CN101957298A - Method for reducing detection error of pulp dichloromethane extract for acetate fiber - Google Patents
Method for reducing detection error of pulp dichloromethane extract for acetate fiber Download PDFInfo
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- CN101957298A CN101957298A CN 201010256174 CN201010256174A CN101957298A CN 101957298 A CN101957298 A CN 101957298A CN 201010256174 CN201010256174 CN 201010256174 CN 201010256174 A CN201010256174 A CN 201010256174A CN 101957298 A CN101957298 A CN 101957298A
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Abstract
The invention relates to a method for detecting an extract, in particular to a method for reducing the detection error of a pulp dichloromethane extract for an acetate fiber. The method for reducing the detection error of the pulp dichloromethane extract for the acetate fiber comprises the following steps of: A, weighing a pulp finished product sample and placing the sample in an extraction tube of an extractor provided with a filtering plate; B, connecting an extraction flask with the extraction tube; C, adding dichloromethane purified through distillation into the extraction flask; D, starting to perform extraction by using a condenser connected with the extractor; and E, after the extraction, placing the extraction flask on a water bath kettle to perform evaporation until a little solution is reserved in the extraction flask and drying the solution to obtain the extract. The method for reducing the detection error of the pulp dichloromethane extract for the acetate fiber has the advantages that: a filtering device is arranged in the extraction tube of the extractor, so the detection error of the extract caused by reflux is reduced on the premise of not influencing the extraction speed; and the filtering device is arranged on the upper part of a reflux pipe orifice at the bottom of the extraction tube, so fine fibers can be effectively filtered so as not to reflow to the flask.
Description
Technical field
The present invention relates to a kind of detection method of extract, specifically is a kind of acetate fiber detects error with pulp methylene chloride extract method that reduces.
Background technology
Acetate fiber has national standard at present with the detection method of pulp methylene chloride extract, but when adopting standard method to detect pulp because pulp is more loose, fiber fines easily is back in the flask with extracting liquid out easily during extraction, because fiber fines proportion is very little, be suspended in easily and be back in the flask in the solvent, there is not filtration unit in the extractor again, can not filter Extract, thereby cause testing result to produce error, influence the accuracy of measurement result, if its testing result is higher, can influence quality assessment to product, and further influence the use of downstream user, it is bigger therefore to detect acetate fiber usefulness pulp methylene chloride extract error with former method.
Summary of the invention
The purpose of this invention is to provide a kind of method that reduces acetate fiber with pulp methylene chloride extract detection error, its particular content is as follows:
A kind of method that reduces acetate fiber with pulp methylene chloride extract detection error, its step comprises:
A, take by weighing pulp finished product sample, put into the extractor extraction tube that is provided with filter;
B, extraction flask is connected with extraction tube;
C, the methylene chloride after will purifying through distillation are added in the extraction flask;
The condenser of D, connection extractor begins to carry out extracting;
After E, extracting finish extraction flask is placed on to be evaporated on the water-bath and remains small volume of solution, oven dry in the extraction flask, obtain extract.
Described filter is arranged on the backflow mouth of pipe of extractor bottom.
Described filter is the quartz sand filtration plate.
Described filter plate hole diameter is 15～40 μ m.
Described extractor is a Soxhlet extractor.
Described extraction flask is a flask.
In the described C step during purification Dichloromethane temperature be 50～60 ℃.
When described D step begins extracting, regulate 70～75 ℃ of bath temperatures, per hour extracting circulation 6-9 time of methylene chloride, and extracting 5～7h.
Be extraction flask to be positioned on the water-bath evaporate in the described E step, with phegma residual in the extraction flask, dry extracting residue 10～12h down to constant weight at 105 ± 2 ℃, weigh after in exsiccator, cooling off 1～2h under the placement normal temperature, by the quality of methylene chloride extract and the over dry mass ratio of sample, try to achieve the content of methylene chloride extract.
The residue small volume of solution is 3～5ml in the described E step.
In concrete operation, extraction flask is placed on to be evaporated on the water-bath remains in the extraction flask small volume of solution, when oven dry, if it is too much to be evaporated to the interior surplus solution of extraction flask, then be unfavorable for next step oven dry, and surplus solution is very few, the surplus solution in this step also might influence the quality of last extract, so should be got 3～5ml.
The invention has the advantages that:
1, utilizing extraction tube inside to be provided with filtration unit at extraction apparatus, under the prerequisite that does not influence extracting speed, error when having reduced the detection extract that causes because reflux, filtration unit is arranged at backflow mouth of pipe top at the bottom of the extraction tube, can effectively filter fiber fines and not allow it be back in the flask.
