WO2017114451A1 - 一种测量纺织物中甲醛的方法 - Google Patents

一种测量纺织物中甲醛的方法 Download PDF

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WO2017114451A1
WO2017114451A1 PCT/CN2016/112936 CN2016112936W WO2017114451A1 WO 2017114451 A1 WO2017114451 A1 WO 2017114451A1 CN 2016112936 W CN2016112936 W CN 2016112936W WO 2017114451 A1 WO2017114451 A1 WO 2017114451A1
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textile
formaldehyde
closed container
content
absorption liquid
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PCT/CN2016/112936
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English (en)
French (fr)
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田琳琳
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田琳琳
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N2030/022—Column chromatography characterised by the kind of separation mechanism
    • G01N2030/027—Liquid chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N2030/062—Preparation extracting sample from raw material

Definitions

  • the present invention relates to a detection method, and more particularly to a method for measuring formaldehyde in a textile, which belongs to the field of product safety inspection.
  • Formaldehyde is a large-scale organic chemical product and intermediate, and has a wide range of uses in many fields such as chemical engineering, wood processing, chemical fiber, medicine, and pesticides.
  • formaldehyde is one of the raw materials for the production of various dyes and textile dyeing and finishing auxiliaries. It is also a cross-linking agent for anti-shrinkage and wrinkle-preventing of fabrics based on cellulose fibers.
  • Formaldehyde-containing textiles gradually release free formaldehyde, and most of them will have direct or indirect contact with the human body, which may cause harm to the human body. Therefore, in order to protect the health and safety of the human body, China has successively formulated indicators for controlling formaldehyde content in the relevant textile product standards.
  • the technical problem to be solved by the present invention is to provide a method for measuring formaldehyde in textiles, which has high accuracy and credibility, and can detect textiles having a very low formaldehyde content. Awakening content, no pollution.
  • the technical solution adopted by the present invention is a method for measuring formaldehyde in a textile, comprising the following steps: (1) placing the object to be tested in a closed container, and then passing through the sealed container; Nitrogen gas 30-40min;
  • the above method for measuring formaldehyde in the textile is optimized, and the absorption liquid in the step (1) is a bottom liquid of the dimethyl ether rectification column.
  • the present invention neither causes damage to the textile, but also can detect the low concentration of formaldehyde in the textile; the invention recovers the formaldehyde in the whole textile, and does not need to cut a small sample from the textile, so It does not cause damage to the object to be measured; the result is high in accuracy and credibility.
  • the invention recovers formaldehyde in the whole textile, and the content of the obtained wake-up result is the average content of formaldehyde in the whole piece of textile, instead of The local content of a certain part or the average content of a certain part, so the accuracy and reliability of the results obtained by applying the invention are higher than those of the existing national standard methods; the textiles having a very low formaldehyde content can be detected. Formaldehyde content.
  • Embodiment 1 is a method for measuring formaldehyde in textiles, comprising the following steps: (1) placing the object to be tested in a closed container, and then introducing nitrogen into the sealed container for 30 minutes;
  • Embodiment 2 is a method for measuring formaldehyde in a textile, comprising the following steps: (1) placing the object to be tested in a closed container, and then introducing nitrogen into the sealed container for 40 minutes; (2) The gas from the closed container is absorbed by the absorption liquid, and the amount of the absorption liquid is in the range of 250 ml; (3) the ultrasonic wave is shaken for 20 minutes, and then extracted and derivatized; (4) the derivatization solution is removed and placed on the centrifuge at 800 r/min.
  • the HPLC column in step (6) is DB-5, 30mx0.25mm, 0.15 ⁇ .
  • the temperature of the closed container in step (1) is 85 degrees.
  • Embodiment 3 is a method for measuring formaldehyde in a textile, comprising the following steps: (1) placing the object to be tested in a closed container, and then introducing nitrogen into the sealed container for 35 minutes; (2) The gas from the closed container is absorbed by the absorption liquid, and the amount of the absorption liquid is in the range of 225 ml; (3) the ultrasonic wave is shaken for 18 minutes, and then extracted and derivatized; (4) the derivatization solution is removed and placed on the centrifuge at 800 r/min.
  • the HPLC column in step (6) is DB-5, 30mx0.25mm, 0.15 ⁇ .
  • the temperature of the closed container in step (1) is 75 degrees.
  • the invention neither causes damage to the textile, but also can detect the low concentration of formaldehyde in the textile; the invention recovers the formaldehyde in the whole textile, and does not need to cut a small sample from the textile, so it will not The object to be measured causes damage; the result is high in accuracy and credibility.
  • the invention recovers formaldehyde in the whole textile, and the content of the obtained wake-up result is the average content of formaldehyde in the whole piece of textile, rather than a certain part.
  • the local content or the average content of certain parts so the accuracy and reliability of the results obtained by applying the invention are higher than the existing national standard methods; the formaldehyde content in textiles with very low formaldehyde content can be detected .

