CN1218905A - 高效液相色谱分析有机阻燃剂的方法 - Google Patents

高效液相色谱分析有机阻燃剂的方法 Download PDF

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CN1218905A
CN1218905A CN 97123374 CN97123374A CN1218905A CN 1218905 A CN1218905 A CN 1218905A CN 97123374 CN97123374 CN 97123374 CN 97123374 A CN97123374 A CN 97123374A CN 1218905 A CN1218905 A CN 1218905A
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detecting device
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efficient liquid
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CN1081331C (zh
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张昌鸣
李爱英
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Shanxi Institute of Coal Chemistry of CAS
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Abstract

一种高效液相色谱分析有机阻燃剂的方法,采用高效液相色谱仪,紫外多波长检测器单独或与示差检测器串联使用,紫外波长为210－350nm,HSG－10分析柱,移动相为C1－C3醇与四氢呋喃的混合物,流量为1.0－3.0ml/分,进样量为5－20μl。本发明具有组份峰呈现性好,分辨率高,重复性好,可表征各种类型的阻燃剂的组成,结构特征的优点。

Description

高效液相色谱分析有机阻燃剂的方法
本发明属于一种分析方法，具体地说涉及一种高效液相色谱分析有机阻燃剂的方法。
目前，对阻燃剂的检测只是进行一般的化学法测定卤素总含量，挥发份含量测定，以及酸值的测定。由于阻燃剂在色谱移动相中的溶解性与组份峰的呈现性、分辨率的矛盾、相互制约性极大，用高效液相色谱法分析其它有机化合物的原有色谱体系，如一般的正相色谱体系，反相色谱体系，凝胶渗透色谱体系，离子色谱体系是难以分离分析阻燃剂的组份。经文献检索，用高效液相色谱法分离分析阻燃剂未见文献报道。
本发明的发明目的是提供一种高效液相色谱分析有机阻燃剂的方法。
本发明的分析方法如下：
1．使用高效液相色谱分析仪，检测器为紫外(UV)多波长检测器，示差检测器(RID)，紫外检测器单独使用或与示差检测器串联使用，紫外波长为210nm-350nm；
2．采用HSG-10分析柱，柱温为室温；
3．把C1-C3醇与四氢呋喃按10∶90～90∶10(V/V)配成移动相，流量为1ml/分-3ml/分；
4．将阻燃剂溶于四氢呋喃配成0.1-10％(重量百分比)待分析溶液；
5．将待分析溶液以5-20μl进样，检测器进行检测，记录器图示谱图。
本发明的分析方法可适用于溴系有机阻燃剂、氯系有机阻燃剂、磷系有机阻燃剂。包括三嗪系列阻燃剂、中间体产品、阻燃增塑剂等各种阻燃剂。
本发明与现有技术相比具有如下优点：
(1)分析方法使用现代仪器，实施目前化学法所不能进行的组份分离分析。
(2)可表征比较各种类型的阻燃剂组成、结构特征。
(3)可测定阻燃剂的纯度，各组份含量。
(4)组份谱峰呈现性好。
(5)色谱分辨率高。
(6)检测结果重复性好。
实施例1
(1)采用LC-3A高效液相色谱仪，检测器为紫外(UV)多波长检测器，紫外波长固定为230nm；(2)分析柱为HSG-10，柱温为室温；(3)移动相配比为甲醇∶四氢呋喃=20∶80(V∶V)，流速为2.0ml/分；(4)将待分析的B-MAP(密胺三聚氰胺)阻燃剂配成0.5％的四氢呋喃溶液，以10μl进样，检测结果见图1。
实施例2
阻燃剂为TBC，即三(2,3二溴丙基)异氰尿酸酯，学名：1,3,5-三(2,3-二溴丙基)-1,3,5-三嗪-2,4,6酮，紫外波长固定在270nm，移动相为甲醇∶四氢呋喃=50∶50(V∶V)，移动相流速为1.8ml/分，进样量为15μl，其余同实施例1，检测结果见图2。
实施例3
阻燃剂为PZ-747(含氯多磷酸酯，分子量为747)。紫外波长固定在310nm。移动相为甲醇∶四氢呋喃=30∶70(V∶V)，移动相流速为2.5ml/分，进样量为15μl，其余同实施例1，检测结果见图3。
实施例4
阻燃剂为BBP，即双(2,3二溴丙基)二氯丙基磷酸酯，检测器为紫外(UV)多波长检测器与示差检测器串联使用，紫外波固定在260nm，移动相为甲醇∶四氢呋喃=10∶30(U/V)其余同实施例1。检测结果见图4。
实施例5
阻燃剂为TBP，即三(2,3二溴丙基磷酸酯，其余同实施例4，检测结果见图5。
实施例6
阻燃剂为亚磷酸三苯酯，紫外波固定在254nm，移动相为甲醇∶四氢呋喃=90∶10(V∶V)，进样量为20μl，其余同实施例4，检测结果见图6。
实施例7
阻燃剂为阻燃增塑剂FR-15，移动相为甲醇∶四氢呋喃=60∶40(V∶U)，其余同实施例6，检测结果见图7。
实施例8
阻燃剂为三(2,3-二溴丙基)硼酸酯，紫外波长为280nm，进样量为10ml/次，其余同实施例6，检测结果见图8。
实施例9
阻燃剂为八溴二苯醚，其余同实施例4，检测结果见图9。

Claims (1)

1．一种高效液相色谱分析有机阻燃剂的方法，其分析方法如下：
(1)．使用高效液相色谱分析仪，检测器为紫外(UV)多波长检测器，示差检测器(RID)，紫外检测器单独使用或于示差检测器串联使用，紫外波长为210nm-350nm；
(2)．采用HSG-10分析柱，柱温为室温；
(3)．把C1-C3醇与四氢呋喃按10∶90～90∶10(V/V)配成移动相，流量为1ml/分-3ml/分；
(4)．将阻燃剂溶于四氢呋喃配成0.1-10％(重量百分比)待分析溶液；
(5)．将待分析溶液以5-20μl进样，检测器进行检测，记录器图示谱图。
CN 97123374 1997-12-04 1997-12-04 高效液相色谱分析有机阻燃剂的方法 Expired - Fee Related CN1081331C (zh)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101216467B (zh) * 2008-01-14 2010-12-15 谱尼测试科技（北京）有限公司 一种电子材料中六溴环十二烷含量的测定方法
CN106501400A (zh) * 2016-10-21 2017-03-15 广东环境保护工程职业学院 一种液相色谱测定水样中tcep的检测方法
CN113125625A (zh) * 2021-06-21 2021-07-16 天地恒一制药股份有限公司 一种富马酸丙酚替诺福韦中基因毒性杂质的检测方法

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101216467B (zh) * 2008-01-14 2010-12-15 谱尼测试科技（北京）有限公司 一种电子材料中六溴环十二烷含量的测定方法
CN106501400A (zh) * 2016-10-21 2017-03-15 广东环境保护工程职业学院 一种液相色谱测定水样中tcep的检测方法
CN106501400B (zh) * 2016-10-21 2017-10-24 广东环境保护工程职业学院 一种液相色谱测定水样中tcep的检测方法
CN113125625A (zh) * 2021-06-21 2021-07-16 天地恒一制药股份有限公司 一种富马酸丙酚替诺福韦中基因毒性杂质的检测方法
CN113125625B (zh) * 2021-06-21 2021-09-03 天地恒一制药股份有限公司 一种富马酸丙酚替诺福韦中基因毒性杂质的检测方法

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