CN104730024A - Method for analysis of magnesium-chelated phenolic resin in chloroprene rubber adhesive - Google Patents
Method for analysis of magnesium-chelated phenolic resin in chloroprene rubber adhesive Download PDFInfo
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- CN104730024A CN104730024A CN201310714834.4A CN201310714834A CN104730024A CN 104730024 A CN104730024 A CN 104730024A CN 201310714834 A CN201310714834 A CN 201310714834A CN 104730024 A CN104730024 A CN 104730024A
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- magnesium
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Abstract
The invention discloses a method for qualitative and quantitative analysis of magnesium-chelated phenolic resin in a chloroprene rubber adhesive. The method utilizes infrared spectroscopy to realize qualitative analysis and utilizes atomic absorption spectrometry and calculation to realize quantitative analysis. The method is related to sample preparation and treatment, apparatus test method and conditions, and calculating steps and formula. The method can be operated simply, can produce accurate test results and can realize detection and analysis of various magnesium-chelated phenolic resins in the chloroprene rubber adhesive. The detection result can be used for product quality identification and scientific research development.
Description
Technical field
The present invention relates to the analytical approach of magnesium chelating phenolics in a kind of chloroprene rubber adhesive agent, is exactly specifically the method that infra-red sepectrometry is used in set, atomic absorption spectrography (AAS) carries out qualitative and quantitative analysis to the magnesium chelating phenolics in chloroprene rubber adhesive agent.The invention belongs to the analysis and testing technology field to macromolecular material.
Background technology
The adhesive property of chloroprene rubber adhesive agent is excellent, affordable, and applicability is extensive, is a kind of high polymer binder generally used in industry and daily life.The matrix composition of chloroprene rubber adhesive agent is solvent-borne type neoprene, its bond effect removes with bonding condition as outside the Pass the phases such as the process of temperature, pressure and gluing of surfaces, largely can depend on the cross-linking reaction under adhesive matrix materials neoprene room temperature, namely matrix material crosslinking degree is higher, and the cohesive strength of tackifier is better.In chloroprene rubber adhesive agent, the component of added vulcanizing agent plays a key effect to the cross-linking reaction under matrix material neoprene room temperature.It is one of conventional vulcanizing agent that phenolics and magnesium oxide share system, set forth the formula of environmental protection chloroprene rubber adhesive agent in national patent CN 101418197A " a kind of environmental protection chloroprene rubber adhesive agent and production method thereof ", namely contain phenolics and magnesium oxide as vulcanizing system.
?in the production process of chloroprene rubber adhesive agent, if add the easy especially layering of the obtained tackifier of two kinds of materials respectively to affect bonding effect.If first by phenolics and magnesium oxide generation pre-reaction, form magnesium chelating phenolics, then the magnesium chelating phenolics of formation is joined in tackifier and then can overcome above-mentioned defect.Magnesium chelating phenolics not only improves the compatibility of phenolics and tackifier, also significantly improves its bonding strength, thermotolerance and bin stability." Fujian chemical industry " 2003 the 4th interim " research of chloroprene rubber adhesive agent thermotolerance " has set forth the impact on chloroprene rubber adhesive agent thermotolerance such as neoprene kind, chelating resin, vulcanization accelerator.The chloroprene rubber adhesive agent that result shows to adopt neoprene, carboxylated neoprene epoxy glue kind to coordinate chelating resin, vulcanization accelerator to be prepared, adhesive property and thermotolerance better.
Therefore visible, whether carry out qualitative and quantitative analysis to the magnesium chelating phenolics in chloroprene rubber adhesive agent can assist production firm's checking pre-reaction successful, tentative prediction is made to the cohesiveness of product, and by this Technology application in the research and development of adhesive products formula technique, can lay the foundation for research and development new product and self product quality of promotion improve.
The national patent CN 102053071A rapid analysis of phenolic resin content " in the phenol resin solution " adopts the content of infra-red sepectrometry to phenolics to introduce." specific rubber goods " the 5th phase " Determination of Composition in Chloroprene Rubber " in 2005 adopts thermogravimetry to analyze its component concentration for neoprene vulcanized rubber.The mensuration of content of magnesium, in current national standard analytical approach, adopts EDTA compleximetry mostly.Complex operation, analyze and measure length consuming time, cost of labor and time cost are all higher.Also have and adopt flame atomic absorption spectrometry, but be only confined to be easier to for water geometric ratio the sample solution prepared.
