CN1094071C - 以碳素为基体的固相微萃取吸附质 - Google Patents

以碳素为基体的固相微萃取吸附质 Download PDF

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CN1094071C
CN1094071C CN98106766A CN98106766A CN1094071C CN 1094071 C CN1094071 C CN 1094071C CN 98106766 A CN98106766 A CN 98106766A CN 98106766 A CN98106766 A CN 98106766A CN 1094071 C CN1094071 C CN 1094071C
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CN1230457A (zh
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方瑞斌
张维昊
涂学炎
张世鸿
高诚伟
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Yunnan University YNU
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Abstract

本发明涉及一种以碳素为基体的固相微萃取吸附质，属化工材料技术领域。本发明由重量比为65-85%的碳素基体、14-30%的无机粘合剂、1-5%的其它辅助材料经常规的工艺制成。碳素基体选用石墨、活性炭或者无定形炭黑。无机粘合剂选用粘土或者硅藻土、三氧化二铝或者二氧化硅。其它辅助材料选用惰性长链有机化合物作为改性添加剂。具有成本低，吸附容量大，分析灵敏度高，使用寿命长，使用方便、应用范围广等优点。

Description

以碳素为基体的固相微萃取吸附质
技术领域：
本发明涉及一种以碳素为基体的固相微萃取吸附质，属化工材料技术领域。
背景技术：
现有的用于固相微萃取装置的吸附质为高分子聚合物(聚二甲硅氧烷或聚丙酸脂等物质)，涂覆在惰性支撑物上制成。该吸附质成本高、吸附量小，痕量样品富集倍数不够高，制作工艺要求严格，使用寿命短(设计正常使用为50-100次/支，但实际因高分子聚合物涂覆膜极易机械划损或热变质损伤)，在推广使用上受到很大限制。
发明内容：
本发明的目的在于克服现有技术之不足，提供一种以碳素为基体的固相微萃取吸附质。
本发明由重量比为65-85％的碳素基体、14-30％的无机粘合剂、1-5％的其它辅助材料经常规的高压成型、烘干、焙烧、活化等工艺制成固相微萃取吸附棒。其中碳素基体选用石墨、活性炭或者无定形炭黑。无机粘合剂选用粘土或者硅藻土、三氧化二铝或者二氧化硅。其它辅助材料选用聚乙稀醇、聚二甲基硅氧烷石蜡、二十四碳一稀酸酯、工业饴糖等惰性添加物制成。
本发明与现有技术相比，具有成本低，吸附容量大，分析灵敏度高，使用寿命长，使用方便等优点。用该吸附质制成的固相微萃取装置可与液相色谱、气相色谱、气质联用分析微量及痕量非极性及小极性有机化合物。
具体实施方式：
实施例1：将70％的鳞状石墨、25％的溧阳粘土、2％的二氧化硅及1％的石蜡粉碎混匀，加水搅拌调和后，经100-220公斤/厘米2的高压捏合成型，随后经600-1100℃高温焙烧后得到石墨基体，再放入浓度为6-12N的硝硫酸中浸泡1-4小时，最后经微波辐射30-300秒钟及超声清洗1-10分钟后得到固相微萃取吸附质。将该吸附质按公知方法装配为固相微萃取装置，该装置与气相色谱联用分析检测环境大气中苯系物。检测时将吸附质纤维暴露于空气中30分钟进行富集吸附，然后直接将其送入色谱气化室内热解吸，色谱分离分析。下表为用该装置分析的结果(而高分子聚合物固定相的固相微萃取装置在此条件下无色谱峰)。下表为环境大气中苯系物的测定结果(单位mg/m3)。
地  点   苯   甲苯   乙苯 二甲苯
云南机床厂喷漆车间 24.7  14.9  58.6  61.5
昆明市区I处 1.8  0.2  0.2  0.1
昆明市区II处 2.3  0.3  0.3  0.3
昆明市区III处 1.9  0.2  0.2  0.2
实施例2：取活性炭65％、三氧化二铝30％、二十四碳一稀酸甘油酯2％、聚乙稀醇改性剂3％按与实施例1相同的制作方法得到吸附质，并装配于固相微萃取装置中。然后分别用该装置及高分子聚合物固定相固相微萃取装置与气相色谱联用分析检测环境水体中有机氯农药含量，检测操作同实施例1。下表为分析结果。
    LOD(ngl-1)     RSD(％)
  分析物 CF  PAC  PDMS  CF  PAC  PDMS
 α-BHC  0.02  1  1  18  5  9
 β-BHC  0.01  1  1  16  5  17
 γ-BHC  0.02  1  1  18  6  7
 δ-BHC  0.14  1  2  18  6  6
 OP2-DDT  0.4  -  -  20  -  -
 PP2-DDT  0.4  1  1  24  11  10
CF是石墨吸附质棒，PAC是95μm聚丙稀酸酯固定相，PDMS100μm聚二甲基硅氧烷是固定相。
由上表分析结果可以看出，采用本发明作为吸附质检测灵敏度显著提高，证明该吸附质有较大的吸附容量及较好的常规气相色谱条件下的可逆解吸附能力。
实施例3：取乙炔碳黑85％、硅藻土12％、聚二甲基硅氧烷改性剂3％按与实施例1相同的制作方法得到吸附质，并装配于固相微萃取装置中。分别用该装置及高分子聚合物固定相固相微萃取装置与气相色谱联用分离烟用香料，操作同实施例1。分析结果表明：石墨类吸附剂有较大的吸附容量及吸附种类范围，对分子量较大、极性较小的化合物有较大的选择性吸附，特别是具有环状结构的化合物的吸附性较大。

Claims (1)

1.一种以碳素为基体的固相微萃取吸附质，其特征在于该吸附质由重量比为65-85％的碳素基体、14-30％的无机粘合剂、1-5％的其它辅助材料经常规工艺制成；碳素基体选用石墨、活性炭或者无定形炭黑；无机粘合剂选用粘土或者硅藻土、三氧化二铝或者二氧化硅；其它辅助材料选用惰性长链有机化合物。
CN98106766A 1998-03-27 1998-03-27 以碳素为基体的固相微萃取吸附质 Expired - Fee Related CN1094071C (zh)

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CN1133477C (zh) * 2000-12-18 2004-01-07 武汉大学 羟基冠醚固相微萃取萃取头及其制备方法
WO2010139813A1 (es) * 2009-06-02 2010-12-09 Desarrollos Tecnicos Mc, S.L. Composicion de un material de grafito y procedimiento de activacion y conversion de un material de grafito a un material adsorbente de carbon activado para la eliminacion de gases contaminantes
CN103188896A (zh) * 2011-12-30 2013-07-03 深圳富泰宏精密工业有限公司 壳体及该壳体的制作方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5576217A (en) * 1995-02-28 1996-11-19 Mallinckrodt Baker, Inc. Solid phase microextraction of trace amounts of organic analytes
US5693228A (en) * 1995-09-28 1997-12-02 Varian Associates, Inc. Method and device for vibration during solid phase microextraction

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5576217A (en) * 1995-02-28 1996-11-19 Mallinckrodt Baker, Inc. Solid phase microextraction of trace amounts of organic analytes
US5693228A (en) * 1995-09-28 1997-12-02 Varian Associates, Inc. Method and device for vibration during solid phase microextraction

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