JPH0618511A - Method for determining boron in sulfuric acid - Google Patents
Method for determining boron in sulfuric acidInfo
- Publication number
- JPH0618511A JPH0618511A JP17245792A JP17245792A JPH0618511A JP H0618511 A JPH0618511 A JP H0618511A JP 17245792 A JP17245792 A JP 17245792A JP 17245792 A JP17245792 A JP 17245792A JP H0618511 A JPH0618511 A JP H0618511A
- Authority
- JP
- Japan
- Prior art keywords
- sulfuric acid
- boron
- solution
- distilled
- acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は硫酸中の硼素の定量方法
に関する。詳しくは高純度硫酸中の微量の硼素の定量方
法に関する。高純度硫酸は近年、特に電子工業用として
有用である。FIELD OF THE INVENTION The present invention relates to a method for determining boron in sulfuric acid. Specifically, it relates to a method for quantifying a trace amount of boron in high-purity sulfuric acid. In recent years, high-purity sulfuric acid is particularly useful for the electronic industry.
【０００２】[0002]
【従来の技術】硼素の定量方法として、蒸留分離吸光光
度法、抽出分離吸光光度法、液体クロマトグラフ法、誘
導結合プラズマ発光分析法、誘導結合プラズマ質量分析
法等が知られている。例えば、試料溶液を濃リン酸、必
要により濃硫酸をまぜ、濃縮して白煙処理し、メタノー
ルを加えて蒸留し、留出する硼酸トリメチルを水酸化カ
ルシウム水溶液に捕集し、これを蒸発乾固した後、クル
クミン−シュウ酸試薬で硼素を吸光定量する方法（JAPA
N ANALYST,Vol.12,120〜125 (1963)）、誘導結合プラズ
マ質量分析法（以下、ＩＣＰ−ＭＳと称する。）による
チタン中の硼素の定量（Analytica Chimica Acta,244(1
991)115-122 ）等が知られている。2. Description of the Related Art Distillation separation absorptiometry, extraction separation absorptiometry, liquid chromatography, inductively coupled plasma emission spectrometry, inductively coupled plasma mass spectrometry and the like are known as methods for quantifying boron. For example, the sample solution is mixed with concentrated phosphoric acid and, if necessary, concentrated sulfuric acid, concentrated, treated with white smoke, distilled by adding methanol, and the distilled trimethyl borate is collected in an aqueous calcium hydroxide solution and evaporated to dryness. After solidification, a method for spectrophotometric determination of boron with curcumin-oxalic acid reagent (JAPA
N ANALYST, Vol.12, 120-125 (1963)), determination of boron in titanium by inductively coupled plasma mass spectrometry (hereinafter referred to as ICP-MS) (Analytica Chimica Acta, 244 (1)
991) 115-122) and the like are known.
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、従来の
方法では定量下限の濃度が高く、硫酸中の１ｐｐｂ以下
の濃度の硼素を定量することは困難であった。かかる事
情に鑑み、硫酸中の低濃度、特に１ｐｐｂ以下の硼素を
定量する方法について鋭意検討した結果、硫酸中の硼素
を硼酸トリメチルとして留出させ、これを糖アルコール
類の水溶液に導入して捕集し、次いで捕集液を雰囲気に
よる汚染をさけるために、窒素気流下に蒸発乾固し、残
渣を酸で溶解して硼素を濃縮し、溶解液中の硼素をＩＣ
Ｐ−ＭＳで測定することにより１ｐｐｂ以下の硼素を精
度良く定量できることを見出し、本発明を完成するに至
った。However, in the conventional method, the lower limit of quantification is high, and it is difficult to quantify boron having a concentration of 1 ppb or less in sulfuric acid. In view of such circumstances, as a result of diligent studies on a method for quantifying boron in a low concentration in sulfuric acid, especially 1 ppb or less, boron in sulfuric acid was distilled as trimethyl borate, and this was introduced into an aqueous solution of sugar alcohols to be captured. In order to avoid contamination of the collected liquid by the atmosphere, the collected liquid is evaporated to dryness under a nitrogen stream, the residue is dissolved with an acid to concentrate boron, and the boron in the dissolved liquid is removed by IC.
The inventors have found that boron of 1 ppb or less can be accurately quantified by measuring with P-MS, and completed the present invention.
