JPS5853858B2 - Determination of trace amounts of selenium using flameless atomic absorption spectrometry - Google Patents
Determination of trace amounts of selenium using flameless atomic absorption spectrometryInfo
- Publication number
- JPS5853858B2 JPS5853858B2 JP53116433A JP11643378A JPS5853858B2 JP S5853858 B2 JPS5853858 B2 JP S5853858B2 JP 53116433 A JP53116433 A JP 53116433A JP 11643378 A JP11643378 A JP 11643378A JP S5853858 B2 JPS5853858 B2 JP S5853858B2
- Authority
- JP
- Japan
- Prior art keywords
- selenium
- atomic absorption
- trace amounts
- interference
- absorption spectrometry
- 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.)
- Expired
Links
Classifications
-
- 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
- G01N21/74—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 flameless atomising, e.g. graphite furnaces
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Environmental & Geological Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Description
【発明の詳細な説明】
本発明はフレームレス原子吸光分析法による微量セレン
の定量法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for quantifying trace amounts of selenium by flameless atomic absorption spectrometry.
通常カーボンアトマイザ−として用いられる抵抗発熱体
は長さ５ｃｒｒＬ、外径６ｍ、内径４閣程度の管状のグ
ラファイトで、その中央に直径１．５−程度の試料注入
孔を設けている。The resistance heating element normally used as a carbon atomizer is a graphite tube with a length of 5 crrL, an outer diameter of 6 m, and an inner diameter of about 4 mm, and a sample injection hole with a diameter of about 1.5 cm is provided in the center.
そしてこの抵抗発熱体の両端に電流を通じて発生するジ
ュール熱によって試料の原子化を行ない、原子化された
セレンの原子吸収をフォトマルにより電流値に変換して
記録計のチャート上に記録し、この記録された吸収ピー
クの高さくｒＩａｎ）から、被検元素の定量を行なうが
、この方法ではセレンに対する酸の干渉および共存元素
の干渉が大きいため、この方法を直接分析法として適用
することは困難である。Then, the sample is atomized by the Joule heat generated through electric current at both ends of this resistance heating element, and the atomic absorption of the atomized selenium is converted into a current value by a photomultiplier and recorded on the chart of the recorder. The analyte element is quantified based on the height of the recorded absorption peak (rIan), but this method is difficult to apply as a direct analysis method because of the large interference of acid with selenium and interference of coexisting elements. It is.
これらのことから酸および共存元素の干渉を抑制する方
法について種々の検討を行なった結果、酸の干渉の抑制
方法としては、カーボンアトマイザ−の試料との接触部
に一定量のジルコニウムＺｒを添加することにより、フ
レームレス原子吸光分析法において最も多く使用される
硝酸の干渉を抑制することができた。Based on these considerations, we conducted various studies on ways to suppress the interference of acids and coexisting elements. As a result, we found that a method for suppressing acid interference is to add a certain amount of zirconium Zr to the part of the carbon atomizer that comes into contact with the sample. This made it possible to suppress the interference of nitric acid, which is most commonly used in flameless atomic absorption spectrometry.
また共存元素の抑制方法としては、酸の抑制方法で見い
出したジルコニウムＺｒの添加法に、さらにキャリヤガ
スとして用いられるアルゴンガス中に酸素ガスを添加す
ることによって抑制できることがわかった。Furthermore, it has been found that coexisting elements can be suppressed by adding oxygen gas to argon gas used as a carrier gas in addition to the method of adding zirconium Zr, which was discovered in the acid suppression method.
本発明は、上記に基づき、カーボンアトマイザ−の試料
との接触部にジルコニウムを添加するとともに、キャリ
ヤガスとして用いるアルゴンガスなどの不活性ガス中に
酸素ガスを添加して、試料中の微量セレンを定量するこ
とを特徴とする。Based on the above, the present invention adds zirconium to the part of the carbon atomizer that comes into contact with the sample, and also adds oxygen gas to an inert gas such as argon gas used as a carrier gas to remove trace amounts of selenium in the sample. Characterized by quantitative determination.
