CN104034811A - Method for analyzing trace contents in printed circuit board assembly (PCBA) board - Google Patents
Method for analyzing trace contents in printed circuit board assembly (PCBA) board Download PDFInfo
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- CN104034811A CN104034811A CN201410301544.1A CN201410301544A CN104034811A CN 104034811 A CN104034811 A CN 104034811A CN 201410301544 A CN201410301544 A CN 201410301544A CN 104034811 A CN104034811 A CN 104034811A
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Abstract
The invention discloses a method for analyzing trace contents in a printed circuit board assembly (PCBA) board. The analysis method comprises the following steps: analyzing anions or cations contained in the trace contents by an ion chromatograph; analyzing metal elements contained in the trace contents by a coupled plasma emission spectrometer; and analyzing organic functional groups contained in the trace contents by an infrared spectrometer. Moreover, a mixed solution consisting of alcohol and water is adopted for extraction and mixed acid dissolution before analysis, so that the detected limiting concentration is greatly improved, and the detection accuracy is greatly improved.
Description
Technical field
The present invention relates to the technical field that material detects qualification, relate in particular to a kind of analytical approach of microinclusion of PCBA plate.
Background technology
PCBA plate is important electronic unit, is the supporter of electronic devices and components, is the supplier of electronic devices and components electrical connection.The foreign organic matter that in use often can run into a lot of trace has a strong impact on the performance of product.The analysis of the microinclusion to PCBA plate in prior art is composition and its surperficial cleanliness factor of surface ion cleanliness technical testing of testing its element by EDS.Because microinclusion is substantially all made up of organo-functional group, zwitterion and metal and nonmetal element, thereby be just the source that is difficult to find out foreign matter by element EDS merely, and foreign matter is all that a small amount of mass spectrometer is also difficult to measure, this causes the accuracy of this analysis lower.
Summary of the invention
In view of this, the invention provides a kind of analytical approach of microinclusion of PCBA plate, the accuracy of this analytical approach is higher.
An analytical approach for the microinclusion of PCBA plate, comprises the following steps:
(1) adopt extraction solvent to extract on PCBA plate sample to be analyzed and be extracted liquid, use ion chromatograph to detect to determine contained negative ion or the kation of PCBA plate sample microinclusion to be analyzed to this extract;
(2) adopt mixed-acid dissolution to obtain acid solution on PCBA plate sample to be analyzed, use coupled plasma emission spectrometer to detect to determine the contained metallic element of PCBA plate sample microinclusion to be analyzed to acid solution;
(3) PCBA plate sample to be analyzed is carried out after pre-treatment, use infrared spectrometer to detect to determine the contained organo-functional group of PCBA plate sample microinclusion to be analyzed.
In said method, the known any detection mode of those skilled in the art all can be implemented the detection of above-mentioned ion chromatograph, coupled plasma emission spectrometer and infrared spectrometer, does not repeat them here.Can not lead to misunderstanding, before above-mentioned three steps titled with sequence number not mean the restriction of the sequencing to its generation, it only represents enumerating three steps.In fact these three steps are mutually independently, do not rely on mutually, and the result that any one step completes all on other steps, any impact does not occur.
Wherein, the mixed liquor of described extraction solvent for being formed by alcohol and water.Alcohol is preferably C
1～C
4alcohol, for example isopropyl alcohol.The volume ratio of alcohol and water is (1.5～5): 1, and for example both volume ratios can be 1.5:1,1.8:1,2:1,2.5:1,3:1,4:1,4.5:1 or 5:1.
Wherein, the temperature of extraction is 45～55 DEG C, and the time of extraction is 0.5～1.5h, and the consumption of the PCBA plate sample to be analyzed extraction solvent used that every 2～3g is to be extracted is 55～65ml.
Wherein, described extraction mode is soxhlet extraction or ultrasonic extraction.Before extraction, use and use nitrogen flushing reduced pressure concentration.
Wherein, described mixed-acid dissolution comprises that adopting is 1:(2～4 by volume ratio) red fuming nitric acid (RFNA) and the acid mixture that forms of concentrated hydrochloric acid dissolve, this acid mixture is for the microinclusion taking metal simple-substance as principal ingredient; Adopting is (2～4) by volume ratio: the acid mixture that 1 red fuming nitric acid (RFNA) and concentrated hydrochloric acid form dissolves, and this acid mixture is for the microinclusion taking organism (particularly superpolymer) as principal ingredient; And adopting is (8～10) by volume ratio: (2～4): the acid mixture that 1 red fuming nitric acid (RFNA), concentrated hydrochloric acid, dense hydrofluorite forms dissolves, this acid mixture is for the microinclusion taking class concrete as principal ingredient.Be understandable that, red fuming nitric acid (RFNA), concentrated hydrochloric acid and dense hydrofluorite are the general concept in this area, its concentration range is specific indication, for example red fuming nitric acid (RFNA) refers to the salpeter solution that massfraction is 65% left and right, it is 50% hydrofluoric acid solution that dense hydrofluorite refers to massfraction, and concentrated hydrochloric acid refers to the hydrochloric acid that massfraction is 37% left and right.
