JPH02226049A - Atomic absorption spectro photometer - Google Patents
Atomic absorption spectro photometerInfo
- Publication number
- JPH02226049A JPH02226049A JP4813089A JP4813089A JPH02226049A JP H02226049 A JPH02226049 A JP H02226049A JP 4813089 A JP4813089 A JP 4813089A JP 4813089 A JP4813089 A JP 4813089A JP H02226049 A JPH02226049 A JP H02226049A
- Authority
- JP
- Japan
- Prior art keywords
- line spectrum
- reactor
- atomic absorption
- bright line
- light source
- 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.)
- Granted
Links
- 238000010521 absorption reaction Methods 0.000 title claims description 28
- 238000001228 spectrum Methods 0.000 claims abstract description 14
- 238000000889 atomisation Methods 0.000 claims description 14
- 238000001514 detection method Methods 0.000 claims 1
- 238000004458 analytical method Methods 0.000 abstract description 8
- 238000002835 absorbance Methods 0.000 abstract description 4
- 230000004907 flux Effects 0.000 abstract description 3
- 239000007787 solid Substances 0.000 description 14
- 239000007789 gas Substances 0.000 description 12
- 239000000779 smoke Substances 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 238000004380 ashing Methods 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 230000035945 sensitivity Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003915 air pollution Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000003891 environmental analysis Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Landscapes
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は、大気汚染、水質汚濁などの環境分析、医薬品
、食品中などの重金属の分析、金属材料分析、生体中微
量金属の分析などに用いる原子吸光分光光度計に関し、
特に試料が固体である場合に好適な原子吸光分光光度計
に関する。[Detailed Description of the Invention] [Field of Industrial Application] The present invention is applicable to environmental analysis such as air pollution and water pollution, analysis of heavy metals in pharmaceuticals and foods, analysis of metal materials, analysis of trace metals in living organisms, etc. Regarding the atomic absorption spectrophotometer used,
The present invention relates to an atomic absorption spectrophotometer suitable particularly when the sample is a solid.
［従来の技術］
従来の原子吸光分光光度計においては、固体試料中の金
属元素を分析（定量）しようとする場合、一般的には固
体試料を溶解し、特に組成が複雑なしの或いは微量元素
の分析のときには、必要に応じて溶媒抽出操作により得
られる溶液をフレーム或いはフレームレス原子吸光分光
光度計に注入して分析するようにしている。[Prior art] In conventional atomic absorption spectrophotometers, when attempting to analyze (quantitate) metal elements in a solid sample, the solid sample is generally dissolved, and especially if the composition is not complex or trace elements are analyzed, the solid sample is dissolved. When performing this analysis, the solution obtained by solvent extraction is injected into a flame or flameless atomic absorption spectrophotometer for analysis, if necessary.
他方、固体試料を前処理なしに直接分析することもおこ
なわれているが、この場合には原子化部を固体熱分解グ
ラファイト管（炉）で構成するようにしている（Ｍえば
、特開昭５９−９４０４３号公報参照）、このとき、試
料の導入は端面の開口部からボート（試料皿）により挿
入する方法をとっている。On the other hand, solid samples are also analyzed directly without pretreatment, but in this case the atomization section is constructed with a solid pyrolytic graphite tube (furnace) (for example, 59-94043), at this time, the sample is introduced through an opening in the end face using a boat (sample dish).
また、固体試料を直接分析する場合には、試料処理が全
く施されておらず、バックグラウンドが非常に大きいた
め、−ａ的にバックグラウンド補正に関し精度の高いゼ
ーマン法を採用した固体試料分析用原子吸光分光光度計
も実用化されている。In addition, when directly analyzing a solid sample, no sample processing is performed and the background is extremely large. Atomic absorption spectrophotometers have also been put into practical use.
［発明が解決しようとする課Ｍ１
従来の原子吸光分光光度計にあっては、固体試料を溶液
試料とする場合は、前処理の操作に多大の時間と労力を
要するため、迅速な分析が達成できないという問題点が
あった。また、前処理において試料ロス、コンタミネー
ション、希釈誤差等を生じるおそれがあるという問題点
もあった。[Problem to be solved by the invention M1 In conventional atomic absorption spectrophotometers, when a solid sample is used as a solution sample, pretreatment operations require a lot of time and effort, so rapid analysis cannot be achieved. The problem was that it couldn't be done. Further, there is a problem that sample loss, contamination, dilution error, etc. may occur during pretreatment.
