CN110687088A - Method for detecting fluorescent substance in toilet paper product - Google Patents
Method for detecting fluorescent substance in toilet paper product Download PDFInfo
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- CN110687088A CN110687088A CN201910995107.7A CN201910995107A CN110687088A CN 110687088 A CN110687088 A CN 110687088A CN 201910995107 A CN201910995107 A CN 201910995107A CN 110687088 A CN110687088 A CN 110687088A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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- Immunology (AREA)
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- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention provides a method for detecting fluorescent substances in toilet paper products, which comprises the following steps: s1, extracting the paper sample by using an extracting agent, filtering the extracted paper sample by using a glass funnel, and then adjusting the pH value of the filtrate to 3.0-5.0 by using a hydrochloric acid solution; immersing clean gauze in the filtrate, heating in a constant-temperature oscillating water bath at the temperature of 38-42 ℃ for 30min, taking out sample gauze by using tweezers, then squeezing the filtrate, folding the filtrate into four layers, and placing the layers on a glass surface dish; s2, carrying out blank control test according to the step S1 except that no sample is added; s3, placing the glass surface vessel on which the sample gauze and the blank control gauze are placed under an ultraviolet lamp to observe the fluorescence phenomenon of the gauzes, and performing at least two parallel measurements on each piece of gauze; and S4, comparing the two parallel measurements of the sample gauze and the blank control gauze to obtain a conclusion, wherein the reliability of the detection result is high.
Description
Technical Field
The invention relates to the technical field of toilet paper detection, in particular to a method for detecting fluorescent substances in a toilet paper product.
Background
In the production process of toilet paper, in order to ensure the whiteness of paper, manufacturers add fluorescent whitening agents into paper pulp, although the visual whiteness of the finished paper is improved, the fluorescent whitening agents are absorbed by human bodies when the fluorescent whitening agents are contacted with skin, and then the fluorescent whitening agents are accumulated in the human bodies, so that the immunity of the human bodies is weakened, the burden of livers is increased, and cell distortion can be caused. When contacting human body, it will enter into body along with pores, and will cause serious harm to human skin, viscera and various systems. Investigations from japan have indicated that fluorescent whitening agents directly enter mammary glands in large quantities with female underwear, directly causing the development of breast cancer and dire lesions such as skin cancer.
One of the disadvantages of the existing detection technology is that the toilet paper product has no fluorescence phenomenon in qualitative detection, and the content of the fluorescent whitening agent can be measured by adopting an ultraviolet quantitative method in the related standard, which has potential influence on the product sale.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for detecting fluorescent substances in toilet paper products, which probes the specific sources of the fluorescent substances, detects and analyzes that no migratable fluorescent whitening agent exists in the raw materials, and is simple and practical.
In order to solve the technical problems, the invention is realized by the following technical scheme:
a method for detecting fluorescent substances in toilet paper products comprises the following steps:
s1, placing the paper sample in a triangular beaker, adding the extraction liquid into the flask, extracting at room temperature under the condition of slowly shaking the flask, filtering by using a glass funnel, and then adjusting the pH value of the filtrate to 3.0-5.0 by using a hydrochloric acid solution; immersing clean gauze in the filtrate, heating in a constant-temperature oscillating water bath at the temperature of 38-42 ℃ for 30min, taking out sample gauze by using tweezers, then squeezing the filtrate, folding the filtrate into four layers, and placing the layers on a glass surface dish;
s2, carrying out a blank control test according to the step S1 except that no sample is added to obtain blank control gauze;
s3, placing the glass surface vessel on which the sample gauze and the blank control gauze are placed under an ultraviolet lamp to observe the fluorescence phenomenon of the gauzes, and performing at least two parallel measurements on each piece of gauze, namely measuring the fluorescence of one piece of gauze at least twice;
s4, two replicates of sample gauze and blank control gauze were compared:
a, judging that the sample has no migratable fluorescent whitening agent if no obvious fluorescent phenomenon exists;
b, if at least one sample gauze has more obvious fluorescence phenomenon than a blank control gauze, performing two parallel tests again, namely if one of the gauzes is found to have the fluorescence phenomenon, re-testing a batch of sample gauzes to confirm, and if the sample gauzes after the re-test and the blank control gauze have no obvious fluorescence phenomenon, judging that the sample has no migratable fluorescent whitening agent; otherwise, judging that the sample has the migratable fluorescent whitening agent.