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Treatment Of Fiber Materials (AREA)

Abstract

一种测量纺织物中甲醛的方法，包括下列步骤：将待测物置于密闭容器内，然后向该密闭容器内通入氮气30-40min；再用吸收液吸收来自该密闭容器的气体，吸收液的用量范围为200-250ml；超声波震荡15-20min后萃取并衍生化；移取衍生化溶液，放置在离心机上以800r/min的转速离心10-12min后静置1.5小时；取下层液加入3ml碳酸氢钠萃取后定容至8ml；采用高效液相色谱仪配合紫外检测器检测即可得出结果。该方法不会对纺织品造成损害，而且还可以测出纺织品中低浓度的甲醛含量；结果准确性和可信度高，是回收整件纺织品中的甲醛进行测定，得到的甲醒的含量结果是整件纺织的甲醛平均含量；可检测出甲醛含量非常低的纺织品中的甲醛含量。

Description

一种测量纺织物中甲醛的方法
技术领域
[0001] 本发明涉及一种检测方法， 尤其是涉及一种测量纺织物中甲醛的方法， 属于产 品安全检测领域。
背景技术
[0002] 甲醛是大宗有机化工产品及中间体， 在化工、 木材加工、 化纤、 医药、 农药等 许多方面有十分广泛的用途。 在纺织行业中， 甲醛是生产多种染料和纺织染整 助剂的原料之一， 也是以纤维素纤维为主的织物的防缩防皱和洗可穿整理的交 联剂。 含甲醛的纺织品会逐渐释放出游离甲醛， 而大多数都会与人体有直接或 间接的接触， 容易对人体造成伤害。 因此为了保障人体的健康和安全， 我国相 继在有关纺织产品标准中制定了控制甲醛含量的指标。
技术问题
[0003] 针对现有技术存在的不足， 本发明所要解决的技术问题是， 提供一种测量纺织 物中甲醛的方法， 结果准确性和可信度高， 可检测出甲醛含量非常低的纺织品 中的甲醒含量， 无污染。
问题的解决方案
技术解决方案
[0004] 为解决上述技术问题， 本发明采取的技术方案是， 一种测量纺织物中甲醛的方 法， 包括下列步骤： （1)将待测物置于密闭容器内， 然后向该密闭容器内通入氮 气 30-40min;
[0005] (2)再用吸收液吸收来自该密闭容器的气体， 吸收液的用量范围为 200-250ml;
[0006] (3)超声波震荡 15-20min后后萃取并衍生化；
[0007] (4)移取衍生化溶液， 放置在离心机上以 800r/min的转速离心 10-12min后静置 1.5 小吋；
[0008] (5)取下层液加入 3ml碳酸氢钠萃取后定容至 8ml;
[0009] (6)采用高效液相色谱仪配合紫外检测器检测即可得出结果。 [0010] 优化的， 上述测量纺织物中甲醛的方法， 其步骤 （6) 中的高效液相色谱仪的 色谱柱为 DB-5， 30mx0.25mm, 0.15μηι。
[0011] 优化的， 上述测量纺织物中甲醛的方法， 其步骤 （1) 中的密闭容器的温度为 7
0-85度。
[0012] 优化的， 上述测量纺织物中甲醛的方法， 其步骤 （1) 中的吸收液为二甲醚精 馏塔的塔底液。
发明的有益效果
有益效果
[0013] 本发明既不会对纺织品造成损害， 而且还可以测出纺织品中低浓度的甲醛含量 ； 本发明是回收整件纺织品中的甲醛进行测定， 无需从纺织品上剪取小块样品 ， 因此不会对所要测定的对象造成损伤； 结果准确性和可信度高， 本发明是回 收整件纺织品中的甲醛进行测定， 得到的甲醒的含量结果是整件纺织的甲醛平 均含量， 而不是某个部位的局部含量或某几个部位的平均含量， 因此应用本发 明检测得到的结果的准确性和可信度比现有的国家标准方法的高； 可检测出甲 醛含量非常低的纺织品中的甲醛含量。
实施该发明的最佳实施例
本发明的最佳实施方式
[0014] 实施例 1本发明为一种测量纺织物中甲醛的方法， 包括下列步骤： （1)将待测物 置于密闭容器内， 然后向该密闭容器内通入氮气 30min;
[0015] (2)再用吸收液吸收来自该密闭容器的气体， 吸收液的用量范围为 200ml;
[0016] (3)超声波震荡 15min后后萃取并衍生化； （4)移取衍生化溶液， 放置在离心机 上以 800r/min的转速离心 lOmin后静置 1.5小吋；
[0017] (5)取下层液加入 3ml碳酸氢钠萃取后定容至 8ml;
[0018] (6)采用高效液相色谱仪配合紫外检测器检测即可得出结果。 步骤 （6) 中的高 效液相色谱仪的色谱柱为 DB-5， 30mx0.25mm, 0.15μηι。 步骤 （1) 中的密闭容 器的温度为 70度。 本发明的实施方式
[0019] 实施例 2本发明为一种测量纺织物中甲醛的方法， 包括下列步骤： （1)将待测物 置于密闭容器内， 然后向该密闭容器内通入氮气 40min; (2)再用吸收液吸收来 自该密闭容器的气体， 吸收液的用量范围为 250ml; (3)超声波震荡 20min后后萃 取并衍生化； （4)移取衍生化溶液， 放置在离心机上以 800r/min的转速离心 12min 后静置 1.5小吋； （5)取下层液加入 3ml碳酸氢钠萃取后定容至 8ml; (6)采用高效 液相色谱仪配合紫外检测器检测即可得出结果。 步骤 （6) 中的高效液相色谱仪 的色谱柱为 DB-5， 30mx0.25mm, 0.15μηι。 步骤 （1) 中的密闭容器的温度为 85 度。
[0020] 实施例 3本发明为一种测量纺织物中甲醛的方法， 包括下列步骤： （1)将待测物 置于密闭容器内， 然后向该密闭容器内通入氮气 35min; (2)再用吸收液吸收来 自该密闭容器的气体， 吸收液的用量范围为 225ml; (3)超声波震荡 18min后后萃 取并衍生化； （4)移取衍生化溶液， 放置在离心机上以 800r/min的转速离心 l lmin 后静置 1.5小吋； （5)取下层液加入 3ml碳酸氢钠萃取后定容至 8ml; (6)采用高效 液相色谱仪配合紫外检测器检测即可得出结果。 步骤 （6) 中的高效液相色谱仪 的色谱柱为 DB-5， 30mx0.25mm, 0.15μηι。 步骤 （1) 中的密闭容器的温度为 75 度。 本发明既不会对纺织品造成损害， 而且还可以测出纺织品中低浓度的甲醛 含量； 本发明是回收整件纺织品中的甲醛进行测定， 无需从纺织品上剪取小块 样品， 因此不会对所要测定的对象造成损伤； 结果准确性和可信度高， 本发明 是回收整件纺织品中的甲醛进行测定， 得到的甲醒的含量结果是整件纺织的甲 醛平均含量， 而不是某个部位的局部含量或某几个部位的平均含量， 因此应用 本发明检测得到的结果的准确性和可信度比现有的国家标准方法的高； 可检测 出甲醛含量非常低的纺织品中的甲醛含量。
工业实用性
[0021] 当然， 上述说明并非是对本发明的限制， 本发明也并不限于上述举例， 本技术 领域的普通技术人员， 在本发明的实质范围内， 作出的变化、 改型、 添加或替 换， 都应属于本发明的保护范围。