2, filter is simple in structure, be easy to practical application, quartzy core silica sand claims pickling silica sand again, it is a kind of silicate mineral of hard, wear-resisting, stable chemical performance, its essential mineral composition is SiO2, high temperature resistant, the acid and alkali-resistance that has, organism etc., but hot investment casting, characteristics such as its shaped article thermal expansivity is little.With quartzy core as filter, in process of the test, can be because of being heated or being subjected to chemical reagent corrosion not influence detection accuracy, and quartzy core can use repeatedly as filter, bore dia is that 15～40 μ m can effectively filter out the small fiber of size.
3, guarantee that the extracting number of times is not less than 40 times, can guarantee effectively that the extraction degree of methylene chloride is higher.
Description of drawings
Fig. 1 is the extractor structural representation;
In the accompanying drawing 1, condenser 2, extraction tube 3, extraction flask 4, recirculatory pipe 5, adapting pipe 6, filtration unit
Embodiment
A kind of method that reduces acetate fiber with pulp methylene chloride extract detection error, its step comprises:
A, take by weighing pulp finished product sample, put into the extractor extraction tube that is provided with filter;
B, extraction flask is connected with extraction tube;
C, the methylene chloride after will purifying through distillation are added in the extraction flask;
The condenser of D, connection extractor begins to carry out extracting;
After E, extracting finish extraction flask is placed on to be evaporated on the water-bath and remains small volume of solution, oven dry in the extraction flask, obtain extract.
Described filter is arranged on the backflow mouth of pipe of bottom, filter is the quartz sand filtration plate, the plate hole diameter is 15～40 μ m, extractor is a Soxhlet extractor, extraction flask is a flask, purification Dichloromethane temperature is 50～60 ℃ in the C step, when the D step begins extracting, regulate 70～75 ℃ of bath temperatures, per hour extracting circulation 6-9 time of methylene chloride, and extracting 5～7h like this are extraction flask to be positioned on the water-bath evaporate in the E step, with phegma residual in the extraction flask, 105 ± 2 ℃ down oven dry extracting residue 10～12h in exsiccator, place and weigh after cooling off 1～2h under the normal temperature, by the quality of methylene chloride extract and the over dry mass ratio of sample to constant weight, try to achieve the content of methylene chloride extract, the residue small volume of solution is 3～5ml in the E step.
The extracting of vegetable fibre organism also can be used this method, as mensuration of paper making raw material alcohol-benzene extractive and ether extract etc.
The employed extraction apparatus structural principle of this method is introduced:
Comprise condenser 1, extraction tube 2 and extraction flask 3, the three is communicated with successively, extraction tube 2 is provided with recirculatory pipe 4 and adapting pipe 5, it is characterized in that: described extraction tube 2 inside are provided with filtration unit 6, and filtration unit 6 is arranged at 4 mouthfuls of tops of recirculatory pipe, 2 end of extraction tube, and filtration unit 6 is a filter, filter is quartzy core filter, the filter bore dia is 15～40 μ m, and condenser 1 is preferred ball condenser 1, and extraction flask 3 is preferably flat bottom flask.
Adapting pipe 5 is sent condensation in the condenser 1 at pure Dichloromethane steam (vapor) outlet with steam; The pure Dichloromethane of condenser 1 cooling evaporation is back in the extraction tube 2 cooled Dichloromethane, effectively contacts with sample, the lipid of sample dissolution, benzene class material; The Dichloromethane phegma of extraction tube 2 splendid attire samples and cooling; Extraction flask 3 dress Dichloromethane and extracts; Recirculatory pipe 4 utilizes siphon principle, is dissolved in the matter in the Dichloromethane having extracted out in the sample, is back in the extraction flask 3; Filtration unit 6 filters fiber fines and impurity.
Embodiment 1
A kind of method that reduces acetate fiber with pulp methylene chloride extract detection error, its step comprises:
Take by weighing and on the backflow mouth of pipe of bottom the quartz sand filtration plate is installed after pulp finished product sample 25g puts into transformation, the plate hole diameter is that what other filtered if desired also can install and use in the 15 μ m filtration unit Soxhlet extractors,
And the flat bottom flask of constant weight is connected on the extractor, because helping in process of the test the stable of flask, puts by flat bottom flask, so the preferred extraction flask of this method is a flat bottom flask.
The methylene chloride that adds after 310ml purifies through distillation is in the flat bottom flask of 500ml and weight in capacity.