Preferably, in step S1, the extract is an aqueous ammonia solution.
Preferably, in the step S2, the ultraviolet lamp has a wavelength of 254nm and 365nm, and the gauze is placed 20cm away from the ultraviolet lamp.
The technical scheme of the invention has the following beneficial effects:
according to the specific source of the fluorescent substance, the invention detects and analyzes whether the migratable fluorescent whitening agent exists in the raw material by a simple and practical method, and the reliability of the detection result is high.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description is given with reference to specific embodiments.
The toilet paper product has no fluorescence phenomenon in qualitative detection, and the content of the fluorescent whitening agent can be measured by adopting an ultraviolet quantitative method in a related standard, so that potential influence is caused on the product sale.
In order to solve the technical problems of the present application, the present invention starts from the research of the test method and studies on the source of the fluorescent whitening agent and the mobility of the fluorescent whitening agent and the corresponding measures. The method mainly comprises the following steps:
1. preparation of experimental materials:
the Sagittaria sagittifolia, the dendrocalamus latiflorus, the yellow bamboos and the green bamboo used in the experiment are all typical bamboo raw materials in the Liangwen paper industry, the raw material base of Chongqing Liangwen paper industry is taken, the age of the selected sample bamboo is 2-3 years, and after each plant is fell down, bamboo sections are cut upwards from several parts of a bamboo pole and marked. Samples with the length of about 5cm are respectively cut from the bamboo joints at the bottom, the middle part and the top of the bamboo pole and the hollow part in a laboratory and are used as samples to be detected of the fluorescence phenomenon. Meanwhile, the bamboo sections are sliced and prepared and then placed in a plastic bag to balance moisture for later use.
2. The systematic research is carried out on more than ten detection standard methods related to paper product fluorescent substances at home and abroad, and the advantages and the disadvantages, the applicability and the influence factors of various methods are compared; the analysis method which is reliable, relatively convenient and suitable for the migratable fluorescent whitening agent in the production process is preferably selected.
3. After comparing more than ten detection standard methods related to paper product fluorescent substances at home and abroad, the various methods have advantages and disadvantages, but standard procedures are needed to ensure the stability of the analysis result of the fluorescent substances. From the aspect of simplicity and practicability, the fluorescent whiteness method can be used for assisting in judging whether the product contains the fluorescent whitening agent, and the method is the simplest and the most practical and is suitable for actual production.
4. The core problem is as follows: the research on the fact that fluorescent whitening agent is not added in the production process of toilet paper products, fluorescent phenomenon does not occur in qualitative detection, and the content of the fluorescent whitening agent can be measured by using an ultraviolet quantitative method in related standards by some media and customers is carried out, and a large amount of research finds that interference caused by shoulders of lignin dissolved in the fluorescent substance detection and extraction process at 330-340 nm and the vicinity of 348nm of the fluorescent whitening agent measurement is the main cause of the problems.
5. Under the specified test conditions, the fluorescent whitening agent transferred to the extraction solution in the paper and board is measured and, after qualitative determination, quantified, to determine whether the "migratable fluorescent whitening agent" is contained in the toilet paper.
6. Sample preparation: extraction of toilet paper product: 2.0g of the sample was accurately weighed and placed in a Erlenmeyer flask. 100ml of an extract-aqueous ammonia solution was added to the flask, and the mixture was extracted at room temperature for 10min while slowly shaking the flask, mainly for adjusting the pH, and then filtered through a glass funnel. And adjusting the pH value of the filtrate to 3.0-5.0 by using a hydrochloric acid solution. Soaking gauze in the filtrate, and heating in constant temperature oscillating water bath at 40 + -2 deg.C for 30 min. The gauze was removed with tweezers to obtain gauze with a sample (sample gauze) and the filtrate was squeezed dry and folded into four layers and placed on a glass petri dish.