【０００４】[0004]
【課題を解決するための手段】すなわち本発明は、硫酸
中にメタノールを加え、不活性ガスを通気しながら加熱
して硫酸中の硼素を硼酸トリメチルとして留出させ、留
出してくる硼酸トリメチルを糖アルコール類の水溶液に
導入して捕集し、捕集液を高純度の不活性ガス雰囲気下
に蒸発し、残渣を酸で溶解し、溶解液中の硼素を誘導結
合プラズマ質量分析法で測定することを特徴とする硫酸
中の硼素の定量方法である。Means for Solving the Problems That is, the present invention is to add methanol to sulfuric acid and heat while aerating an inert gas to distill boron in sulfuric acid as trimethyl borate. It is introduced into an aqueous solution of sugar alcohols and collected, the collected solution is evaporated in a high-purity inert gas atmosphere, the residue is dissolved with an acid, and boron in the solution is measured by inductively coupled plasma mass spectrometry. The method for quantifying boron in sulfuric acid is characterized by
【０００５】本発明に用いる機器は充分洗浄したもの、
試薬は高純度試薬または精製して用いる。例えばメタノ
ールおよびエタノールは精密分析用のメタノールに特級
の水酸化ナトリウムを加え、蒸留精製したものを用い
る。純水としては蒸留水をＭｉｌｌ−Ｑ装置で精製して
用いる。機器は充分洗浄後、密閉して保管しておいたも
のを用いる。特に１ｐｐｂ以下の濃度の硼素を定量する
際には、雰囲気中に存在する硼素による汚染の影響が大
きいので注意が必要である。一度蒸留操作を行って汚染
された硼素を除いた後に本測定を行うのが好ましい。The equipment used in the present invention has been thoroughly washed,
The reagent is a high-purity reagent or is used after purification. For example, methanol and ethanol are prepared by distilling and refining methanol for precision analysis with special grade sodium hydroxide. As pure water, distilled water is used after being purified with a Mill-Q device. Use equipment that has been thoroughly cleaned, sealed, and stored. In particular, when quantifying boron having a concentration of 1 ppb or less, care must be taken because the influence of contamination by boron present in the atmosphere is great. It is preferable to perform the main measurement after performing a distillation operation once to remove contaminated boron.
【０００６】本発明に用いる糖アルコール類としては、
グリセリン等のトリット、エリトリット等のテトリッ
ト、アラビット、アドニット等のペンチット、マンニッ
ト、ズルシット、タリット、アリット等のヘキシット等
が挙げられる。The sugar alcohols used in the present invention include
Examples thereof include trit such as glycerin, tetrit such as erythritol, penchit such as arabite and adnit, and hexit such as mannitol, dulcitt, talit, and arit.
【０００７】本発明を実施する際に用いる装置の一例を
図１に示す。石英製の蒸留器６に高純度の不活性ガス、
通常、窒素ガスをボンベ１から流量計２、フィルター
３、シリンダー（テフロン製）４経由して供給するライ
ンが設けられている。更に留出液を冷却し、捕集する冷
却器７とシリンダー（テフロン製）８が連結されてい
る。留出液を捕集するシリンダー８には糖アルコール類
の水溶液が入れられ、留出管がその中に挿入されてい
る。蒸留器はスターラー付プレート上のウオーターバス
で加熱できるようになっている。An example of an apparatus used to carry out the present invention is shown in FIG. A quartz distiller 6 with a high-purity inert gas,
Usually, a line for supplying nitrogen gas from a cylinder 1 via a flow meter 2, a filter 3, and a cylinder (made of Teflon) 4 is provided. Further, a cooler 7 for cooling and collecting the distillate and a cylinder (made of Teflon) 8 are connected. An aqueous solution of sugar alcohols is put in a cylinder 8 for collecting the distillate, and a distilling pipe is inserted therein. The distiller can be heated in a water bath on a stirrer plate.
【０００８】蒸留器に測定試料の硫酸を入れ、冷却す
る。硫酸量は限定されるものではないが、通常、約１０
０ｇ用いられる。これに冷却したメタノールを液温が４
０℃以上にならないように徐々に加える。メタノールは
約１００ｍｌ加えられる。蒸留器を熱水浴中に入れ、不
活性ガスを通気しながら蒸留する。その後メターノール
を約２０ｍｌ追加して更に蒸留する。これを２〜３回繰
り返すことにより硼素を１００％留出回収することがで
きる。追加するメタノールの代わりにエタノールを用い
ることにより少ない回数で硼素を１００％留出回収する
ことができる。Sulfuric acid as a measurement sample is placed in a distiller and cooled. The amount of sulfuric acid is not limited, but is usually about 10
0 g is used. Liquid temperature of methanol cooled to this is 4
Add gradually so that the temperature does not rise above 0 ° C. About 100 ml of methanol is added. Place the still in a hot water bath and distill with an inert gas bubble. Thereafter, about 20 ml of methanol is added and further distilled. By repeating this 2 to 3 times, 100% of boron can be distilled and recovered. By using ethanol instead of additional methanol, it is possible to distill and recover 100% of boron in a small number of times.
