CN104614416A - Detecting method of fluoride in soldering paste - Google Patents
Detecting method of fluoride in soldering paste Download PDFInfo
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- CN104614416A CN104614416A CN201310535976.4A CN201310535976A CN104614416A CN 104614416 A CN104614416 A CN 104614416A CN 201310535976 A CN201310535976 A CN 201310535976A CN 104614416 A CN104614416 A CN 104614416A
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Abstract
The invention provides a detecting method of fluoride in soldering paste. According to the detecting method, oxygen bomb combustion method and electrochemical ion electrode method are combined for detection. In a step of oxygen bomb combustion, a soldering paste sample is treated with acetone, halide ions are dissolved so as to obtain an acetone halogen solution, the acetone halogen solution is subjected to volatilizing concentration so as to obtain a concentrate, the concentrate is subjected to oxygen bomb combustion treatment so as to obtain a sample liquid containing fluorine ions. The obtained sample liquid is subjected to electrochemical ion electrode analysis, wherein a fluorine ion standard sample solution is delivered into a measuring circuit and a sample liquid pool of an ion selective electrode, electric potential determination is realized, and fluorine ion concentration is calculated. The detecting method is capable of realizing sample and rapid detection of fluoride content in soldering paste, and instrument cost is low.
Description
Technical field
The present invention relates to solder(ing) paste detection technique field, particularly relate to the detection method of fluoride in a kind of solder(ing) paste.
Background technology
Solder(ing) paste is a kind of Novel welding material arisen at the historic moment along with SMT.SMT is surface mounting technology (Surface Mount Technology, be called for short SMT), refer to printing, applying solder paste on printed circuit board pad, and Surface Mount Component is placed with accurately scribbles on the pad of solder(ing) paste, according to specific reflux temperature curve heater circuit plate, allow solder(ing) paste melt, between components and parts with printed circuit board, form solder joint after its alloying component cooled and solidified and realize the metallurgical technology be connected.
Solder(ing) paste is mixed by solder powder, scaling powder and other additive, the creaminess potpourri of formation.The massfraction of scaling powder is usually between 8 ~ 10%, and all the other overwhelming majority are ultra-fine (20-75 μm) spherical alloy welding powders.Scaling powder can help and promote welding process in welding technology, has protective effect simultaneously, stops the generation etc. of oxidation reaction.Often containing fluoride in scaling powder, the content of fluoride decides usability and the feature of environmental protection of solder(ing) paste.Therefore, need content by measuring fluoride in solder(ing) paste to solder(ing) paste Progressive symmetric erythrokeratodermia energy and feature of environmental protection evaluation.
At present, in international industrial standard ANSI/J-STD-004, siliver chromate test paper method of testing can only chlorine, the bromine of qualitative detection ionic species, cannot detect the existence of fluoride.Japanese Industrial Standards JIS Z3284-1994 is also a quilitative method about the detection of fluoride.Adopt By Oxygen Bomb Combustion-chromatography of ions quantitative measurement can comprise the content of all halogens of fluoride in EN14582, this method of testing is that lotion makes all organic substances at high temperature burn completely by By Oxygen Bomb Combustion, and remaining residue contains halogen and other dead matter; This residue is carried out chromatography of ions test, the content that halogenide is definite can be obtained.The chromatography of ions has the advantages such as accuracy is high, reproducible, but the instrument stabilizer time is longer, instrument cost and analysis cost all higher, operating personnel are required high, also require suspension <0.45 μm (aperture) in sample simultaneously, in case the sampling system of plug ion chromatographic apparatus, cause sample pre-treatments loaded down with trivial details, time-consuming.
Therefore, for accurately detecting the content of fluoride in solder(ing) paste, be necessary to study a kind ofly use simply cheap instrument to carry out analyzing, cost is low, the simple fluoride detection method of method.
Summary of the invention
The object of the present invention is to provide fluoride detection method in a kind of solder(ing) paste, quantitatively can detect content of fluoride, instrument cost is low, analyze simple and quick.
The invention provides fluoride detection method in a kind of solder(ing) paste, be utilize oxygen bomb combustion to combine with electrochemical ion electrode method to detect, comprise the steps:
Step one: by soldering paste sample by acetone treatment, dissolves halide ion and obtains acetone halogen solutions, and by concentrated in concentrate for the solution evaporation obtained, concentrate, by oxygen bomb combustion process, obtains the test sample liquid of fluoride ion;
Step 2: above-mentioned test sample liquid is analyzed by electrochemical ion electrode method, in the metering circuit and test sample liquid pool device of ion-selective electrode, add fluorine ion standard model solution, to measure current potential, and calculate fluorinion concentration by concentration formula.