7. And (4) carrying out a blank control test according to the step (6) except that no sample is added, so as to obtain blank control gauze.
8. And (3) testing: the glass surface vessel on which the sample gauze and the blank test gauze are placed is placed in an ultraviolet lamp (with the wavelength of 254nm and the wavelength of 365nm) in a dark room or a dark box, the ultraviolet lamp and the sample gauze are simultaneously turned on, and the fluorescence phenomenon of the gauze is observed at the position of about 20cm below the ultraviolet lamp. Two replicates of each sample were performed.
9. And (4) judging a result: if the sample gauze of the two parallel tests has no obvious fluorescence phenomenon compared with the blank test gauze, judging that the sample has no migratable fluorescent whitening agent; if one of the sample gauzes in the two parallel tests has a fluorescence phenomenon more obvious than that of the blank test gauze, performing the two parallel tests again; if the sample gauze after the retest does not have obvious fluorescence phenomenon compared with the blank test gauze, judging that the sample does not have the migratable fluorescent whitening agent; otherwise, judging that the sample has the migratable fluorescent whitening agent.
10. In order to further confirm whether the toilet paper products, bamboo raw materials and handsheets with different bleaching nodes contain the migratable fluorescent whitening agent; and whether the bamboo raw material has the migration of the migratable fluorescent whitening agent in the pulping process is explored, and a high performance liquid chromatography (HPLC-FLD) method with a fluorescence detector with higher precision is adopted to qualitatively and quantitatively determine toilet paper products, the bamboo raw material and samples of all nodes in the pulping process.
11. The results after the measurement show that although individual fluorescent point phenomena can be observed in the bamboo raw materials and the handsheets, the subsequent qualitative and quantitative detection results of HPLC-FLD show that no migratable fluorescent whitening agent is found in the four bamboo raw materials of natural color toilet paper, white toilet paper, Sasa albo-marginata, dendrocalamus latiflorus, yellow bamboo and Phyllostachys glauca and the cooking black liquor in the pulping process thereof, and the handsheets and bleaching wastewater of each node in the D0-E-D1 bleaching process. The result of the qualitative analysis is consistent, and the detection method is proved to have high reliability.
12. After systematic study on the problem of fluorescence of toilet paper, four countermeasures are studied for the problem of fluorescent substance of toilet paper.
And (4) conclusion: through fluorescence phenomenon detection, migration fluorescent whitening agent qualitative determination and high performance liquid chromatography reconfirmation with a fluorescence detector, liquid and solid samples of each node in the process of producing pulp by a typical bamboo raw material are subjected to systematic analysis and test, and although individual fluorescent point phenomena can be observed in the bamboo raw material and handsheets, the fluorescent phenomena are originated from natural bamboo raw materials and are specific fluorescent effects existing in some plants in the nature, and systematic detection and analysis do not find the migration.
Compared with the prior art, the application has the following positive effects:
1. the specific source of the fluorescent substance is explored, and the detection and analysis show that no migratable fluorescent whitening agent exists in the raw material.
2. The selection and attention points of raw and auxiliary materials in the production process are researched.
3. Promotes the establishment of relevant policy standards and protects the vital interests of companies.
4. Discloses a method for detecting the fluorescent substance, protects the right of the consumer to know and allows the consumer to purchase the fluorescent substance at ease.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (3)
1. A method for detecting fluorescent substances in toilet paper products is characterized by comprising the following steps:
s1, placing the paper sample in a triangular beaker, adding the extraction liquid into the flask, extracting at room temperature under the condition of slowly shaking the flask, filtering by using a glass funnel, and then adjusting the pH value of the filtrate to 3.0-5.0 by using a hydrochloric acid solution; immersing clean gauze in the filtrate, heating in a constant-temperature oscillating water bath at the temperature of 38-42 ℃ for 30min, taking out sample gauze by using tweezers, then squeezing the filtrate, folding the filtrate into four layers, and placing the layers on a glass surface dish;
s2, carrying out a blank control test according to the step S1 except that no sample is added to obtain blank control gauze;
s3, placing the glass surface vessel on which the sample gauze and the blank control gauze are placed under an ultraviolet lamp to observe the fluorescence phenomenon of the gauzes, and performing at least two parallel measurements on each piece of gauze, namely measuring the fluorescence of one piece of gauze at least twice;
s4, two replicates of sample gauze and blank control gauze were compared:
a, judging that the sample has no migratable fluorescent whitening agent if no obvious fluorescent phenomenon exists;
b, if at least one sample gauze has more obvious fluorescence phenomenon than a blank control gauze, performing two parallel tests again, namely if one of the gauzes is found to have the fluorescence phenomenon, re-testing a batch of sample gauzes to confirm, and if the sample gauzes after the re-test and the blank control gauze have no obvious fluorescence phenomenon, judging that the sample has no migratable fluorescent whitening agent; otherwise, judging that the sample has the migratable fluorescent whitening agent.
