JP5140519B2 - Solder composition analysis method - Google Patents
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- JP5140519B2 JP5140519B2 JP2008212839A JP2008212839A JP5140519B2 JP 5140519 B2 JP5140519 B2 JP 5140519B2 JP 2008212839 A JP2008212839 A JP 2008212839A JP 2008212839 A JP2008212839 A JP 2008212839A JP 5140519 B2 JP5140519 B2 JP 5140519B2
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- 229910000679 solder Inorganic materials 0.000 title claims description 55
- 239000000203 mixture Substances 0.000 title claims description 30
- 238000004458 analytical method Methods 0.000 title claims description 21
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 48
- 239000002253 acid Substances 0.000 claims description 39
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 30
- 229910017604 nitric acid Inorganic materials 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 14
- 238000009616 inductively coupled plasma Methods 0.000 claims description 7
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 238000004993 emission spectroscopy Methods 0.000 claims description 2
- 238000004949 mass spectrometry Methods 0.000 claims description 2
- 238000004445 quantitative analysis Methods 0.000 claims description 2
- 239000000523 sample Substances 0.000 description 31
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 14
- 239000000243 solution Substances 0.000 description 13
- 229910045601 alloy Inorganic materials 0.000 description 6
- 239000000956 alloy Substances 0.000 description 6
- 239000000470 constituent Substances 0.000 description 6
- 238000004090 dissolution Methods 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 239000012488 sample solution Substances 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000005259 measurement Methods 0.000 description 4
- 150000007513 acids Chemical class 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- AUYOHNUMSAGWQZ-UHFFFAOYSA-L dihydroxy(oxo)tin Chemical compound O[Sn](O)=O AUYOHNUMSAGWQZ-UHFFFAOYSA-L 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000012085 test solution Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Sampling And Sample Adjustment (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Description
本発明は、「鉛フリーはんだ」と呼ばれる鉛の含有量が０．１質量％以下のはんだの組成分析に適用して有効な技術である。 The present invention is a technique that is effective when applied to a composition analysis of a solder having a lead content of 0.1% by mass or less, referred to as “lead-free solder”.
欧州連合（ＥＵ）によるＲｏＨＳ（Ｒｅｓｔｒｉｃｔｉｏｎ ｏｆ Ｈａｚａｒｄｏｕｓ Ｓｕｂｓｔａｎｃｅｓ）指令に基づき、我が国からＥＵ加盟国向けに輸出される電気・電子機器に含まれるＰｂ、Ｈｇ、Ｃｄ、Ｃｒ（ＶＩ）、特定臭素系難燃剤の含有量は一定量以下に規制されることになった。 Pb, Hg, Cd, Cr (VI), and specific brominated flame retardants contained in electrical and electronic equipment exported from Japan to EU member countries based on the European Union (EU) RoHS (Restriction of Hazardous Sub- stances) The content of was to be regulated below a certain amount.
例えば、従来の電子機器では、電子回路にＰｂを主成分とするはんだを使用していたが、ＲｏＨＳ指令により規制の対象になった。そして、現在の電子機器では、「鉛フリーはんだ」と呼ばれる鉛含有量が０．１質量％以下のはんだが使用されるようになった。 For example, in a conventional electronic device, solder containing Pb as a main component is used in an electronic circuit, but has been regulated by the RoHS directive. And in the present electronic device, the solder whose lead content called 0.1 mass% or less called "lead free solder" came to be used.
この鉛フリーはんだの分析法としては、ＪＩＳ Ｚ３９１０(はんだ分析法)があるが、銀の定量に滴定法が採用されており、規定された全ての合金構成元素および不純物元素を一度に分析することができないため、測定に手間と時間を要する。 There is JIS Z3910 (solder analysis method) as an analysis method of this lead-free solder, but the titration method is adopted for the determination of silver, and all specified alloy constituent elements and impurity elements should be analyzed at once. Because it is not possible, measurement takes time and effort.