Connect condenser and also begin to carry out extracting, regulate 70 ℃ of bath temperatures, guarantee per hour extracting circulation 9 times of methylene chloride, and about 5h of extracting like this, it is 40 times that total extracting cycle index is not less than.
After extracting finishes flat bottom flask is placed on the water-bath and evaporates, to the residual about 7ml phegma of flat bottom flask, 103 ℃ down oven dry extracting residues be no more than 12h, and dry to constant weight, in exsiccator, be placed on and weigh after cooling off 1h under the normal temperature.By the quality of methylene chloride extract and the over dry mass ratio of sample, try to achieve the content of methylene chloride extract.
Embodiment 2
A kind of method that reduces acetate fiber with pulp methylene chloride extract detection error, its step comprises:
Take by weighing and on the backflow mouth of pipe of bottom the quartz sand filtration plate is installed after pulp finished product sample 25g puts into transformation, the plate hole diameter is that what other filtered if desired also can install and use in the 40 μ m filtration unit Soxhlet extractors.
And the flat bottom flask of constant weight is connected on the extractor, because helping in process of the test the stable of flask, puts by flat bottom flask, so the preferred extraction flask of this method is a flat bottom flask.
The methylene chloride that adds after 290ml purifies through distillation is in the flat bottom flask of 500ml and weight in capacity.
Connect condenser and also begin to carry out extracting, regulate 75 ℃ of bath temperatures, guarantee per hour extracting circulation 6 times of methylene chloride, and about 7h of extracting like this, it is 40 times that total extracting cycle index is not less than.
After extracting finishes flat bottom flask is placed on the water-bath and evaporates, to the residual about 4ml phegma of flat bottom flask, 107 ℃ down oven dry extracting residues be no more than 10h, and dry to constant weight, in exsiccator, be placed on and weigh after cooling off 2h under the normal temperature.By the quality of methylene chloride extract and the over dry mass ratio of sample, try to achieve the content of methylene chloride extract.
Embodiment 3
A kind of method that reduces acetate fiber with pulp methylene chloride extract detection error, its step comprises:
Take by weighing and on the backflow mouth of pipe of bottom the quartz sand filtration plate is installed after pulp finished product sample 25g puts into transformation, the plate hole diameter is: in the 25 μ m filtration unit Soxhlet extractors, what other filtered if desired also can install and use.
And the flat bottom flask of constant weight is connected on the extractor, because helping in process of the test the stable of flask, puts by flat bottom flask, so the preferred extraction flask of this method is a flat bottom flask.
The methylene chloride that adds after 300ml purifies through distillation is in the flat bottom flask of 500ml and weight in capacity.
Connect condenser and also begin to carry out extracting, regulate 72 ℃ of bath temperatures, guarantee per hour extracting circulation 8 times of methylene chloride, and about 6h of extracting like this, it is 40 times that total extracting cycle index is not less than.
After extracting finishes flat bottom flask is placed on the water-bath and evaporates, to the residual about 5ml phegma of flat bottom flask, 105 ℃ down oven dry extracting residues be no more than 11h, and dry to constant weight, in exsiccator, be placed on and weigh after cooling off 1.5h under the normal temperature.By the quality of methylene chloride extract and the over dry mass ratio of sample, try to achieve the content of methylene chloride extract
The invention is not restricted to above embodiment, all patent claims of the present invention institute content all belongs to this patent protection domain.
Claims (10)
1. one kind is reduced the method that acetate fiber is used pulp methylene chloride extract detection error, and its step comprises:
A, take by weighing pulp finished product sample, put into the extractor extraction tube that is provided with filter;
B, extraction flask is connected with extraction tube;
C, the methylene chloride after will purifying through distillation are added in the extraction flask;
The condenser of D, connection extractor begins to carry out extracting;
After E, extracting finish extraction flask is placed on to be evaporated on the water-bath and remains small volume of solution in the extraction flask, oven dry obtains extract.
2. a kind of method that reduces acetate fiber with pulp methylene chloride extract detection error according to claim 1, it is characterized in that: described filter is arranged on the backflow mouth of pipe of extractor bottom.
3. a kind of method that reduces acetate fiber with pulp methylene chloride extract detection error according to claim 1, it is characterized in that: described filter is the quartz sand filtration plate.
4. a kind of method that reduces acetate fiber with pulp methylene chloride extract detection error according to claim 1, it is characterized in that: described filter plate hole diameter is 15～40 μ m.
5. a kind of method that reduces acetate fiber with pulp methylene chloride extract detection error according to claim 1, it is characterized in that: described extractor is a Soxhlet extractor.
