CN1050770A - 氮含量测定方法 - Google Patents
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title abstract description 23
- 238000005336 cracking Methods 0.000 claims abstract description 30
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000012047 saturated solution Substances 0.000 claims abstract description 16
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000004448 titration Methods 0.000 claims abstract description 11
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 10
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 8
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 8
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 8
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 7
- 238000010521 absorption reaction Methods 0.000 claims abstract description 4
- 229960001759 cerium oxalate Drugs 0.000 claims abstract description 4
- ZMZNLKYXLARXFY-UHFFFAOYSA-H cerium(3+);oxalate Chemical compound [Ce+3].[Ce+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O ZMZNLKYXLARXFY-UHFFFAOYSA-H 0.000 claims abstract description 4
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 claims abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims abstract description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 11
- 229910052736 halogen Inorganic materials 0.000 claims description 10
- 239000005864 Sulphur Substances 0.000 claims description 9
- 150000002367 halogens Chemical class 0.000 claims description 9
- 229910000765 intermetallic Inorganic materials 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 7
- 238000012856 packing Methods 0.000 claims description 7
- 239000005955 Ferric phosphate Substances 0.000 claims description 3
- 238000005443 coulometric titration Methods 0.000 claims description 3
- 229940032958 ferric phosphate Drugs 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910000399 iron(III) phosphate Inorganic materials 0.000 claims description 3
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(ii,iv) oxide Chemical compound O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 229910002026 crystalline silica Inorganic materials 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 abstract description 5
- 239000011593 sulfur Substances 0.000 abstract description 5
- 229910052759 nickel Inorganic materials 0.000 abstract description 4
- 239000003209 petroleum derivative Substances 0.000 abstract description 4
- 150000002894 organic compounds Chemical class 0.000 abstract description 3
- -1 sulfur halide Chemical class 0.000 abstract description 3
- 239000010453 quartz Substances 0.000 abstract description 2
- 150000002736 metal compounds Chemical class 0.000 abstract 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 abstract 1
- 229910000398 iron phosphate Inorganic materials 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 8