【０００９】硼素を捕集した糖アルコール類の水溶液を
蒸発皿に移し、内部標準のベリリウムと塩酸を加え、高
純度の不活性ガス雰囲気下に加熱し、蒸発、濃縮する。
この時、周囲の大気に曝して蒸発すると汚染されるの
で、周囲の大気に接触しないよう硼素を含有しない高純
度の不活性ガス、通常、窒素ガス雰囲気下に行う必要が
ある。乾固直前に加熱を止め、酸と純水を加えて残渣を
溶解する。酸としては硝酸、硫酸、塩酸が挙げられる
が、通常、硝酸が用いられる。溶解液をポリエチレン試
験管に移し、洗浄し、液量を５ｍｌ程度にする。これを
ＩＣＰ−ＭＳで 9Beと11B を測定する。An aqueous solution of sugar alcohols in which boron is collected is transferred to an evaporation dish, beryllium as an internal standard and hydrochloric acid are added, and the mixture is heated in a high-purity inert gas atmosphere to evaporate and concentrate.
At this time, since it is contaminated by being exposed to the ambient air and evaporating, it is necessary to perform it in a high-purity inert gas containing no boron, usually a nitrogen gas atmosphere, so as not to come into contact with the ambient air. Immediately before drying, stop heating and add acid and pure water to dissolve the residue. Examples of the acid include nitric acid, sulfuric acid and hydrochloric acid, and nitric acid is usually used. The solution is transferred to a polyethylene test tube and washed to make the solution volume about 5 ml. 9 Be and 11 B are measured by ICP-MS.
【００１０】少量、約２ｇの硫酸について上記と同様な
操作、すなわち空試験を行い。上記で得られた測定値を
補正し、硫酸中の硼素濃度を求める。The same operation as above, that is, a blank test, was carried out with a small amount of about 2 g of sulfuric acid. The measured value obtained above is corrected to determine the boron concentration in sulfuric acid.
【００１１】[0011]
【発明の効果】本発明の方法により、低濃度（０．Ｘｐ
ｐｂ）の硫酸中の硼素を精度良く測定することができ
る。According to the method of the present invention, a low concentration (0.Xp
It is possible to accurately measure boron in sulfuric acid of pb).
【００１２】[0012]
【実施例】本発明を実施例で更に詳細に説明するが、本
発明はこの実施例に限定されるものではない。The present invention will be described in more detail with reference to examples, but the present invention is not limited to these examples.
【００１３】（使用試薬およびその調整） （１）メタノール：和光精密分析用５００ｍｌに和光特
級水酸化ナトリウム１ｇを加えて溶解後、８０〜８３℃
の熱水浴中で蒸留精製する。留出初めから３０〜４００
ｍｌを取得し用いる。 （２）エタノール：和光精密分析用５００ｍｌに和光特
級水酸化ナトリウム１ｇを加えて溶解後、８５〜８８℃
の熱水浴中で蒸留精製する。留出初めから３０〜４００
ｍｌを取得し用いる。 （３）糖アルコール水溶液：糖アルコールとしてマンニ
ットを用いた。和光特級マンニット０．２ｇを純水１０
０ｍｌに溶解した（２ｍｇ／ｍｌ）。 （４）塩酸 ：多摩化学 ３０％ ＡＡ−１０００ （５）硝酸 ：多摩化学 ６８％ ＡＡ−１０００ （６）純水 ：蒸留水をＭｉｌｌ−Ｑ装置で精製し
た水 （７）硼素標準液：和光原子吸光用１０００ｐｐｍ溶液
を純水で希釈し、０．１ｐｐｍ溶液とした。 （８）ベリリウム溶液：和光原子吸光用１０００ｐｐｍ
溶液を純水で希釈し、１ｐｐｍ溶液とした。(Reagents Used and Their Preparation) (1) Methanol: 1 g of Wako special grade sodium hydroxide was added to 500 ml for Wako precision analysis and dissolved, and then at 80 to 83 ° C.
Purify by distillation in a hot water bath. 30 to 400 from the beginning of distillation
Obtain and use ml. (2) Ethanol: 1 g of Wako special grade sodium hydroxide was added to 500 ml for Wako precision analysis and dissolved, and then 85 to 88 ° C.