Inductivity coupled plasma mass spectrometry analysis is adopted to measure the content of magnesium in the national patent CN 103134849A fast method of potassium sodium calcium-magnesium content " in a kind of Simultaneously test cigarette paper ".The national patent CN 102735515A assay method of iron, manganese, copper, tin and content of magnesium " in titanium sponge, the titanium or titanium alloy ", adopts the content of magnesium in flame atom spectrum measuring metal.
Integrated employing infrared spectrum is qualitative carries out qualitative, quantitative analysis and research with atomic absorption spectrum for magnesium chelating phenolics in chloroprene rubber adhesive agent, there is not yet relevant open report.
The present invention proposes a kind ofly to have carried out qualitative, quantitative analysis and research method to the magnesium chelating phenolics in chloroprene rubber adhesive agent, namely chemical method is adopted to be separated and sample preparation resin, infra-red sepectrometry is adopted to carry out qualitative analysis to phenolics, adopt atomic absorption spectrography (AAS) by the quantitative test to magnesium elements in sample, and then by calculating, magnesium chela phenolics is quantitatively determined.Result shows that this research can magnesium chelating phenolics accurately in qualitative and quantitative analysis chloroprene rubber adhesive agent.
Summary of the invention
Content of the present invention is to provide a kind of analytical approach to the qualitative, quantitative of magnesium chelating phenolics in chloroprene rubber adhesive agent.
technical scheme
Adopt the method for usual chemical test process sample to carry out pre-treatment to two parts of chloroprene rubber adhesive agent samples from same sample, that is: dry solvent contained in sample, adopt the good solvent of magnesium chelating phenolics to extract object on soxhlet type apparatus.
Infra-red sepectrometry is adopted to carry out qualitative analysis a copy of it after process in sample, to the phenolics of known component structure at infrared spectrometer middle-infrared band 400cm
-1~ 4000cm
-1gather spectrogram, spectrogram is gathered to extract simultaneously, by the characteristic absorption peak of comparison two spectrograms, qualitative magnesium chelating phenolics.
Adopt an atomic absorption spectrography (AAS) to carry out quantitative test another after process in sample part, ashing removing phenolic resin moiety, being then clear transparent solutions by sample pretreating, is that anti-interference reagent is tested with strontium chloride.Select suitable magnesium test job condition.
In certain concentration range, absorbance and the concentration of magnesium follow langbobier law, linear.By the test of series standard solution, set up the typical curve of magnesium, the content of magnesium in working sample solution, and the content being converted into magnesium chelating phenolics.Then according to the following step, sample is analyzed.
A, respectively get chloroprene rubber adhesive agent about 2g in two conical flasks, be placed in (100 ± 5) DEG C baking oven, dry to constant weight, by solvent volatilization completely.Adopt acetone as extraction solvent, sample extracting 4 hours after soxhlet type apparatus will be dried.
B, dissolve 0.1g magnesium chelating phenolics known sample by proper amount of acetone, be evenly coated on the bromination sylvite sheet of surfacing, at the middle-infrared band 400cm of infrared spectrometer
-1~ 4000cm
-1gather spectrogram as reference spectrogram.
C, be evenly coated on bromination sylvite sheet, at the middle-infrared band 400cm of infrared spectrometer to the chloroprene rubber adhesive agent sample extract that wherein bottle is obtained by steps A
-1~ 4000cm
-1gather sample spectrogram.
D, duplicate spectrogram and reference spectrogram, the magnesium chelating phenolics characteristic absorption peak position in reference spectrogram all exists in sample spectrogram, then contain magnesium chelating phenolics in qualitative chloroprene rubber adhesive agent sample.
E, dry another bottle by steps A gained chloroprene rubber adhesive agent sample extract to constant weight.