ＪＩＳ Ｚ３９１０より迅速にはんだの組成分析を行うことができる方法として、はんだを無機酸とオキシカルボン酸とで加熱溶解してはんだ試料溶液を調製した後、プラズマ発光分析法により試料溶液中の元素を測定する方法が提案されている（例えば特許文献１参照）。 The solder composition analysis can be performed more quickly than JIS Z3910 by preparing a solder sample solution by heating and dissolving the solder with an inorganic acid and an oxycarboxylic acid, and then analyzing the elements in the sample solution by plasma emission analysis. A measuring method has been proposed (see, for example, Patent Document 1).
また、はんだの組成分析を高精度に行えるようにした方法として、はんだ試料を硝酸により溶解し、試料溶液中の元素を定量分析する方法が提案されている（例えば特許文献２参照）。
しかしながら、特許文献１に記載の提案は、鉛を多く含む従来のはんだを対象とした分析方法であり、鉛含有率が低い鉛フリーはんだの分析には対応していない。 However, the proposal described in Patent Document 1 is an analysis method for a conventional solder containing a large amount of lead, and does not support analysis of lead-free solder having a low lead content.
また、特許文献２の提案は、不溶残渣が生じないようにするには、実質的に試料を溶解する際の温度を２０〜３５℃と厳密に制御する必要がある。しかも、低温度で溶解するため、溶解に時間を要して迅速性に欠ける。 Further, in the proposal of Patent Document 2, it is necessary to strictly control the temperature at which the sample is substantially dissolved to 20 to 35 ° C. in order to prevent insoluble residues from being generated. And since it melt | dissolves at low temperature, time is required for melt | dissolution and lacks in speediness.
本発明の目的は、鉛フリーはんだに含まれる全合金構成元素と不純物元素とを同時に分析する方法を提供することにある。 An object of the present invention is to provide a method for simultaneously analyzing all alloy constituent elements and impurity elements contained in lead-free solder.
本発明の前記ならびにその他の目的と新規な特徴は、本明細書の記述および添付図面から明らかになるであろう。 The above and other objects and novel features of the present invention will be apparent from the description of this specification and the accompanying drawings.
本願において開示される発明のうち、代表的なものの概要を簡単に説明すれば、次のとおりである。 Of the inventions disclosed in the present application, the outline of typical ones will be briefly described as follows.
すなわち、鉛の含有量が０．１質量％以下のはんだの組成分析方法であって、前記はんだを溶解する酸として、硫酸３．６ｍｏｌ／Ｌ以上１３．４ｍｏｌ／Ｌ以下、硝酸１．３ｍｏｌ／Ｌ以上３．４ｍｏｌ／Ｌ以下の濃度であり、且つ硫酸と硝酸のモル比が２．６：１以上７．９：１以下である混酸を用い、前記はんだの組成成分を完全に溶解させた後、この組成成分を定量分析する。 That is, it is a composition analysis method for a solder having a lead content of 0.1% by mass or less, and as an acid for dissolving the solder, sulfuric acid of 3.6 mol / L or more and 13.4 mol / L or less, nitric acid 1.3 mol / L The composition component of the solder was completely dissolved by using a mixed acid having a concentration of L to 3.4 mol / L and a molar ratio of sulfuric acid to nitric acid of 2.6: 1 to 7.9: 1. Then, this composition component is quantitatively analyzed.
なお、本願発明において「はんだの組成成分を完全に溶解させた」とは、はんだの組成成分が溶液中に溶解して残渣が目視で見えなくなった状態を意味する。 In the present invention, “the solder composition component is completely dissolved” means a state in which the solder composition component is dissolved in the solution and the residue becomes invisible.
本願において開示される発明のうち、代表的なものによって得られる効果を簡単に説明すれば以下のとおりである。 Among the inventions disclosed in the present application, effects obtained by typical ones will be briefly described as follows.