Further, in described solder(ing) paste, in fluoride detection method, concentration formula is
wherein, C
xfor fluorinion concentration, V
sfor the volume of fluorine ion standard model solution, C
sfor the concentration of fluorine ion standard model solution, V
xfor the volume of institute's extracting sample solution, △ C is the concentration increments adding fluorine ion in test solution after standard solution, and S is the slope of electrode; In solder(ing) paste former state, content of fluoride ion is drawn by following formula:
wherein m is soldering paste sample quality, m
2-m
1for solder(ing) paste sample through acetone extraction, concentrated after quality, m
3for the quality of making test sample liquid taken in halogen sample in solder(ing) paste sample.
Further, by the slope formula of electrode,
calculate slope S; Wherein E
2, E
3for the potential value that potentiometer measures; △ C is drawn by following formula, Δ C=C
s× V
s/ V
x.
Further, described step one also specifically comprises the following steps:
A, get a dry centrifuge tube, load soldering paste sample m gram, in described centrifuge tube, add acetone, and put into hydro-extractor and carry out centrifuging, leave standstill, pour out upper strata acetone soln, put into drying receptacle, container mass is m
1gram; Repeat said process repeatedly, fully to obtain the halide ion in solder(ing) paste;
B, by concentrated for the acetone volatilization in container, weighing container and content quality obtain m
2gram; Therefrom accurately take concentrate m
3gram, put into platinum crucible;
Add absorbing liquid in advance in C, cylinder, screw oxygen bomb lid, oxygen bomb, to 4MPa, is placed in water-bath by oxygenate pressure, igniting; Product to be combusted is completely absorbed, and takes out cylinder, is proceeded to by absorbing liquid in volumetric flask, and rinse each several part in oxygen bomb with absorbing liquid, washing fluid is incorporated to volumetric flask, adds TISAB solution, obtains test sample liquid.
Further, it is characterized in that: described step 2 also specifically comprises the following steps:
D, preparation fluoride ion selective electrode, mix up potentiometer on request, load onto fluoride ion selective electrode and contrast electrode, fluoride ion selective electrode is immersed in 1.0 × 10
-1in the fluorine ion standard solution of mol/L, then with washed with de-ionized water several, until the electrode potential value recorded reaches background values, this value is indicated by the factory of electrode;
Content of fluoride ion in E, standard addition method test samples, draws V
xtest sample liquid, puts into plastic beaker, starts stirrer, immerses fluoride ion selective electrode and contrast electrode, after current potential is stable, and record equilibrium potential; Accurately add V
sconcentration is C
sfluorine ion standard solution, fluorine ion standard solution needs to add TISAB solution preparation, records potential value E
2;
F, blank assay, replace sample with deionized water, repeat above-mentioned experiment, as blank value;
G, result calculate and measure E
2after test solution blank reagent dilute one times, then record potential value E
3.
Further, described C
sbe 1.00 × 10
-4molL
-1or 1.00 × 10
-3molL
-1.
Further, the compound method of TISAB solution is as follows: take sodium chloride 58g, sodium citrate 10g, be dissolved in 800mL deionized water, add glacial acetic acid 57mL again, the NaOH solution with 40% regulates pH to 5.0-6.0, and then adding deionized water, to be diluted to cumulative volume be 1L.
In solder(ing) paste of the present invention, By Oxygen Bomb Combustion is combined with electrochemical ion electrode method by fluoride detection method, quantitatively detects the content of fluoride in solder(ing) paste, and instrument cost is low, it is simple and quick to analyze.
Accompanying drawing explanation
Fig. 1 is the diagram of the By Oxygen Bomb Combustion device of fluoride detection method in solder(ing) paste of the present invention.
Fig. 2 is metering circuit and the sample pool device of the fluoride ion selective electrode of fluoride detection method in solder(ing) paste of the present invention.
Embodiment
Form is by the following examples described in further detail foregoing of the present invention again, but this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following embodiment, all technology realized based on foregoing of the present invention all belong to scope of the present invention.
In embodiment of the present invention solder(ing) paste, oxygen bomb combustion mainly combines with electrochemical ion electrode method by the detection method of fluoride, and then realizes quantitatively detecting content of fluoride in solder(ing) paste.Detection method comprises the steps:
Step one: during oxygen bomb combustion, by soldering paste sample by acetone treatment, dissolves halide ion and obtains acetone halogen solutions, and by concentrated in concentrate for the solution evaporation obtained, concentrate, by oxygen bomb combustion process, obtains the test sample liquid of fluoride ion;
Step 2: during electrochemical ion electrode method, in the metering circuit and test sample liquid pool device of ion-selective electrode, adds fluorine ion standard model solution, to measure current potential.
