1、方法原理根据偶氮二异丁腈热分解所析出氮气，量取其体积，换算为偶氮二异丁腈的纯度。测定步骤称取 0.5g 试样置于比重瓶中，加入 10ml 环己酮，将比重瓶接入如图所示之装置，在水准瓶中加入 200ml 水，将 150ml 丙三醇倒入烧杯，将三通阀转向排气阀，调节水准瓶使气体排出，并使量气管内液面处于零位，关闭三通阀，10 分钟后检查零点不变，确认系统无漏气后，开始加热升温至 1355，并保持 10 分钟，使试样分解完全，停止加热，冷却至室温。将水准瓶与量气管液面保持同一水平，读出量气管内的氮气体积，10分钟后再次读数，以两次读数不变或相差不超过 0.3ml 为准，记录氮气体积、大气压和水银温度
2、计所示室温（精确至 0.5） 。结果的表示发气量 V0按下式计算：V0=VK/m式中：V 0 在 20、101325P 条件下的试样发气量,ml/gV 实测试样的发气量，mlK 测定时室温和大气压的换算系数（见附录）m 试样质量,g纯度结果的表示X= （V 0/149.88）100%式中：V 0 在 20，101352Pa 下试样的发气量, ml/g附录 1 气体体积换算成 20，101325Pa（1atm ）状态下的系数室温， 大气压，Pa12 13 14 15 16 17 18 19 20 21 22 23906 667 0.9272 0.9229 0.9185 0.9141 0.9096
3、 0.9057 0.9011 0.8964 0.8923 0.8875 0.8833 0.8784909 333 0.9300 0.9257 0.9213 0.9168 0.9123 0.9084 0.9038 0.8991 0.8950 0.8902 0.8860 0.8810912 000 0.9328 0.9284 0.9240 0.9196 0.9151 0.9111 0.9065 0.9018 0.8977 0.8929 0.8887 0.8837914 667 0.9355 0.9312 0.9268 0.9223 0.9178 0.9139 0.9092 0.9405 0.900
4、4 0.8956 0.8913 0.8864917 333 0.9383 0.9339 0.9295 0.9250 0.9205 0.9166 0.9119 0.9072 0.9031 0.8983 0.8940 0.8890920 000 0.9411 0.9367 0.9323 0.9278 0.9233 0.9193 0.9146 0.9099 0.9058 0.9009 0.8967 0.8917922 667 0.9438 0.9395 0.9350 0.9305 0.9260 0.9220 0.9174 0.9126 0.9085 0.9036 0.8994 0.8944925 3
5、33 0.9466 0.9422 0.9378 0.9332 0.9287 0.9248 0.9201 0.9153 0.9112 0.9063 0.9020 0.8970928 000 0.9494 0.9450 0.9405 0.9360 0.9314 0.9275 0.9228 0.9180 0.9139 0.9090 0.9047 0.8997930 667 0.9522 0.9477 0.9433 0.9387 0.9342 0.9302 0.9255 0.9207 0.9166 0.9117 0.9074 0.9024933 333 0.9549 0.9505 0.9460 0.9
6、415 0.9639 0.9329 0.9282 0.9234 0.9193 0.9144 0.9101 0.9050936 000 0.9577 0.9533 0.9488 0.9442 0.9396 0.9356 0.9309 0.9261 0.9220 0.9170 0.9127 0.9077938 667 0.9604 0.9560 0.9515 0.9470 0.9424 0.9384 0.9336 0.9288 0.9247 0.9197 0.9154 0.9104941 333 0.9632 0.9588 0.9543 0.9497 0.9451 0.9411 0.9363 0.