F, by the solid transfer that obtains in step e in platinum crucible, put into muffle furnace, (450 ~ 500) DEG C slow ashing.Add the concentrated hydrochloric acid of (3 ~ 5) ml after cooling, drip several hydrofluorite, on electric furnace, volatilization is near dry, adds 1:1 dissolving with hydrochloric acid, is filtered in volumetric flask.
Add strontium chloride solution, constant volume in G, the solution that obtains in step F, shake up, be sample solution.
The preparation of H, sample blank solution: under the condition not having chloroprene rubber adhesive agent, carries out above-mentioned A, E, F, G step simultaneously, obtains sample blank solution.
The absorbance of I, atomic absorption spectrometry magnesium standard solution, drawing standard curve, in test sample solution, the concentration of magnesium, calculates the content W of magnesium in chloroprene rubber adhesive agent
mg; Finally, the content of magnesium chelating phenolics is calculated by formula 1.
Formula 1:Wr=W
mg*24.305/ M
w*100%
wherein: the content of magnesium chelating phenolics in Wr-chloroprene rubber adhesive agent;
W
mgthe content of magnesium in-chloroprene rubber adhesive agent;
M
wthe molecular weight of-magnesium chelating phenolics;
24.305 the relative atomic mass of-magnesium atom.
Acetone in described steps A, B is commercial chemicals (analyzing pure); Hydrochloric acid in described step F, hydrofluorite are commercial chemicals (analyzing pure); Strontium chloride in described step G is commercial chemicals (analyzing pure).
useful achievement
Phenolics characteristic absorption peak is pointed out according to infrared spectroscopy, can the existence of qualitative phenolics class material, by infrared spectrogram and the comparison of sample spectrogram of known kind magnesium chelating phenolics, can the kind of qualitative magnesium chelating phenolics; Adopt the absorbance of magnesium in air acetylene aas determination mark liquid and sample solution, according to the typical curve of magnesium, obtain content of magnesium, calculate the content of magnesium chelating phenolics.The method is easy and simple to handle, accurate, precision is high.
Accompanying drawing explanation
Fig. 1 is to the infrared spectrogram of tert-butyl group magnesium chelating phenolics.
The infrared spectrogram of Fig. 2 sample.
Embodiment
The present invention can be had a clear understanding of further by several specific embodiment given below, but they are not limitation of the invention, the related personnel of this area is to be understood that, equivalent replacement or amendment can be carried out to technical scheme of the present invention, and not departing from purport and the scope of technical solution of the present invention, it all should be encompassed in right of the present invention.
1, sample process in early stage: respectively get two portions of chloroprene rubber adhesive agents about 2 grams, be placed in (100 ± 5) DEG C baking oven and solvent is volatilized, take out sample after 2 hours and be placed in exsiccator, weigh after half an hour, until sample constant weight.By solvent volatilization completely.Adopt acetone as extraction solvent, after drying in water-bath with soxhlet type apparatus, sample extracting 4 hours, concentrates and collects extract, to be measured.
2, sample qualitative analysis: using magnesium chelating phenolics known for composition as reference sample, analyze with infrared spectrometer; Analyze according to the sample after aforementioned 1, step process, the infrared spectrogram of duplicate and reference sample, judges the concrete kind of magnesium chelating phenolics in sample, carries out following steps operation simultaneously.
(1) 0.1g magnesium chelating phenolics known sample is dissolved by proper amount of acetone, sample is dissolved completely, draw acetone soln with the kapillary that internal diameter is 1mm ± 0.1mm, be coated in uniformly on the bromination sylvite sheet of surfacing, and toast 1min under being placed in infrared lamp.
(2) observe the coated film of sample on salt sheet, if sample film is evenly distributed, be arranged on the specimen holder of infrared spectrometer, at middle-infrared band 400cm
-1~ 4000cm
-1gather infrared spectrogram as reference spectrogram.
(3) get 1, extract after process, according to the step of (1), sample to be tested is coated on bromination sylvite sheet, at middle-infrared band 400cm
-1~ 4000cm
-1gather sample spectrogram.
(4) duplicate spectrogram and reference spectrogram, the magnesium chelating phenolics characteristic absorption peak position in reference spectrogram all exists in sample spectrogram, then contain magnesium chelating phenolics in qualitative chloroprene rubber adhesive agent sample.
