CN107422072A - A kind of alkalescence goes the analysis method of flash agent - Google Patents

A kind of alkalescence goes the analysis method of flash agent Download PDF

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Publication number
CN107422072A
CN107422072A CN201710428778.6A CN201710428778A CN107422072A CN 107422072 A CN107422072 A CN 107422072A CN 201710428778 A CN201710428778 A CN 201710428778A CN 107422072 A CN107422072 A CN 107422072A
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sample
analysis
alkalescence
goes
analysis method
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陈仲校
高煜林
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Sheng Longshunfa Electronic Science And Technology Wuxi Co Ltd
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Sheng Longshunfa Electronic Science And Technology Wuxi Co Ltd
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0001—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00 by organoleptic means
    • 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
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
    • 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
    • G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
    • G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
    • G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
    • 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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
    • 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
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR

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Abstract

The invention discloses the analysis method that a kind of alkalescence goes flash agent, including following analytical procedure：The first step, the judgement to sample Back ground Information；Second step, each composition of sample is separated；3rd step, is detected and structure elucidation to sample；4th step, sample analysis result is integrated, to obtain required analysis result.Using the analysis method of the present invention, it can therefrom obtain useful information with faster, the accurate information for obtaining sample composition and content, help enterprise to solve above-mentioned problem.