7、9315 0.9274 0.9224 0.9181 0.9130944 000 0.9660 0.9615 0.9570 0.9524 0.9478 0.9438 0.9391 0.9342 0.9301 0.9251 0.9208 0.9157946 667 0.9687 0.9643 0.9598 0.9552 0.9508 0.9465 0.9418 0.9369 0.9328 0.9278 0.9234 0.9183949 333 0.9715 0.9671 0.9625 0.9579 0.9533 0.9493 0.9445 0.9396 0.9355 0.9304 0.9261 0
8、.9210952 000 0.9743 0.9698 0.9653 0.9607 0.9560 0.9520 0.9472 0.9423 0.9381 0.9331 0.9288 0.9237954 667 0.9771 0.9726 0.9680 0.9634 0.9588 0.9547 0.9499 0.9451 0.9408 0.9358 0.9315 0.9263957 333 0.9799 0.9753 0.9708 0.9661 0.9615 0.9574 0.9526 0.9478 0.9435 0.9385 0.9342 0.9220960 000 0.9826 0.9781
9、0.9735 0.9689 0.9642 0.9601 0.9553 0.9505 0.9462 0.9412 0.9368 0.9317962 667 0.9854 0.9809 0.9763 0.9716 0.9669 0.9629 0.9580 0.9532 0.9489 0.9439 0.9395 0.9343965 333 0.9882 0.9836 0.9790 0.9744 0.9697 0.9656 0.9608 0.9559 0.9516 0.9465 0.9422 0.9370968 000 0.9909 0.9864 0.9818 0.9771 0.9724 0.9683
10、 0.9635 0.9586 0.9543 0.9492 0.9449 0.9397970 667 0.9937 0.9891 0.9845 0.9798 0.9751 0.9710 0.9662 0.9613 0.9570 0.9519 0.9475 0.9423附录 2 气体体积换算成 20，101325Pa（1atm ）状态下的系数室温， 大气压，Pa24 25 26 27 28 29 30 31 32 33 34 35906 667 0.8740 0.8689 0.8643 0.8590 0.8543 0.8495 0.8439 0.8389 0.8338 0.8285 0.82259
11、09 333 0.8767 0.8715 0.8670 0.8617 0.8569 0.8521 0.8465 0.8415 0.8364 0.8311 0.8251912 000 0.8793 0.8742 0.8696 0.8643 0.8596 0.8547 0.8491 0.8441 0.8390 0.8337 0.8277914 667 0.8820 0.8768 0.8722 0.8669 0.8622 0.8573 0.8517 0.8467 0.8415 0.8363 0.8302917 333 0.8846 0.8795 0.8749 0.8696 0.8648 0.8600
12、 0.8544 0.8493 0.8441 0.8389 0.8328920 000 0.8873 0.8821 0.8775 0.8722 0.8674 0.8626 0.8570 0.8519 0.8467 0.8414 0.8354922 667 0.8900 0.8848 0.8802 0.8748 0.8701 0.8652 0.8596 0.8545 0.8493 0.8440 0.8380925 333 0.8926 0.8874 0.8828 0.8775 0.8727 0.8678 0.8622 0.8571 0.8519 0.8466 0.8405928 000 0.895
13、3 0.8901 0.8854 0.8801 0.8753 0.8704 0.8648 0.8597 0.8545 0.8492 0.8431930 667 0.8979 0.8927 0.8881 0.8827 0.8779 0.8730 0.8674 0.8623 0.8571 0.8518 0.8457933 333 0.9006 0.8953 0.8907 0.8853 0.8805 0.8756 0.8700 0.8649 0.8597 0.8543 0.8482936 000 0.9032 0.8980 0.8934 0.8880 0.8832 0.8783 0.8720 0.86
14、75 0.8622 0.8569 0.8508938 667 0.9059 0.9006 0.8960 0.8905 0.8858 0.8809 0.8752 0.8701 0.8647 0.8595 0.8534941 333 0.9086 0.9033 0.8986 0.8932 0.8884 0.8835 0.8778 0.8727 0.8674 0.8621 0.8559944 000 0.9112 0.9059 0.9013 0.8959 0.8910 0.8861 0.8804 0.8752 0.8700 0.8647 0.8585946 667 0.9139 0.9086 0.9
15、039 0.8985 0.8936 0.8887 0.8830 0.8778 0.8726 0.8672 0.8611949 333 0.9165 0.9112 0.9066 0.9011 0.8963 0.8913 0.8856 0.8804 0.8752 0.8698 0.8637952 000 0.9192 0.9139 0.9092 0.9038 0.8989 0.8939 0.8882 0.8830 0.8778 0.8724 0.8662954 667 0.9218 0.9165 0.9118 0.9064 0.9015 0.8966 0.8908 0.8856 0.8804 0.
