CN102128899B - Method for measuring N,N-dimethyl formamide residue - Google Patents
Method for measuring N,N-dimethyl formamide residue Download PDFInfo
- Publication number
- CN102128899B CN102128899B CN 201010607598 CN201010607598A CN102128899B CN 102128899 B CN102128899 B CN 102128899B CN 201010607598 CN201010607598 CN 201010607598 CN 201010607598 A CN201010607598 A CN 201010607598A CN 102128899 B CN102128899 B CN 102128899B
- Authority
- CN
- China
- Prior art keywords
- sample
- reaction tube
- extraction
- residual quantity
- assay method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention discloses a method for measuring N,N-dimethyl formamide residue. The method comprises the following steps of: (1) shearing a sample; (2) weighing a certain amount of sample, and putting the sample into a reaction tube; (3) adding methanol solution of naphthalene-D8 into the reaction tube filled with the sample, wherein the mass ratio of the sample to the naphthalene-D8 is 100+/-1:5;(4) putting the reaction tube into an extraction device to perform extraction; (5) cooling the reaction tube after the extraction is completed; and (6) filling partial extracted solution into an injector, filtering the extracted solution through a polytetrafluoroethylene filter head, then filling the filtrated extracted solution into a sample injection bottle, and analyzing the extracted solutionin the sample injection bottle through a gas chromatograph-mass spectrometer. The method for measuring the N,N-dimethyl formamide residue is simple in operation, quick and high in accuracy.
Description
Technical field
The present invention relates to a kind of assay method of chemical industry material residual quantity, especially relate to a kind of assay method of DMF residual quantity.
Background technology
DMF is the extremely wide industrial chemicals of a kind of purposes, also is a kind of good solvent of having many uses.DMF is good solvent to multiple superpolymer such as tygon, Polyvinylchloride, polyacrylonitrile, polyamide etc., can be used for wet spinning silk, polyurethane synthetic of the synthon such as polyacrylonitrile fibre; Be used for the plastics masking; Also can remove the paint stripper of paint; It can also dissolve the pigment of some low solubility, makes pigment with the characteristics of dyestuff.DMF in use can remain in the product when the industrial solvent more or less, and DMF has very large injury to eye, the upper respiratory tract, liver and skin of people etc.For example, in the quality monitoring of textile, need the residual quantity of DMF is analyzed mensuration, to guarantee the quality of product.Yet, there is not now corresponding assay method, how the residual quantity of DMF being analyzed mensuration has become the problem that needs to be resolved hurrily.
Summary of the invention
The defective that the present invention be directed to the existence of above-mentioned background technology provides a kind of assay method of DMF residual quantity, and the method is simple to operate, quick, accuracy is high.
For achieving the above object, the invention discloses a kind of assay method of DMF residual quantity, it comprises the steps:
Further, described extraction equipment is the ultrasonic extraction device.
Further, the water temperature of described extraction equipment is 40 ℃.
Further, the time that extracts in the described extraction equipment is 60 minutes.
Further, described step
For the reaction tube after extraction is finished is cooled to room temperature (20-25 ℃).
Further, described step
For sample being cut into the blockage of 5 * 5 mm in sizes, and sample mix is even.
In sum, N of the present invention, the assay method of dinethylformamide residual quantity passes through naphthalene-D8 as internal standard compound, it can be separated by chromatographic column, the again not interference of other component peaks in the test sample, as long as measure peak area and the relative response of internal standard compound and component to be measured, can obtain the percentage composition of component to be measured in sample, thereby simple to operate, to reach accuracy fast high.
Embodiment
For further understanding feature of the present invention, technological means and the specific purposes that reach, function, below in conjunction with embodiment the present invention is described in further detail.
The assay method of DMF residual quantity of the present invention comprises the steps:
, sample is cut into the blockage of 5 * 5 mm in sizes, and sample mix is even.
, by electronic balance take by weighing 1 ± 0.01 the gram sample place 40 milliliters with the reaction tube of screw top.
, pipette 10 milliliters of methanol solutions that contain naphthalene-D8 of 5mg/mL with transfer pipet, in the reaction tube that fills sample.
, reaction tube is placed water temperature is 40 ℃ ± 2 ℃ ultrasonic extraction device, extracts 60 minutes.
, extraction is cooled to room temperature (20-25 ℃) with reaction tube after finishing.