Purify by distillation in a hot water bath. 30 to 400 from the beginning of distillation
Obtain and use ml. (3) Sugar alcohol aqueous solution: Mannitol was used as sugar alcohol. 0.2 g of Wako special grade mannite is added to pure water 10
It was dissolved in 0 ml (2 mg / ml). (4) Hydrochloric acid: Tama Chemical Co., Ltd. 30% AA-1000 (5) Nitric acid: Tama Chemical Co., Ltd. 68% AA-1000 (6) Pure water: distilled water purified by Mill-Q equipment (7) Boron standard solution: Wako atom The 1000 ppm solution for light absorption was diluted with pure water to give a 0.1 ppm solution. (8) Beryllium solution: 1000 ppm for Wako atomic absorption
The solution was diluted with pure water to give a 1 ppm solution.
【００１４】（検量線の作成）ポリエチレン試験管に純
水１ｍｌを取り、硝酸０．２ｍｌとマンニット水溶液
０．５ｍｌを加える。ベリリウム溶液０〜０．５ｍｌ
（０〜５００ｎｇ）および硼素標準液０〜０．５ｍｌ
（０〜５０ｎｇ）を段階的に加え、純水を加えて５ｍｌ
とした。これらについてＩＣＰ−ＭＳ装置（ＶＧ社製
ＰＱ−II型）を用いて測定し検量線を作成した。なお、
ＩＣＰ−ＭＳの測定は通常用いられる条件で行った。(Preparation of calibration curve) 1 ml of pure water is placed in a polyethylene test tube, and 0.2 ml of nitric acid and 0.5 ml of an aqueous mannite solution are added. Beryllium solution 0-0.5 ml
(0-500 ng) and boron standard solution 0-0.5 ml
(0 to 50 ng) is added stepwise, and pure water is added to 5 ml.
And About these, ICP-MS device (made by VG)
(PQ-II type) was used to make a calibration curve. In addition,
The ICP-MS measurement was performed under the conditions usually used.
【００１５】実施例１ 図１に示す装置を用いて８９％の高純度硫酸中の硼素の
定量を行った。石英蒸留器のフラスコに硫酸１０２ｇを
取り、水で冷却した。これに水で冷却したメタノール１
００ｍｌを、液温が４０℃以上にならないように徐々に
加えた。捕集用１００ｍｌテフロン製シリンダーにマン
ニット水溶液０．５ｍｌと純水２５ｍｌを取り、この液
中に留出管を投入し、フラスコに蒸留ヘッドを取りつけ
た。更に窒素ガスの通気設備を取りつけた。Example 1 Boron in 89% highly pure sulfuric acid was quantified using the apparatus shown in FIG. 102 g of sulfuric acid was placed in a flask of a quartz distiller and cooled with water. Methanol 1 cooled with water
00 ml was gradually added so that the liquid temperature did not exceed 40 ° C. 0.5 ml of an aqueous mannite solution and 25 ml of pure water were placed in a 100 ml Teflon cylinder for collection, a distilling tube was put into this liquid, and a distillation head was attached to the flask. Furthermore, a nitrogen gas ventilation facility was attached.
【００１６】蒸留器を約９３℃の熱水浴中に入れ、窒素
ガスを１００ｍｌ／分で通気し、回転子を６０ｒｐｍで
回転させた。１０分間加熱蒸留した。次にテフロンシリ
ンダー４にメタノール２０ｍｌを入れ、蒸留器に送り込
み、２０分間蒸留した。更にエタノール１０ｍｌを同様
にして蒸留器に送り込み、３０分間蒸留した。捕集液を
７５ｍｍφの透明蒸発皿に移し、ベリリウム溶液０．５
ｍｌと３０％塩酸１ｍｌを加えた。これをホットプレー
トに載せ、窒素ガスの流入口、流出口を有するカバーを
かぶせ、窒素ガスを供給してカバー内を窒素ガス雰囲気
にし、ホットプレートを約２００℃に加熱して蒸発、濃
縮を行った。液量５ｍｌ程度から温度を８０℃に下げ、
乾固直前に蒸発皿をホットプレートからおろした。The distiller was placed in a hot water bath at about 93 ° C., nitrogen gas was bubbled at 100 ml / min, and the rotor was rotated at 60 rpm. It was heated and distilled for 10 minutes. Next, 20 ml of methanol was put into the Teflon cylinder 4, fed into a distiller, and distilled for 20 minutes. Further, 10 ml of ethanol was similarly fed into the distiller and distilled for 30 minutes. Transfer the collected solution to a transparent evaporation dish of 75 mmφ and place the beryllium solution at 0.5.
ml and 30% hydrochloric acid 1 ml were added. Place this on a hot plate, cover with a cover having a nitrogen gas inlet and outlet, supply nitrogen gas to create a nitrogen gas atmosphere in the cover, heat the hot plate to about 200 ° C. to evaporate and concentrate. It was From about 5 ml of liquid, lower the temperature to 80 ℃,
Immediately before drying, the evaporation dish was removed from the hot plate.