他方、固体試料を前処理なしに直接分析する場合は、大
口径グラファイト管（炉）を用いると、その発光強度が
大きくなり、相対的に光源強度が低くなって、ベースラ
インノイズの増大、ピーク値のバラツキが大きくなるた
め、大口径グラファイト管を採用することができず、原
子化炉への試料導入が困難であるという問題点があった
。On the other hand, when directly analyzing a solid sample without pretreatment, using a large-diameter graphite tube (furnace) increases the emission intensity and relatively lowers the light source intensity, increasing baseline noise and peak Because of the large variation in values, it was not possible to use a large-diameter graphite tube, and there was a problem in that it was difficult to introduce the sample into the nuclear reactor.
才な、ゼーマン原子吸光分光光度計の場合は、もともと
偏光子による光量ロスがあるため、固体試料からのバッ
クグラウンドによる光量ロスとも相俟ってかなりのエネ
ルギーロスがおこり、ＳＺＮ比が著しく低下するという
問題点があった。In the case of the Zeeman atomic absorption spectrophotometer, there is originally a loss of light amount due to the polarizer, and this together with the loss of light amount due to the background from the solid sample causes a considerable energy loss, resulting in a significant drop in the SZN ratio. There was a problem.
本発明は、固体試料を前処理なしに直接分析する方式で
、試料導入を容易にするため原子化炉を大口径化しても
ノイズの増大、ピーク値のバラツキが大きくならず、高
精度の分析ができる原子吸光分光光度計を得ることを目
的としている。The present invention is a method that directly analyzes solid samples without pretreatment, and in order to facilitate sample introduction, even if the diameter of the nuclear reactor is increased, noise increases and peak value variations do not become large, and high-precision analysis can be achieved. The aim is to obtain an atomic absorption spectrophotometer that can perform
「課題を解決するための手段］
上記目的を達成するために、本発明の原子吸光分光光度
計においては、小電流と大電流を交互に流して点灯され
るランプを光源に用いると共に、通過する輝線スペクト
ルの原子化炉の入口または出口の窓のうち少なくとも一
方を着脱可能に構成したものである。原子化炉には、円
筒状等のグラファイト炉を用いる。"Means for Solving the Problems" In order to achieve the above object, the atomic absorption spectrophotometer of the present invention uses a lamp that is lit by alternately passing a small current and a large current as a light source. At least one of the entrance and exit windows of the atomization reactor for bright line spectra is configured to be removable.A cylindrical graphite furnace is used as the atomization reactor.
また、原子化炉内に導入するインナーガスや加熱中に試
料から発生するガスを炉外に排出するため、原子化炉の
外壁または窓にガス噴出口を設けるのが効果的である。Furthermore, in order to discharge the inner gas introduced into the reactor and the gas generated from the sample during heating to the outside of the reactor, it is effective to provide a gas outlet in the outer wall or window of the reactor.
さらに、原子化炉の着脱可能に構成した窓は、原子化炉
内への試料の挿入後に、例えば原子化炉の昇温プログラ
ム（乾燥、灰化、原子化）と連動して駆動させるとよい
。Furthermore, the removable window of the nuclear reactor is preferably driven after the sample is inserted into the reactor, for example in conjunction with the temperature increase program (drying, ashing, atomization) of the reactor. .