Wherein, described extraction mode is soxhlet extraction or ultrasonic extraction.
Wherein, the described process by PCBA plate sample employing mixed-acid dissolution to be analyzed completes by micro-wave digestion mode.Micro-wave digestion mode can accelerate dissolution process carrying out.
Wherein, described pre-treatment comprises and shattering.The testable granularity of infrared test that the size shattering is known to those skilled in the art dawn.Certainly, pre-treatment also comprises and sample to be tested through shattering is adopted the organic solvents such as acetone, methylene chloride extract organic principle, then extract is adopted to KBr compressing tablet.
The present invention uses ion chromatograph to analyze the contained negative ion of microinclusion or kation, use coupled plasma emission spectrometer to analyze the contained metallic element of microinclusion, use infrared spectrometer to analyze the contained organo-functional group of microinclusion.And before above-mentioned analysis, adopt respectively that the mixed liquor being made up of alcohol and water extracts, mixed-acid dissolution, greatly improved thus the limiting concentration of its detection, greatly improved thus the accuracy detecting.
Embodiment
Further illustrate technical scheme of the present invention below in conjunction with embodiment.
Embodiment 1
First, adopt the mixed solution of the isopropyl alcohol and water that volume ratio is 1.5:1 to carry out extracting 1.5h at 45 DEG C on PCBA plate sample to be analyzed, the consumption of the PCBA plate sample to be analyzed extraction solvent used that every 2g is to be extracted is 65ml, to be extracted liquid and use ion chromatograph to this extract, obtain contained negative ion or the kation of microinclusion.Then, the acid mixture that the acid mixture that the red fuming nitric acid (RFNA) that the acid mixture that the red fuming nitric acid (RFNA) that to adopt respectively by volume ratio be 1:2 and concentrated hydrochloric acid form dissolves, be 2:1 by volume ratio and concentrated hydrochloric acid form dissolves and be 8:2:1 by volume ratio red fuming nitric acid (RFNA), concentrated hydrochloric acid, dense hydrofluorite forms dissolves, in these three kinds of mixed-acid dissolution processes, adopt micro-wave digestion mode, use ICP-OES to measure its lysate, obtain the contained metallic element of microinclusion.Then, by PCBA plate sample to be analyzed shatter, organic solvent extraction and make KBr compressing tablet after adopt FTIR to carry out examination of infrared spectrum, obtain microinclusion contained organo-functional group.Finally, obtain the qualitative analysis of the microinclusion of PCBA plate sample to be analyzed for above-mentioned three pacing test results.
Embodiment 2
In this example, the mixed solution of the isopropyl alcohol and water that extraction solvent volume ratio is 5:1, extraction extracts 0.5h at 55 DEG C, and the consumption of the PCBA plate sample to be analyzed extraction solvent used that every 3g is to be extracted is 55ml; The mixed-acid dissolution that the mixed-acid dissolution that the mixed-acid dissolution that the red fuming nitric acid (RFNA) that it is 1:3 that mixed-acid dissolution is respectively by volume ratio and concentrated hydrochloric acid form, the red fuming nitric acid (RFNA) that is 3:1 by volume ratio and concentrated hydrochloric acid form and red fuming nitric acid (RFNA), concentrated hydrochloric acid, the dense hydrofluorite that is 9:3:1 by volume ratio form; Except above-mentioned condition, other conditions are all same as embodiment 1.
Embodiment 3:
In this example, the mixed solution of the isopropyl alcohol and water that extraction solvent volume ratio is 3.5:1, extraction extracts 1h at 50 DEG C, and the consumption of the PCBA plate sample to be analyzed extraction solvent used that every 2.5g is to be extracted is 60ml; The mixed-acid dissolution that the mixed-acid dissolution that the mixed-acid dissolution that the red fuming nitric acid (RFNA) that it is 1:4 that mixed-acid dissolution is respectively by volume ratio and concentrated hydrochloric acid form, the red fuming nitric acid (RFNA) that is 4:1 by volume ratio and concentrated hydrochloric acid form and red fuming nitric acid (RFNA), concentrated hydrochloric acid, the dense hydrofluorite that is 10:4:1 by volume ratio form; Except above-mentioned condition, other conditions are all same as embodiment 1.
Embodiment 4:
In this example, the mixed solution of the isopropyl alcohol and water that extraction solvent volume ratio is 3:1, extraction extracts 1h at 60 DEG C, and the consumption of the PCBA plate sample to be analyzed extraction solvent used that every 2.5g is to be extracted is 60ml; The mixed-acid dissolution that the mixed-acid dissolution that the mixed-acid dissolution that the red fuming nitric acid (RFNA) that it is 1:3 that mixed-acid dissolution is respectively by volume ratio and concentrated hydrochloric acid form, the red fuming nitric acid (RFNA) that is 3:1 by volume ratio and concentrated hydrochloric acid form and red fuming nitric acid (RFNA), concentrated hydrochloric acid, the dense hydrofluorite that is 9:3:1 by volume ratio form; Except above-mentioned condition, other conditions are all same as embodiment 1.