Pass through concentration formula:
Calculate fluorinion concentration;
Wherein, V
sfor the volume of fluorine ion standard solution, C
sfor the concentration of fluorine ion standard model solution, V
xfor the volume of institute's extracting sample solution, △ C is the concentration increments adding fluorine ion in test solution after standard solution, Δ C=C
s× V
s/ V
x, S is the slope of electrode, C
xfor fluorinion concentration.
Wherein, slope S is by the slope formula of electrode:
draw, survey electrode slope by standard solution, E
2, E
3for the potential value that potentiometer measures.
Again according to following formula:
Draw content of fluoride ion in solder(ing) paste former state, and then analyze the performance of solder(ing) paste.
Wherein, m is soldering paste sample quality, m
2-m
1for solder(ing) paste sample through acetone extraction, concentrated after quality, m
3for the quality of making test sample liquid taken in halogen sample in solder(ing) paste sample.
Below for being obtained the specific embodiment of test sample test solution in the detection method of fluoride in solder(ing) paste of the present invention by oxygen bomb combustion, comprise the steps: further
A, get the dry centrifuge tube of 10mL, (quality is m), adds 5-8mL acetone, stir evenly in described centrifuge tube, and puts into hydro-extractor and carry out centrifuging, and rotating speed is 2000r/min, centrifugal 10 minutes, leaves standstill 5 minutes to load 10 grams, soldering paste sample; Pour out upper strata acetone soln, (container mass is m to put into drying receptacle
1); In centrifuge tube, add 5-6mL acetone again, stir evenly, centrifugal, leave standstill, upper strata is poured out, and puts into same container, repeats said process 5 ~ 6 times, fully to dissolve the halide ion in solder(ing) paste.
B, by concentrated in concentrate for the acetone volatilization in container, weighing container and content quality obtain m
2.Therefrom accurately taking concentrate, to be about 0.5g(quality be m
3, be accurate to 0.1 milligram), put into platinum crucible 1(as Fig. 1);
C, as Fig. 1, add deionized water 20.00ml in cylinder 2 in advance as absorbing liquid, screw oxygen bomb lid, oxygenate pressure is to 4MPa.Oxygen bomb is placed in water-bath, igniting; After 30min, product to be combusted is completely absorbed, and takes out cylinder 2, slowly exits, open bullet lid, proceeded to by absorbing liquid in 100ml volumetric flask, carefully rinse each several part in oxygen bomb with deionized water, washing fluid is incorporated to volumetric flask, add 10.00ml TISAB, constant volume, shake up, obtain test sample liquid.
Below for being analyzed the specific embodiment of fluorinion concentration in test sample test solution in the detection method of fluoride in solder(ing) paste of the present invention by electrochemical ion electrode method, comprise the steps: further
D, preparation fluoride ion selective electrode, mix up potentiometer 3 on request, namely PHS-3C type pH meter (a kind of numerical monitor pH meter) is to mV shelves, loads onto fluoride ion selective electrode 4 and contrast electrode 5(saturated calomel electrode, SCE).Fluoride ion selective electrode 4 is immersed in 1.0 × 10
-1in the fluorine ion standard solution of mol/L, about 30min, then the washed with de-ionized water using made fresh for several times, can use (this value each electrode difference, is indicated by the factory of electrode) until the electrode potential value recorded reaches background values (about-370mV).
E, as Fig. 2, by content of fluoride ion in standard addition method test samples, absorption 25.00ml(is V
x) test sample liquid 6, put into 50ml plastic beaker, start stirrer, immerse fluoride ion selective electrode 4 and contrast electrode 5, after current potential is stable, record equilibrium potential (E
1).
Accurately adding 1.00mL(is V
s) 1.00 × 10
-4molL
-1(C
s) fluorine ion standard solution, fluorine ion standard solution needs to add TISAB solution preparation, records potential value E
2if (the potential value changes delta E read is less than 20mV, should use 1.00 × 10
-3molL
-1
F
-standard solution, now experiment need restart).
F, blank assay, replace sample with deionized water, repeat above-mentioned experiment, as blank value.
G, result calculate
Measure E
2after test solution blank reagent dilute one times, then record potential value E
3, by the slope formula (2) of electrode, calculate slope S.At V
s, C
s, V
x, when △ C and S is known, by concentration formula (1), calculate fluorinion concentration C
x.
Again according to formula (3), C
x, m, m
2, m
1and m
3when known, calculate the content of fluorine ion in solder(ing) paste former state, and then analyze the performance of solder(ing) paste.
