JPH087142B2 - Frameless atomic absorption spectrometric method for trace metal analysis - Google Patents
Frameless atomic absorption spectrometric method for trace metal analysisInfo
- Publication number
- JPH087142B2 JPH087142B2 JP17079887A JP17079887A JPH087142B2 JP H087142 B2 JPH087142 B2 JP H087142B2 JP 17079887 A JP17079887 A JP 17079887A JP 17079887 A JP17079887 A JP 17079887A JP H087142 B2 JPH087142 B2 JP H087142B2
- Authority
- JP
- Japan
- Prior art keywords
- sample
- atomic absorption
- succinic acid
- trace metal
- added
- 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 - Fee Related
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
Description
【発明の詳細な説明】 （技術分野） 本発明は、フレームレス原子吸光法により微少量の金
属を分析する方法に関する。TECHNICAL FIELD The present invention relates to a method for analyzing a trace amount of metal by a flameless atomic absorption method.
（従来技術） 微小量金属の分析にはフレームレス原子吸光法が適用
されているが、試料中のマトリックスやグラファイトチ
ューブの形状等の影響を受けやすく、検出感度の低下を
来たすという問題がある。(Prior Art) Although a flameless atomic absorption method is applied to the analysis of a minute amount of metal, there is a problem that it is easily affected by the shape of a matrix or a graphite tube in a sample and the detection sensitivity is lowered.
このため、例えば、微小量のカドミウムを分析する場
合には、ジチゾン−クロロホルムにより抽出を行ない、
これを塩酸により逆抽出して濃縮する、いわゆる抽出法
によりサンプルを作成してから原子化させることが行な
われているが、サンプル作成に手間と時間を要するとい
う問題がある。Therefore, for example, when analyzing a small amount of cadmium, extraction with dithizone-chloroform is performed,
A sample is prepared and atomized by a so-called extraction method in which this is back-extracted with hydrochloric acid to be concentrated, but there is a problem that it takes time and time to prepare the sample.
（目的） 本発明はこのような問題に鑑みてなされたものであっ
て、その目的とするところは、抽出作業を不要として、
高い検出感度と再現性でもって微小量の金属を分析する
ことができる方法を提案することにある。(Purpose) The present invention has been made in view of such a problem, and an object of the present invention is to eliminate extraction work,
It is to propose a method capable of analyzing a minute amount of metal with high detection sensitivity and reproducibility.
（発明の概要） すなわち、本発明が特徴とするところは、試料にコハ
ク酸化合物を添加して灰化工程において比較的熱に安定
なコハク酸と金属との化合物を形成させ、もって灰化時
における金属の揮散を防止するようにした点にある。(Summary of the Invention) That is, the feature of the present invention is that a succinic acid compound is added to a sample to form a relatively heat-stable compound of succinic acid and a metal in the ashing step, and thus, during ashing. The point is to prevent the volatilization of the metal.
（実施例） そこで以下に本発明の詳細を実施例に基づいて説明す
る。(Examples) Therefore, details of the present invention will be described below based on Examples.
第１図は本発明に使用するフレームレス原子吸光分析
装置の一例を示すものであって、図中符号１は、原子化
炉を構成するグラファイトチューブで、グラファイト製
柱体に軸方向の通孔1aを穿設し、試料収容部の外壁に通
孔を穿設して試料注入口1bを設けるとともに、両端の電
極２、３からの通電により発熱させて、通孔12から透過
して来る光ビームを測定するように構成されている。FIG. 1 shows an example of a flameless atomic absorption spectroscope used in the present invention. In the figure, reference numeral 1 is a graphite tube constituting an atomization furnace, and an axial through hole is formed in a graphite column. 1a is provided, a through hole is provided in the outer wall of the sample storage portion to provide a sample injection port 1b, and heat is generated by energization from the electrodes 2 and 3 at both ends, and the light is transmitted through the through hole 12. It is configured to measure the beam.