すなわち、はんだを溶解する酸として、硫酸３．６ｍｏｌ／Ｌ以上１３．４ｍｏｌ／Ｌ以下、硝酸１．３ｍｏｌ／Ｌ以上３．４ｍｏｌ／Ｌ以下の濃度であり、且つ硫酸と硝酸のモル比が２．６：１以上７．９：１以下である混酸を用い、はんだの組成成分を完全に溶解させた後、この組成成分を定量分析する。 That is, the acid for dissolving the solder has a concentration of 3.6 mol / L to 13.4 mol / L of sulfuric acid, 1.3 mol / L to 3.4 mol / L of nitric acid, and a molar ratio of sulfuric acid to nitric acid of 2. Using a mixed acid of 6: 1 or more and 7.9: 1 or less and completely dissolving the composition component of the solder, the composition component is quantitatively analyzed.
つまり、はんだ試料を溶解する混酸を、予め硝酸と硫酸とが所定濃度になるように混合調製し、試料を混酸で溶解して試料検液を作製する。そして、この作製した試料検液を定量分析する。 That is, a mixed acid that dissolves the solder sample is mixed and prepared in advance so that nitric acid and sulfuric acid have a predetermined concentration, and the sample is dissolved with the mixed acid to prepare a sample test solution. Then, the prepared sample test solution is quantitatively analyzed.
これにより、鉛フリーはんだに含まれる全合金構成元素と不純物元素とを同時に分析することができる。 Thereby, all the alloy constituent elements and impurity elements contained in lead-free solder can be analyzed simultaneously.
以下、本発明の実施の形態を説明する。図１は本発明の一実施の形態であるはんだの組成分析方法の工程を示すフロー図である。図１に示すように、本発明のはんだの組成分析方法は、溶液化工程Ｓ１と測定工程Ｓ２とからなる。 Embodiments of the present invention will be described below. FIG. 1 is a flowchart showing the steps of a solder composition analysis method according to an embodiment of the present invention. As shown in FIG. 1, the solder composition analysis method of the present invention comprises a solution forming step S1 and a measuring step S2.
溶液化工程Ｓ１は、試料を秤量する工程、酸を混合する工程、および試料に混酸を加えて溶解する工程から構成される。 The solution forming step S1 includes a step of weighing a sample, a step of mixing an acid, and a step of adding a mixed acid to the sample and dissolving it.
まず、試料を秤量する工程について説明する。試料は、鉛の含有量が０．１質量％以下のいわゆる鉛フリーはんだである。鉛フリーはんだの成分としては、例えばＳｎ、Ａｇ、Ｃｕなどが一般的であるが、さらに他の元素が含まれていてもよい。はんだとしては、はんだ接合に使用する前のはんだであってもよいし、例えば半導体チップ、プリント基板、パッケージ材、フレキシブル基板などの電子部品中に存在するはんだであってもよい。秤量は、精密分析で一般的な方法であれば特に制限はない。 First, the process of weighing a sample will be described. The sample is a so-called lead-free solder having a lead content of 0.1% by mass or less. As a component of lead-free solder, for example, Sn, Ag, Cu and the like are common, but other elements may be further included. The solder may be a solder before being used for solder joining, or may be a solder present in an electronic component such as a semiconductor chip, a printed board, a package material, or a flexible board. The weighing is not particularly limited as long as it is a general method for precise analysis.