Description

A kind of alkalescence goes the analysis method of flash agent
Technical field
The present invention relates to the analysis method that a kind of alkalescence goes flash agent.
Background technology
Flash is to flow to the fifth wheel on pin and exposed carrier during integrated circuit plastic packaging at present.The plastic packaging material of spilling It is covered on terminal pin, multiple performance defect can be brought to product, therefore removes the indispensable link that flash is integrated circuit.At present Occur on the market it is a variety of remove flash product, there is acidity to go flash agent, alkalescence to go flash agent etc., if a suitable production of selection Product, how to know a active ingredient gone in flash agent, how formula improvement is carried out to existing product, to most use For person, all exist greatly difficult.
Although some enterprises possess certain research and development power of test, also possess certain analysis analytic ability, due to Different product system, composition and content differ greatly, and the component of addition has acid alkalescence, has low boiling and high boiling substance, Organic matter inorganic matter mixes, it is difficult to be analyzed with unified analysis method different samples, it is necessary to according to product body System is different, suits the remedy to the case, and proposes more flexible changeable separation method and corresponding means of testing.
This patent combination modern analysis means, it is desirable to provide a kind of fast and convenient analysis method for going flash agent, therefrom obtain Useful information is taken, helps enterprise to solve above-mentioned problem.
The content of the invention
The defects of the present invention seeks to exist for prior art, provides the analysis method that a kind of alkalescence goes flash agent, can be with Faster, the accurate information for obtaining sample composition and content.
The present invention to achieve the above object, adopts the following technical scheme that：A kind of alkalescence goes the analysis method of flash agent, including Following analytical procedure：
The first step, the judgement to sample Back ground Information；
Second step, each composition of sample is separated；
3rd step, is detected and structure elucidation to sample；
4th step, sample analysis result is integrated, to obtain required analysis result.
Further, the specific steps of the judgement to sample Back ground Information are mainly：First, after touching sample, to sample The outward appearance and state of product judged, then the pH value of test sample, density and solid content；If sample is more sticky, survey The viscosity of test agent.
Further, the specific method separated to each composition of sample includes：
Distillation under vacuum, mainly for separating of the different material of the high and low boiling point in sample；
Extraction, it is mainly used in coming organic matter in sample is separated from the water；
Gradient Elution Method, by preparing the eluent of opposed polarity, the different component of polarity in sample is separated；
Chromatogram column technique is prepared, using the attached ability of the Adsorption and desorption of pillar, complicated organic moiety in sample is separated； Muffle furnace ashing method, for organic compound combustion to be obtained into inorganic component.
Further, detection and the specific method of structure elucidation are carried out to sample to be included：Fourier transform infrared spectroscopy (FT-IR), gas chromatography combined with mass spectrometry (GCMS), nuclear magnetic resonance (1H-NMR), X-fluorescence elementary analysis (XRF), X ray monocrystalline Diffraction (XRD), karl Fischer moisture measurement and carbonate, titration hydroxy.
Further, comprised the following steps that to what sample analysis result was integrated：Include qualitative analysis and quantitative analysis Two aspects；Qualitative analysis is carried out first, so that quantitative analysis is carried out to it again after determining a certain composition, and various materials are qualitative Quantitative result combines, and just obtains the complete analysis result of whole sample.
Beneficial effects of the present invention：Using the present invention analysis method, can with it is faster, it is accurate acquisition sample composition with And the information of content, useful information is therefrom obtained, helps enterprise to solve above-mentioned problem.
Brief description of the drawings
Fig. 1 is the infrared test figure of present invention drying sample；
Fig. 2 is the XRD test charts of present invention drying sample；
Fig. 3-1 is the total ion chromatogram of GCMS of the present invention tests；
Fig. 3-2 to Fig. 3-4 is the matching figure corresponding to GCMS each retention time after processing as former state of the invention；
Fig. 4-1 to Fig. 4-4 be inventive samples in component 1 to component 4 hydrogen spectrogram.
Embodiment
Embodiment：
Select certain excellent performance goes flash agent, carries out constituent analysis：
1st, the preliminary judgement of sample message
First, after touching sample, judgement be exactly appearance color smell etc., it can be deduced that this sample be transparency liquid slightly Jaundice, has strong ammonia taste, there is volatility, crystalloid precipitate is arranged at bottom；
Then, the pH value of test sample, density, water content etc., test result is shown in Table 1.It was found from test data, sample is Please alkaline system, contain substantial amounts of volatile-resistant substance.
Table 1：The essential information of sample
2nd, the separation of sample
The formula of flash agent is gone to form by information such as the pH value of sample, solid contents, and with reference to alkalescence, wherein often containing： Highly basic, alcohol ether solvents, organic amine material, complexing agent, micro surfactant etc., according to these information, can tentatively it make Separation scheme.Sample can be evaporated under reduced pressure, drying and processing, drying sample can use and elute step by step, can use solvent as former state Wherein lower boiling component of extraction etc..
