WO2017114406A1 - 一种测量液体中甲醛含量的方法 - Google Patents

一种测量液体中甲醛含量的方法 Download PDF

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Publication number
WO2017114406A1
WO2017114406A1 PCT/CN2016/112577 CN2016112577W WO2017114406A1 WO 2017114406 A1 WO2017114406 A1 WO 2017114406A1 CN 2016112577 W CN2016112577 W CN 2016112577W WO 2017114406 A1 WO2017114406 A1 WO 2017114406A1
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liquid
formaldehyde
taking
cuvette
ultrafiltration
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PCT/CN2016/112577
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田琳琳
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田琳琳
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour

Definitions

  • the present invention relates to a detection method, and more particularly to a method for measuring the formaldehyde content in a liquid, which belongs to the field of safety inspection.
  • the technical problem to be solved by the present invention is to provide a method for measuring the formaldehyde content in a liquid, which has high accuracy and credibility, is convenient to use, has obvious phenomena, and has high sensitivity, and Low cost and safe operation.
  • the technical solution adopted by the present invention is a method for measuring the formaldehyde content in a liquid, comprising the following steps: (1) taking 10 g of the liquid to be tested and centrifuging on a high-speed centrifuge to obtain an upper layer liquid; Take the above supernatant liquid, transfer it to the ultrafiltration cup, use ultrafiltration membrane ultrafiltration at room temperature, and collect the filtered clear color liquid, and store it at minus 10 degrees for measurement; (3) Add formaldehyde to the clean UV cuvette; (4) Weigh 10-15g of sodium hydroxide in the volumetric flask, add 20-28ml of distilled water and shake it into the above UV cuvette; (5) Take O. lmg colorless clear liquid, gradually add it to the UV cuvette with a micro-injector, add formaldehyde coloring agent while adding sample, let stand for 20-30min and test on UV-visible spectrophotometer You can judge the result.
  • the method for measuring the formaldehyde content in the liquid, the formaldehyde developer in the step (5) is a phenol reagent
  • the color development reaction of the invention is fast, only about one minute, the measurement conditions are relatively loose, and the sensitivity is high, the cost is low, and the interference in the raw milk detection is also small.
  • it is a A method for rapidly detecting formaldehyde in liquids that is very suitable for popularization.
  • Embodiment 1 is a method for measuring the formaldehyde content in a liquid, comprising the following steps: (1) taking 10 g of the liquid to be tested and centrifuging on a high-speed centrifuge to obtain an upper layer liquid; (2) taking the above-mentioned upper layer liquid, transferring Ultrafiltration cup, ultrafiltration using ultrafiltration membrane at room temperature, collecting filtered colorless clear liquid, stored at minus 10 degrees for measurement; (3) adding formaldehyde developer to clean In the ultraviolet cuvette; (4) Weigh 10g of sodium hydroxide in a volumetric flask, add 20ml of distilled water and shake it into the above UV cuvette; (5) take O.lmg colorless clear liquid, gradually use trace The sampler is added to the ultraviolet cuvette, and the formaldehyde coloring agent is added while the sample is applied.
  • the formaldehyde coloring agent in the step (5) is a phenol reagent; the concentration of the phenol reagent is 0.015 g/ml.
  • Embodiment 2 is a method for measuring the formaldehyde content in a liquid, comprising the following steps: (1) taking 10 g of the liquid to be tested and centrifuging on a high-speed centrifuge to obtain an upper layer liquid; (2) taking the above-mentioned upper layer liquid, transferring Ultrafiltration cup, ultrafiltration using ultrafiltration membrane at room temperature, collecting filtered colorless clear liquid, stored at minus 10 degrees for measurement; (3) adding formaldehyde developer to clean In the ultraviolet cuvette; (4) Weigh 15g of sodium hydroxide in a volumetric flask, add 28ml of distilled water and shake it into the above-mentioned UV cuvette; (5) then take O.
  • the injector is added to the UV cuvette, and the formaldehyde developer is added while the sample is being applied. After 30 minutes, the result can be judged by detecting on a UV-visible spectrophotometer.
  • the formaldehyde developer in the step (5) is a phenol reagent; the concentration of the phenol reagent is 0.015 g/ml.
  • Embodiment 3 is a method for measuring the formaldehyde content in a liquid, comprising the following steps: (1) taking 10 g of the liquid to be tested and centrifuging on a high-speed centrifuge to obtain an upper layer liquid; (2) taking the above upper layer liquid and transferring to the ultrafiltration cup Ultrafiltration with ultrafiltration membrane at room temperature, ultrafiltration of ultrafiltration, collection of colorless clear liquid, stored at minus 10 degrees for measurement; (3) addition of formaldehyde developer to clean UV colorimetric (4) Weigh 12g of sodium hydroxide in a volumetric flask, add 24ml of distilled water and shake it into the above UV cuvette; (5) take O.
  • the formaldehyde developer in the step (5) is a phenol reagent; the concentration of the phenol reagent is 0.015 g/ml.
  • the color development reaction of the invention is fast, only about one minute, the measurement conditions are relatively loose, and the sensitivity is high, the cost is low, and the interference in the raw milk detection is also small, which is very suitable for large and medium-sized dairy companies or beverage companies.