, get the part extraction solution syringe of packing into, by gas chromatograph-mass spectrometer the extraction solution in the sample introduction bottle is analyzed by internal standard method in the sample introduction bottle of after the teflon filtering head filters, packing into.
Parameter when with the chromatographic column gas chromatograph-mass spectrometer extraction solution in the sample introduction bottle being analyzed arranges as follows: one, chromatographic column: (5% phenyl) methyl polysiloxane, nonpolar chromatographic column.Two, the gas chromatograph-mass spectrometer parameter arranges: a, injection port setting: temperature: 250 ℃, and sample introduction pattern: Splitless injecting samples general pressure: 51kpa.B, chromatographic column and furnace temperature setting: post flow: 1mL/min, total flow: 19 mL/min, heating schedule: 40 ℃ (keeping 1 minute), rise to 100 with the programming rate of 10 ℃/min, then the programming rate with 60 ℃/min rises to 300(maintenance 1 minute).C, mass spectrum setting: mass spectrometer interface temperature: 300 ℃; Ion source temperature: 250 ℃; The quadrupole rod temperature: 150 ℃, monitoring ion (m/z): 42,43,56,58,72,73.By measuring peak area and the relative response of internal standard compound naphthalene-D8 and component DMF to be measured, can obtain the percentage composition of component to be measured in sample.
In sum, N of the present invention, the assay method of dinethylformamide residual quantity passes through naphthalene-D8 as internal standard compound, it can be separated by chromatographic column, the again not interference of other component peaks in the test sample, as long as measure peak area and the relative response of internal standard compound and component to be measured, can obtain the percentage composition of component to be measured in sample, thereby simple to operate, to reach accuracy fast high.
The above embodiment has only expressed one embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as limitation of the scope of the invention.Should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with claims.
Claims (6)
1. the assay method of a DMF residual quantity is characterized in that: comprise the steps:
2. the assay method of DMF residual quantity according to claim 1, it is characterized in that: described extraction equipment is the ultrasonic extraction device.
3. the assay method of DMF residual quantity according to claim 1 and 2, it is characterized in that: the water temperature of described extraction equipment is 40 ℃.
4. the assay method of DMF residual quantity according to claim 1 and 2, it is characterized in that: the time that extracts in the described extraction equipment is 60 minutes.
5. the assay method of DMF residual quantity according to claim 1 and 2 is characterized in that: described step
For the reaction tube after extraction is finished is cooled to room temperature 20-25 ℃.
6. the assay method of DMF residual quantity according to claim 1 and 2 is characterized in that: described step
For sample being cut into the blockage of 5 * 5 mm in sizes, and sample mix is even.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010607598 CN102128899B (en) | 2010-12-28 | 2010-12-28 | Method for measuring N,N-dimethyl formamide residue |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010607598 CN102128899B (en) | 2010-12-28 | 2010-12-28 | Method for measuring N,N-dimethyl formamide residue |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102128899A CN102128899A (en) | 2011-07-20 |
| CN102128899B true CN102128899B (en) | 2013-04-10 |
Family
ID=44267065
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010607598 Active CN102128899B (en) | 2010-12-28 | 2010-12-28 | Method for measuring N,N-dimethyl formamide residue |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102128899B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102854265A (en) * | 2012-09-11 | 2013-01-02 | 广州广电计量检测股份有限公司 | Analyzing method of N,N-dimethylformamide in leather and textile products |
| CN103512996B (en) * | 2013-10-22 | 2014-10-22 | 广州广电计量检测股份有限公司 | Analysis method for amide compounds |
| CN104764841A (en) * | 2014-12-30 | 2015-07-08 | 东莞市正明检测技术有限公司 | Detection method for dimethyl formamide content of exhaust gas |
| CN104792887A (en) * | 2014-12-30 | 2015-07-22 | 东莞市正明检测技术有限公司 | A method of measuring the content of dimethylformamide in soil |
| CN108362786B (en) * | 2018-01-10 | 2022-03-08 | 杭州中一检测研究院有限公司 | Rapid solvent extraction analysis method for N, N-dimethylformamide in soil |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2484566Y (en) * | 2001-06-21 | 2002-04-03 | 浙江江山化工股份有限公司 | Chromatographic column determining micro impurity in dimethyl formamide |