本発明によれば、フレームレス原子吸光分析法で最も多
く使用される硝酸の溶液にして、硝酸及びＺｎｔＴｅな
との共存元素による干渉を抑制することかできる。According to the present invention, a solution of nitric acid, which is most commonly used in flameless atomic absorption spectrometry, can be used to suppress interference caused by elements coexisting with nitric acid and ZntTe.
以下、本発明の詳細な説明する。The present invention will be explained in detail below.
まず次表にセレン濃度１００ｐｐｂ溶液を用いて、種々
の測定条件について検討を行なった結果から定めたセレ
ンの最適測定条件を示す。First, the following table shows the optimum measurement conditions for selenium determined from the results of studies on various measurement conditions using a solution with a selenium concentration of 100 ppb.
次に前記表と同様にセレン濃度１００ｐｐｂ溶液を用い
て、前記表の測定条件にしたがい、各種酸の干渉および
各種共存元素の干渉をくわしく調べた。Next, using a solution with a selenium concentration of 100 ppb as in the table above, and according to the measurement conditions in the table above, interference of various acids and interference of various coexisting elements was investigated in detail.
初めに各種酸濃度をＯから２ＯＮの範囲内で段階的に変
化させてその影響を調べた。First, various acid concentrations were varied stepwise within the range of O to 2ON, and the effects thereof were investigated.
その結果を第１図に示す。The results are shown in FIG.
この第１図における縦軸はピーク値間であり、横軸は酸
濃度Ｎである。The vertical axis in FIG. 1 is the peak value, and the horizontal axis is the acid concentration N.
この結果より、いずれの酸も犬きく減感干渉を示すため
。This result shows that both acids exhibit strong desensitization interference.
これらの酸が共存する場合にはセレンを直接分析するこ
とは不可能であった。Direct analysis of selenium was impossible when these acids coexisted.
これらのことから、使用する酸を硝酸に限定して、その
干渉抑制方法を確立するために種々の検討を行なった。For these reasons, we limited the acid used to nitric acid and conducted various studies to establish a method for suppressing its interference.
その結果、カーボンアトマイザ−の試料接触部にジルコ
ニウムＺｒを添加する方法に効果を見い出した。As a result, we found that a method of adding zirconium Zr to the sample contacting part of the carbon atomizer was effective.
第２図にセレン１００ ｐｐｂ の硝酸濃度０１ＩＮ溶
液を用いて、抑制効果に対するジルコニウムＺｒ添加量
の影響を調べた結果を示す。FIG. 2 shows the results of investigating the influence of the amount of zirconium Zr added on the suppression effect using a nitric acid concentration 01 IN solution containing 100 ppb of selenium.
この第２図における縦軸はピーク値間であり、横軸はジ
ルコニウムＺｒの添加量μグである。In FIG. 2, the vertical axis is the peak value, and the horizontal axis is the amount μg of zirconium Zr added.
この結果より、セレンの原子吸収によるピーク値間はジ
ルコニウムＺｒ添加量３００−１４００μノの範囲で一
定値を示し、充分実用性が認められる。From this result, the peak value due to selenium atomic absorption shows a constant value in the range of zirconium Zr addition amount of 300 to 1400 μm, and sufficient practicality is recognized.
第３図はジルコニウムＺｒ添加量を５００μ２にし、硝
酸濃度をＯから０．５ Ｎの範囲で段階的に変化させ、
硝酸濃度の影響を調べた結果である。Figure 3 shows that the amount of zirconium Zr added was 500 μ2, and the nitric acid concentration was changed stepwise from O to 0.5 N.
This is the result of investigating the influence of nitric acid concentration.
この第３図における縦軸はセレンの原子吸収によるピー
ク値間であり、横軸は硝酸濃度Ｎである。In FIG. 3, the vertical axis is the peak value due to atomic absorption of selenium, and the horizontal axis is the nitric acid concentration N.
この結果より、０．０５Ｎ以下の低濃度では低い値を示
したが、０．０５Ｎから０．５Ｎの範囲内では一定値を
示し、充分実用性がある。From this result, a low value was shown at a low concentration of 0.05N or less, but a constant value was shown within the range of 0.05N to 0.5N, which is sufficiently practical.
次にセレン１００ｐｐｂ標準溶液に各種の元素を添加し
、この溶液をＯ，Ｉ Ｎ硝酸酸性に調製後、上記と同様
、前記表の測定条件に従って共存元素濃度による影響を
調べた。Next, various elements were added to a 100 ppb selenium standard solution, and after the solution was acidified with O, IN nitric acid, the influence of the coexisting element concentration was investigated in accordance with the measurement conditions shown in the table above, in the same manner as above.
この場合のカーボンアトマイザ−は、セレンに対スる硝
酸の干渉抑制剤としてジルコニウムＺｒ５００μ？を試
料接触部に添加したものを用いた。The carbon atomizer in this case uses zirconium Zr500μ as an interference inhibitor of nitric acid with selenium. was added to the sample contact area.
その結果を第４図に示す。The results are shown in FIG.
これより、Ｎａ、Ｋ。Ｓｒ 、Ｃａ ｓ Ｂａ ） Ｚ
ｎ ｓ ＴｅおよびＩｎは増感干渉を、ｐｂおよびＣｄ
は減感干渉を示し、これらの元素を含む試料中のセレン
を直接分析法により測定することは困難であった。From this, Na, K. Sr, Cas Ba) Z
n s Te and In cause sensitizing interference, pb and Cd
showed desensitizing interference, making it difficult to measure selenium in samples containing these elements by direct analytical methods.
これらのことから、共存元素の干渉抑制法について種々
の検討を行なった結果、キャリヤガスとして用いるアル
ゴンガス中に酸素ガスを添加する方法に優れた抑制効果
が認められることを発明した。Based on these considerations, we conducted various studies on methods for suppressing the interference of coexisting elements, and as a result, we discovered that a method of adding oxygen gas to argon gas used as a carrier gas has an excellent suppressing effect.
第５図に共存元素としてＺｎおよびＴｅをｌｐｐｍ添加
した試料を用いて行なった場合の抑制効果に対する酸素
濃度の影響を示した。FIG. 5 shows the influence of oxygen concentration on the suppression effect when using a sample to which lppm of Zn and Te were added as coexisting elements.
また同様に共存元素が存在しない場合のセレンに対する
酸素濃度の影響についても調べた。We also investigated the effect of oxygen concentration on selenium in the absence of coexisting elements.
この結果より、酸素濃度０．２５から１．２５％Ｖ／Ｖ
の薄囲内で完全に共存元素の影響を抑制することができ
た。From this result, oxygen concentration 0.25 to 1.25%V/V
It was possible to completely suppress the influence of coexisting elements within a thin range of .
この第５図における縦軸はセレン原子吸収によるピーク
値間を、横軸はアルゴンガス中の酸素濃度（係Ｖ／Ｖ）
を示す。In Fig. 5, the vertical axis indicates the peak value due to selenium atomic absorption, and the horizontal axis indicates the oxygen concentration in argon gas (V/V ratio).
shows.
第６図に干渉を示す共存元素に適用した結果を示す。Figure 6 shows the results when applied to coexisting elements that exhibit interference.
この場合の酸素濃度は０．７５ ％ Ｖ／Ｖで行なった
。The oxygen concentration in this case was 0.75% V/V.
この結果より、Ｔｅについては５ｐｐｍ以上で干渉を示
したが、その他の元素については１０ｐｐｍまでの範囲
内では完全に干渉抑制することができた。From this result, interference was observed for Te at 5 ppm or more, but interference could be completely suppressed for other elements up to 10 ppm.
また本発明の定量法における再現性を調べた結果、セレ
ン濃度１００ ｐｐｂの場合で変動係数Ｃ−Ｖ−（ｎ＝
１ｏ ）は１．２０％であり、検量線は１５０ｐｐｂ
までの範囲内ではピーク値の間に良好な直線関係が成立
するため充分に実用性が認められた。Furthermore, as a result of investigating the reproducibility of the quantitative method of the present invention, the coefficient of variation C-V-(n=
1o) is 1.20%, and the calibration curve is 150 ppb
Since a good linear relationship was established between the peak values within the range of 1 to 3, the practicality was recognized to be sufficient.
その検量線の１例を第１図に示す。An example of the calibration curve is shown in FIG.
以上のように本発明によれば、低濃度のセレンを硝酸溶
液および共存元素中より、溶媒抽出法などにより抽出分
離することなく、直接分析できるため、分析時間が大幅
に短縮できる。As described above, according to the present invention, low-concentration selenium can be directly analyzed from a nitric acid solution and coexisting elements without being extracted and separated by a solvent extraction method or the like, so that the analysis time can be significantly shortened.
第１図はセレンに対する各種酸濃度の影響を示すグラフ
、第２図は硝酸の干渉抑制効果に対するＺｒ添加量の影
響を示すグラフ、第３図ばＺｒを添加した場合の硝酸の
影響を示すグラフ、第４図はセレンに対する各種元素の
干渉を示すグラフ、第５図は干渉抑制効果に対する酸素
濃度の影響とセレンに対する酸素濃度の影響を示すグラ
フ、第６図は各種共存元素の干渉に対する抑制効果を示
すグラフ、第７図は検量線の１例を示したものである。Figure 1 is a graph showing the effect of various acid concentrations on selenium, Figure 2 is a graph showing the effect of Zr addition amount on the interference suppression effect of nitric acid, and Figure 3 is a graph showing the effect of nitric acid when Zr is added. , Fig. 4 is a graph showing the interference of various elements with selenium, Fig. 5 is a graph showing the influence of oxygen concentration on the interference suppression effect and the effect of oxygen concentration on selenium, and Fig. 6 is the suppression effect on the interference of various coexisting elements. The graph shown in FIG. 7 shows an example of a calibration curve.
Claims (1)
ウムを添加するとともに、キャリヤガスとして用いる不
活性ガス中に酸素ガスを添加して、試料中の微量セレン
な定量することを特徴とするフレームレス原子吸光分析
法による微量セレンの定量法。 ２ ジルコニウムの添加量が３００μｍから１４００μ
ｍの範囲である特許請求の範囲第１項記載のフレームレ
ス原子吸光分析法による微量セレンの定量法。 ３ 酸素ガスの添加量が０．２５から１．２５％Ｖ／Ｖ
の範囲である特許請求の範囲第１項記載のフレームレス
原子吸光分析法による微量セレンの定量法。[Claims] 1. A carbon atomizer that is characterized by adding zirconium to the contact portion with the sample and adding oxygen gas to an inert gas used as a carrier gas to quantify trace amounts of selenium in the sample. A method for quantifying trace amounts of selenium using flameless atomic absorption spectrometry. 2 The amount of zirconium added is from 300μm to 1400μm
A method for quantifying trace amounts of selenium by flameless atomic absorption spectrometry according to claim 1, wherein the amount of selenium is within the range of m. 3 Addition amount of oxygen gas is 0.25 to 1.25%V/V
A method for quantifying trace amounts of selenium by flameless atomic absorption spectrometry according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP53116433A JPS5853858B2 (en) | 1978-09-20 | 1978-09-20 | Determination of trace amounts of selenium using flameless atomic absorption spectrometry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP53116433A JPS5853858B2 (en) | 1978-09-20 | 1978-09-20 | Determination of trace amounts of selenium using flameless atomic absorption spectrometry |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5542083A JPS5542083A (en) | 1980-03-25 |
| JPS5853858B2 true JPS5853858B2 (en) | 1983-12-01 |
Family
ID=14686973
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP53116433A Expired JPS5853858B2 (en) | 1978-09-20 | 1978-09-20 | Determination of trace amounts of selenium using flameless atomic absorption spectrometry |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5853858B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104964941B (en) * | 2015-06-29 | 2017-02-22 | 浙江大学 | Method and separating and collecting device for detecting elemental selenium quickly and quantitatively |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5211087A (en) * | 1975-07-16 | 1977-01-27 | Matsushita Electric Ind Co Ltd | Carbon atomizer |
| JPS5851615B2 (en) * | 1976-05-27 | 1983-11-17 | 松下電器産業株式会社 | Frameless atomic absorption spectrometry |
| JPS5364592A (en) * | 1976-11-19 | 1978-06-09 | Matsushita Electric Ind Co Ltd | Flameless atomic absorption anlysis method |
-
1978
- 1978-09-20 JP JP53116433A patent/JPS5853858B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5542083A (en) | 1980-03-25 |
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