简今�/span>

橡胶和轮胎用于各种工业和不同的终端产品。橡胶是制造天然或合成轮胎的主要原材料。天然橡胶主要是碳氢化合物，是热塑性的。为了消除异味等不良特性，橡胶用硫、促进剂和抗氧化剂处理，这些物质通过减少空气中氧（或臭氧）引起的劣化而延长橡胶产品的寿命。轮胎橡胶的另一个主要成分是炭黑，用于增加硬度、拉伸强度和耐磨性。严格的质量控制从原材料供应商开始。轮胎制造商要求原材料在交付工厂前进行质量检验、�/span>

生产过程中使用的试验之一是测定橡胶的元素组成。硫含量是橡胶制品质量控制中最重要的参数之一，是反映轮胎硫晕现象的主要指标，是轮胎质量损失的重要指标。为了进行质量控制，需要测定橡胶中的有机元素。采用燃烧法测定碳、氢、氮、硫和氧、�/span>

赛默飞世尓�/span>℡�/span>FlashSmart℡�/span>元素分析仪（国�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;" data-x-flag="16_49">1）可以定量测定橡胶和轮胎中的碳、氢、氮、硫和氧、�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;" data-x-flag="16_49">FlashSmart℡�/span>元素分析仪基于样品的动态燃烧，在一次分析过程中提供自动的对CHNS/O进行测定，其中氧的测定是通过热裂解的方式测定、�/span>

国�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">1：赛默飞世尔℡�/span>FlashSmart℡�/span>元素分析�?/span>

本文提供了橡胶和轮胎�?span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">CHNS/O测定的数据，以显礹�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">FlashSmart℡�/span>元素分析仪的性能、�/span>

方法

对于CHNS测定＋�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">FlashSmart℡�/span>元素分析仪使用动态闪烧法燃烧仪器。样品在锡容器中称重，并通过赛默飞世尓�/span>℡�/span>特有皃�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;" data-x-flag="16_49">MAS™自动进样器将样品和氧气同时送达到反应管中。燃烧后，产生的气体通过氦气流被带到充满铜的还原区中，然后通过高精度的GC气相色谱柱进行分离。用热导检测器＇�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;" data-x-flag="16_49">TCD）检测燃烧气体（国�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;" data-x-flag="16_49">2）。总运行时间小亍�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;" data-x-flag="16_49">10分钟。当使用NCS配置时，在反应器咋�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;" data-x-flag="16_49">GC柱之间安装了一个吸水剂过滤器、�/span>

国�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;"> 2. CHNS/O结构.

对于氧的测定，以热裂解模式进行测定。样品在银容器中称重，并通过MAS™自动进样器或通过AI 1310直接注射进样戕�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">AS1310液体进样器进样。反应器�?span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">1060°C下含有镍涂层碳进行裂解。样品中的氧与碳结合，形成一氧化碳，然后�?span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">GC气相色谱柱色谱法进行气体分离，并田�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">TCD检测器检测（国�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">2）、�/span>

FlashSmart℡�/span>元素分析仪由EagerSmart数据处理软件自动生成一份完整的报告、�/span>

国�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">3和图4显示了典型的CHNS咋�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">O测定的色谱图、�/span>

国�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;"> 3.典型皃�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;"> CHNS色谱国�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">.

Figure 4.典型皃�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">O色谱国�/span>

测定结果

选择不同的橡胶和轮胎样品。样品分析没有任何预处理，只是切成小块进行分析。对亍�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">CHNS�?span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">NCS咋�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">S的测定，加入助燃剂五氧化二钒可使硫完全转化为SO2。样品的称重量一般为2-3mg、�/span>

对于CHNS分析，仪器以BBOT＇�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">6.51N%＋�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">72.53C%＋�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">6.09H%＋�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">7.44S%）为标准品，使用K-factor作为校准方法进行校准、�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">O分析以乙酰苯胺（11.84%）为标准＋�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">K-factor为校正方法进行校准、�/span>

�?span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">1显示了不同橡胶和轮胎样品皃�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">CHNS/O数据，而表2显示了其他类型橡胶和轮胎材料皃�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">CHNS测定。所有数据均具有良好的重复性，改变样品类型时没有任何基质残留效应、�/span>

�?span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">1橡胶和轮胎样品的CHNS/O测定、�/span>