-
2010
- 2010-12-28 CN CN 201010607598 patent/CN102128899B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2484566Y (en) * | 2001-06-21 | 2002-04-03 | 浙江江山化工股份有限公司 | Chromatographic column determining micro impurity in dimethyl formamide |
Non-Patent Citations (4)
| Title |
|---|
| N, N- 二甲基甲酰胺的气相色谱分析;高亚琳 等;《河南化工》;20060720;第23卷(第7期);44-45 * |
| 王昊, 王晓宁, 廖青.静态顶空-气相色谱-质谱联用法同时检测涂层织物中的6种异味物质.《北京服装学院学报》.2010,第30卷(第2期), |
| 静态顶空-气相色谱-质谱联用法同时检测涂层织物中的6种异味物质;王昊, 王晓宁, 廖青;《北京服装学院学报》;20100430;第30卷(第2期);54-60 * |
| 高亚琳等.N N- 二甲基甲酰胺的气相色谱分析.《河南化工》.2006 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102128899A (en) | 2011-07-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102128899B (en) | Method for measuring N,N-dimethyl formamide residue | |
| CN106841490A (en) | A kind of method of contained polycyclic aromatic hydrocarbon in detection surrounding air | |
| US10514365B2 (en) | Cooling-assisted inside needle capillary adsorption trap device for analyzing complex solid samples using nano-sorbent | |
| CN103399102B (en) | Method for determining total solanesol in tobaccos and tobacco products | |
| CN104020243B (en) | Detection method for solvent gasoline in air in working place | |
| CN101726533A (en) | Rapid and sensitive method for detecting melamine | |
| CN105891374A (en) | Detection method for measuring eight preservatives in reconstituted tobaccos simultaneously | |
| CN103706146A (en) | Column extraction system and extraction method for organic materials in solid particles | |
| CN103837396B (en) | The digestion procedure of a kind of crystal glass and the assay method of crystal glass lead content | |
| DE102010039275A1 (en) | Method and apparatus for the online determination of the isotopic ratio of chlorine, bromine or sulfur in an organic sample | |
| CN105865891A (en) | Internal standard substance release and escape product enrichment combination device for thermal analyzer and use method of device | |
| CN105181868A (en) | Method for simultaneous detection of 13 benzene compounds and phthalic acid ester compounds in water-borne adhesive and application thereof | |
| CN203965395U (en) | A kind of hyperchannel micro-extraction and washing device | |
| CN103852534A (en) | Detecting method for PBDEs (polybrominated diphenyl ethers) in plastic component of electronic element | |
| CN107543870A (en) | Semi-preparative supercritical fluid chromatograph | |
| CN104807902B (en) | The detection method of benzyldithio toluene and antioxidant in insulating oil | |
| Rossi et al. | Optimization of a flow injection analysis system for multiple solvent extraction | |
| CN105717238A (en) | Method for detecting nuciferine in lotus leaf through liquid chromatography | |
| CN105467054A (en) | Method for measuring PBB (polybrominated biphenyl) and PBDE (polybrominated diphenyl ether) fire retardants in textile with ultra-high performance liquid chromatography | |
| Ayre et al. | Supercritical fluid extraction-a green paradigm in the area of separation science | |
| CN105158382A (en) | Method for detecting fluopicolide in fruits and vegetables | |
| CN203519375U (en) | Airflow type combustible liquid sample extraction device | |
| CN106932421B (en) | A kind of preparation method of organic phase plutonium and organic phase neptunium standard solution | |
| CN203337620U (en) | Pretreatment device suitable for residue analysis of pesticide and veterinary drug | |
| CN106383193A (en) | Detection method for phenylethanolamine in pork |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee | ||
| CP02 | Change in the address of a patent holder |
Address after: 523000, No. four, No. 7 industrial North Road, Songshan hi tech Industrial Development Zone, Guangdong, Dongguan Patentee after: Consumer Testing Technology Co., Ltd. Address before: 523000, B, 8, North Industrial Town, Songshan Lake Science and Technology Industrial Park, Guangdong, Dongguan Patentee before: Consumer Testing Technology Co., Ltd. |
|
| CP01 | Change in the name or title of a patent holder |
Address after: No.7, Gongye North 4th Road, Songshanhu high tech Industrial Development Zone, Dongguan City, Guangdong Province, 523000 Patentee after: Guangdong Zhongding Testing Technology Co.,Ltd. Address before: No.7, Gongye North 4th Road, Songshanhu high tech Industrial Development Zone, Dongguan City, Guangdong Province, 523000 Patentee before: DONGGUAN CONSUMER TESTING TECHNOLOGY Co.,Ltd. |
|
| CP01 | Change in the name or title of a patent holder |