3, sample quantitative test pre-treatment: dry acetone solvent in another bottle of extract to constant weight.The solid transfer obtained, in platinum crucible, puts into muffle furnace, 500 DEG C of slow ashing.Add the concentrated hydrochloric acid of 5ml after cooling, and drip 3 hydrofluorite, on electric furnace, volatilization is near dry, adds the 1:1 dissolving with hydrochloric acid of 5ml, is filtered in 100ml volumetric flask.Add the 50g/L strontium chloride solution of 5ml, constant volume, shakes up, and is sample solution.Under the condition not having chloroprene rubber adhesive agent, carry out this operation simultaneously, obtain sample blank solution.
4, sample quantitative test: be divided into configuration quantitative criterion solution, standard solution measures, sample solution measures three steps.
(1) quantitative criterion solution is configured: State Standard Matter Research Centre 1000 μ g/ml magnesium standard solution, draw 1mL magnesium standard solution (1000 μ g/mL) in 100mL volumetric flask, be diluted to 10 μ g/ml Standard Stock solutions, Standard Stock solutions is diluted to 6 series standard solution, is respectively 0.05,0.1,0.2,0.3,0.4,0.5 μ g/mL.
(2) standard solution measures: first optimize air acetylene Atomic Absorption Spectrometer condition of work, lamp current 2mA, wavelength 285.20nm, slit 0.20nm, acetylene flow 1.5L/min, air mass flow 10L/min, calibration mode is linear least square.Bioassay standard solution absorbance, drawing standard curve.
(3) sample solution measures: the absorbance of magnesium in test sample, obtains the concentration of magnesium in sample solution, calculate the content W of magnesium in chloroprene rubber adhesive agent according to typical curve
mg.
Embodiment 1: qualitative analysis is carried out to the chloroprene rubber adhesive agent containing tert-butyl group magnesium chelating phenolics.
(1) by embodiment step 2, to known to tert-butyl group magnesium chelating phenolics gather infrared spectrogram, obtain accompanying drawing 1.Wherein wave number 3200-3400cm-1 place is that the stretching vibration absorption peak of O-H is strong and wide, and 2948.4cm-1 place is the stretching vibration absorption peak of C-H; 1611.1cm-1,1481.7cm-1 place is the stretching vibration absorption peak of phenyl ring C=C double bond; 1216.7cm-1 place is Ph-O stretching vibration absorption peak of phenolic hydroxyl group; 1126.9cm-1 place is the symmetrical stretching vibration absorption peak of ehter bond CH2-O-CH2; 1034.4cm-1 place is PhCH2-O stretching vibration absorption peak of benzyl hydroxyl; 874.8 cm-1 are that on 1,2,4,6-substituted benzene, C-H out-of-plane bending vibration absorption peak illustrates that the tert-butyl group replaces in contraposition.
(2) according to embodiment step 2, to step 1, process after known sample gather infrared spectrogram, obtain accompanying drawing 2.
(3) the characteristic spectrum peak of analysis chart 1 and Fig. 2 magnesium chelating phenolics, learns that in Fig. 1, characteristic spectrum peak can all confirm in fig. 2.Illustrate that the resin used in chloroprene rubber adhesive agent to be measured is to tert-butyl group magnesium chelating phenolics, in table 1.
Embodiment 2: quantitative test is carried out to the tert-butyl group magnesium chelating phenolics of chloroprene rubber adhesive agent sample.
1, according to concrete implementation step 4, test standard solution, test result is in table 2.
2, by containing in embodiment 1, sample solution being processed into the chloroprene rubber adhesive agent sample 2.0120g of tert-butyl group magnesium chelating phenolics, testing after diluting 200 times; According to typical curve, the concentration obtaining magnesium is 0.400 mcg/ml, and calculating content of magnesium in chloroprene rubber adhesive agent sample is 0.40%; Calculate finally by use formula 1, to learn in this chloroprene rubber adhesive agent to the content of tert-butyl group magnesium chelating phenolics to be 6.77%.
