CN102879344A - Method for detecting primary amine in anti-aging agents TMQ - Google Patents
Method for detecting primary amine in anti-aging agents TMQ Download PDFInfo
- Publication number
- CN102879344A CN102879344A CN2012103620863A CN201210362086A CN102879344A CN 102879344 A CN102879344 A CN 102879344A CN 2012103620863 A CN2012103620863 A CN 2012103620863A CN 201210362086 A CN201210362086 A CN 201210362086A CN 102879344 A CN102879344 A CN 102879344A
- Authority
- CN
- China
- Prior art keywords
- solution
- tmq
- primary amine
- aniline
- hydrochloric acid
- 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.)
- Pending
Links
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention relates to a method for detecting primary amine in anti-aging agents TMQ. The method comprises the following steps of: preparing aniline standard solutions with different concentrations and a standard reference solution, respectively measuring the absorbance of the different aniline standard solutions under the condition of the wavelength of 437 nanometers by using an ultraviolet and visible spectrophotometer and the 1cm optical path of a cuvette, and drawing a standard curve of the aniline standard solutions by using the standard reference solution as a comparison solution; measuring the absorbance of a sample solution by the same method by using a sample reference solution as a comparison solution; performing quantitative analysis by the aniline standard curve to obtain the content of the primary amine in the anti-agents TMQ in a sample. By the method, the content of the primary amine in the anti-aging agents TMQ can be accurately detected, instruments are simple, and the method is easy and convenient to operate and high in accuracy.
Description
Technical field
The present invention relates to a kind of detection method of primary amine, particularly rubber antioxidant 2,2, the detection method of primary amine in the 4-trimethyl-1,2-dihyaroquinoline polymkeric substance (TMQ).Belong to the rubber antioxidant analysis technical field.
Background technology
Aging resister TMQ is one of rubber antioxidant kind of performance brilliance, and the existence meeting of the objectionable constituent primary amine in this product exerts an influence to the reversion of insoluble sulfur, when primary amine content is higher, with its half finished rubber that makes the bloom phenomenon occurs easily.Detection to primary amine content is the important means that guarantees aging resister TMQ quality.But only have now the HPLC method to measure the aniline content of one of primary amine, can not measure whole primary amine content by the HPLC method.Existing method can not detect the content of primary amine fully, can only detect the aniline content in the primary amine.This experimental technique is exactly in order to detect the content of the primary amine among the aging resister TMQ, can to reduce its content by process modification in order to advance.
Summary of the invention
The object of the present invention is to provide the detection method of primary amine among a kind of aging resister TMQ, this method is utilized spectrophotometric determination, and is simple to operate, error is little.
Technical scheme of the present invention is as follows:
The detection method of primary amine among a kind of aging resister TMQ comprises that preparation, ultraviolet-visible pectrophotometer analysis operation, the result of reagent calculates three detection computations unit compositions; Concrete steps are as follows:
1) preparation variable concentrations aniline standard solution and criterion referenced solution, use ultraviolet-visible pectrophotometer, cuvette 1cm light path, measure respectively the absorbance of different aniline standard solution at 437nm, do reference solution with criterion referenced solution, draw the typical curve of aniline standard solution;
2) same method is measured the absorbance of sample solution, does reference solution with sample with reference to solution;
3) carry out quantitative test by the aniline typical curve and draw in the sample content of primary amine among the aging resister TMQ.
The detection method of primary amine among the aging resister TMQ of the present invention when preparing the aniline standard solution of variable concentrations, accurately adds paradime thylaminobenzaldehyde solution in each volumetric flask.
Aniline criterion referenced solution: in volumetric flask, add the 2N hydrochloric acid solution, then add paradime thylaminobenzaldehyde solution, add to scale mark, leave standstill more than 30 minutes as aniline criterion referenced solution with methyl alcohol.
The preparation sample solution: aging resister TMQ sample places separating funnel, adds the chloroform dissolving; Add the 2N hydrochloric acid solution, shake fast after being divided into two solution phases, below chloroform phase solution phase is separated from funnel, will contain the top solution phase of hydrochloric acid, use the funnel with filter paper to filter, collect; Add paradime thylaminobenzaldehyde solution and hydrochloric acid solution, be diluted to scale with methyl alcohol.