- 238000003556 assay Methods 0.000 description 7
- 238000004939 coking Methods 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 238000009835 boiling Methods 0.000 description 4
- WQAQPCDUOCURKW-UHFFFAOYSA-N butanethiol Chemical compound CCCCS WQAQPCDUOCURKW-UHFFFAOYSA-N 0.000 description 4
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- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000007868 Raney catalyst Substances 0.000 description 3
- 229910000564 Raney nickel Inorganic materials 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
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- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- FZERHIULMFGESH-UHFFFAOYSA-N N-phenylacetamide Chemical compound CC(=O)NC1=CC=CC=C1 FZERHIULMFGESH-UHFFFAOYSA-N 0.000 description 1
- FULZLIGZKMKICU-UHFFFAOYSA-N N-phenylthiourea Chemical compound NC(=S)NC1=CC=CC=C1 FULZLIGZKMKICU-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
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- DMLAVOWQYNRWNQ-UHFFFAOYSA-N azobenzene Chemical compound C1=CC=CC=C1N=NC1=CC=CC=C1 DMLAVOWQYNRWNQ-UHFFFAOYSA-N 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
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- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical group [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
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- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
本说明涉及有机化合物和石油产品等的氮含量
测定方法。本方法采用石英裂解管、酸性气体吸收
管、滴定池、微库仑仪和记录仪等组成的微库仑滴定
仪,本方法的特征是在裂解管内镍系催化剂填料段
前,增添适量铬粉作除硫卤剂和烃类裂解催化剂的填
料段,滴定池的参比电极由Pt/难溶的金属化合物
饱和溶液构成,该金属化合物饱和溶液是由二氧化
铈、草酸铈、四氧化三铁、磷酸铁和四氧化三铅中选择
一种配制的。
Description
本发明是关于有机化合物和石油产品等的氮含量测定方法的。
目前,正在采用SY2507-83和ASTM D3431-80石油产品痕量氮的微库仑测定方法。方法概要如下:把样品注入或用进样舟导入通有氢气流的裂解管中,经镍系催化剂填料段,样品中氮化物裂解加氢转化成氨,硫化物和卤化物等所生成的酸性气体被碱性吸附剂吸收,氨进入滴定池中与电解液中的氢离子反应,所消耗的氢离子由电解补充,测量补充氢离子所需电量,按电解定律求出样品的氮含量。
用已知的微库仑测定方法测定N-N键型化合物的氮含量,当裂解管入口温度高于650℃时,因为N-N键型化合物裂解后易形成分子态N2,减少NH3的生成量,所以为了提高氮的回收率,需将裂解管入口温度控制在500℃以下,並需增加氢气的流量。由此可见,已知的微库仑测定方法不适于测定高沸点的N-N键型化合物,其中也包括润滑剂用的一些高沸点的N-N键型添加剂。
用已知的测定方法,在高温裂解时,含硫大于5%的试样,裂解出较多H2S,易使镍系催化剂中毒。将CaO放于催化剂前,虽然CaO能排除硫的干扰,解决了镍系催化剂中毒的问题,但CaO不具有催化烃类裂解为CH4的性能,裂解管内积碳和结焦较多的问题依然存在。在裂解管内壁和催化剂表面积碳和结焦较多,不仅降低催化剂的活性,而且碳和焦质吸附少量的NH3,还使氮的回收率偏低。
为了减少裂解管内积碳和结焦,人们采取改进裂解管结构,适当降低裂解管温度,减少每次进样量等措施。虽然积碳和结焦有所减少,但也未彻底解决问题。
已知的微库仑测定方法采用Pb/PbSO4饱合溶液作滴定池的参比电极。由于参比电极的Pb浸在Na2SO4水溶液中,表面缓慢形成一层不溶盐保护膜,造成电极电位不稳定,其使用寿命仅为数日。采用镀Pb电极时,其镀制技术较难掌握。以前,许多人试图研制一种更稳定的电极取代Pb/PbSO4饱和溶液的参比电极,由于他们局限于从金属/同种金属的难溶盐的范围考虑,因而都未如愿以偿。因此,在现行的微库仑测定方法(标准方法)中,仍采用Pb/PbSO4饱和溶液的参比电极。
本发明的目的是解决现行的氮含量微库仑测定方法(标准方法)存在的上述各方面问题,提供一种不受硫卤干扰,参比电极稳定的氮含量测定方法。
为了达到上述目的,我们研究了阻N2剂、除硫卤剂和烃类裂解催化剂以及新的参比电极。我们用铁粉作阻N2剂,用铬粉作除硫卤剂和烃类裂解催化剂,参比电极由铂和难溶的氧化态和还原态的金属化合物饱和溶液组成,从而完成了本发明。