It will be understood by those skilled in the art that all kinds of magnesium chelating phenolics that the present invention can be actually used in chloroprene rubber adhesive agent exists carry out determination and analysis, test result can be used for the objects such as product quality qualification and scientific research and development.
Claims (5)
1., to an analytical approach for magnesium chelating phenolics in chloroprene rubber adhesive agent, it is characterized in that using infra-red sepectrometry to carry out qualitative analysis; Atomic absorption spectrography (AAS) and calculating is used to carry out quantitative test.
2. a kind of analytical approach to magnesium chelating phenolics in chloroprene rubber adhesive agent according to claim 1, is characterized in that: before carrying out qualitative and quantitative analysis, carry out process in early stage to chloroprene rubber adhesive agent sample, the steps include:
A. respectively materials about 2g in two conical flasks, be placed in (100 ± 5) DEG C baking oven and dry to constant weight;
B. using acetone as extraction solvent, sample extracting 4 hours after soxhlet type apparatus will be dried.
3. a kind of analytical approach to magnesium chelating phenolics in chloroprene rubber adhesive agent according to claim 1, is characterized in that using infra-red sepectrometry to carry out qualitative analysis, the steps include:
A. dissolve 0.1g magnesium chelating phenolics known sample by proper amount of acetone, be evenly coated on the bromination sylvite sheet of surfacing, at the middle-infrared band 400cm of infrared spectrometer
-1~ 4000cm
-1gather spectrogram as reference spectrogram;
B. be evenly coated on bromination sylvite sheet, at the middle-infrared band 400cm of infrared spectrometer to wherein obtaining chloroprene rubber adhesive agent sample extract according to method described in claim 2
-1~ 4000cm
-1gather sample spectrogram;
C. duplicate spectrogram and reference spectrogram, the magnesium chelating phenolics characteristic absorption peak position in reference spectrogram all exists in sample spectrogram, then contain magnesium chelating phenolics in qualitative chloroprene rubber adhesive agent sample.
4. a kind of analytical approach to magnesium chelating phenolics in chloroprene rubber adhesive agent according to claim 1, is characterized in that using atomic absorption spectrography (AAS) and calculating to carry out quantitative test, the steps include:
A. the preparation of sample solution: dry and obtain another bottle of chloroprene rubber adhesive agent sample according to method described in claim 2, extract is to constant weight; The solid transfer obtained, in platinum crucible, puts into muffle furnace, (450 ~ 500) DEG C slow ashing; Add (3-5) ml concentrated hydrochloric acid after cooling, and drip several hydrofluorite, on electric furnace, volatilization is near dry, adds 1:1 dissolving with hydrochloric acid, is filtered in volumetric flask; Add strontium chloride solution, constant volume, shake up, be sample solution;
B. the preparation of sample blank solution: under the condition not having chloroprene rubber adhesive agent, carries out the step A of the claims 2 and 4 simultaneously, obtains sample blank solution;
C. using the absorbance of magnesium in aas determination sample, being learnt the concentration of magnesium in sample solution by typical curve, finally by calculating magnesium chelating phenolic resin content Wr in chloroprene rubber adhesive agent.
5. a kind of analytical approach to magnesium chelating phenolics in chloroprene rubber adhesive agent according to claim 1, it is characterized in that using atomic absorption spectrography (AAS) and calculating to carry out quantitative test, in chloroprene rubber adhesive agent, the computing formula 1 of magnesium chelating phenolic resin content is:
Wr= W
Mg*24.305/ M
W* 100%
wherein: the content of magnesium chelating phenolics in Wr-chloroprene rubber adhesive agent;
W
mgthe content of magnesium in-chloroprene rubber adhesive agent;
M
wthe molecular weight of-magnesium chelating phenolics;
24.305 the relative atomic mass of-magnesium atom.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112908541A (en) * | 2021-01-27 | 2021-06-04 | 上海起帆电线电缆技术有限公司 | High-temperature-resistant vulcanized longitudinal watertight cable for sonar system and twisting mold |
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| CN112908541B (en) * | 2021-01-27 | 2022-10-14 | 上海起帆电线电缆技术有限公司 | High-temperature-resistant vulcanized longitudinal watertight cable for sonar system and twisting mold |
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