Claims

权利要求书
[权利要求 1] 一种测量纺织物中甲醛的方法， 包括下列步骤： （1)将待测物置于密 闭容器内， 然后向该密闭容器内通入氮气 30-40min;
(2)
再用吸收液吸收来自该密闭容器的气体， 吸收液的用量范围为 200-25 0ml;
(3)超声波震荡 15-20min后萃取并衍生化；
(4)移取衍生化溶液， 放置在离心机上以 800r/min的转速离心 10-12min 后静置 1.5小吋；
(5)取下层液加入 3ml碳酸氢钠萃取后定容至 8ml;
(6)采用高效液相色谱仪配合紫外检测器检测即可得出结果。
[权利要求 2] 根据权利要求 1所述的测量纺织物中甲醛的方法， 其特征在于： 所述 步骤 （6) 中的高效液相色谱仪的色谱柱为 DB-5， 30mx0.25mm, 0.15 μηι。
[权利要求 3] 根据权利要求 1所述的测量纺织物中甲醛的方法， 其特征在于： 所述 步骤 （1) 中的密闭容器的温度为 70-85度。
[权利要求 4] 根据权利要求 1所述的测量纺织物中甲醛的方法， 其特征在于： 所述 步骤 （1) 中的吸收液为二甲醚精馏塔的塔底液。
PCT/CN2016/112936 2015-12-30 2016-12-29 一种测量纺织物中甲醛的方法 WO2017114451A1 (zh)

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