The detection method of primary amine among the aging resister TMQ of the present invention, its quantitative analysis method is:
The consistent mg level amine content of the maximum absorbance at 437nm place has following rule:
C%=A*M*a/W*1000*b*100%
C represents the primary amine concentration of percentage composition
A represents that unit is mg/ml according to the concentration of the definite primary amine of typical curve
W represents the TMQ sample quality, and unit is g,
The volume of M volumetric flask, unit are ml,
The volume of a hydrochloric acid phase, unit are ml,
B pipettes the volume of hydrochloric acid phase, and unit is ml.
The present invention can detect the content of primary amine among the aging resister TMQ exactly, and instrument is simple, and is easy and simple to handle, and degree of accuracy is high.
Description of drawings
Fig. 1: concentration of aniline absorbance relation curve.
Embodiment
One, reagent preparation:
1.1% paradime thylaminobenzaldehyde (DMAB) solution: in the 500ml volumetric flask, take by weighing 5g DMAB and be dissolved in 250ml 7% hydrochloric acid, be diluted to 500ml with methyl alcohol;
2.1g/L the aniline standard solution: 100.0+/-0.1mg aniline is dissolved in the 100ml volumetric flask in the 30ml 2N hydrochloric acid.Then, solution is diluted to the volumetric flask groove with methyl alcohol.Attention: because the near room temperature of temperature is treated in hydrochloric acid and methyl alcohol reaction, supply the volume of contraction with methyl alcohol.
Two, drawing standard curve:
1. the standard solution for preparing 6 concentration differences (1%, 2%, 3%, 4%, 5%, 6%): in 6 100ml volumetric flasks, move into respectively 1ml, 2ml, 3ml, 4ml, 5ml, 6ml aniline standard solution with transfer pipet, add successively again 2N hydrochloric acid solution 39ml, 38ml, 37ml, 36ml, 35ml, 34ml, in every part of solution, add 20ml DMAB solution, then, add methyl alcohol vacant most of volume is filled it up with, mixed solution is shaken in rotation gently.Solution left standstill to room temperature, is diluted to the groove place with methyl alcohol.
2. after reacting 30 to 60 minutes, do the reference record absorption spectrum with methyl alcohol.According to each bar absorption curve, the maximum absorbance that record shows about the 437nm place, drawing standard curve such as Fig. 1.
Three, analysis operation:
Take by weighing an amount of TMQ sample W gram (being accurate to 0.0001g), be dissolved in the chloroform with separating funnel.Then, add the hydrochloric acid of a milliliter, shook fast 2 minutes.After being divided into two solution phases, below solution phase (chloroform phase) is separated from funnel, abandon.The top solution phase that will contain hydrochloric acid with funnel and groove Filter paper filtering, is collected and is revolved in mouthful bottle.In solution, pipette in the volumetric flask that the b milliliter changes the M milliliter over to transfer pipet, wherein contain 20% DMAB solution and 20% 2N hydrochloric acid solution.Then, add methyl alcohol vacant most of volume is filled it up with, mixed solution is shaken in rotation gently.Solution left standstill to room temperature, is diluted to the groove place with methyl alcohol.React after 30 to 60 minutes, do the reference record absorption spectrum with methyl alcohol.Be recorded in the maximum absorption wavelength at 437nm place.
Four, computational analysis:
The consistent mg level amine content of the maximum absorbance at 437nm place has following rule:
C%=A*M*a/W*1000*b*100%
C represents the primary amine concentration of percentage composition
A represents that unit is mg/ml according to the concentration of the definite primary amine of typical curve
W represents the TMQ sample quality, and unit is g
The volume of M volumetric flask, unit are ml
The volume of a hydrochloric acid phase, unit are ml
B pipettes the volume of hydrochloric acid phase, and unit is ml.
Embodiment one:
Taking by weighing analysis purified petroleum benzin amine 0.1044g is dissolved in the 100ml volumetric flask in the 30ml 2N hydrochloric acid.Then, solution is diluted to the volumetric flask groove with methyl alcohol, as the aniline standard solution.
In 6 100ml volumetric flasks, move into respectively 1ml, 2ml, 3ml, 4ml, 5ml, 6ml aniline standard solution with transfer pipet, add successively again 2N hydrochloric acid solution 39ml, 38ml, 37ml, 36ml, 35ml, 34ml, in every part of solution, add 20ml DMAB solution, then, add methyl alcohol vacant most of volume is filled it up with, mixed solution is shaken in rotation gently.Left standstill 5 minutes, and be diluted to the groove place with methyl alcohol.