2. The method for detecting fluorescent substances in toilet paper products according to claim 1, wherein the extract in step S1 is an aqueous ammonia solution.
3. The method for detecting fluorescent substances in a hygiene paper product according to claim 1, wherein the ultraviolet lamp has a wavelength of 254nm or 365nm and the gauze is placed at a distance of 20cm from the ultraviolet lamp in step S2.
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| CN201910995107.7A CN110687088A (en) | 2019-10-18 | 2019-10-18 | Method for detecting fluorescent substance in toilet paper product |
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| CN201910995107.7A CN110687088A (en) | 2019-10-18 | 2019-10-18 | Method for detecting fluorescent substance in toilet paper product |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113376272A (en) * | 2021-05-28 | 2021-09-10 | 江苏天成纸业有限公司 | Efficient detection method capable of detecting multiple fluorescent whitening agents in paper product |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101122567A (en) * | 2007-05-11 | 2008-02-13 | 广东出入境检验检疫局检验检疫技术中心 | Method and device for quickly detecting fluorescent whitening agent of paper and paper board |
| CN103063638A (en) * | 2012-12-27 | 2013-04-24 | 通标标准技术服务(上海)有限公司 | Rapid detection method for fluorescent whitening agent on fabrics |
| CN105823738A (en) * | 2015-01-05 | 2016-08-03 | 广东省东莞市质量监督检测中心 | Method for measuring content of transportable fluorescent brightener in paper product |
| CN107084936A (en) * | 2017-04-24 | 2017-08-22 | 沃奇中 | The assay method of transportable property fluorescent whitening agent in toilet paper |
-
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- 2019-10-18 CN CN201910995107.7A patent/CN110687088A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101122567A (en) * | 2007-05-11 | 2008-02-13 | 广东出入境检验检疫局检验检疫技术中心 | Method and device for quickly detecting fluorescent whitening agent of paper and paper board |
| CN103063638A (en) * | 2012-12-27 | 2013-04-24 | 通标标准技术服务(上海)有限公司 | Rapid detection method for fluorescent whitening agent on fabrics |
| CN105823738A (en) * | 2015-01-05 | 2016-08-03 | 广东省东莞市质量监督检测中心 | Method for measuring content of transportable fluorescent brightener in paper product |
| CN107084936A (en) * | 2017-04-24 | 2017-08-22 | 沃奇中 | The assay method of transportable property fluorescent whitening agent in toilet paper |
Non-Patent Citations (3)
| Title |
|---|
| 华人民共和国卫生部: "《GB11680-89食品包装用原纸卫生标准》", 30 July 1990, 中国标准出版社, pages: 1 - 4 * |
| 屈鹏峰 等: "纱布吸附_紫外灯照射法测定食品接触纸及其制品中荧光增白剂", 《中国食品卫生杂志》 * |
| 屈鹏峰 等: "纱布吸附_紫外灯照射法测定食品接触纸及其制品中荧光增白剂", 《中国食品卫生杂志》, vol. 28, no. 3, 31 December 2016 (2016-12-31), pages 352 - 355 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113376272A (en) * | 2021-05-28 | 2021-09-10 | 江苏天成纸业有限公司 | Efficient detection method capable of detecting multiple fluorescent whitening agents in paper product |
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