［作 用］
上記のように構成された原子吸光分光光度計の光源を点
灯すると、周知のとおり、ランプの輝線スペクトルは大
電流時にはバックグラウンド吸収を受ける中心が凹んだ
形となり、他方小電流時にはバックグラウンド吸収と原
子吸光の双方の吸収を受ける一本のピークとなるので、
両者の吸光度の策よりバックグラウンド吸収の補正され
た原子吸光が測定できるが、このような点灯手法の光源
は光量ロスがなく光強度が強いため、原子化炉の大口径
化にともなう原子化炉と光源との発光強度の相対的な低
下を緩和し、原子化炉の大口径を可能にする。[Function] When the light source of an atomic absorption spectrophotometer configured as described above is turned on, as is well known, the emission line spectrum of the lamp becomes concave at the center where background absorption occurs at high currents, while at low currents the light source of the lamp becomes concave. Since it becomes a single peak that absorbs both background absorption and atomic absorption,
Using both absorbance measures, it is possible to measure atomic absorption with background absorption corrected.However, the light source using this lighting method has no loss of light quantity and has a strong light intensity, so it is possible to measure the atomic absorption with the background absorption corrected. This alleviates the relative decrease in emission intensity between the light source and the light source, and enables a large diameter nuclear reactor.
また、原子化炉の外壁または窓に設けたガス噴出口は、
特に乾燥、灰化時に試料から発生する煙を、炉内に導入
する不活性なインナーガスの作用により炉外に排出する
のに役立ち、バックグラウンドの影響を受けにくくする
。なお、試料から発生する煙は原子化炉の両端の入口及
び出口を開口端とすることにより効果的に拡散するが、
反面、炉外の空気が炉内に流入することにより原子化炉
（グラファイト炉）の寿命を縮め、原子化時には原子化
元素の拡散をもたらし、感度の低下をきたすことになる
。In addition, the gas outlet installed on the outer wall or window of the nuclear reactor is
In particular, the inert inner gas introduced into the furnace helps to discharge smoke generated from the sample during drying and ashing to the outside of the furnace, making it less susceptible to background effects. Note that the smoke generated from the sample can be effectively diffused by making the inlet and outlet at both ends of the reactor open.
On the other hand, air from outside the reactor flows into the reactor, shortening the life of the atomization reactor (graphite reactor), causing diffusion of atomized elements during atomization, and reducing sensitivity.
このような理由から、原子化炉の着脱可能に構成した窓
を原子化炉の昇温プログラムと連動して駆動し、例えば
特に煙が多量に発生する固体試料の場合には乾燥、灰化
時には窓を開成状態に維持して煙の拡散を効果的におこ
ない、原子化時に開成して感度の低下を回避するのが好
ましい、もちろん、煙の発生がさほど多くない試料の場
合には、炉内への試料の導入後から窓を開成状態に維持
し、煙を炉壁または窓のガス噴出口より排出すればよい
［実施例］
実施例について図面を参照して説明すると、第１図にお
いて、光源１はホロカソードランプで、小電流、大電流
及び予備点灯（ベース）もしくは電流オフの３状悪を１
サイクルとして高速周波数（１００Ｈｚ）点灯する。こ
のような点灯手法のランプは原子化炉の発光ノイズの影
響を受けず、光量ロスがなく、大電流時の光強度は小電
流時の１００倍以上になる。ホロカソードランプ１に小
電流と大電流を交互に流すと、ランプの輝線スペクトル
は大電流時には中心が凹んだ形となり、主にバックグラ
ウンド吸収を受け、他方小電流時には一本のピークとな
り、バックグラウンド吸収と原子吸光の双方の吸収を受
けるので、したがって両者の吸光度の差を求めれば、バ
ックグラウンド吸収の補正された真の原子吸光が測定で
きる。For this reason, the removable window of the reactor is operated in conjunction with the reactor's temperature increase program, for example, for drying solid samples that generate a lot of smoke, and for ashing. It is preferable to keep the window open to effectively diffuse smoke, and open it during atomization to avoid a decrease in sensitivity. Of course, if the sample does not generate much smoke, After introducing the sample into the chamber, the window may be kept open and the smoke may be discharged from the furnace wall or the gas outlet of the window [Example] An example will be described with reference to the drawings. Light source 1 is a hollow cathode lamp, which can handle three conditions: small current, large current, preliminary lighting (base), or current off.
Lights up at high speed frequency (100Hz) as a cycle. Lamps using this lighting method are not affected by the light emission noise of the nuclear reactor, there is no loss of light quantity, and the light intensity at high current is more than 100 times that at low current. When a small current and a large current are applied alternately to the hollow cathode lamp 1, the emission line spectrum of the lamp becomes concave at the center at high currents and is mainly subject to background absorption, while at small currents it becomes a single peak with no background absorption. Since it receives both ground absorption and atomic absorption, by finding the difference between the two absorbances, it is possible to measure the true atomic absorption with background absorption corrected.