React after 45 minutes, do reference with methyl alcohol, the maximum absorbance that record shows about the 437nm place:
Take by weighing TMQ sample 0.7257g, be dissolved in the 50ml chloroform with separating funnel.Then, add 50ml 2N hydrochloric acid, shook fast 2 minutes.After being divided into two solution phases, below solution phase (chloroform phase) is separated from funnel, abandon.The top solution phase that will contain hydrochloric acid with funnel and groove Filter paper filtering, is collected 50ml and is revolved in mouthful bottle.Draw wherein that 5ml hydrochloric acid layer solution changes in the 100ml volumetric flask, wherein contain 20ml DMAB solution and 20ml 2N hydrochloric acid solution.Then, add methyl alcohol vacant most of volume is filled it up with, mixed solution is shaken in rotation gently.Left standstill 5 minutes, and be diluted to the groove place with methyl alcohol.Solution left standstill to room temperature, is diluted to the groove place with methyl alcohol.React after 45 minutes, do reference with methyl alcohol, the maximum absorbance value at the 437nm place is 1.469.
Calculate: A=0.033453*Q+0.00044
=0.033453*1.469+0.00044
=0.0496mg/ml
C%=A*M*a/W*1000*b*100%
=0.0496*100*50/0.7257*1000*5*100%
=6.83%
Embodiment two:
Take by weighing 8 parts with same aging resister TMQ sample is parallel, utilize the typical curve of making among the embodiment one, carry out sample analysis by the analysis operation method in the embodiment, the result is as follows:
Claims (5)
1. the detection method of primary amine among the aging resister TMQ, the preparation, ultraviolet-visible pectrophotometer analysis operation, the result that comprise reagent calculate three detection computations unit and form; It is characterized in that:
1) preparation variable concentrations aniline standard solution and criterion referenced solution, use ultraviolet-visible pectrophotometer, cuvette 1cm light path, measure respectively the absorbance of different aniline standard solution at 437nm, do reference solution with criterion referenced solution, draw the typical curve of aniline standard solution;
2) same method is measured the absorbance of sample solution, does reference solution with sample with reference to solution;
3) carry out quantitative test by the aniline typical curve and draw in the sample content of primary amine among the aging resister TMQ.
2. the detection method of primary amine among the aging resister TMQ as claimed in claim 1 when it is characterized in that preparing the aniline standard solution of variable concentrations, accurately adds paradime thylaminobenzaldehyde solution in each volumetric flask.
3. the detection method of primary amine among the aging resister TMQ as claimed in claim 1, it is characterized in that aniline criterion referenced solution: in volumetric flask, add the 2N hydrochloric acid solution, then add paradime thylaminobenzaldehyde solution, add to scale mark, leave standstill more than 30 minutes as aniline criterion referenced solution with methyl alcohol.
4. the detection method of primary amine among the aging resister TMQ as claimed in claim 1, it is characterized in that preparing sample solution: aging resister TMQ sample places separating funnel, adds the chloroform dissolving; Add the 2N hydrochloric acid solution, shake fast after being divided into two solution phases, below chloroform phase solution phase is separated from funnel, will contain the top solution phase of hydrochloric acid, use the funnel with filter paper to filter, collect; Add paradime thylaminobenzaldehyde solution and hydrochloric acid solution, be diluted to scale with methyl alcohol.