【００１７】蒸発皿に硝酸０．２ｍｌと純水約３ｍｌを
加えて残渣を溶かし、ポリエチレン試験管に移した。蒸
発皿を純水で洗浄し、液を合わせて５ｍｌとした。これ
をＩＣＰ−ＭＳで測定した結果。硼素を２０ｎｇ検出し
た。0.2 ml of nitric acid and about 3 ml of pure water were added to the evaporating dish to dissolve the residue, which was then transferred to a polyethylene test tube. The evaporating dish was washed with pure water, and the liquids were combined to make 5 ml. The result of measuring this by ICP-MS. 20 ng of boron was detected.
【００１８】硫酸２ｇを取り、上記と同様に操作して空
試験を行い、硼素を６ｎｇ検出した。硼素の検出値から
硫酸中の硼素濃度を求めた〔（Ａ−Ｂ）／１００〕とこ
ろ０．１ｐｐｂであった。2 g of sulfuric acid was taken and a blank test was conducted in the same manner as above to detect 6 ng of boron. The boron concentration in sulfuric acid was determined from the detected value of boron [(AB) / 100], and it was 0.1 ppb.
【００１９】同一日に２サンプリングして５日間分析し
た場合の繰り返し再現性は、変動係数で５％、回収率は
９０％であった。The reproducibility was 5% in terms of coefficient of variation and 90% in recovery when two samples were taken on the same day and analyzed for 5 days.
【図１】本発明を実施する際に用いる装置の一例を示
す。FIG. 1 shows an example of an apparatus used for carrying out the present invention.
１ 高純度窒素ガスボンベ ２ 流量計 ３ フィルター ４ テフロンシリンダー（５０ｍｌ） ５ ウオーターバス、スターラー付プレート ６ 蒸留器 ７ 冷却器 ８ テフロンシリンダー（１００ｍｌ） 1 High-purity nitrogen gas cylinder 2 Flow meter 3 Filter 4 Teflon cylinder (50 ml) 5 Water bath, stirrer plate 6 Distiller 7 Cooler 8 Teflon cylinder (100 ml)
Claims (2)
を通気しながら加熱して硫酸中の硼素を硼酸トリメチル
として留出させ、留出してくる硼酸トリメチルを糖アル
コール類の水溶液に導入して捕集し、捕集液を高純度の
不活性ガス雰囲気下に蒸発し、残渣を酸で溶解し、溶解
液中の硼素を誘導結合プラズマ質量分析法で測定するこ
とを特徴とする硫酸中の硼素の定量方法。1. Methanol is added to sulfuric acid and heated while aerating an inert gas, boron in sulfuric acid is distilled as trimethyl borate, and the distilled trimethyl borate is introduced into an aqueous solution of sugar alcohols. Collected, the collected solution is evaporated under a high-purity inert gas atmosphere, the residue is dissolved with an acid, and boron in the solution is measured by inductively coupled plasma mass spectrometry. Determination method of boron.
項１記載の硫酸中の硼素の定量方法。2. The method for quantifying boron in sulfuric acid according to claim 1, wherein the sugar alcohol is mannite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP04172457A JP3144065B2 (en) | 1992-06-30 | 1992-06-30 | Determination of boron in sulfuric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP04172457A JP3144065B2 (en) | 1992-06-30 | 1992-06-30 | Determination of boron in sulfuric acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0618511A true JPH0618511A (en) | 1994-01-25 |
| JP3144065B2 JP3144065B2 (en) | 2001-03-07 |
Family
ID=15942350
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP04172457A Expired - Fee Related JP3144065B2 (en) | 1992-06-30 | 1992-06-30 | Determination of boron in sulfuric acid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3144065B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112279220A (en) * | 2020-12-29 | 2021-01-29 | 苏州香榭轩表面工程技术咨询有限公司 | Continuous production method of high-purity sulfuric acid |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1932242B (en) * | 2006-10-02 | 2010-05-12 | 中国矿业大学 | Well wall with steel plate aquifuge and construction method thereof |
-
1992
- 1992-06-30 JP JP04172457A patent/JP3144065B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112279220A (en) * | 2020-12-29 | 2021-01-29 | 苏州香榭轩表面工程技术咨询有限公司 | Continuous production method of high-purity sulfuric acid |
| CN112279220B (en) * | 2020-12-29 | 2021-03-23 | 苏州香榭轩表面工程技术咨询有限公司 | Continuous production method of high-purity sulfuric acid |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3144065B2 (en) | 2001-03-07 |
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