16、8750 0.8688957 333 0.9245 0.9192 0.9145 0.9090 0.9041 0.8992 0.8934 0.8882 0.8830 0.8776 0.8714960 000 0.9272 0.9218 0.9171 0.9116 0.9068 0.9018 0.8960 0.8908 0.8855 0.8801 0.8740962 667 0.9298 0.9245 0.9198 0.9143 0.9094 0.9044 0.8986 0.8934 0.8881 0.8827 0.8765965 333 0.9325 0.9271 0.9224 0.9169 0
17、.9120 0.9070 0.9012 0.8960 0.8907 0.8853 0.8791968 000 0.9351 0.9298 0.9250 0.9195 0.9146 0.9096 0.9038 0.8986 0.8933 0.8879 0.8816970 667 0.9378 0.9324 0.9277 0.9222 0.9172 0.9122 0.9064 0.9012 0.8959 0.8905 0.8842附录 3 气体体积换算成 20，101325Pa（1atm ）状态下的系数室温， 大气压，Pa 12 13 14 15 16 17 18 19 20 21 22 2397
18、3 333 0.9965 0.9919 0.9873 0.9826 0.9779 0.9738 0.9689 0.9640 0.9597 0.9546 0.9502 0.9450976 000 0.9992 0.9947 0.9900 0.9853 0.9806 0.9765 0.9716 0.9667 0.9624 0.9573 0.9529 0.9477978 667 1.0020 0.9974 0.9928 0.9881 0.9833 0.9792 0.9743 0.9694 0.9651 0.9599 0.9556 0.9503981 333 1.0048 1.0002 0.9955
19、0.9908 0.9861 0.9819 0.9770 0.9721 0.9678 0.9626 0.9582 0.9530984 000 1.0076 1.0030 0.9983 0.9935 0.9888 0.9846 0.9797 0.9748 0.9705 0.9653 0.9609 0.9557986 667 1.0103 1.0057 1.0010 0.9963 0.9915 0.9874 0.9824 0.9775 0.9732 0.9680 0.9636 0.9583989 333 1.0131 1.0085 1.0038 0.9990 0.9943 0.9901 0.9852
20、 0.9802 0.9759 0.9707 0.9663 0.9610992 000 1.0159 1.0112 1.0065 1.0018 0.9970 0.9928 0.9879 0.9829 0.9786 0.9732 0.9689 0.9637994 667 1.0186 1.0140 1.0093 1.0045 0.9997 0.9955 0.9906 0.9856 0.9812 0.9761 0.9716 0.9663997 333 1.0214 1.0168 1.0120 1.0072 1.0024 0.9983 0.9933 0.9883 0.9839 0.9788 0.974
21、3 0.9690100 000 1.0242 1.0195 1.0148 1.0100 1.0052 1.0010 0.9960 0.9910 0.9866 0.9815 0.9770 0.9717100 267 1.0269 1.0223 1.0175 1.0127 1.0079 1.0037 0.9987 0.9937 0.9893 0.9842 0.9796 0.9743100 533 1.0297 1.0250 1.0203 1.0456 1.0106 1.0064 1.0014 0.9964 0.9920 0.9869 0.9823 0.9770100 800 1.0325 1.02
22、78 1.0230 1.0182 1.0134 1.0091 1.0041 0.9991 0.9947 0.9895 0.9850 0.9797101 067 1.0353 1.0306 1.0258 1.0209 1.0161 1.0119 1.0069 1.0018 0.9974 0.9922 0.9877 0.9823101 325 1.0380 1.0333 1.0285 1.0237 1.0188 1.0146 1.0096 1.0045 1.0001 0.9949 0.9903 0.9850101 600 1.0408 1.0361 1.0313 1.0264 1.0216 1.0
23、173 1.0123 1.0072 1.0028 0.9976 0.9930 0.9877101 867 1.0436 1.0388 1.0340 1.0292 1.0243 1.0200 1.0150 1.0099 1.0055 1.0003 0.9957 0.9903102 133 1.0463 1.0416 1.0368 1.0319 1.0270 1.0228 1.0177 1.0126 1.0082 1.0030 0.9984 0.9930102 400 1.0491 1.0444 1.0395 1.0346 1.0298 1.0255 1.0204 1.0153 1.0109 1.