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Plasma & Fusion (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Separation Using Semi-Permeable Membranes (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)

Abstract

一种测量液体中甲醛含量的方法,包括下列步骤:取10g待测液体在高速离心机上离心得上层液;取上述上层液,转入超滤杯,在室温条件下使用超滤膜用超滤器超滤,收取滤出的无色清亮液,在零下10度保存,以供测量;将甲醛显色剂加到洁净的紫外比色皿中;称取10-15g氢氧化钠于容量瓶中,再加入20-28ml蒸馏水摇匀加入上述紫外比色皿中;再取0.1mg无色清亮液,逐渐用微量进样器加到紫外比色皿中,边加样边加入甲醛显色剂,静置20-30min后在紫外可见分光光度仪上检测即可判断结果。

Description

一种测量液体中甲醛含量的方法 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液体中甲醛含量的方法, 属于 安全检测领域。
背景技术
[0002] 目前在我国原奶等惨假的现象屡禁未止, 而且越来越严重和普遍。 由于甲醛有 防腐消毒作用, 在利益的驱使下, 一些奶户在原奶中加入甲醛以达到收奶吋的 微生物指标, 孰不知甲醛为较高毒性的物质, 在我国有毒化学品优先控制名单 上甲醛高居第二位。 甲醛已经被世界卫生组织确定为致癌和致畸形物质, 是公 认的变态反应源, 也是潜在的强致突变物之一, 它可以破坏生物细胞蛋白, 可 引起人体过敏、 肠道刺激反应、 食物中毒等疾病。 目前对原奶等液体中甲醛的 快速检测有相应的几种检测方法, 但因不易于安全操作、 显色现象不明显或灵 敏度不高的缺点, 使其质量不能得到保证。
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, 提供一种测量液体 中甲醛含量的方法, 结果准确性和可信度高, 使用方便, 现象明显、 灵敏度高 , 而且成本低廉、 操作安全。
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, 一种测量液体中甲醛含量的 方法, 包括下列步骤: (1)取 10g待测液体在高速离心机上离心得上层液; (2)取 上述上层液, 转入超滤杯, 在室温条件下使用超滤膜用超滤器超滤, 收取滤出 的无色清亮液, 在零下 10度保存, 以供测量; (3)将甲醛显色剂加到洁净的紫外 比色皿中; (4)称取 10-15g氢氧化钠于容量瓶中, 再加入 20-28ml蒸馏水摇匀加入 上述紫外比色皿中; (5)再取 O. lmg无色清亮液, 逐渐用微量进样器加到紫外比色 皿中, 边加样边加入甲醛显色剂, 静置 20-30min后在紫外可见分光光度仪上检测 即可判断结果。
[0005] 优化的, 上述测量液体中甲醛含量的方法, 其步骤 (5)中的甲醛显色剂为酚试剂
[0006] 优化的, 上述测量液体中甲醛含量的方法, 其酚试剂的浓度为 0.015g/ml。
发明的有益效果
有益效果
[0007] 本发明显色反应快, 只需大约一分钟, 测定条件相对也宽松, 而且灵敏度高, 成本低, 在原奶检测中干扰也小, 对于大中型乳品企业或饮料企业来说, 是一 种非常适用于普及的快速检测液体中含甲醛的方法。
实施该发明的最佳实施例
本发明的最佳实施方式