次に、酸を混合する工程について説明する。酸としては硫酸および硝酸を混合した混酸を用いる。硝酸のみであると、メタスズ酸の沈殿が生じてしまう虞がある。硫酸と硝酸は、体積比２：１から６：１までの範囲で混合し、硫酸濃度が３．６ｍｏｌ／Ｌ以上１３．４ｍｏｌ／Ｌ以下、硝酸濃度が１．３ｍｏｌ／Ｌ以上３．４ｍｏｌ／Ｌ以下、硫酸と硝酸のモル比が２．６：１以上７．９：１以下となるように水で希釈して混酸を調製する。混酸の組成は、操作を容易にする観点から、硫酸濃度が３．６ｍｏｌ／Ｌ以上４．５ｍｏｌ／Ｌ以下、硝酸濃度が１．３ｍｏｌ／Ｌ以上１．７ｍｏｌ／Ｌ以下であるとより好ましい。硫酸濃度および硝酸濃度がそれぞれ３．６ｍｏｌ／Ｌ未満、１．３ｍｏｌ／Ｌ未満であると、試料が完全に溶解しないことがある。 Next, the step of mixing the acid will be described. A mixed acid in which sulfuric acid and nitric acid are mixed is used as the acid. If only nitric acid is used, precipitation of metastannic acid may occur. Sulfuric acid and nitric acid are mixed in a volume ratio range of 2: 1 to 6: 1, the sulfuric acid concentration is 3.6 mol / L or more and 13.4 mol / L or less, and the nitric acid concentration is 1.3 mol / L or more and 3.4 mol / L. A mixed acid is prepared by diluting with water so that the molar ratio of sulfuric acid and nitric acid is 2.6: 1 or more and 7.9: 1 or less. From the viewpoint of facilitating the operation, the mixed acid composition is more preferably a sulfuric acid concentration of 3.6 mol / L to 4.5 mol / L and a nitric acid concentration of 1.3 mol / L to 1.7 mol / L. When the sulfuric acid concentration and the nitric acid concentration are less than 3.6 mol / L and less than 1.3 mol / L, the sample may not be completely dissolved.
そして、試料に混酸を加えて溶解する工程では、試料を例えばビーカー等の容器に移し、混酸を適量加えて完全に試料を溶解させる。この際の溶解温度には特に制限はないが、通常８０〜１００℃で行われる。 In the step of adding mixed acid to the sample and dissolving it, the sample is transferred to a container such as a beaker, and an appropriate amount of mixed acid is added to completely dissolve the sample. Although there is no restriction | limiting in particular in the melting temperature in this case, Usually, it carries out at 80-100 degreeC.
測定工程Ｓ２は、上述の溶液化工程で調製した試料溶液を測定し、試料中の元素を定量分析する工程である。つまり、溶液化工程で溶液とした試料を例えば全量フラスコ等に移し、純水で希釈してこの希釈溶液を試料溶液として定量分析する。 The measurement step S2 is a step of measuring the sample solution prepared in the above-described solution forming step and quantitatively analyzing elements in the sample. That is, the sample made into a solution in the solution forming step is transferred to, for example, a whole flask, diluted with pure water, and this diluted solution is quantitatively analyzed as a sample solution.
分析方法としては、一般に定量分析に適用される方法であれば特に制限はないが、微量成分を迅速かつ高精度に分析できる観点から、例えば、ＩＣＰ（Ｉｎｄｕｃｔｉｖｅｌｙ Ｃｏｕｐｌｅｄ Ｐｌａｓｍａ）発光分析法、ＩＣＰ質量分析法、原子吸光法などが好適に挙げられる。 The analysis method is not particularly limited as long as it is a method generally applied to quantitative analysis. From the viewpoint of analyzing trace components quickly and with high accuracy, for example, ICP (Inductively Coupled Plasma) emission spectrometry, ICP mass spectrometry The method, atomic absorption method and the like are preferable.
このように本発明では、鉛フリーはんだにおいて、酸として所定濃度の硫酸および硝酸を混合した混酸を用いて組成成分を完全に溶解させるので、鉛フリーはんだに含まれる全合金構成元素と不純物元素とを同時に分析することができる。 As described above, in the present invention, in the lead-free solder, the composition components are completely dissolved by using a mixed acid in which sulfuric acid and nitric acid at a predetermined concentration are mixed as acids. Therefore, all the alloy constituent elements and impurity elements contained in the lead-free solder Can be analyzed simultaneously.