3rd, test
According to separating resulting, the method for testing of selection has：IR, NMR, XRF, XRD, GCMS, chemistry titration, water content test Analyzed Deng means of testing.
Specific to method of testing it is as follows：
IR is tested：Isolated each component is carried out respectively IR tests (according to state, can use pellet technique, Liquid cell method and ATR methods).
X-fluorescence elementary analysis (XRF)：XRF tests (can use and pass through filter paper method) are directly carried out as former state；
X ray single crystal diffraction (XRD)：Isolated solid constituent is subjected to XRD tests；
GCMS is tested：Former state is made into 1 with isopropanol:1000 solution and after drying, carries out GCMS tests；
Or GCMS detections are carried out after being extracted with ethyl acetate as former state；
Nmr analysis (NMR)：Respectively to the component of each separation, carry out1(deuterated reagent selects heavy water or deuterium for H-NMR tests For methanol)
ICP-AES：After former state multiple is diluted, specific aim carries out ICP tests；
Carbonate, bicarbonate radical, hydroxyl titration：Take as former state, titrated according to national standard method；
Water content is tested：Directly take as former state, water content test is carried out with the karl Fischer moisture tester of volumetric method
4th, data analysis (spectrum analysis)
4.1 IR are analyzed
Fig. 1 is the infrared test figure for drying sample；As seen from the figure, 3600~3200cm-1For the stretching vibration of hydroxyl active hydrogen； 1450cm-1For the asymmetric stretching vibration peak of carbonate, 1064cm-1Inhaled for the symmetrical stretching vibration peak flexural vibrations of carbonate Receive peak, 890cm-1For carbonate out-of-plane bending vibration, 680cm-1For the in-plane bending vibration of carbonate.In 1671cm-1、 1574cm-1Deng there is the characteristic absorption peak of some carboxylates.
4.2 XRF analysis
Table 1-1 is former state XRF test result.As can be seen from the table, dry in sample mainly containing the element such as potassium, sodium and The elements such as micro chlorine, iron, sulphur, silicon；With reference to pH and infrared test result, potassium hydroxide, hydrogen may be contained by guessing in former state The materials such as sodium oxide molybdena, potassium carbonate.
The XRF test results of table 1-1 former states
[Quantitative Result]
4.3 XRD analysis
Fig. 2 is the test chart for drying sample XRD.As shown in the figure：The XRD spectrum of drying sample is mainly matched as potassium hydroxide, carbon The materials such as sour potassium.
4.4 GCMS are analyzed
Fig. 3-1 to Fig. 3-4 is the matching figure corresponding to GCMS test chart and each retention time after processing as former state.By Analysis, mainly detect the materials such as ethylenediamine, cyclohexylamine, butyl glycol ether.
4.5 NMR are analyzed
Fig. 4-1 is the hydrogen spectrogram of component 1, and Fig. 4-2 is the hydrogen spectrogram of component 2；Fig. 4-3 is the hydrogen spectrum for being evaporated under reduced pressure residue Figure；Fig. 4-4 is the hydrogen spectrogram for drying sample.
From Fig. 4-1,2.687ppm (4H) corresponds to the chemical shift of proton on ethylenediamine；
From Fig. 4-2,2.85ppm (1H), 1.82~1.65ppm (4H), 1.60~1.43ppm (3H), 1.05~ 0.88ppm (2H) corresponds to the chemical shift of proton on cyclohexylamine；
From Fig. 4-3：3.8~3.6ppm (6H), 1.6ppm (2H), 1.2ppm (2H), 0.9ppm (3H) are ethylene glycol The chemical shift of proton on butyl ether；2.85ppm, 1.82~1.65ppm, 1.60~1.43ppm, 1.05~0.88ppm are corresponded to The chemical shift of proton on cyclohexylamine；Illustrate that the boiling point of cyclohexylamine is higher, vacuum distillation is not kept completely separate out；Butyl glycol ether Boiling point it is higher, do not distill substantially.
From Fig. 4-4：4.0~3.2ppm (6H) is the chemical shift of proton on sodium gluconate；2.8ppm (8H)、 2.35ppm (42H) is the chemical shift of proton on the sodium of EDTA tetra-.
4.6 ICP-AES are tested
Table 2 is the test result of ICP-AES after more times of dilutions as former state.
Sample ID Test event Assay (mg/L) Normative reference Detection limit
Alkalescence goes flash agent Potassium (K) 107.21 EPA 3052-1996 10ppm
Alkalescence goes flash agent Sodium (Na) 12.04 EPA 3052-1996 10ppm
Alkalescence goes flash agent Silicon (Si) 1.67 EPA 3052-1996 2ppm
4.7 hydroxyls, carbonate titration
Table 3 is to carry out hydroxyl, the titration results of carbonate using National Standard Method as former state.Take being averaged for titration results three times It is worth, it is 5.47% that hydroxyl is contained in former state, carbonate 0.86%.
4.8 moisture measurement
Table 4 is as former state using the result of volumetric method karl Fischer moisture tester test water content.It was found from test result, Aqueous about 48.6% in sample.
The moisture measurement of the sample of table 4
Sample ID Test event Assay Normative reference Detection limit
Alkalescence goes flash agent Water content is tested 52.6% GB/T606-2003 0.05%
5th, integration analysis result
Comprehensive IR, XRF, XRD, GCMS, NMR, the analyze data such as IC, moisture measurement, contain in former state：Potassium hydroxide 15- 20%；Potassium carbonate 1-3%；Ethylenediamine 5-10%；Cyclohexylamine 5-10；Ethylene glycol monobutyl ether 2-5%；Sodium gluconate 1-2%； The sodium 1-2% of EDTA tetra-；Metasilicate pentahydrate sodium 0.3-1.0%；Water 50-55%.
It is that a kind of case of the embodiment of the present invention is described above, commercially available most of alkalescence remove the composition of flash agent With present case relatively, analysis method used is referred to present case, no longer will repeat one by one.
By the foregoing description of the disclosed embodiments, professional and technical personnel in the field are enable to realize or use this hair It is bright.A variety of modifications to these embodiments will be apparent for those skilled in the art, determine herein The analysis method of justice can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, originally Invention is not intended to be limited to embodiment illustrated herein, and is to fit to and principles disclosed herein and features of novelty phase one The most wide scope caused.