Use the method can not be confined to only have metal qualitative, use the method to understand more extensive, can learn more micro-ly, and detecting lower concentration, makes the indium addition material can be out qualitative, has and detects more accurately effect.
Applicant's statement, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, and the selections of the equivalence replacement to the each raw material of product of the present invention and the interpolation of auxiliary element, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
Claims (9)
1. an analytical approach for the microinclusion of PCBA plate, is characterized in that, comprises the following steps:
(1) adopt extraction solvent to extract on PCBA plate sample to be analyzed and be extracted liquid, use ion chromatograph to detect to determine contained negative ion or the kation of microinclusion in PCBA plate sample to be analyzed to this extract;
(2) adopt mixed-acid dissolution to obtain acid solution on PCBA plate sample to be analyzed, use coupled plasma emission spectrometer to detect to determine the contained metallic element of PCBA plate sample microinclusion to be analyzed to acid solution;
(3) PCBA plate sample to be analyzed is carried out after pre-treatment, use infrared spectrometer to detect to determine the contained organo-functional group of PCBA plate sample microinclusion to be analyzed.
2. method according to claim 1, is characterized in that, the mixed liquor of described extraction solvent for being made up of alcohol and water.
3. method according to claim 2, is characterized in that, the volume ratio of described alcohol and water is (1.5～5): 1.
4. method according to claim 2, is characterized in that, described alcohol is isopropyl alcohol.
5. method according to claim 1, is characterized in that, the temperature of described extraction is 45～55 DEG C, and the time of extraction is 0.5～1.5h, and the consumption of the PCBA plate sample to be analyzed extraction solvent used that every 2～3g is to be extracted is 55～65ml.
6. method according to claim 1, is characterized in that, described extraction mode is soxhlet extraction or ultrasonic extraction.
7. method according to claim 1, it is characterized in that, described mixed-acid dissolution comprises that adopting is 1:(2～4 by volume ratio) red fuming nitric acid (RFNA) and the acid mixture that forms of concentrated hydrochloric acid dissolve, adopting is (2～4) by volume ratio: the acid mixture that 1 red fuming nitric acid (RFNA) and concentrated hydrochloric acid form dissolves, and adopting is (8～10) by volume ratio: (2～4): the acid mixture that 1 red fuming nitric acid (RFNA), concentrated hydrochloric acid, dense hydrofluorite forms dissolves.
8. method according to claim 1, is characterized in that, the process of described employing mixed-acid dissolution completes by micro-wave digestion mode.
9. method according to claim 1, is characterized in that, described pre-treatment comprises and shattering.
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| CN201410301544.1A CN104034811A (en) | 2014-06-27 | 2014-06-27 | Method for analyzing trace contents in printed circuit board assembly (PCBA) board |
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| CN201410301544.1A CN104034811A (en) | 2014-06-27 | 2014-06-27 | Method for analyzing trace contents in printed circuit board assembly (PCBA) board |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110412200A (en) * | 2019-08-13 | 2019-11-05 | 江西瑞林稀贵金属科技有限公司 | The analysis method of chlorinity in a kind of measurement electroplating sludge |
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| WO2004054931A1 (en) * | 2002-12-18 | 2004-07-01 | Showa Denko K. K. | Barium titanate and electronic parts using the material |
| CN103033498A (en) * | 2012-12-21 | 2013-04-10 | 深圳市谱尼测试科技有限公司 | Method for simultaneously detecting substances of very high concern (SVHC) boric acid and borax of registration, evaluation, authorization and restriction of chemicals (REACH) law of European Union |
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2014
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2004054931A1 (en) * | 2002-12-18 | 2004-07-01 | Showa Denko K. K. | Barium titanate and electronic parts using the material |
| CN103033498A (en) * | 2012-12-21 | 2013-04-10 | 深圳市谱尼测试科技有限公司 | Method for simultaneously detecting substances of very high concern (SVHC) boric acid and borax of registration, evaluation, authorization and restriction of chemicals (REACH) law of European Union |
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| 孙静: "微波诱导热解废旧印刷电路板（WPCB）的实验和机理研究", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》, no. 05, 15 May 2013 (2013-05-15), pages 51 - 54 * |
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| 陈胜文等: "微波消解 ICP-AES 测定废弃线路板中金属元素", 《上海第二工业大学学报》, vol. 26, no. 3, 30 September 2009 (2009-09-30), pages 183 - 187 * |
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| CN110412200A (en) * | 2019-08-13 | 2019-11-05 | 江西瑞林稀贵金属科技有限公司 | The analysis method of chlorinity in a kind of measurement electroplating sludge |
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Application publication date: 20140910 |