つまり、鉛フリーはんだでは、酸溶解時に不溶残渣が生じることが問題となっていたが、所定濃度の硫酸および硝酸を混合した混酸により鉛フリーはんだを、残渣を生じさせずに完全に溶解することができ、結果として鉛フリーはんだに含まれる全合金構成元素と不純物元素とを同時に高精度に分析できるのである。 In other words, lead-free solder has a problem that insoluble residues are generated during acid dissolution, but lead-free solder can be completely dissolved without any residue by a mixed acid mixed with sulfuric acid and nitric acid at a predetermined concentration. As a result, all alloy constituent elements and impurity elements contained in the lead-free solder can be simultaneously analyzed with high accuracy.
また、所定濃度の硫酸および硝酸を混合した混酸によれば、不溶残渣が生じる虞がないので、溶解する際の温度を厳密に制御する必要がなく、高温溶解が可能であり、例えば４０分以内と極めて迅速に鉛フリーはんだを完全に溶解させることができる。 Moreover, according to the mixed acid in which sulfuric acid and nitric acid of a predetermined concentration are mixed, there is no possibility that an insoluble residue is generated. Therefore, it is not necessary to strictly control the temperature at the time of dissolution, and high temperature dissolution is possible, for example, within 40 minutes And lead-free solder can be completely dissolved very quickly.
以下、実施例によって、本発明をさらに説明する。なお、本発明は、これらの実施例によって限定されない。 Hereinafter, the present invention will be further described by way of examples. In addition, this invention is not limited by these Examples.
(実施例)
〔溶液化工程〕
試料(千住金属工業製：Ｍ７０５)０．５ｇを採取し、質量を０．１ｍｇの桁まで精度良く秤量した。
(Example)
[Solution process]
A sample (manufactured by Senju Metal Industry Co., Ltd .: M705) 0.5 g was collected and weighed accurately to the order of 0.1 mg.
ついで、表１に示すように、硫酸および硝酸からなる７種類の酸濃度および体積比の混酸を調製した。 Next, as shown in Table 1, seven acid concentrations and volume ratios of sulfuric acid and nitric acid were prepared.
試料を３００ｍＬビーカーに移して、上述の７種類の混酸２０ｍＬをそれぞれ加えて８０℃で４０分溶解した。この際の試料の溶解状態を表１に示す。 The sample was transferred to a 300 mL beaker, and 20 mL of the above-mentioned seven mixed acids were added and dissolved at 80 ° C. for 40 minutes. The dissolved state of the sample at this time is shown in Table 1.
表１の結果から、混酸中の硫酸濃度が３．６ｍｏｌ／Ｌ未満、硝酸濃度が１．３ｍｏｌ／Ｌ未満であると、はんだの組成成分の残渣が溶液中に残り、完全には溶解しなかった。このため、はんだの組成成分の残渣を残さずに、完全に溶解させるには、硫酸濃度３．６ｍｏｌ／Ｌ以上１３．４ｍｏｌ／Ｌ以下、硝酸濃度１．３ｍｏｌ／Ｌ以上３．４ｍｏｌ／Ｌ以下であり、且つ硫酸と硝酸のモル比が２．６：１以上７．９：１以下である混酸が好適であることがわかった。 From the results in Table 1, when the sulfuric acid concentration in the mixed acid is less than 3.6 mol / L and the nitric acid concentration is less than 1.3 mol / L, the residue of the solder component remains in the solution and does not completely dissolve. It was. For this reason, in order to dissolve completely without leaving the residue of the solder composition component, the sulfuric acid concentration is 3.6 mol / L or more and 13.4 mol / L or less, and the nitric acid concentration is 1.3 mol / L or more and 3.4 mol / L or less. And a mixed acid having a molar ratio of sulfuric acid to nitric acid of 2.6: 1 or more and 7.9: 1 or less was found to be suitable.