24、0056 1.0011 0.9957102 667 1.0519 1.0471 1.0423 1.0374 1.0325 1.0282 1.0231 1.0180 1.0136 1.0083 1.0037 0.9983102 933 1.0546 1.0499 1.0450 1.0401 1.0352 1.0309 1.0258 1.0207 1.0163 1.0110 1.0064 1.0010103 200 1.0574 1.0526 1.0478 1.0429 1.0379 1.0336 1.0286 1.0234 1.0190 1.0137 1.0091 1.0037103 467 1
25、.0602 1.0554 1.0505 1.0456 1.0407 1.0364 1.0313 1.0261 1.0217 1.0164 1.0118 1.0063103 733 1.0630 1.0582 1.0533 1.0483 1.0434 1.0391 1.0340 1.0288 1.0244 1.0190 1.0144 1.0090104 000 1.0657 1.0609 1.0560 1.0511 1.0461 1.0418 1.0367 1.0315 1.0270 1.0217 1.0171 1.0117附录 4 气体体积换算成 20，101325Pa（1atm ）状态下的系
26、数室温， 大气压，Pa24 25 26 27 28 29 30 31 32 33 34 35973 333 0.9405 0.9351 0.9303 0.9248 0.9199 0.9149 0.9090 0.9038 0.8985 0.8930 0.8868976 000 0.9431 0.9377 0.9330 0.9274 0.9225 0.9175 0.9116 0.9064 0.9011 0.8956 0.8894978 667 0.9458 0.9404 0.9356 0.9301 0.9251 0.9201 0.9142 0.9090 0.9037 0.8982 0.891998
27、1 333 0.9484 0.9430 0.9382 0.9327 0.9277 0.9227 0.9168 0.9116 0.9062 0.9008 0.8945984 000 0.9511 0.9457 0.9409 0.9353 0.9304 0.9253 0.9195 0.9142 0.9088 0.9034 0.8971986 667 0.9537 0.9483 0.9435 0.9379 0.9330 0.9279 0.9221 0.9168 0.9114 0.9059 0.8996989 333 0.9564 0.9510 0.9462 0.9406 0.9356 0.9305
28、0.9247 0.9194 0.9140 0.9085 0.9022992 000 0.9511 0.9536 0.9488 0.9432 0.9382 0.9331 0.9273 0.9220 0.9166 0.9111 0.9048994 667 0.9617 0.9563 0.9514 0.9458 0.9408 0.9358 0.9299 0.9246 0.9192 0.9137 0.9073997 333 0.9644 0.9589 0.9541 0.9485 0.9435 0.9384 0.9325 0.9272 0.9218 0.9163 0.9099100 000 0.9670
29、 0.9615 0.9567 0.9511 0.9461 0.9410 0.9351 0.9298 0.9244 0.9188 0.9125100 267 0.9697 0.9642 0.9594 0.9537 0.9487 0.9436 0.9377 0.9324 0.9269 0.9214 0.9151100 533 0.9723 0.9668 0.9620 0.9564 0.9513 0.9462 0.9403 0.9350 0.9295 0.9240 0.9176100 800 0.9750 0.9695 0.9646 0.9590 0.9540 0.9488 0.9429 0.937
30、5 0.9321 0.9266 0.9202101 067 0.9777 0.9721 0.9673 0.9616 0.9566 0.9514 0.9455 0.9401 0.9347 0.9292 0.9228101 325 0.9803 0.9748 0.9699 0.9642 0.9592 0.9541 0.9481 0.9421 0.9373 0.9317 0.9253101 600 0.9830 0.9774 0.9726 0.9669 0.9618 0.9567 0.9507 0.9453 0.9399 0.9343 0.9279101 867 0.9856 0.9801 0.97
31、52 0.9695 0.9644 0.9593 0.9533 0.9479 0.9425 0.9369 0.9305102 133 0.9883 0.9827 0.9778 0.9721 0.9671 0.9619 0.9559 0.9505 0.9451 0.9395 0.9330102 400 0.9910 0.9854 0.9805 0.9748 0.9697 0.9645 0.9585 0.9531 0.9477 0.9421 0.9356102 667 0.9936 0.9880 0.9831 0.9774 0.9723 0.9671 0.9611 0.9557 0.9502 0.9
32、446 0.9382102 933 0.9963 0.9907 0.9858 0.9800 0.9750 0.9697 0.9637 0.9583 0.9528 0.9472 0.9408103 200 0.9989 0.9933 0.9884 0.9827 0.9776 0.9724 0.9663 0.9609 0.9554 0.9498 0.9433103 467 1.0016 0.9960 0.9910 0.9853 0.9802 0.9750 0.9689 0.9635 0.9580 0.9524 0.9459103 733 1.0042 0.9986 0.9937 0.9879 0.9828 0.9776 0.9715 0.9661 0.9606 0.9550 0.9485104 000 1.0069 1.0013 0.9963 0.9905 0.9854 0.9802 0.9741 0.9687 0.9632 0.9575 0.9510
