (r2) | LOD/ (mg/L) | LOQ/ (mg/L) | RSDs/%(n=5) | |
---|---|---|---|---|---|---|
Retention time | Peak area | |||||
HMX | 0.49-50 | 0.9973 | 0.150 | 0.49 | 0.17 | 4.2 |
RDX | 0.35-50 | 0.9999 | 0.112 | 0.35 | 0.14 | 4.2 |
TNB | 0.31-10 | 0.9931 | 0.089 | 0.31 | 0.15 | 5.0 |
1,3-Dinitrobenzene | 0.29-50 | 0.9996 | 0.085 | 0.29 | 0.14 | 4.2 |
TNT | 0.18-10 | 0.9997 | 0.057 | 0.18 | 0.13 | 4.5 |
2,4-Dinitrotoluene | 0.13-50 | 0.9978 | 0.043 | 0.13 | 0.04 | 3.6 |
Cl- | 0.016-25 | 0.9991 | 0.005 | 0.016 | 0.28 | 5.0 |
N | 0.049-40 | 0.9991 | 0.016 | 0.049 | 0.28 | 3.5 |
N | 0.059-40 | 0.9993 | 0.020 | 0.059 | 0.25 | 1.6 |
Analyte | Added/ (mg/L) | Recoveries/% | RSDs/% | Analyte | Added/ (mg/L) | Recoveries/% | RSDs/% | ||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Soil | Water | Soil | Water | Soil | Water | Soil | Water | ||||||||
HMX | 0.22 | 98.27 | 90.83 | 2.7 | 6.7 | 2,4-Dinitrotoluene | 0.56 | 102.11 | 91.34 | 7.3 | 7.4 | ||||
0.56 | 101.98 | 92.07 | 9.3 | 8.2 | 1.25 | 92.92 | 91.47 | 8.0 | 11.3 | ||||||
1.45 | 100.05 | 103.62 | 5.0 | 9.5 | 2.78 | 88.20 | 89.95 | 8.1 | 5.1 | ||||||
RDX | 0.28 | 92.63 | 96.63 | 7.1 | 2.1 | Cl- | 0.12 | 88.61 | 91.67 | 4.1 | 2.8 | ||||
0.56 | 105.38 | 93.96 | 11.5 | 5.3 | 1.25 | 91.73 | 88.43 | 11.0 | 2.4 | ||||||
1.45 | 98.32 | 98.41 | 5.5 | 3.6 | 10.0 | 98.47 | 89.75 | 2.0 | 5.1 | ||||||
TNB | 0.22 | 96.49 | 96.50 | 2.7 | 5.0 | N | 0.25 | 95.18 | 97.92 | 9.5 | 5.1 | ||||
0.45 | 98.25 | 89.89 | 9.9 | 4.5 | 2.50 | 100.88 | 89.37 | 3.1 | 3.7 | ||||||
1.15 | 102.06 | 96.66 | 8.2 | 7.7 | 20.0 | 97.57 | 91.46 | 6.2 | 4.5 | ||||||
1,3-Dinitrobenzene | 0.56 | 91.48 | 92.43 | 7.8 | 9.1 | N | 0.25 | 94.84 | 90.63 | 6.1 | 9.1 | ||||
1.25 | 100.41 | 91.57 | 8.5 | 6.6 | 2.50 | 97.64 | 94.06 | 4.3 | 2.1 | ||||||
2.78 | 98.33 | 94.23 | 11.4 | 8.3 | 20.0 | 89.88 | 91.57 | 8.7 | 2.2 | ||||||
TNT | 0.40 | 99.33 | 96.87 | 7.9 | 9.3 | ||||||||||
0.55 | 103.61 | 90.40 | 7.3 | 4.9 | |||||||||||
1.15 | 102.00 | 94.33 | 5.4 | 4.7 |
Table 3 Spiked recoveries and RSDs of the six nitroaromatic compounds and three anions (n=6)
Analyte | Added/ (mg/L) | Recoveries/% | RSDs/% | Analyte | Added/ (mg/L) | Recoveries/% | RSDs/% | ||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Soil | Water | Soil | Water | Soil | Water | Soil | Water | ||||||||
HMX | 0.22 | 98.27 | 90.83 | 2.7 | 6.7 | 2,4-Dinitrotoluene | 0.56 | 102.11 | 91.34 | 7.3 | 7.4 | ||||
0.56 | 101.98 | 92.07 | 9.3 | 8.2 | 1.25 | 92.92 | 91.47 | 8.0 | 11.3 | ||||||
1.45 | 100.05 | 103.62 | 5.0 | 9.5 | 2.78 | 88.20 | 89.95 | 8.1 | 5.1 | ||||||
RDX | 0.28 | 92.63 | 96.63 | 7.1 | 2.1 | Cl- | 0.12 | 88.61 | 91.67 | 4.1 | 2.8 | ||||
0.56 | 105.38 | 93.96 | 11.5 | 5.3 | 1.25 | 91.73 | 88.43 | 11.0 | 2.4 | ||||||
1.45 | 98.32 | 98.41 | 5.5 | 3.6 | 10.0 | 98.47 | 89.75 | 2.0 | 5.1 | ||||||
TNB | 0.22 | 96.49 | 96.50 | 2.7 | 5.0 | N | 0.25 | 95.18 | 97.92 | 9.5 | 5.1 | ||||
0.45 | 98.25 | 89.89 | 9.9 | 4.5 | 2.50 | 100.88 | 89.37 | 3.1 | 3.7 | ||||||
1.15 | 102.06 | 96.66 | 8.2 | 7.7 | 20.0 | 97.57 | 91.46 | 6.2 | 4.5 | ||||||
1,3-Dinitrobenzene | 0.56 | 91.48 | 92.43 | 7.8 | 9.1 | N | 0.25 | 94.84 | 90.63 | 6.1 | 9.1 | ||||
1.25 | 100.41 | 91.57 | 8.5 | 6.6 | 2.50 | 97.64 | 94.06 | 4.3 | 2.1 | ||||||
2.78 | 98.33 | 94.23 | 11.4 | 8.3 | 20.0 | 89.88 | 91.57 | 8.7 | 2.2 | ||||||
TNT | 0.40 | 99.33 | 96.87 | 7.9 | 9.3 | ||||||||||
0.55 | 103.61 | 90.40 | 7.3 | 4.9 | |||||||||||
1.15 | 102.00 | 94.33 | 5.4 | 4.7 |
Analyte | Surface water samples/(mg/L) | Soil samples/(mg/kg) | ||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|
1 | 2 | 3 | 4 | 5 | 1 | 2 | 3 | 4 | 5 | |||
Cl- | 25.3 | 36.3 | 27.4 | 55.3 | 41.4 | 25.1 | 30.2 | 15.5 | 18.2 | 23.2 | ||
N | - | 0.41 | - | 0.54 | 0.72 | - | 0.56 | 0.63 | 1.50 | - | ||
N | 1.38 | 1.82 | 2.16 | 1.49 | 1.33 | 0.65 | 1.35 | 2.39 | 2.16 | 2.01 |
Table 4 Test results of five surface water samples and five soil samples
Analyte | Surface water samples/(mg/L) | Soil samples/(mg/kg) | ||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|
1 | 2 | 3 | 4 | 5 | 1 | 2 | 3 | 4 | 5 | |||
Cl- | 25.3 | 36.3 | 27.4 | 55.3 | 41.4 | 25.1 | 30.2 | 15.5 | 18.2 | 23.2 | ||
N | - | 0.41 | - | 0.54 | 0.72 | - | 0.56 | 0.63 | 1.50 | - | ||
N | 1.38 | 1.82 | 2.16 | 1.49 | 1.33 | 0.65 | 1.35 | 2.39 | 2.16 | 2.01 |
Fig. 4 (a) HPLC and (b) IC chromatograms of a standard sample and soil sample No. 1 Peak identifications: 1. HMX; 2. RDX; 3. TNB; 4. 1,3-dinitrobenzene; 5. TNT; 6. 2,4-dinitrotoluene; 7. Cl-; 8. N O 2 -; 9. N O 3 -.
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