また、上述の硫酸濃度および硝酸濃度の範囲の混酸であれば、はんだの組成成分を完全に溶解することはできるが、硫酸濃度が４．５ｍｏｌ／Ｌ、硝酸濃度が１．７ｍｏｌ／Ｌをそれぞれ超えると、発熱が観られた。このため、操作を容易にすることを考慮すると、硫酸濃度が３．６ｍｏｌ／Ｌ以上４．５ｍｏｌ／Ｌ以下、硝酸濃度が１．３ｍｏｌ／Ｌ以上１．７ｍｏｌ／Ｌ以下である混酸がより好適であることがわかった。 In addition, if the mixed acid is in the range of the sulfuric acid concentration and nitric acid concentration described above, the solder composition components can be completely dissolved, but the sulfuric acid concentration is 4.5 mol / L and the nitric acid concentration is 1.7 mol / L. When exceeded, fever was observed. For this reason, in view of facilitating the operation, a mixed acid having a sulfuric acid concentration of 3.6 mol / L to 4.5 mol / L and a nitric acid concentration of 1.3 mol / L to 1.7 mol / L is more preferable. I found out that
なお、図２に、試料が完全に溶解した状態の一例を写真で示す。図２から、試料が完全に溶解した状態では、目視で残渣が観られず、溶液がほぼ透明となっていることがわかる。 FIG. 2 shows an example of a state in which the sample is completely dissolved. FIG. 2 shows that in the state where the sample is completely dissolved, no residue is visually observed, and the solution is almost transparent.
〔測定工程〕
溶液化工程で溶液とした試料全量を５０ｍＬフラスコに移し入れ、純水で標線まで希釈した。この希釈溶液を試料溶液とし、ＩＣＰ発光分析装置で測定した。結果を表２に示す。
[Measurement process]
The total amount of the sample made into a solution in the solution forming step was transferred to a 50 mL flask and diluted to the marked line with pure water. This diluted solution was used as a sample solution and measured with an ICP emission spectrometer. The results are shown in Table 2.
表２に示すように、はんだに含まれる合金構成元素である銀、銅に加えて数多くの不純物元素を一度に測定できた。 As shown in Table 2, in addition to silver and copper, which are alloy constituent elements contained in solder, many impurity elements could be measured at once.
（比較例）
比較例として硝酸、塩酸およびその混酸を用いた場合のはんだの溶解について検討した。つまり、混酸として、表３に示す６種類の酸濃度の酸または混酸を用いた以外は実施例と同様にして試料を溶解させた。この際の試料の溶解状態を表３および図３の写真に示す。なお、表３の上から順に記載された各酸濃度が、図３の左から順に示した結果に対応している。
(Comparative example)
As a comparative example, the dissolution of solder in the case of using nitric acid, hydrochloric acid and mixed acid thereof was examined. That is, the sample was dissolved in the same manner as in the example except that six acid concentrations shown in Table 3 or mixed acids were used as the mixed acid. The dissolved state of the sample at this time is shown in Table 3 and the photograph in FIG. In addition, each acid density | concentration described in order from the top of Table 3 respond | corresponds to the result shown in order from the left of FIG.
表３および図３の結果から、硝酸のみを用いた場合にはメタスズ酸の沈殿が生じて試料を溶解できないことがわかった。硝酸および塩酸を混合した混酸を用いた場合にも殆どでメタスズ酸等の沈殿が生じて試料の溶解が困難なことがわかった。 From the results of Table 3 and FIG. 3, it was found that when only nitric acid was used, precipitation of metastannic acid occurred and the sample could not be dissolved. It was found that even when a mixed acid in which nitric acid and hydrochloric acid were mixed was used, precipitation of metastannic acid or the like occurred in most cases, and it was difficult to dissolve the sample.