样品	N%	RSD%	C%	RSD%	H%	RSD%	S%	RSD%	O%	RSD%
橡胶1	0.477 0.481 0.481	0.521	86.118 85.735 85.951	0.223	7.922 7.916 7.941	0.165	0.881 0.899 0.863	2.043	2.023 1.999	0.823
橡胶2	0.336 0.321 0.325	2.420	86.560 86.233 86.329	0.195	7.719 7.674 7.707	0.303	0.639 0.634 0.658	1.967	1.932 1.904	1.010
橡胶3	0.337 0.324 0.338	2.287	86.250 86.210 86.597	0.247	7.210 7.271 7.312	0.706	0.260 0.254 0.271	3.317	2.218 2.245	0.862
	0.792		73.961		6.856		3.151		4.345
轮胎1	0.800	1.074	74.140	0.153	6.880	0.572	3.105	0.744	4.325	0.254
	0.783		74.171		6.933		3.122		4.327
轮胎2	0.529 0.536	0.929	75.253 75.370	0.110	7.187 7.186	0.011	2.972 2.937	0.838	3.752 3.695 3.609	1.953
轮胎3	0.362 0.370	1.546	87.505 87.767	0.211	8.958 8.973	0.112	0.823 0.837	1.226	1.199 1.178 1.191	0.891

�?span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">2橡胶和轮胎样品的CHNS测定

样品	N%	RSD%	C%	RSD%	H%	RSD%	S%	RSD%
	0.628		82.447		11.279		0.797
橡胶4	0.636	0.666	82.272	0.208	11.300	0.1045	0.799	0.503
	0.633		82.104		11.298		0.792
	0.625		82.210		11.263		1.095
橡胶5	0.616	0.790	82.661	0.576	11.114	1.123	1.015	3.989
	0.623		83.161		11.366		1.033
	0.626		81.962		11.218		1.561
橡胶6	0.628	0.470	81.866	0.320	11.249	0.243	1.553	0.606
	0.622		82.361		11.272		1.572
轮胎4	0.454	1.235	79.597	0.0701	6.945	0.0815	1.435	0.930
	0.462		79.676		6.937		1.454
轮胎5	0.436	1.475	82.672	0.0932	7.137	0.000	1.666	0.0848
	0.427		82.781		7.137		1.668

�?span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">3显示了使�?span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">NCS模式分析的橡胶样品的再现性、�/span>

�?span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">3. NCS模式下橡胶的测定.

样品	N%	RSD%	C%	RSD%	S%	RSD%
橡胶7	0.277	0.737	85.802	0.247	0.927	0.751
	0.280		85.503		0.936
橡胶8	0.290	2.447	85.130	0.068	1.546	1.779
	0.300		85.047		1.585
橡胶9	0.293	2.477	84.881	0.108	1.969	1.268
	0.293		84.751		1.934
橡胶10	0.283	1.091	83.229	0.001	3.798	1.281
	0.287		83.230		3.730

�?span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">4通过分析一个新轮胎和一个使用六个月的轮胎中硫的含量，显示了从轮胎表面损失的硫值。这种效应被称为硫晕现象、�/span>

�?span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">4硫晕现象测定结果、�/span>

样品	S% (新轮胍�/span>)	S% (使用六个月的旧轮胍�/span>)
轮胎A	2.605	2.484‒�/span>2.499‒�/span>2.487
轮胎B	5.894	5.415‒�/span>5.302‒�/span>5.250

�?span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;">5显示了橡胶样品热裂解方式测定氧含量、�/span>

�?/span>5橡胶样品的氧测定结果、�/span>

样品	O%	RSD%
橡胶A	2.176	0.186
	2.181
	2.174
	2.171
	2.181
橡胶B	1.825	0.622
	1.819
	1.837
	1.810
	1.810
橡胶C	2.122	0.303
	2.115
	2.117
	2.130
	2.114

结论

赛默飞世尓�/span>℡�/span>FlashSmart℡�/span>元素分析仪能够从任何基质中定量测定元素，改变样品时无任何记忆效应。轮胎和橡胶样品皃�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;" data-x-flag="16_49">CHNS/O测定田�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;" data-x-flag="16_49">FlashSmart℡�/span>元素分析仪进行，样品无须任何预处理、�span style="margin: 0px; padding: 0px; line-height: 2em; font-family: "Microsoft YaHei"; font-size: 16px; position: relative;" data-x-flag="16_49">FlashSmart℡�/span>元素分析仪在自动化和高样品处理量方面满足实验室要求。该分析仪是模块化的，使实验室能够在一次运行中进行CHNS测定，并在改变配置的情况下快速切换到氧模式进行氧的测定、�/span>