光源１からの光束は窓板３から入射し、原子化炉２を通
過して分光器６に入る。原子化炉２はグラファイト炉で
、周知のとおり、供給する電流をル制御することにより
炉内の設定加熱温度、すなわち乾燥、灰化及び原子化の
各段階に応じた温度に制御する。原子化炉２内にはイン
ナーガスとして不活性ガスを導入し、炉外壁に開口した
ガス噴出口５または／及び窓板３．４に設けたガス噴出
口５ （第２図参照）より乾燥、灰化時に試料より発生
する煙を炉外に排出する０通常は、試料をボート（試料
皿）に載せて原子化炉２内に挿入した後に可動窓板４を
閉成するが、試料によって多量に煙が発生する場合、可
動窓板４を、好ましくは固定窓板３も可動として両窓板
を乾燥、灰化時には開成させるのがよい、原子化時には
、窓板４はｍ成し、不活性ガスの炉内への導入も停止す
る。A light beam from a light source 1 enters through a window plate 3, passes through an atomization reactor 2, and enters a spectrometer 6. The atomization reactor 2 is a graphite reactor, and as is well known, by controlling the supplied current, the atomization reactor 2 is controlled to a set heating temperature in the reactor, that is, a temperature corresponding to each stage of drying, ashing, and atomization. An inert gas is introduced into the reactor 2 as an inner gas, and the gas is dried through the gas outlet 5 opened in the outer wall of the reactor or/and the gas outlet 5 provided in the window plate 3.4 (see Fig. 2). Normally, the movable window plate 4 is closed after the sample is placed on a boat (sample tray) and inserted into the reactor 2, but smoke generated by the sample during ashing is discharged outside the reactor. When smoke is generated, it is better to make the movable window plate 4, preferably also the fixed window plate 3, movable and open both window plates when drying and ashing.When atomizing, the window plate 4 becomes m-formed and non-formed. The introduction of active gas into the furnace is also stopped.
原子化された目的元素が拡散し、感度が低下するのを防
止するためである。This is to prevent the atomized target element from diffusing and reducing sensitivity.
可動窓板４の駆動は適宜の手段によっておこなうことが
できるが、そのタイミングは上述の点を考慮すれば、原
子化炉２の昇温プログラムと連動しておこなうのがよい
が、分析開始のための押しボタンの操作と連動させるこ
とも可能である。The movable window plate 4 can be driven by any appropriate means, but considering the above-mentioned points, it is best to do it in conjunction with the temperature increase program of the nuclear reactor 2, It is also possible to link this to the operation of the push button.
原子化炉２を通過した光束は、輝線スペクトルを選択的
に強く吸収し、分光器６でこの輝線スペクトルを分光し
て、検出器７で電気信号として検出する。前述したよう
に、大電流時の輝線スペクトルと小電流時の輝線スペク
トルの吸光度の差が信号処理部８で求められ、これを目
的元素の濃度に比例した値として制御部９を通じて表示
部１１に指示する。これら信号処理系は周知のとおりで
ある。なお、１０はキーボード等の操作部である。The luminous flux that has passed through the atomization reactor 2 selectively and strongly absorbs the bright line spectrum, the spectrometer 6 separates the bright line spectrum, and the detector 7 detects the bright line spectrum as an electric signal. As mentioned above, the difference in absorbance between the bright line spectrum at a large current and the bright line spectrum at a small current is determined by the signal processing section 8, and is displayed on the display section 11 through the control section 9 as a value proportional to the concentration of the target element. Instruct. These signal processing systems are well known. Note that 10 is an operation unit such as a keyboard.
［発明の効果］
本発明は、以上説明したように構成されているので、原
子化炉を大形化（大口径）することができ、固体試料の
原子化炉内への導入が容易となり、そして原子化炉内の
煙を効果的に拡散させることができ、固体試料を高感度
で、かつ高精度に直接分析することができる。[Effects of the Invention] Since the present invention is configured as described above, the nuclear reactor can be made larger (large diameter), and solid samples can be easily introduced into the reactor. The smoke inside the nuclear reactor can be effectively diffused, and solid samples can be directly analyzed with high sensitivity and precision.
第１図は本発明の原子吸光分光光度計のシステムブロッ
ク図で、第２図は窓板の形状を示す図である。
１・・・光源、２・・・原子化炉、３．４・・・窓板５
．５−・・・ガス噴出口、６−・・分光器、７・・・検
出器、８・・・信号処理部
特許出願人 株式会社島津制作所FIG. 1 is a system block diagram of the atomic absorption spectrophotometer of the present invention, and FIG. 2 is a diagram showing the shape of the window plate. 1... Light source, 2... Nuclear reactor, 3.4... Window plate 5
．． 5-...Gas outlet, 6-...Spectrometer, 7...Detector, 8...Signal processing unit Patent applicant Shimadzu Corporation
Claims (1)
る目的元素を原子化する原子化炉を通過させ、分光器で
目的元素の輝線のみ選択し、これを検出器で検出する原
子吸光分光光度計において、 前記光源に小電流と大電流を交互に流して 点灯されるランプを用いると共に、前記原子化炉の前記
輝線スペクトルの入口又は出口の窓のうち少なくとも一
方を着脱可能に構成したことを特徴とする原子吸光分光
光度計。[Claims] 1. The emission line spectrum from the light source is passed through an atomization reactor that atomizes the target element contained in the sample, only the emission line of the target element is selected by the spectrometer, and this is detected by the detector. In the atomic absorption spectrophotometer for detection, a lamp is used that is lit by alternately passing a small current and a large current through the light source, and at least one of the windows at the entrance or exit of the bright line spectrum of the atomization reactor is attached or detached. An atomic absorption spectrophotometer characterized in that the atomic absorption spectrophotometer is configured to enable
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1048130A JPH0762649B2 (en) | 1989-02-27 | 1989-02-27 | Atomic absorption spectrophotometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1048130A JPH0762649B2 (en) | 1989-02-27 | 1989-02-27 | Atomic absorption spectrophotometer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02226049A true JPH02226049A (en) | 1990-09-07 |
| JPH0762649B2 JPH0762649B2 (en) | 1995-07-05 |
Family
ID=12794747
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1048130A Expired - Lifetime JPH0762649B2 (en) | 1989-02-27 | 1989-02-27 | Atomic absorption spectrophotometer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0762649B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0694607A (en) * | 1992-09-11 | 1994-04-08 | Shimadzu Corp | Flameless atomic absorption spectro photometer |
| CN111307733A (en) * | 2018-11-27 | 2020-06-19 | 株式会社岛津制作所 | Atomic absorption spectrophotometer |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS51134687A (en) * | 1975-05-16 | 1976-11-22 | Jeol Ltd | Atomic extinction analysis method |
| JPS6126919U (en) * | 1984-07-25 | 1986-02-18 | 株式会社ノーリツ | oil vaporization burner |
| JPS6145478U (en) * | 1984-08-24 | 1986-03-26 | 鹿島建設株式会社 | drain for sanitary appliances |
-
1989
- 1989-02-27 JP JP1048130A patent/JPH0762649B2/en not_active Expired - Lifetime
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS51134687A (en) * | 1975-05-16 | 1976-11-22 | Jeol Ltd | Atomic extinction analysis method |
| JPS6126919U (en) * | 1984-07-25 | 1986-02-18 | 株式会社ノーリツ | oil vaporization burner |
| JPS6145478U (en) * | 1984-08-24 | 1986-03-26 | 鹿島建設株式会社 | drain for sanitary appliances |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0694607A (en) * | 1992-09-11 | 1994-04-08 | Shimadzu Corp | Flameless atomic absorption spectro photometer |
| CN111307733A (en) * | 2018-11-27 | 2020-06-19 | 株式会社岛津制作所 | Atomic absorption spectrophotometer |
| CN111307733B (en) * | 2018-11-27 | 2023-06-09 | 株式会社岛津制作所 | Atomic absorption spectrophotometer |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0762649B2 (en) | 1995-07-05 |
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