ここで、硝酸濃度０．３ｍｏｌ／Ｌ、塩酸濃度５．９ｍｏｌ／Ｌである混酸を用いた場合、試料を完全に溶解させることができた。これは、分解時の塩酸濃度が高いため、Ａｇ＋がクロライド錯体となり水溶性を示すことが原因と考えられる。しかし、水で５０ｍＬに定容すると、塩酸濃度が低下するため錯体が維持できなくなり、ＡｇＣｌ沈殿が生じたため、試料の組成成分の分析が不可能であった。 Here, when a mixed acid having a nitric acid concentration of 0.3 mol / L and a hydrochloric acid concentration of 5.9 mol / L was used, the sample could be completely dissolved. This is presumably because Ag + becomes a chloride complex and exhibits water solubility because the hydrochloric acid concentration during decomposition is high. However, when the volume was adjusted to 50 mL with water, the complex concentration could not be maintained because the concentration of hydrochloric acid was lowered, and AgCl precipitation occurred, making it impossible to analyze the composition components of the sample.
また、塩酸のみを用いた場合には沈殿は生じないが、塩酸濃度が高く測定工程で分析装置に負荷を与え、試料を完全に溶解するための酸としては不適当であった。 Further, when only hydrochloric acid was used, precipitation did not occur, but the concentration of hydrochloric acid was high and it was unsuitable as an acid for completely dissolving the sample by applying a load to the analyzer during the measurement process.
本発明は、「鉛フリーはんだ」と呼ばれる鉛の含有量が０．１質量％以下のはんだの組成分析に有効に利用することができる。 The present invention can be effectively used for the composition analysis of solder called “lead-free solder” with a lead content of 0.1 mass% or less.
Claims (3)
前記はんだを溶解する酸として、硫酸３．６ｍｏｌ／Ｌ以上１３．４ｍｏｌ／Ｌ以下、硝酸１．３ｍｏｌ／Ｌ以上３．４ｍｏｌ／Ｌ以下の濃度であり、且つ硫酸と硝酸のモル比が２．６：１以上７．９：１以下である混酸を用い、前記はんだの組成成分を完全に溶解させた後、この組成成分を定量分析することを特徴とするはんだの組成分析方法。 A method for analyzing the composition of a solder having a lead content of 0.1% by mass or less,
The acid for dissolving the solder has a concentration of sulfuric acid of 3.6 mol / L or more and 13.4 mol / L or less, nitric acid of 1.3 mol / L or more and 3.4 mol / L or less, and the molar ratio of sulfuric acid and nitric acid is 2. A solder composition analysis method, comprising: using a mixed acid of 6: 1 or more and 7.9: 1 or less to completely dissolve the composition component of the solder, and then quantitatively analyzing the composition component.
前記混酸に含まれる酸の組成が、硫酸３．６ｍｏｌ／Ｌ以上４．５ｍｏｌ／Ｌ以下、硝酸１．３ｍｏｌ／Ｌ以上１．７ｍｏｌ／Ｌ以下であることを特徴とするはんだの組成分析方法。 In the solder composition analysis method according to claim 1,
A composition analysis method for solder, wherein a composition of an acid contained in the mixed acid is from 3.6 mol / L to 4.5 mol / L of sulfuric acid and from 1.3 mol / L to 1.7 mol / L of nitric acid.
前記組成成分の定量分析を、ＩＣＰ（Ｉｎｄｕｃｔｉｖｅｌｙ Ｃｏｕｐｌｅｄ Ｐｌａｓｍａ）発光分析法、ＩＣＰ質量分析法および原子吸光法のいずれかにより行うことを特徴とするはんだの組成分析方法。 In the solder composition analysis method according to any one of claims 1 and 2,
A solder composition analysis method, wherein the quantitative analysis of the composition component is performed by any one of ICP (Inductively Coupled Plasma) emission spectrometry, ICP mass spectrometry, and atomic absorption.
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