Claims (5)

1. a kind of alkalescence goes the analysis method of flash agent, it is characterised in that including following analytical procedure：
The first step, the judgement to sample Back ground Information；
Second step, each composition of sample is separated；
3rd step, is detected and structure elucidation to sample；
4th step, sample analysis result is integrated, to obtain required analysis result.
2. a kind of alkalescence as claimed in claim 1 goes the analysis method of flash agent, it is characterised in that to sample Back ground Information The specific steps of judgement are mainly：First, after touching sample, the outward appearance and state of sample is judged, then tested PH value, density and the solid content of sample；If sample is more sticky, the viscosity of test sample.
3. a kind of alkalescence as claimed in claim 1 goes the analysis method of flash agent, it is characterised in that each composition of sample is entered The specific method of row separation includes：
Distillation under vacuum, mainly for separating of the different material of the high and low boiling point in sample；
Extraction, it is mainly used in coming organic matter in sample is separated from the water；
Gradient Elution Method, by preparing the eluent of opposed polarity, the different component of polarity in sample is separated；
Chromatogram column technique is prepared, using the attached ability of the Adsorption and desorption of pillar, complicated organic moiety in sample is separated；Muffle Stove ashing method, for organic compound combustion to be obtained into inorganic component.
4. a kind of alkalescence as claimed in claim 1 goes the analysis method of flash agent, it is characterised in that sample is carried out detection with The specific method of structure elucidation includes：Fourier transform infrared spectroscopy (FT-IR), gas chromatography combined with mass spectrometry (GCMS), nuclear-magnetism Resonance (1H-NMR), X-fluorescence elementary analysis (XRF), X ray single crystal diffraction (XRD), karl Fischer moisture measurement and carbonate, Titration hydroxy.
5. a kind of alkalescence as claimed in claim 1 goes the analysis method of flash agent, it is characterised in that sample analysis result is entered Row is comprehensive to be comprised the following steps that：Include two aspects of qualitative analysis and quantitative analysis；Qualitative analysis is carried out first, to determine certain Carry out quantitative analysis after one composition to it again, and the result of various material qualitative, quantitatives is combined, just obtain whole sample The complete analysis result of product.
CN201710428778.6A 2017-06-08 2017-06-08 A kind of alkalescence goes the analysis method of flash agent Pending CN107422072A (en)

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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19739659A1 (en) * 1997-09-10 1999-03-11 Hubertus Dipl Ing Meyer Processing used lubricating grease for recycling
US20040064265A1 (en) * 2000-01-31 2004-04-01 Myers David F. Assay methods for hydratable cementitious compositions
CN101027554A (en) * 2004-09-17 2007-08-29 英国石油国际有限公司 Method of assaying a hydrocarbon-containing feedstock
CN102169111A (en) * 2011-05-18 2011-08-31 通标标准技术服务有限公司 Method for detecting high-attention substance in European Union REACH rule
CN102565259A (en) * 2011-11-10 2012-07-11 深圳天祥质量技术服务有限公司 Method for detecting SVHC (Substance of Very High Concern)
CN103235081A (en) * 2013-05-23 2013-08-07 福建省纤维检验局 Method for measuring phenolic compounds in textiles and leather products
CN104020236A (en) * 2014-06-27 2014-09-03 宜特科技(昆山)电子有限公司 Qualitative analytical method of substance
CN104049046A (en) * 2014-06-18 2014-09-17 南京麦思德餐饮管理有限公司 Method for detecting dimethyl fumarate in body lotion
CN104181254A (en) * 2014-09-03 2014-12-03 云南中烟工业有限责任公司 Method for determining polycyclic aromatic hydrocarbon in hot melt adhesive by separation

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19739659A1 (en) * 1997-09-10 1999-03-11 Hubertus Dipl Ing Meyer Processing used lubricating grease for recycling
US20040064265A1 (en) * 2000-01-31 2004-04-01 Myers David F. Assay methods for hydratable cementitious compositions
CN101027554A (en) * 2004-09-17 2007-08-29 英国石油国际有限公司 Method of assaying a hydrocarbon-containing feedstock
CN102169111A (en) * 2011-05-18 2011-08-31 通标标准技术服务有限公司 Method for detecting high-attention substance in European Union REACH rule
CN102565259A (en) * 2011-11-10 2012-07-11 深圳天祥质量技术服务有限公司 Method for detecting SVHC (Substance of Very High Concern)
CN103235081A (en) * 2013-05-23 2013-08-07 福建省纤维检验局 Method for measuring phenolic compounds in textiles and leather products
CN104049046A (en) * 2014-06-18 2014-09-17 南京麦思德餐饮管理有限公司 Method for detecting dimethyl fumarate in body lotion
CN104020236A (en) * 2014-06-27 2014-09-03 宜特科技(昆山)电子有限公司 Qualitative analytical method of substance
CN104181254A (en) * 2014-09-03 2014-12-03 云南中烟工业有限责任公司 Method for determining polycyclic aromatic hydrocarbon in hot melt adhesive by separation

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Application publication date: 20171201