6. a kind of method that reduces acetate fiber with pulp methylene chloride extract detection error according to claim 1, it is characterized in that: described extraction flask is a flask.
7. detect the method for error according to any described a kind of acetate fiber that reduces of claim 1-4 with pulp methylene chloride extract, it is characterized in that: in the described C step during purification Dichloromethane temperature be 50～60 ℃.
8. according to any described a kind of acetate fiber detects error with pulp methylene chloride extract the method that reduces of claim 1-4, it is characterized in that: when described D step begins extracting, regulate 70～75 ℃ of bath temperatures, per hour extracting circulation 6-9 time of methylene chloride, and extracting 5～7h.
9. according to any described a kind of acetate fiber detects error with pulp methylene chloride extract the method that reduces of claim 1-4, it is characterized in that: be extraction flask to be positioned on the water-bath evaporate in the described E step, with phegma residual in the extraction flask, dry extracting residue 10～12h down to constant weight at 105 ± 2 ℃, weigh after in exsiccator, cooling off 1～2h under the placement normal temperature, by the quality of methylene chloride extract and the over dry mass ratio of sample, try to achieve the content of methylene chloride extract.
10. according to any described a kind of method that reduces acetate fiber with pulp methylene chloride extract detection error of claim 1-4, it is characterized in that: the residue small volume of solution is 3～5ml in the described E step.
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| CN 201010256174 CN101957298A (en) | 2010-08-18 | 2010-08-18 | Method for reducing detection error of pulp dichloromethane extract for acetate fiber |
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| CN 201010256174 CN101957298A (en) | 2010-08-18 | 2010-08-18 | Method for reducing detection error of pulp dichloromethane extract for acetate fiber |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103992880A (en) * | 2014-05-15 | 2014-08-20 | 河北中烟工业有限责任公司 | Volatile oil high-efficiency extraction separator |
| CN106932300A (en) * | 2017-01-10 | 2017-07-07 | 国家纺织服装产品质量监督检验中心（浙江桐乡） | The method whether silk floss increases weight is detected and evaluated using organic solvent |
| CN108181198A (en) * | 2018-01-24 | 2018-06-19 | 苏州中汽检测技术服务有限公司 | A kind of atomization measure device and method |
| CN111912733A (en) * | 2020-08-12 | 2020-11-10 | 威海拓展纤维有限公司 | Method for testing mass fraction of fibers in carbon fiber reinforced nylon plastic |
| CN108181198B (en) * | 2018-01-24 | 2024-05-31 | 苏州中汽检测技术服务有限公司 | Atomization testing device and method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85201170U (en) * | 1985-04-01 | 1986-02-05 | 四川大学 | Soxhlef extractor with the ability of sampling |
| CN2184930Y (en) * | 1993-02-24 | 1994-12-07 | 杨运才 | YS-fully automatic multifunction extractor |
-
2010
- 2010-08-18 CN CN 201010256174 patent/CN101957298A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85201170U (en) * | 1985-04-01 | 1986-02-05 | 四川大学 | Soxhlef extractor with the ability of sampling |
| CN2184930Y (en) * | 1993-02-24 | 1994-12-07 | 杨运才 | YS-fully automatic multifunction extractor |
Non-Patent Citations (1)
| Title |
|---|
| 《GB/T 7979-2005 纸浆 二氯甲烷抽出物的测定》 20050926 中华人民共和国国家质量监督检验检疫局 《GB/T 7979-2005 纸浆 二氯甲烷抽出物的测定》 1-10 , 1 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103992880A (en) * | 2014-05-15 | 2014-08-20 | 河北中烟工业有限责任公司 | Volatile oil high-efficiency extraction separator |
| CN103992880B (en) * | 2014-05-15 | 2015-12-09 | 河北中烟工业有限责任公司 | A kind of volatile oil high efficiency extraction separator |
| CN106932300A (en) * | 2017-01-10 | 2017-07-07 | 国家纺织服装产品质量监督检验中心（浙江桐乡） | The method whether silk floss increases weight is detected and evaluated using organic solvent |
| CN108181198A (en) * | 2018-01-24 | 2018-06-19 | 苏州中汽检测技术服务有限公司 | A kind of atomization measure device and method |
| CN108181198B (en) * | 2018-01-24 | 2024-05-31 | 苏州中汽检测技术服务有限公司 | Atomization testing device and method |
| CN111912733A (en) * | 2020-08-12 | 2020-11-10 | 威海拓展纤维有限公司 | Method for testing mass fraction of fibers in carbon fiber reinforced nylon plastic |
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Application publication date: 20110126 |