JPS6322254B2 - - Google Patents
Info
- Publication number
- JPS6322254B2 JPS6322254B2 JP4896581A JP4896581A JPS6322254B2 JP S6322254 B2 JPS6322254 B2 JP S6322254B2 JP 4896581 A JP4896581 A JP 4896581A JP 4896581 A JP4896581 A JP 4896581A JP S6322254 B2 JPS6322254 B2 JP S6322254B2
- Authority
- JP
- Japan
- Prior art keywords
- sample
- interference
- carrier fluid
- present
- atomization
- 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
- 239000012530 fluid Substances 0.000 claims description 12
- 238000000889 atomisation Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 238000001479 atomic absorption spectroscopy Methods 0.000 claims description 4
- 239000000523 sample Substances 0.000 description 49
- 239000007788 liquid Substances 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 239000002737 fuel gas Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
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
- G01N21/72—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 flame burners
Landscapes
- Health & Medical Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (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】
本発明は化学干渉を除くようにした原子吸光分
析方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an atomic absorption spectrometry method that eliminates chemical interference.
原子吸光分析において、例えばアルカリ土類元
素を定量測定しようとする場合試料中にAl、Si
等の陽イオン或は燐酸等が存在すると目的元素の
濃度が実際よりも低く測定される。これは試料原
子化部においてアルカリ土類元素がAl等と結合
することにより原子化するアルカリ土類元素の原
子数が減るからで、原子吸光分析でこのような或
る物質の存在により目的元素の濃度が実際と異つ
て測定される現象が化学干渉と云われる現象であ
る。このような現象は試料に適当な物質を混入す
ることにより除くことができる。例えばアルカリ
土類元素に対するAl、Si、燐酸等の干渉は試料
にLaとかSr等を添加すると、試料原子化部にお
いてはLaとかSrの方がアルカリ土類よりもAl等
との親和性が強くこれらと結合してしまうので、
上述した干渉が除去される。このような干渉を除
去する添加物質を干渉抑制剤と云つている。 In atomic absorption spectrometry, for example, when attempting to quantitatively measure alkaline earth elements, Al and Si may be present in the sample.
If such cations or phosphoric acid are present, the concentration of the target element will be measured lower than the actual concentration. This is because the number of atoms of the alkaline earth element that is atomized decreases as the alkaline earth element combines with Al etc. in the sample atomization section. A phenomenon in which the concentration is measured differently from the actual concentration is a phenomenon called chemical interference. Such a phenomenon can be eliminated by mixing an appropriate substance into the sample. For example, when Al, Si, phosphoric acid, etc. interfere with alkaline earth elements, when La or Sr is added to the sample, La or Sr has a stronger affinity with Al etc. than alkaline earth elements in the sample atomization part. Because it combines with these
The interference mentioned above is removed. Additives that remove such interference are called interference suppressants.
原子吸光分析装置は従来第１図に示すような構
成になつていた。Ｆは試料原子化部である炎でＢ
は炎Ｆで形成するバーナ本体である。Ｔは試料供
給管で一端がバーナ本体Ｂ内に挿入されており、
他端は試料容器Ｃ中の試料溶液Ｓ中に入れてあ
る。バーナ本体の後部から燃料ガスｆと助燃ガス
の空気等ａが供給されており、これらの供給ガス
による霧吹き作用で試料液Ｓは試料供給管Ｔを通
して吸引されバーナ本体Ｂ内に噴霧され、燃料ガ
ス、助燃ガス、試料の三者が混合されてノズルＮ
より噴出し炎Ｆを形成する。この構成では試料毎
に容器Ｃを取換え、試料毎に干渉抑制剤と試料と
を調合して容器Ｃに入れると云う手順になり試料
の調整が大変面倒である。 An atomic absorption spectrometer has conventionally had a configuration as shown in FIG. F is the flame that is the sample atomization part, and B
is the burner body formed by flame F. T is a sample supply tube, one end of which is inserted into the burner body B.
The other end is placed in a sample solution S in a sample container C. A fuel gas F and a combustion assisting gas such as air a are supplied from the rear of the burner body, and by the atomizing action of these supplied gases, the sample liquid S is sucked through the sample supply pipe T and atomized into the burner body B, and the fuel gas , auxiliary gas, and sample are mixed into the nozzle N.
From this, a flame F is formed. In this configuration, the procedure is to change the container C for each sample, mix the interference suppressant and the sample for each sample, and put the mixture into the container C, which makes sample preparation very troublesome.
本発明は干渉抑制剤を添加した試料を調整する
場合の上述した調合操作の繁雑さを解消すること
を目的としてなされたものである。 The present invention has been made with the aim of solving the above-mentioned complexity of the compounding operation when preparing a sample to which an interference suppressor has been added.
本発明はバーナ本体内に干渉抑制剤を添加した
溶媒のみ噴霧させておき、この溶媒供給路に外部
から間欠部に試料を注入するようにした原子吸光
分析方法を提案するものである。以下実施例によ
つて本発明を説明する。 The present invention proposes an atomic absorption spectrometry method in which only a solvent containing an interference suppressor is sprayed into the burner body, and a sample is injected from the outside into the solvent supply path at intervals. The present invention will be explained below with reference to Examples.
第２図は本発明方法において用いられる試料原
子化用バーナの一実施例である。第１図のバーナ
と殆んど同じ構造であり第１図の各部と対応する
部分には同じ符号がつけてある。このバーナの特
徴は試料供給管Ｔの途中にシリコンゴムの栓Ｇで
閉鎖した試料導入室Ｘを形成した点で、ゴム栓Ｇ
に注射針Ｉを貫通させマイクロシリンダＭで微量
の試料を注入できるようになつている。燃料ガス
及び助燃ガスが供給されると容器Ｃ中の液Ｌが管
Ｔを通して吸引されバーナ本体Ｂ内に噴出し霧化
せしめられる。本発明方法の特徴は容器Ｃ中の液
Ｌには試料を含ませず、液Ｌは干渉抑制剤を添加
した溶媒だけより成つている点にある。液Ｌは試
料導入室Ｘを通過して流通しており、同室Ｘに注
入された試料をバーナ本体内に運搬するキヤリヤ
の作用を果すものである。試料導入室Ｘに注入さ
れた試料は上述したキヤリヤ流体Ｌと混合しなが
らバーナ本体Ｂまで運ばれてバーナ本体内に噴霧
する。キヤリヤ流体Ｌ中には干渉抑制剤が添加し
てあるから試料はこの干渉抑制剤と混合してノズ
ルＮより噴出し炎Ｆ内に係給される。 FIG. 2 shows an example of a sample atomization burner used in the method of the present invention. It has almost the same structure as the burner shown in FIG. 1, and parts corresponding to those shown in FIG. 1 are given the same reference numerals. The feature of this burner is that a sample introduction chamber X is formed in the middle of the sample supply tube T, which is closed with a silicone rubber stopper G.
The syringe needle I is passed through the micro cylinder M so that a minute amount of sample can be injected. When the fuel gas and the auxiliary combustion gas are supplied, the liquid L in the container C is sucked through the pipe T and sprayed into the burner body B to be atomized. The method of the present invention is characterized in that the liquid L in the container C does not contain a sample, and the liquid L consists only of a solvent to which an interference suppressor has been added. The liquid L flows through the sample introduction chamber X, and acts as a carrier for transporting the sample injected into the chamber X into the burner body. The sample injected into the sample introduction chamber X is conveyed to the burner body B while being mixed with the carrier fluid L mentioned above, and is sprayed into the burner body. Since an interference suppressant is added to the carrier fluid L, the sample is mixed with the interference suppressant and ejected from the nozzle N into the flame F.
第３図は従来方法による分析結果の一例のカー
ブで、Mgを定量するものである。試料にAlを添
加したときの干渉現象を示している。測定結果の
カーブは矩形波パルスの形になつている。一つの
パルスが一試料であつて、第１図の容器Ｃに入れ
た試料液全部を吸引しつくす迄の間Mg検出信号
が出力されているから矩形波パルスになる。第４
図は本発明方法においてキヤリヤ流体Ｌに水を用
い干渉抑制剤を添加しないときの測定例で、Mg
検出においてAlを干渉物質として添加した例で
ある。測定出力がスパイク状であるのは微量の試
料をキヤリヤ流体で運んで炎Ｆに送る構成だから
であり、Alによる干渉が現れている。第５図は
第４図と同じ試料を用い、本発明方法を実施した
場合の測定結果であり、キヤリヤ流体にはLaを
4000ppm含む水を用したものである。Alを
50ppmから1000ppmまで含んだ各試料ともMg単
独の試料と同レベルの出力を得ており、干渉抑制
剤の効果は充分に発揮されている。 FIG. 3 is a curve showing an example of the analysis results according to the conventional method, and is used to quantify Mg. This shows the interference phenomenon when Al is added to the sample. The curve of the measurement result is in the form of a square wave pulse. One pulse corresponds to one sample, and since the Mg detection signal is output until all the sample liquid in the container C in FIG. 1 is sucked out, it becomes a rectangular wave pulse. Fourth
The figure shows an example of measurement when water is used in the carrier fluid L and no interference suppressant is added in the method of the present invention.
This is an example in which Al is added as an interference substance during detection. The spike-like shape of the measured output is due to the configuration in which a small amount of sample is carried by a carrier fluid and sent to flame F, and interference by Al appears. Figure 5 shows the measurement results when the method of the present invention was carried out using the same sample as in Figure 4, with La added to the carrier fluid.
This uses water containing 4000ppm. Al
Each sample containing Mg from 50ppm to 1000ppm obtained the same level of output as the sample containing Mg alone, and the effect of the interference suppressor was fully demonstrated.
本発明方法によれば上述したように干渉抑制剤
を添加したキヤリヤ流体を継続的に試料原子化部
に供給し、このキヤリヤ流体の流路の途中に試料
を注入するので、試料毎に干渉抑制剤を添加する
と云う面倒な試料調整操作が不要となり、試料原
子化装置上例で云えばバーナ本体内は常時キヤリ
ヤ流体と燃料及び助燃両ガスの混合ガスで洗われ
ており、試料が間欠的に供給される結果、試料原
子化装置内の前回分析試料による汚染がなく、一
試料の分析時間が短かく、一つの試料注入と次の
試料注入との間が自然に装置洗滌期間になるか
ら、分析能率が向上する。 According to the method of the present invention, as described above, the carrier fluid added with the interference suppressant is continuously supplied to the sample atomization section, and the sample is injected into the flow path of this carrier fluid, so that interference is suppressed for each sample. This eliminates the need for troublesome sample preparation operations such as adding reagents, and in the example of sample atomization equipment, the inside of the burner body is constantly flushed with a mixture of carrier fluid, fuel, and auxiliary gas, and the sample is intermittently flushed. As a result, there is no contamination from the previous analysis sample in the sample atomization device, the analysis time for one sample is short, and there is a natural device cleaning period between one sample injection and the next sample injection. Analysis efficiency is improved.
第１図は従来の試料原子化用バーナの略側面
図、第２図は本発明方法において用いる試料原子
化用バーナの略側面図、第３図は従来方法による
測定結果のグラフ、第４図は本発明において干渉
抑制剤を用いなかつたときの測定結果のグラフ、
第５図は本発明方法による測定結果のグラフであ
る。
Ｂ…バーナ本体、Ｔ…試料供給管、Ｃ…容器、
Ｌ…キヤリヤ流体、Ｘ…試料導入室、Ｆ…炎、ｆ
…燃料ガス、ａ…助燃ガス。
Figure 1 is a schematic side view of a conventional sample atomization burner, Figure 2 is a schematic side view of a sample atomization burner used in the method of the present invention, Figure 3 is a graph of measurement results by the conventional method, and Figure 4. is a graph of measurement results when no interference suppressor is used in the present invention,
FIG. 5 is a graph of measurement results according to the method of the present invention. B...burner body, T...sample supply tube, C...container,
L...Carrier fluid, X...sample introduction chamber, F...flame, f
...fuel gas, a...assistant gas.
Claims (1)
みを添加したキヤリヤ流体を継続的に供給し、こ
のキヤリヤ流体の流路の途中に試料導入室を設
け、間欠的に干渉抑制剤を添加してない微量の試
料を上記試料導入室に注入し、上記キヤリヤ流体
によつて試料原子化部まで移送させるようにした
ことを特微とする原子吸光分析方法。1. Continuously supply a carrier fluid that does not contain a sample but only an interference suppressor to the sample atomization device, provide a sample introduction chamber in the middle of the flow path of this carrier fluid, and add the interference suppressor intermittently. An atomic absorption spectrometry method characterized in that a very small amount of a sample that has not been oxidized is injected into the sample introduction chamber and transported to a sample atomization section by the carrier fluid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4896581A JPS57161638A (en) | 1981-03-31 | 1981-03-31 | Method for atomic absorption analysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4896581A JPS57161638A (en) | 1981-03-31 | 1981-03-31 | Method for atomic absorption analysis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS57161638A JPS57161638A (en) | 1982-10-05 |
| JPS6322254B2 true JPS6322254B2 (en) | 1988-05-11 |
Family
ID=12817988
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4896581A Granted JPS57161638A (en) | 1981-03-31 | 1981-03-31 | Method for atomic absorption analysis |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS57161638A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9719961B2 (en) | 2008-10-08 | 2017-08-01 | Sage Science, Inc. | Multichannel preparative electrophoresis system |
| US10131901B2 (en) | 2014-10-15 | 2018-11-20 | Sage Science, Inc. | Apparatuses, methods and systems for automated processing of nucleic acids and electrophoretic sample preparation |
| US10473619B2 (en) | 2012-10-12 | 2019-11-12 | Sage Science, Inc. | Side-eluting molecular fractionator |
| US11542495B2 (en) | 2015-11-20 | 2023-01-03 | Sage Science, Inc. | Preparative electrophoretic method for targeted purification of genomic DNA fragments |
| US11867661B2 (en) | 2017-04-07 | 2024-01-09 | Sage Science, Inc. | Systems and methods for detection of genetic structural variation using integrated electrophoretic DNA purification |
-
1981
- 1981-03-31 JP JP4896581A patent/JPS57161638A/en active Granted
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9719961B2 (en) | 2008-10-08 | 2017-08-01 | Sage Science, Inc. | Multichannel preparative electrophoresis system |
| US10473619B2 (en) | 2012-10-12 | 2019-11-12 | Sage Science, Inc. | Side-eluting molecular fractionator |
| US10131901B2 (en) | 2014-10-15 | 2018-11-20 | Sage Science, Inc. | Apparatuses, methods and systems for automated processing of nucleic acids and electrophoretic sample preparation |
| US10738298B2 (en) | 2014-10-15 | 2020-08-11 | Sage Science, Inc. | Apparatuses, methods and systems for automated processing of nucleic acids and electrophoretic sample preparation |
| US11542495B2 (en) | 2015-11-20 | 2023-01-03 | Sage Science, Inc. | Preparative electrophoretic method for targeted purification of genomic DNA fragments |
| US11867661B2 (en) | 2017-04-07 | 2024-01-09 | Sage Science, Inc. | Systems and methods for detection of genetic structural variation using integrated electrophoretic DNA purification |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS57161638A (en) | 1982-10-05 |
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