马拉硫磷实验

马拉硫磷实验
马拉硫磷保温反应液：未稀释进样0.1uL
色谱柱Rtx-1，柱温110度，5度/min 到150度，20度/min 到250度，保持18min 。

气化和检测温度：250度
棕色：保温9h ，蓝色12h ，玫瑰色14h ，黑色16h ，（均为44#保温反应液加入少量丙酮）绿色：二乙酯反应液48#
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15.0
min
0.0
0.10.20.30.40.50.60.70.80.91.01.11.21.31.41.5uV(x10,000,000)2.0
3.0
4.0
5.0
6.0
7.0
8.0
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min
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0.10.20.30.40.50.60.70.80.91.01.11.21.31.41.51.61.71.8uV(x1,000,000)3.6
3.7
3.8
3.9
4.0
4.1
4.2
4.3
4.4
4.5
4.6
4.7
min
0.0
0.51.01.52.02.53.03.54.04.55.05.56.0uV(x10,000)
uV(x10,000)
3.00
2.75
2.50
2.25
2.00
1.75
1.50
1.25
1.00
0.75
0.50
0.25
0.00
1.5
2.0 2.5
3.0 3.5
4.0 4.5
5.0 5.5
6.0 6.5
7.07.5min
uV(x10,000)
3.50
3.25
3.00
2.75
2.50
2.25
2.00
1.75
1.50
1.25
1.00
0.75
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0.00
44#保温反应液扣除丙酮峰后归一化结果
9h
峰号保留时间组分名面积面积%
1 1.779 398196.5 3.2365
2 2.148 4349.2 0.0353
3 2.562 9610.5 0.0781
4 2.631 5021.0 0.0408
5 3.167 硫化物316179.5 2.5699
6 3.322 2227.4 0.0181
7 3.719 4634.9 0.0377
8 3.929 二乙酯4748.2 0.0386
9 4.138 90224.0 0.7333
10 4.210 111069.2 0.9028
11 5.552 2338.0 0.0190
12 6.208 8430.4 0.0685
13 6.297 27271.8 0.2217
14 6.638 263501.9 2.1417
15 7.049 10883.3 0.0885
16 8.235 3434.5 0.0279
17 9.087 3971.7 0.0323
18 9.250 14492.1 0.1178
19 11.376 2273.1 0.0185
20 11.942 5147.2 0.0418
21 12.442 3523.0 0.0286
22 12.568 4635.7 0.0377
23 13.026 219178.3 1.7814
24 13.450 232555.0 1.8902
25 13.716 马拉硫磷10266349.8 83.4432
26 13.872 51275.6 0.4168
27 14.348 70933.4 0.5765
28 14.518 3467.4 0.0282
29 14.597 20886.8 0.1698
30 14.675 67403.5 0.5478
31 15.122 55259.8 0.4491
32 17.288 7600.8 0.0618
33 17.512 2749.6 0.0223
34 17.598 2462.3 0.0200
35 21.009 4608.7 0.0375
36 21.220 2504.6 0.0204 12h
峰号保留时间组分名面积面积%
1 1.779 206823.9 1.6293
2 2.149 4582.
3 0.0361
3 2.562 9702.
4 0.0764
4 2.631 5256.1 0.0414
5 3.167 硫化物337940.
6 2.6621
6 3.719 3852.4 0.0303
7 3.927 二乙酯2078.6 0.0164
8 4.136 76259.1 0.6007
9 4.209 37046.6 0.2918
10 6.207 6507.6 0.0513
11 6.295 27784.9 0.2189
12 6.636 238739.9 1.8807
13 7.047 8747.0 0.0689
14 8.232 2079.8 0.0164
15 9.085 4205.1 0.0331
16 9.249 14444.8 0.1138
17 9.896 4811.7 0.0379
18 11.376 2008.2 0.0158
19 11.942 5670.0 0.0447
20 12.447 2360.8 0.0186
21 12.566 3318.0 0.0261
22 13.033 227106.9 1.7890
23 13.455 239882.9 1.8897
24 13.722 马拉硫磷10928360.4 86.0885
25 13.875 55357.5 0.4361
26 13.984 2092.0 0.0165
27 14.349 49444.9 0.3895
28 14.528 4168.3 0.0328
29 14.599 26917.4 0.2120
30 14.677 78393.3 0.6175
31 15.124 59511.4 0.4688
32 17.288 3861.9 0.0304
33 17.513 3450.3 0.0272
34 17.599 3059.1 0.0241
35 21.008 5539.7 0.0436
36 21.232 2972.9 0.0234 14h
峰号保留时间组分名面积面积%
1 1.779 200910.5 1.6299
2 2.149 3731.0 0.0303
3 2.562 9568.2 0.0776
4 2.631 5068.1 0.0411
5 3.168 硫化物356492.7 2.8921
6 3.718 3434.0 0.0279
7 3.927 二乙酯2881.9 0.0234
8 4.136 70413.3 0.5712
9 4.208 55855.4 0.4531
10 6.207 4663.5 0.0378
11 6.296 26889.6 0.2181
12 6.638 259697.2 2.1068
13 7.050 9380.9 0.0761
14 9.087 3809.3 0.0309
15 9.250 17077.9 0.1385
16 9.896 5767.9 0.0468
17 11.376 2424.8 0.0197
18 11.941 5274.0 0.0428
19 12.565 3493.6 0.0283
20 13.030 228159.7 1.8510
21 13.455 221844.6 1.7997
22 13.718 马拉硫磷10578980.2 85.8225
23 13.873 52303.3 0.4243
24 14.347 48796.1 0.3959
25 14.528 2697.3 0.0219
26 14.597 20076.6 0.1629
27 14.673 56045.2 0.4547
28 15.122 52454.8 0.4255
29 17.288 4363.2 0.0354
30 17.513 3041.7 0.0247
31 17.597 2782.6 0.0226
32 21.004 5265.0 0.0427
33 21.230 2942.9 0.0239 16h
峰号保留时间组分名面积面积%
1 1.780 216015.
2 1.6736
2 2.150 3915.6 0.0303
3 2.562 10154.5 0.0787
4 2.632 5145.9 0.0399
5 3.168 硫化物363619.1 2.8172
6 3.719 4235.9 0.0328
7 3.927 二乙酯2255.9 0.0175
8 4.137 78379.2 0.6072
9 4.210 35616.5 0.2759
10 6.208 6120.7 0.0474
11 6.296 27896.0 0.2161
12 6.638 271308.8 2.1020
13 7.050 13019.8 0.1009
14 8.234 2637.3 0.0204
15 9.087 4661.1 0.0361
16 9.249 14985.9 0.1161
17 9.896 5493.4 0.0426
18 11.377 4005.5 0.0310
19 11.942 5462.8 0.0423
20 12.442 2569.3 0.0199
21 12.567 2805.0 0.0217
22 13.035 273711.8 2.1206
23 13.454 234030.1 1.8132
24 13.723 马拉硫磷11007397.6 85.2807
25 13.876 55493.5 0.4299
26 13.985 2433.5 0.0189
27 14.350 59596.2 0.4617
28 14.533 3423.7 0.0265
29 14.601 28110.2 0.2178
30 14.677 73680.7 0.5708
31 15.125 68199.6 0.5284
32 17.289 5546.9 0.0430
33 17.513 3241.3 0.0251
34 17.599 2902.8 0.0225
35 21.012 5931.9 0.0460 36 21.229 3253.9 0.0252 二乙酯反应液（未扣除前面乙醇与苯） 峰号 保留时间 组分名 面积 面积% 1 1.642 421998.4 1.3358 2 1.716 4173.9 0.0132 3 1.777 18618326.0 58.9345 4 1.874 2409.2 0.0076 5 1.986 7105.2 0.0225 6 2.189 2225.2 0.0070 7 2.635 8980.8 0.0284 8 3.225 6136.5 0.0194 9 4.053 二乙酯
12150629.3 38.4616 10 4.234 94646.7 0.2996 11 4.336 229128.4 0.7253 12 5.238 7686.9 0.0243 13 6.299 23097.4 0.0731 14 12.952 2238.6 0.0071 15 13.535 12779.7
0.0405
二乙酯成品
2.5
5.0
7.5
10.0
12.5
15.0
17.5
20.0
22.5
25.0
27.5
30.0min
-0.25
0.000.250.500.75
1.001.251.501.75
2.002.252.50
2.75
3.00uV(x1,000,000)0.0
25.050.075.0100.0125.0
150.0175.0200.0225.0250.0
275.0300.0325.0350.0
375.0400.0425.0C 色谱
峰号 保留时间 组分名
面积 面积% 1 1.641 56163.7 0.2630 2 1.778 192064.1 0.8993 3 2.276 2370.1 0.0111 4 2.633 5183.9 0.0243 5 3.227 5641.7 0.0264 6 4.100 二乙酯 20841422.7 97.5878 7 4.254 98955.3 0.4633 8 4.326 96966.6 0.4540 9 4.788 10106.7 0.0473 10 5.124 3266.0 0.0153 11 5.243 4320.6 0.0202 12 6.302 37044.7 0.1735 13
13.536
3085.8
0.0144
二乙酯反应液48#与纯品二乙酯对比
黑色：二乙酯反应液红色：纯品二乙酯随着含量增加二乙酯出峰时间拖后，但刚开始出峰时间不变
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min
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0.250.500.75
1.00
1.251.501.75
2.002.252.502.75
3.003.253.503.75
4.004.25
4.50uV(x10,000)0.02
5.050.075.0
100.0
125.0
150.0175.0200.0225.0250.0275.0300.0325.0350.0375.0400.0
425.0C 色谱
46#合成保温
棕色：保温9h ，蓝色12h ，玫瑰色14h ，黑色16h ，
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0.10.20.30.40.50.60.70.80.91.01.11.21.31.41.51.6uV(x10,000,000)1.5
2.5
3.0
4.0
4.5
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6.5
0.00
0.250.500.751.001.251.501.752.002.252.502.753.003.253.503.754.004.25uV(x10,000)1.0
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min
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0.250.500.751.001.251.501.752.002.252.50uV(x1,000,000)
uV(x10,000)
4.25
4.00
3.75
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3.00
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0.75
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7.0
8.0
9.010.011.012.013.014.015.016.017.018.0min
uV(x10,000)
3.00
2.75
2.50
2.25
2.00
1.75
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0.75
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3.0 3.1 3.2 3.3 3.4 3.5 3.6 3.7 3.8 3.9
4.0 4.1 4.2 4.3 4.4 4.5 4.6min
uV(x100,000)
1.4
1.3
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1.0
0.9
0.8
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0.3
0.2
0.1
0.0
1.75
2.00 2.75
3.00 3.50 3.75
4.00
9h
峰号保留时间组分名面积面积%
1 1.781 177522.8 1.3928
2 2.151 7859.
3 0.0617
3 2.565 9781.2 0.0767
4 2.634 5039.9 0.0395
5 3.171 硫化物360984.5 2.8322
6 3.721 3000.9 0.0235
7 3.931 二乙酯3188.9 0.0250
8 4.140 70490.3 0.5531
9 4.212 80543.5 0.6319
10 6.214 3195.5 0.0251
11 6.301 27688.7 0.2172
12 6.642 233022.0 1.8282
13 7.056 11614.8 0.0911
14 8.241 2053.2 0.0161
15 9.091 3507.9 0.0275
16 9.252 10126.7 0.0795
17 9.899 9432.2 0.0740
18 11.379 2339.3 0.0184
19 11.943 5505.4 0.0432
20 12.446 2544.0 0.0200
21 12.568 4703.9 0.0369
22 13.036 271638.7 2.1312
23 13.459 239469.0 1.8788
24 13.726 马拉硫磷10926249.5 85.7253
25 13.877 54389.2 0.4267
26 13.987 2449.8 0.0192
27 14.351 55704.4 0.4370
28 14.537 2840.4 0.0223
29 14.601 23756.1 0.1864
30 14.677 59578.0 0.4674
31 15.127 57442.8 0.4507
32 17.292 3775.9 0.0296
33 17.517 2485.0 0.0195
34 17.603 2220.8 0.0174
35 21.012 6046.3 0.0474
36 21.233 3463.0 0.0272 12h
峰号保留时间组分名面积面积%
1 1.781 167790.8 1.3220
2 1.94
3 2365.1 0.0186
3 2.151 8700.2 0.0685
4 2.564 9767.3 0.0770
5 2.634 5247.5 0.0413
6 3.169 硫化物343416.5 2.7057
7 3.721 3022.1 0.0238
8 3.928 二乙酯2234.7 0.0176
9 4.139 77720.6 0.6124
10 4.211 50221.0 0.3957
11 6.210 3949.0 0.0311
12 6.298 27589.7 0.2174
13 6.639 252336.9 1.9881
14 7.053 10791.3 0.0850
15 8.236 2150.6 0.0169
16 9.088 3909.5 0.0308
17 9.250 10482.6 0.0826
18 9.897 9088.0 0.0716
19 11.377 2844.4 0.0224
20 11.943 5375.7 0.0424
21 12.446 2539.3 0.0200
22 12.567 3674.9 0.0290
23 13.035 273961.6 2.1585
24 13.459 237607.6 1.8721
25 13.723 马拉硫磷10882217.3 85.7396
26 13.876 53872.4 0.4245
27 13.984 2410.8 0.0190
28 14.350 61957.7 0.4882
29 14.532 2930.0 0.0231
30 14.600 26070.9 0.2054
31 14.676 64149.6 0.5054
32 15.125 63676.1 0.5017
33 17.289 3749.3 0.0295
34 17.514 2477.7 0.0195
35 17.601 2195.6 0.0173
36 21.007 6071.8 0.0478
37 21.227 3602.8 0.0284 14h
峰号保留时间组分名面积面积%
1 1.781 166082.1 1.2940
2 1.942 2142.1 0.0167
3 2.151 9148.0 0.0713
4 2.564 9943.
5 0.0775
5 2.634 5169.5 0.0403
6 3.169 硫化物341556.
7 2.6611
7 3.720 3302.8 0.0257
8 3.929 二乙酯2138.6 0.0167
9 4.139 80392.0 0.6263
10 4.211 39521.9 0.3079
11 6.210 4965.4 0.0387
12 6.297 27540.3 0.2146
13 6.639 253247.5 1.9731
14 7.053 10591.0 0.0825
16 9.087 3933.5 0.0306
17 9.249 10076.8 0.0785
18 9.896 11970.5 0.0933
19 11.378 3841.1 0.0299
20 11.942 5356.6 0.0417
21 12.442 2625.1 0.0205
22 12.567 3809.5 0.0297
23 13.033 276796.7 2.1565
24 13.459 233897.4 1.8223
25 13.723 11017779.4 85.8404
26 13.875 55121.0 0.4295
27 13.985 2540.3 0.0198
28 14.350 68609.3 0.5345
29 14.600 27188.2 0.2118
30 14.677 67827.6 0.5285
31 15.126 67358.6 0.5248
32 17.290 3557.2 0.0277
33 17.514 2497.4 0.0195
34 17.600 2242.0 0.0175
35 21.011 6393.1 0.0498
36 21.231 3670.3 0.0286 16h
峰号保留时间组分名面积面积%
1 1.781 180415.7 1.3906
2 2.150 9593.0 0.0739
3 2.562 10163.3 0.0783
4 2.632 4871.3 0.0375
5 3.167 硫化物323888.9 2.4964
6 3.319 2880.1 0.0222
7 3.718 3392.1 0.0261
8 3.928 二乙酯2463.2 0.0190
9 4.138 116823.3 0.9004
10 4.211 33756.7 0.2602
11 5.549 2934.4 0.0226
12 6.209 6384.9 0.0492
13 6.297 28224.6 0.2175
14 6.642 318919.3 2.4581
15 7.052 10518.6 0.0811
16 8.235 3782.4 0.0292
17 9.088 4168.4 0.0321
18 9.250 10497.2 0.0809
19 9.897 12700.1 0.0979
21 11.376 3409.6 0.0263
22 11.942 5327.0 0.0411
23 12.305 2326.2 0.0179
24 12.447 2081.7 0.0160
25 12.567 2581.0 0.0199
26 13.035 254707.8 1.9632
27 13.455 242279.0 1.8674
28 13.724 马拉硫磷11046687.2 85.1436
29 13.877 55558.2 0.4282
30 13.985 2429.9 0.0187
31 14.354 89890.7 0.6928
32 14.601 25377.3 0.1956
33 14.678 66434.4 0.5121
34 15.127 67004.8 0.5164
35 17.292 7998.8 0.0617
36 17.515 2061.5 0.0159
37 21.009 5844.6 0.0450
38 21.232 3343.9 0.0258。