[0008] 实施例 1本发明为一种测量液体中甲醛含量的方法, 包括下列步骤: (1)取 10g 待测液体在高速离心机上离心得上层液; (2)取上述上层液, 转入超滤杯, 在室 温条件下使用超滤膜用超滤器超滤, 收取滤出的无色清亮液, 在零下 10度保存 , 以供测量; (3)将甲醛显色剂加到洁净的紫外比色皿中; (4)称取 10g氢氧化钠 于容量瓶中, 再加入 20ml蒸馏水摇匀加入上述紫外比色皿中; (5)再取 O.lmg无 色清亮液, 逐渐用微量进样器加到紫外比色皿中, 边加样边加入甲醛显色剂, 静置 20min后在紫外可见分光光度仪上检测即可判断结果。 步骤 (5)中的甲醛显色 剂为酚试剂; 酚试剂的浓度为 0.015g/ml。
本发明的实施方式
[0009] 实施例 2本发明为一种测量液体中甲醛含量的方法, 包括下列步骤: (1)取 10g 待测液体在高速离心机上离心得上层液; (2)取上述上层液, 转入超滤杯, 在室 温条件下使用超滤膜用超滤器超滤, 收取滤出的无色清亮液, 在零下 10度保存 , 以供测量; (3)将甲醛显色剂加到洁净的紫外比色皿中; (4)称取 15g氢氧化钠 于容量瓶中, 再加入 28ml蒸馏水摇匀加入上述紫外比色皿中; (5)再取 O. lmg无色 清亮液, 逐渐用微量进样器加到紫外比色皿中, 边加样边加入甲醛显色剂, 静 置 30min后在紫外可见分光光度仪上检测即可判断结果。 步骤 (5)中的甲醛显色剂 为酚试剂; 酚试剂的浓度为 0.015g/ml。 实施例 3本发明为一种测量液体中甲醛含 量的方法, 包括下列步骤: (1)取 10g待测液体在高速离心机上离心得上层液; (2)取上述上层液, 转入超滤杯, 在室温条件下使用超滤膜用超滤器超滤, 收取 滤出的无色清亮液, 在零下 10度保存, 以供测量; (3)将甲醛显色剂加到洁净的 紫外比色皿中; (4)称取 12g氢氧化钠于容量瓶中, 再加入 24ml蒸馏水摇匀加入 上述紫外比色皿中; (5)再取 O. lmg无色清亮液, 逐渐用微量进样器加到紫外比色 皿中, 边加样边加入甲醛显色剂, 静置 25min后在紫外可见分光光度仪上检测即 可判断结果。 步骤 (5)中的甲醛显色剂为酚试剂; 酚试剂的浓度为 0.015g/ml。 本 发明显色反应快, 只需大约一分钟, 测定条件相对也宽松, 而且灵敏度高, 成 本低, 在原奶检测中干扰也小, 对于大中型乳品企业或饮料企业来说, 是一种 非常适用于普及的快速检测液体中含甲醛的方法。
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
一种测量液体中甲醛含量的方法, 包括下列步骤: ω取 iog待测液体 在高速离心机上离心得上层液; (2)取上述上层液, 转入超滤杯, 在 室温条件下使用超滤膜用超滤器超滤, 收取滤出的无色清亮液, 在零 下 10度保存, 以供测量; (3)将甲醛显色剂加到洁净的紫外比色皿中 ; (4)称取 10-15g氢氧化钠于容量瓶中, 再加入 20-28ml蒸馏水摇匀加 入上述紫外比色皿中; (5)再取 O.lmg无色清亮液, 逐渐用微量进样器 加到紫外比色皿中, 边加样边加入甲醛显色剂, 静置 20-30min后在紫 外可见分光光度仪上检测即可判断结果。
根据权利要求 1所述的测量液体中甲醛含量的方法, 其特征在于: 所 述步骤 (5)中的甲醛显色剂为酚试剂。
根据权利要求 2所述的测量液体中甲醛含量的方法, 其特征在于: 所 述酚试剂的浓度为 0.015g/ml。
PCT/CN2016/112577 2015-12-30 2016-12-28 一种测量液体中甲醛含量的方法 WO2017114406A1 (zh)

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CN105606603A (zh) * 2015-12-30 2016-05-25 田琳琳 一种测量液体中甲醛含量的方法
CN109856068B (zh) * 2019-01-17 2021-08-24 浙江理工大学 一种基于Mannich反应的甲醛检测试剂及检测方法

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