ICS 75.140 CCS E 43 中华人民共和国石油化工行业标准 NB/SH/T 6087—2024 重馏分油四组分的测定 中压液相色谱法 Standard test method for separation of heavy distillate into four fractions— Medium pressure liquid chromatography 2024-12-25发布 2025-06-25实施 NB/SH/T 6087—2024 I 目 次 前言 ······························································································································I I 1 范 围 ························································································································· 1 2 规范性引用文件 ·········································································································· 1 3 术语和定义 ················································································································ 1 4 方法概要 ··················································································································· 1 5 仪器设备 ··················································································································· 1 5.1 中压液相色谱仪 ····································································································· 1 6 试剂或材料 ················································································································ 2 7 取 样 ························································································································· 3 8 试验步骤 ··················································································································· 3 8.1 仪器的准备 ··········································································································· 3 8.2 样品的分析 ··········································································································· 3 9 试验数据处理 ············································································································· 4 10 精密度 ····················································································································· 5 10.1 重复性（ 95%置信水平） ························································································ 5 10.2 再现性（ 95%置信水平） ························································································ 5 11 试验报告 ·················································································································· 5 NB/SH/T 6087—2024 II 前 言 本文件按照 GB/T 1.1 —2020《标准化工作导则 第1部分：标准化文件的结构和起草规则》的规定 起草。 请注意本文件的某些内容可能涉及专利。本文件的发布机构不承担识别专利的责任。 本文件由中国石油化工集团有限公司提出。 本文件由全国石油产品和润滑剂标准化技术委员会石油沥青分技术委员会（ SAC/TC280/SC4 ）归口。 本文件起草单位：中国石油天然气股份有限公司石油化工研究院、中石化石油化工科学研究院、中 国石油天然气股份有限公司大连石化分公司、中国石油大学（北京） 、中国石油天然气股份有限公司广 西石化分公司、中国石油天然气股份有限公司华北石化分公司、中海油天津化工研究设计院有限公司、 中石油燃料油有限责任公司研究院、北京橙达仪器有限公司、山东亿维新材料有限责任公司。 本文件主要起草人：曹青、修远、文大为、陈芬芬、史军歌、杨孟智、薛聚彦、薛慧峰、邴德媚、 何京、韩晔华、杨定忠、赫丽娜、郝萌、冯永年、卫玉磊、毛三鹏、邹雯、郝亚苹、何礼军、隋芝宇。 本文件于 2024年首次发布。 NB/SH/T 6087—2024 1 重馏分油四组分的测定 中压液相色谱法 警示—使用本文件的人员应有正规实验室的实践经验。本文件并未指出所有可能的安全问题。 使用者有责任采取适当的安全和健康措施，并保证符合国家有关法规规定的条件。 1 范围 1.1 本文件规定了使用中压液相色谱将重馏分油分离为四组分（饱和分、芳香分、胶质、沥青质）并 测定其含量的方法。 1.2 本文件适用于沥青质含量不大于 30%的渣油、蜡油和石油沥青，其他初馏点＞ 350℃的石油馏分 及产品可参照使用。 2 规范性引用文件 下列文件中的内容通过文中的规范性引用而构成本文件必不可少的条款。其中，注日期的引用文件， 仅该日期对应的版本适用于本文件。不注日期的引用文件，其最新版本（包括所有的修改单）适用于本 文件。 GB/T 679 化学试剂 乙醇（ 95%） GB/T 4756 石油液体手工取样法 GB/T 11147 沥青取样法 SH/T 0229 固体和半固体石油产品取样法 3 术语和定义 本文件没有需要界定的术语和定义。 4 方法概要 将试样分散于正庚烷中，分散液经沥青质过滤膜上样到色谱柱上，沥青质被保留在过滤膜上，脱沥 青组分经色谱柱分离洗脱为饱和分、芳香分和胶质，沥青质不经色谱柱直接用甲苯冲洗后溶解收集。蒸 干溶剂后即可得到沥青质、饱和分、芳香分和胶质。分别称重计算每个组分的质量分数。 5 仪器设备 5.1 中压液相色谱仪 5.1.1 仪器组成：由流动相控制单元、分离单元、组分接收单元 3个模块组成，仪器各单元之间的连 接方式可参照图 1。 NB/SH/T 6087—2024 2 图 1 中压液相色谱仪的结构示意图 a） 流动相控制单元：该单元由至少 3个溶剂罐、至少 2个柱塞泵及溶剂混合装置组成。柱塞及柱 塞腔室应当使用耐受甲苯、正庚烷、乙醇的材质制成。流动相的流速由柱塞泵控制，可控制样 品洗脱流速范围： 0.5mL/min ～2.5mL/min ，精确到 0.1mL/min 。如仪器具有多路平行分离功能， 应当能够保证通过每一路的流量之间最大差异不超过体积流速绝对值的 5%。 b） 分离单元：由色谱柱、沥青质过滤膜和柱温箱组成，色谱柱和沥青质过滤膜均可竖直放置于 （50±2）℃的柱温箱中。设备应当能够使操作者方便地单独安装和拆卸色谱柱及过滤膜，并 在不接入色谱柱的情况下直接将沥青质过滤膜与组分接收单元连接。 c） 组分接收单元：用于收集洗脱的组分，能够容纳至少 4个铝杯（ 6.6），能通过主动排风装置或 其他方式保证试验过程中溶剂蒸气的浓度低于其爆炸极限。