The wherein preparation of reagent:
1.TISAB solution: take sodium chloride 58g, sodium citrate 10g, is dissolved in 800mL deionized water, then adds glacial acetic acid 57mL, and the NaOH solution with 40% regulates pH to 5.0-6.0, and then adding deionized water, to be diluted to cumulative volume be 1L.TISAB is that total ionic strength regulates buffer solution, can control the pH value of test solution, keeps solution to have suitable pH scope (5-8).Can also as screening agent, with iron aluminium plasma formed complex compound with eliminate they because of with fluorine ion generation association reaction and produce interference, eliminate the ionic strength difference of standard solution and detected solution simultaneously, ionic activity coefficient be consistent.
2.0.100molL
-1naF Standard Reserving Solution: accurately take 2.100g NaF (drying more than 2h at 120 DEG C) and put into 500mL beaker, be transferred to after adding 100mLTISAB solution and 300mL deionized water dissolving in 500mL volumetric flask, scale is diluted to deionized water, shake up, be stored in vinyon bottle for subsequent use.
In solder(ing) paste of the present invention, By Oxygen Bomb Combustion is combined with electrochemical ion electrode method by the detection method of fluoride, quantitatively detects the content of fluoride in solder(ing) paste, and instrument cost is low, it is simple and quick to analyze.
Claims (7)
1. a fluoride detection method in solder(ing) paste, is utilize oxygen bomb combustion to combine with electrochemical ion electrode method to detect, comprises the steps:
Step one: by soldering paste sample by acetone treatment, dissolves halide ion and obtains acetone halogen solutions, and by concentrated in concentrate for the solution evaporation obtained, concentrate, by oxygen bomb combustion process, obtains the test sample liquid of fluoride ion;
Step 2: above-mentioned test sample liquid is analyzed by electrochemical ion electrode method, in the metering circuit and test sample liquid pool device of ion-selective electrode, add fluorine ion standard model solution, to measure current potential, and calculate fluorinion concentration by concentration formula.
2. fluoride detection method in solder(ing) paste as claimed in claim 1, is characterized in that: concentration formula
wherein, C
xfor fluorinion concentration, V
sfor the volume of fluorine ion standard model solution, C
sfor the concentration of fluorine ion standard model solution, V
xfor the volume of institute's extracting sample solution, △ C is the concentration increments adding fluorine ion in test solution after standard solution, and S is the slope of electrode; In solder(ing) paste former state, content of fluoride ion is drawn by following formula:
wherein m is soldering paste sample quality, m
2-m
1for solder(ing) paste sample through acetone extraction, concentrated after quality, m
3for the quality of making test sample liquid taken in halogen sample in solder(ing) paste sample.
3. fluoride detection method in solder(ing) paste as claimed in claim 2, is characterized in that: by the slope formula of electrode,
calculate slope S; Wherein E
2, E
3for the potential value that potentiometer measures; △ C is drawn by following formula, Δ C=C
s× V
s/ V
x.
4. fluoride detection method in solder(ing) paste as claimed in claim 1, is characterized in that: described step one also specifically comprises the following steps:
A, get a dry centrifuge tube, load soldering paste sample m gram, in described centrifuge tube, add acetone, and put into hydro-extractor and carry out centrifuging, leave standstill, pour out upper strata acetone soln, put into drying receptacle, container mass is m
1gram; Repeat said process repeatedly, fully to obtain the halide ion in solder(ing) paste;
B, by concentrated for the acetone volatilization in container, weighing container and content quality obtain m
2gram; Therefrom accurately take concentrate m
3gram, put into platinum crucible;
Add absorbing liquid in advance in C, cylinder, screw oxygen bomb lid, oxygen bomb, to 4MPa, is placed in water-bath by oxygenate pressure, igniting; Product to be combusted is completely absorbed, and takes out cylinder, is proceeded to by absorbing liquid in volumetric flask, and rinse each several part in oxygen bomb with absorbing liquid, washing fluid is incorporated to volumetric flask, adds TISAB solution, obtains test sample liquid.
5. fluoride detection method in solder(ing) paste as claimed in claim 1, is characterized in that: described step 2 also specifically comprises the following steps:
D, preparation fluoride ion selective electrode, mix up potentiometer on request, load onto fluoride ion selective electrode and contrast electrode, fluoride ion selective electrode is immersed in 1.0 × 10
-1in the fluorine ion standard solution of mol/L, then with washed with de-ionized water several, until the electrode potential value recorded reaches background values, this value is indicated by the factory of electrode;
Content of fluoride ion in E, standard addition method test samples, draws VX test sample liquid, puts into plastic beaker, start stirrer, immerse fluoride ion selective electrode and contrast electrode, after current potential is stable, and record equilibrium potential; Accurately add the fluorine ion standard solution that VS concentration is CS, fluorine ion standard solution needs to add TISAB solution preparation, records potential value E2;
F, blank assay, replace sample with deionized water, repeat above-mentioned experiment, as blank value;
G, result calculate the test solution blank reagent after measuring E2 and dilute one times, then record potential value E3.