5. the detection method of primary amine among the aging resister TMQ as claimed in claim 1 is characterized in that quantitative analysis method is:
The mg level amine content that the maximum absorbance at 437nm place is consistent:
C%=A*M*a/W*1000*b*100%
C represents the primary amine concentration of percentage composition
A represents that unit is mg/ml according to the concentration of the definite primary amine of typical curve
W represents the TMQ sample quality, and unit is g,
The volume of M volumetric flask, unit are ml,
The volume of a hydrochloric acid phase, unit are ml,
B pipettes the volume of hydrochloric acid phase, and unit is ml.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103620863A CN102879344A (en) | 2012-09-25 | 2012-09-25 | Method for detecting primary amine in anti-aging agents TMQ |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103620863A CN102879344A (en) | 2012-09-25 | 2012-09-25 | Method for detecting primary amine in anti-aging agents TMQ |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102879344A true CN102879344A (en) | 2013-01-16 |
Family
ID=47480752
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012103620863A Pending CN102879344A (en) | 2012-09-25 | 2012-09-25 | Method for detecting primary amine in anti-aging agents TMQ |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102879344A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106632102A (en) * | 2016-09-14 | 2017-05-10 | 华南理工大学 | Application of hyper branched polytriazole in detection of diarylamines antioxidant |
| CN106752063A (en) * | 2016-12-06 | 2017-05-31 | 浙江力禾集团有限公司 | A kind of method of one pot process AZOpigments |
| CN114057638A (en) * | 2020-08-06 | 2022-02-18 | 中石化南京化工研究院有限公司 | Method for removing impurity primary amine in anti-aging agent TMQ |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102062728A (en) * | 2010-12-13 | 2011-05-18 | 武汉大学 | Method for measuring concentration of octadecylamine |
-
2012
- 2012-09-25 CN CN2012103620863A patent/CN102879344A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102062728A (en) * | 2010-12-13 | 2011-05-18 | 武汉大学 | Method for measuring concentration of octadecylamine |
Non-Patent Citations (1)
| Title |
|---|
| 林新花 等: "硫化胶中防老剂NLB含量的测定", 《橡胶工业》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106632102A (en) * | 2016-09-14 | 2017-05-10 | 华南理工大学 | Application of hyper branched polytriazole in detection of diarylamines antioxidant |
| CN106632102B (en) * | 2016-09-14 | 2019-06-18 | 华南理工大学 | A kind of application of hyperbranched poly triazole in detection diarylamines anti-aging agent |
| CN106752063A (en) * | 2016-12-06 | 2017-05-31 | 浙江力禾集团有限公司 | A kind of method of one pot process AZOpigments |
| CN114057638A (en) * | 2020-08-06 | 2022-02-18 | 中石化南京化工研究院有限公司 | Method for removing impurity primary amine in anti-aging agent TMQ |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102967568B (en) | Method for testing dual-wavelength of light splitting luminosity | |
| CN102590383A (en) | Method for determining content of potassium, sodium, calcium and magnesium in cigarette paper simultaneously | |
| CN101762653B (en) | Method for determining main phenolic compounds in main stream smoke of cigarette | |
| CN103149309A (en) | Measuring method for the furfural content of transformer oil | |
| CN102879344A (en) | Method for detecting primary amine in anti-aging agents TMQ | |
| CN109324004A (en) | The method of content of bisphenol A is remained in a kind of measurement polycarbonate | |
| CN110672769A (en) | Method for measuring residual quantity of cantharidin yellow pigment in poultry eggs | |
| CN102818782B (en) | Determination method of total 2-(2-phenethyl) chromone compound content | |
| CN103293119A (en) | Method for rapidly detecting contents of amaranthus red and brilliant blue in foods | |
| CN102507466B (en) | Improved spectrophotometry method for determining proteins by using Coomassie brilliant blue | |
| CN101639438A (en) | Detection method of lead content in gasoline | |
| CN102353739A (en) | Rapid detection method of nicotine in tobacco | |
| CN101762575A (en) | Method for identifying authenticity and determining content of lycium barbarum polysaccharides | |
| CN102954942A (en) | Palladium content testing method | |
| CN102879349A (en) | Method for detecting primary amine in anti-aging agents FR | |
| CN103743690B (en) | A kind of quantitative analysis method of fullerene | |
| JP2006329641A (en) | Analyzing method of solvent soluble coloring matter | |
| CN110361479A (en) | A kind of methods and applications detecting a variety of sulfa drug residues | |
| CN105628861A (en) | Method for quickly measuring content of vitamin C in Fructus lycii | |
| CN110895264A (en) | Method for determining ethyl bromide in tenofovir alafenamide | |
| CN101957303A (en) | Method for analyzing turbidity of colored solution | |
| CN105572240A (en) | Method for detecting content of pharmaceutic adjuvant carmine by using high performance liquid chromatography | |
| CN103048407A (en) | Content detection method for lysine of compound ketoacid tablet | |
| CN107300531A (en) | The detection method of N methylimidazoles content in a kind of glyoxaline ion liquid | |
| CN102539340A (en) | Method for determining oil content and organic matter content in synthetic ammonia |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130116 |