本发明方法中,进样方式视情况而定,可以采用注射器和/或进样舟。采用进样舟时,在进样舟内加入适量铁粉,该铁粉是N-N键型化合物高温裂解的阻N2剂,它能有效地防止N2的形式,使N-N键型化合物在裂解管入口温度850℃的高温下的氮回收率不低于95%。成功地解决了高沸点N-N键型化合物氮含量测定中存在的问题。我们发现,铬粉在高温下,不仅能除去样品中硫化合物和卤化物的干扰,起除硫卤剂的作用,而且还能降低裂解管内的积碳和结焦量,起烃类裂解催化剂的作用。Pt/难溶的金属化合物饱和溶液作参比电极,不仅制备简便、性能稳定,而且使用寿命长。
本发明的氮含量测定方法,采用同已知的标准方法相类似的仪器,如石英裂解管、酸性气体吸收管、滴定池、微库仑仪和记录仪等组成的微库仑滴定仪。裂解管内装有镍系催化剂,滴定池装有测量一参比电极对,本发明的特征在于在裂解管内镍系催化剂填料段前,增添适量铬粉作除硫卤剂和烃类裂解催化剂的填料段,滴定池的参比电极由Pt/难溶的金属化合物饱和溶液构成,该金属化合物饱和溶液是由二氧化铈、草酸铈、四氧化三铁、磷酸铁和四氧化三铅中选择一种,加入0.2%硫酸钠水溶液配制而成的,最好是把适量二氧化铈粉加入0.2%硫酸钠水溶液中配制的二氧化铈饱和溶液。
本发明所用的镍系催化剂是常用的粒状镍、峰窝状镍、粒状Ni-Pt和Ni-MgO催化剂,最好选择粒状镍催化剂。
本发明所用的铬粉的粒度,虽然並无特别的限定,但最好选择20~80目的。本发明所用的铬粉填料的装入量,虽然也无特别的限定,但最好是充满管长4~6cm的量。用量过少时,不能起有效的除硫卤剂和烃类裂解催化剂的作用;过多时,造成浪费和阻力增大。
本发明的方法,适用范围广泛,主要用于有机化合物和石油产品,也可以用于环境污水的含氮量测定,通常可直接测定含氮量为1~5000PPm的样品。
下面举出本发明的实验例和参照的比较例,具体地说明本发明。
实验例1
采用符合SY2507-83标准方法的微库仑滴定仪,同SY2507-83相类似的操作方法和标样配制方法。並作下述四点改进:
一、裂解管汽化区和催化区的内径都是φ1cm,在催化区用镍粒催化剂填满21cm长的管子后,再用φ0.1mm的镍丝填满1cm长的管子,起分隔铬粉和镍催化剂的作用。将镍催化剂活化之后,装入60~80目的铬粉,充满6cm长的管子。
二、用Pt/二氧化铈饱和溶液作滴定池的参比电极。
三、由于用Pt/二氧化铈饱和溶液作参比电极,库仑仪工作偏压应为-880~-920mV,而所用的DKD-201数字式库仑仪的偏压仅有±750mV,因而在库仑仪输入回路中加上一个固定偏压。
四、采用注射器和装有铁粉的石英舟进样。
裂解炉各段的温度:汽化段为850℃,催化段为800℃,吸收段为300℃。
氢气流量:干燥氢气为50ml/min,增湿氢气为350ml/min。
进样量:5μl/次。
用上述本发明的方法测定7个标样的含氮量。结果列入表1中。
实验例2
采用同实验例1相类似的本发明的方法,测定並计算出7个标样的氮回收率。结果列入表2中。
实验例3
采用同实验例1相类似的本发明的方法,测定配入丁硫醇和三氯甲烷的3个标样的含氮量。结果列入表3中。
实验例4
除了配制参比电极的饱和溶液的难溶的金属化合物不同,並且相应调整偏压以外,其余采用同实验例1相类似的方法,测定7个标样的含氮量。结果列入表4中。
比较例1
除了不用铬粉以外,其余采用同实验例3相类似的方法,测定配入丁硫醇和三氯甲烷的3个标准的含氮量。结果列入表5中。
比较例2
用含氮的商品齿轮油作样品,除了不用铬粉(比较的方法)和用铬粉(本发明的方法)以外,其余采用同实验例1相类似的方法进行实验,观察裂解管内积碳和结焦的情况。结果列入表6中。
由表1~5看出,本发明的方法用于高沸点N-N键型化合物含氮量的测定,也给出满意的结果;不仅可以用于硫含量低于5%,卤素含量低于20%的样品(SY2507-83指定范围),而且还可以用于硫含量高于5%,卤素含量高于20%的样品,通常认为,可以用于硫含量低于20%,卤素含量低于50%的样品含氮量的测定。本发明的方法具有很高的精密度。由表6看出,本发明的方法,在裂解管积碳和结焦的性能上,显著地优于已知的方法。此外,本发明方法的参比电极的使用寿命全部达到3个月以上。
表1
化合物 | 计算值ppm | 测定值ppm | 平均值ppm | 绝对误差ppm | 相对标准偏差% |
乙酰替苯胺 | 152.1 | 151.5 150.8 152.1148.4 147.5 153.2154.4 155.1 154.0 | 151.9 | -0.2 | 1.74 |
对硝基苯按 | 130.9 | 129.9 131.0 128.5128.3 130.4 127.6132.0 134.7 130.9133.6 | 130.7 | -0.2 | 1.75 |
8-羟基喹啉* | 20.4 | 19.3 20.1 19.920.2 20.7 20.220.3 20.9 21.121.0 | 20.4 | 0 | 2.74 |
偶氮苯 | 168.0 | 166.8 168.1 165.9165.5 162.4 161.2162.8 163.7 | 164.6 | -3.4 | 1.45 |
55′-氧撑双苯骈三唑 | 155.5 | 150.2 149.6 149.6149.9 146.9 147.7149.4 144.8 | 148.5 | -7.0 | 1.27 |
续表1
化合物 | 计算值ppm | 测定值ppm | 平均值ppm | 绝对误差ppm | 相对标准偏差% |
苯基硫脲 | 200.6 | 195.7 197.9 198.3194.6 196.1 194.6199.0 195.7 199.0200.9 | 197.2 | -3.4 | 1.07 |
盐酸芐基硫脲 | 191.8 | 188.4 189.9 189.9189.1 182.8 186.9193.9 192.4 | 189.2 | -2.6 | 1.79 |
*进样量为30μl/次
续表4
配制该参比电极的饱和溶液时,(1)和(2)用草酸铈,(3)和(4)用四氧化三铁,(5)和(6)用磷酸铁,(7)用四氧化三铅。
表5
Claims (3)
1、一种氮含量测定方法,采用石英裂解管、酸性气体吸收管、滴定池、微库仑仪和记录仪等组成的微库仑滴定仪,其特征在于在裂解管内镍系催化剂填料段前,增添适量铬粉作除硫卤剂和烃类裂解催化剂的填料段,滴定池的参比电极由Pt/难溶的金属化合物饱和溶液构成,该金属化合物饱和溶液是由二氧化铈、草酸铈、四氧化三铁、磷酸铁和四氧化三铅中选择一种配制的。
2、如权利要求1所述的氮含量测定方法,其特征在于铬粉填料段的装入量为充满管长4~6cm的量。
3、如权利要求1和2所述的任何一种氮含量测定方法,其特征在于滴定池的参比电极由Pt/二氧化铈饱和溶液构成。
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