このように構成された装置において、液状に調製した
サンプルを試料注入口1bからグラファイトチューブ１内
に注入し、ついで無水コハク酸、コハク酸アミド、コハ
ク酸アンモニューム等の溶液を添加すると、これら２種
類の液体は、試料収容部内に溜まることになる。このよ
うな状態においてグラファイトチューブ１を、150℃に
昇温させて、試料やコハク酸溶液の水分を乾燥させたの
ち500℃まで昇温させて灰化を行なうと、試料中の金属
はコハク酸化合物と結合して熱的に安定な物質を形成す
る。このようにして灰化が終了した段階で、グラファイ
トチューブを分析対象金属に適してた温度に昇温させる
と、この昇温過程において分析対象金属とコハク酸との
化合物は、比較的熱的に安定であるため、チューブ１か
ら揮散する量が抑えられて原子化工程に入り初期の濃度
を可及的に維持して吸光度が検出されることになる。In the apparatus configured as described above, a sample prepared in a liquid state is injected into the graphite tube 1 through the sample injection port 1b, and then a solution of succinic anhydride, succinic acid amide, ammonium succinate or the like is added to The liquid of the type will collect in the sample container. In such a state, the temperature of the graphite tube 1 is raised to 150 ° C., the water content of the sample and the succinic acid solution is dried, and then the temperature is raised to 500 ° C. to incinerate, and the metal in the sample is succinic acid. Combines with compounds to form thermally stable materials. When the graphite tube is heated to a temperature suitable for the metal to be analyzed at the stage where the ashing is completed in this way, the compound of the metal to be analyzed and succinic acid in the temperature rising process becomes relatively thermally. Since it is stable, the amount of volatilization from the tube 1 is suppressed and the atomization step is started to maintain the initial concentration as much as possible and the absorbance is detected.
［実施例］ 鉛、カドミウムを各10ppb、また鉄を50ppb、さらに銅
を20ppbの濃度で含む水溶液を試料に、またコハク酸、
無水コハク酸、コハク酸アミド、コハク酸アンモニウム
をそれぞれ５％含む水溶液を増感溶液に用意し、乾燥温
度150℃、灰化温度500℃とする一方、原子化温度をカド
ミウムについては1600℃、鉛については1800℃、及び
鉄、銅については2300℃に設定して分析したところ、表
１に示したような結果を得た。[Example] An aqueous solution containing 10 ppb each of lead and cadmium, 50 ppb iron, and 20 ppb copper was used as a sample, and succinic acid,
Prepare an aqueous solution containing 5% each of succinic anhydride, succinamide, and ammonium succinate as a sensitizing solution and set the drying temperature to 150 ° C and the ashing temperature to 500 ° C, while the atomization temperature is 1600 ° C for cadmium and lead. The results were as shown in Table 1 when the analysis was carried out by setting the temperature to 1800 ° C and the temperature to 2300 ° C for iron and copper.
すなわち、鉛に対しては、無水コハク酸を添加すると
検出感度が1.5倍となり、カドミウムに対してはコハク
酸アミドを添加すると感度が5.8倍にも増大し、また鉄
に対しては、コハク酸と無水コハク酸が1.7〜1.8倍とな
り、さらに銅に対しては無水コハク酸とコハク酸アミド
を添加すると測定感度が1.5〜1.6倍となることが解っ
た。 That is, for lead, the detection sensitivity was increased 1.5 times when succinic anhydride was added, and when succinic acid amide was added for cadmium, the sensitivity was increased 5.8 times, and for iron, succinic acid was added. It was found that succinic anhydride increased 1.7 to 1.8 times, and that the addition of succinic anhydride and succinamide to copper increased the measurement sensitivity to 1.5 to 1.6 times.
また、カドミウムを含む同一試料を用いて、無水コハ
ク酸とコハク酸アミドを添加して分析したところ、表２
に示したような結果を得た。In addition, the same sample containing cadmium was used and analyzed by adding succinic anhydride and succinic acid amide.
The result is shown in.
すなわち、無水コハク酸を添加して分析すると、前述
の抽出法によりサンプルを調製した場合に比較して高い
感度と再現性を得ることができ、またコハク酸アミドを
使用したものにあっても、略々抽出法と同様の再現性を
得ることができた。このことから、コハク酸化合物溶液
を添加するという簡単な操作により、濃縮操作を用いる
ことなく水溶液中のカドミウムを高い再現性で高感度で
分析できることが判明した。 That is, when succinic anhydride is added and analyzed, higher sensitivity and reproducibility can be obtained compared to the case where a sample is prepared by the above-mentioned extraction method, and even in the case of using succinic acid amide, Almost the same reproducibility as the extraction method could be obtained. From this, it was revealed that by a simple operation of adding a succinic acid compound solution, cadmium in an aqueous solution can be analyzed with high reproducibility and high sensitivity without using a concentration operation.