6. fluoride detection method in solder(ing) paste as claimed in claim 5, is characterized in that: described C
sbe 1.00 × 10
-4molL
-1or 1.00 × 10
-3molL
-1.
7. fluoride detection method in solder(ing) paste as claimed in claim 5, it is characterized in that: the compound method of TISAB solution is as follows: take sodium chloride 58g, sodium citrate 10g, be dissolved in 800mL deionized water, add glacial acetic acid 57mL again, NaOH solution with 40% regulates pH to 5.0-6.0, and then adding deionized water, to be diluted to cumulative volume be 1L.
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| CN105651851A (en) * | 2015-12-29 | 2016-06-08 | 中核北方核燃料元件有限公司 | Measuring method of fluorine content in thorium tetrafluoride |
| CN106525906A (en) * | 2016-09-29 | 2017-03-22 | 江苏国泰超威新材料有限公司 | Method for detecting content of fluorine ions in perfluoroalkyl sulfonyl imine salts |
| CN107192629A (en) * | 2017-04-27 | 2017-09-22 | 甘肃东兴铝业有限公司 | A kind of ion regulating agent and its application in aluminum fluoride in fluorine content determination method |
| CN107271530A (en) * | 2017-07-17 | 2017-10-20 | 云南云天化股份有限公司 | A kind of method of Oil repellent in fluorine-containing organic solvent of Accurate Determining |
| CN108802149A (en) * | 2018-06-19 | 2018-11-13 | 湖南师范大学 | A kind of Oxygen Bomb Combustion quickly measures the detection method of PAHs in coal content |
| CN110057896A (en) * | 2019-05-25 | 2019-07-26 | 江门市崖门新财富环保工业有限公司 | The analysis method of content of fluoride in a kind of hazardous waste |
| CN110057881A (en) * | 2019-05-16 | 2019-07-26 | 瓮福（集团）有限责任公司 | The rapid assay methods of fluorine in a kind of fluorine-containing slag |
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| CN104849112B (en) * | 2015-05-13 | 2017-09-29 | 中国科学院长春应用化学研究所 | A kind of Oxygen bottle combustion sample treatment |
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| CN104849113B (en) * | 2015-05-13 | 2017-09-22 | 中国科学院长春应用化学研究所 | The sample treatment of microwave igniting Oxygen bottle combustion |
| CN105651851A (en) * | 2015-12-29 | 2016-06-08 | 中核北方核燃料元件有限公司 | Measuring method of fluorine content in thorium tetrafluoride |
| CN105651851B (en) * | 2015-12-29 | 2018-07-27 | 中核北方核燃料元件有限公司 | The assay method of fluorine content in a kind of thorium tetrafluoride |
| CN106525906A (en) * | 2016-09-29 | 2017-03-22 | 江苏国泰超威新材料有限公司 | Method for detecting content of fluorine ions in perfluoroalkyl sulfonyl imine salts |
| CN106525906B (en) * | 2016-09-29 | 2019-07-23 | 江苏国泰超威新材料有限公司 | A method of content of fluoride ion in detection per-fluoroalkyl sulfonyl inferior amine salt |
| CN107192629A (en) * | 2017-04-27 | 2017-09-22 | 甘肃东兴铝业有限公司 | A kind of ion regulating agent and its application in aluminum fluoride in fluorine content determination method |
| CN107271530A (en) * | 2017-07-17 | 2017-10-20 | 云南云天化股份有限公司 | A kind of method of Oil repellent in fluorine-containing organic solvent of Accurate Determining |
| CN108802149A (en) * | 2018-06-19 | 2018-11-13 | 湖南师范大学 | A kind of Oxygen Bomb Combustion quickly measures the detection method of PAHs in coal content |
| CN110057881A (en) * | 2019-05-16 | 2019-07-26 | 瓮福（集团）有限责任公司 | The rapid assay methods of fluorine in a kind of fluorine-containing slag |
| CN110057896A (en) * | 2019-05-25 | 2019-07-26 | 江门市崖门新财富环保工业有限公司 | The analysis method of content of fluoride in a kind of hazardous waste |
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Application publication date: 20150513 |