さらに、検量性を調査すべく、濃度が異なるカドミウ
ム溶液を用意するとともに、これに無水コハク酸溶液と
コハク酸アミド溶液を添加して分析したところ、第２図
に示すように無水コハク酸溶液を添加したもの（図中
Ａ）とコハク酸アミド溶液を添加したもの（Ｂ）は、抽
出法Ｃに劣ることのない高い直線性を示した。Furthermore, in order to investigate the calibratability, cadmium solutions with different concentrations were prepared, and a succinic anhydride solution and a succinic acid amide solution were added to this and analyzed. As shown in FIG. The added one (A in the figure) and the one to which the succinamide solution was added (B) showed high linearity comparable to that of the extraction method C.
また、検出限界点を調査したとこと、本発明法では0.
2pgとなり、従来行なわれていた抽出法の1.0pgに比較し
て1/5程度の低濃度のものまで検出可能であることが解
った。Further, that the detection limit point was investigated, the method of the present invention is 0.
It became 2 pg, and it was found that even a low concentration of about 1/5 can be detected compared to 1.0 pg of the conventional extraction method.
なお、上述の実施例においては、コハク酸化合物を別
に添加するようにしているが、コハク酸の添加によって
沈澱を生じない試料にあっては両者を混合した状態でグ
ラファイトチューブに注入しても同様の作用を奏するこ
とは云うまでもない。In the above-mentioned examples, the succinic acid compound is added separately, but in the case of a sample in which precipitation does not occur due to the addition of succinic acid, the same can be obtained by injecting both into a graphite tube. It goes without saying that the effect of is exerted.
（効果） 以上説明したように本発明によれば、試料にコハク酸
化合物を添加して灰化するようにしたので、灰化工程中
における目的金属の揮散を可及的に少なくして鉄、銅、
鉛、カドミウムを高い感度と、再現性でもって検出で
き、特にカドミウムに対しては、極めて高い増感効果を
示すため、排水中のカドミウムを抽出等の前処理を必要
とすることなく分析することが可能をなる。(Effect) As described above, according to the present invention, the succinic acid compound is added to the sample for ashing, so that volatilization of the target metal during the ashing step is reduced as much as possible, iron, copper,
Lead and cadmium can be detected with high sensitivity and reproducibility, and especially for cadmium, it shows an extremely high sensitizing effect, so analyze cadmium in wastewater without requiring pretreatment such as extraction. Will be possible.
第１図は本発明に使用する装置の一例を示す断面図、第
２図は分析結果の一例を示す線図である。 １……グラファイトチューブ 1a……通孔、1b……試料注入口 ２、３……電極FIG. 1 is a sectional view showing an example of an apparatus used in the present invention, and FIG. 2 is a diagram showing an example of analysis results. 1 ... Graphite tube 1a ... Through hole, 1b ... Sample inlet 2, 3 ... Electrode
Claims (1)
原子化させることを特徴とするフレームレス原子吸光法
による微量金属の分析方法。1. A succinic acid compound is added to a sample to be incinerated,
A method for analyzing trace metals by flameless atomic absorption spectrometry, which is characterized by atomization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17079887A JPH087142B2 (en) | 1987-07-07 | 1987-07-07 | Frameless atomic absorption spectrometric method for trace metal analysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17079887A JPH087142B2 (en) | 1987-07-07 | 1987-07-07 | Frameless atomic absorption spectrometric method for trace metal analysis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6413437A JPS6413437A (en) | 1989-01-18 |
| JPH087142B2 true JPH087142B2 (en) | 1996-01-29 |
Family
ID=15911548
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17079887A Expired - Fee Related JPH087142B2 (en) | 1987-07-07 | 1987-07-07 | Frameless atomic absorption spectrometric method for trace metal analysis |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH087142B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2510339B2 (en) * | 1990-07-19 | 1996-06-26 | 株式会社日立製作所 | Sample sampling method and apparatus for flameless atomic absorption spectrometry |
| CN102175630A (en) * | 2010-12-14 | 2011-09-07 | 北京市理化分析测试中心 | Method for measuring trace cadmium in vinegar |
| CN105057572A (en) * | 2015-07-27 | 2015-11-18 | 明光市留香泵业有限公司 | Mesoporous-silica-contained high-adsorbability water-based paint for evaporative pattern casting and preparation method for mesoporous-silica-contained high-adsorbability water-based paint |
-
1987
- 1987-07-07 JP JP17079887A patent/JPH087142B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6413437A (en) | 1989-01-18 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |