JPS5851615B2 - Frameless atomic absorption spectrometry - Google Patents
Frameless atomic absorption spectrometryInfo
- Publication number
- JPS5851615B2 JPS5851615B2 JP6211776A JP6211776A JPS5851615B2 JP S5851615 B2 JPS5851615 B2 JP S5851615B2 JP 6211776 A JP6211776 A JP 6211776A JP 6211776 A JP6211776 A JP 6211776A JP S5851615 B2 JPS5851615 B2 JP S5851615B2
- Authority
- JP
- Japan
- Prior art keywords
- sodium sulfate
- oxygen
- atomic absorption
- lead
- 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
- 238000001479 atomic absorption spectroscopy Methods 0.000 title claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 26
- 239000001301 oxygen Substances 0.000 claims description 26
- 229910052760 oxygen Inorganic materials 0.000 claims description 26
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 21
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 21
- 235000011152 sodium sulphate Nutrition 0.000 claims description 21
- 239000011261 inert gas Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 4
- 238000000889 atomisation Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 6
- 238000002347 injection Methods 0.000 description 5
- 239000007924 injection Substances 0.000 description 5
- 238000005259 measurement Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000004380 ashing Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000002655 kraft paper Substances 0.000 description 1
- PIJPYDMVFNTHIP-UHFFFAOYSA-L lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 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
- G01N21/74—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】
鉛のフレームレス原子吸光分析において、多量の硫酸ナ
トリウムが共存すると鉛の原子吸収に大きな影響を与え
、硫酸ナトリウムが１１００ｐｐ以上含まれるとほとん
ど分析不可能となる。DETAILED DESCRIPTION OF THE INVENTION In flameless atomic absorption spectrometry of lead, the coexistence of a large amount of sodium sulfate greatly affects the atomic absorption of lead, and if 1100 pp or more of sodium sulfate is contained, analysis becomes almost impossible.
硫酸ナトリウムは排水処理における中和工程から排出さ
れるほか板ガラス製造、クラフトパルプ製造、合成繊維
製造等の工程から排出されている。Sodium sulfate is emitted from the neutralization process in wastewater treatment, as well as from processes such as plate glass manufacturing, kraft pulp manufacturing, and synthetic fiber manufacturing.
これらのことから排水中に多量に含まれる可能性が大き
く、現在これら多量の硫酸ナトリウムを含む排水中の鉛
を測定する場合は複雑な分離操作を行なう必要があり、
時間がか＼る上に分析精度も良好でない欠点があった。For these reasons, there is a high possibility that lead may be contained in large amounts in wastewater, and currently, when measuring lead in wastewater containing large amounts of sodium sulfate, it is necessary to perform complex separation operations.
The drawbacks were that it was time consuming and the analysis accuracy was poor.
本発明はフレームレス原子吸光分析による鉛の測定にお
いて特に大きな干渉影響を与える硫酸ナトリウムが共存
する試料を測定する際の干渉の抑制を行うもので、次に
その原理について述べる。The present invention suppresses interference when measuring a sample in which sodium sulfate, which has a particularly large interference effect when measuring lead by flameless atomic absorption spectrometry, coexists.The principle thereof will be described next.
硫酸ナトリウムが鉛の測定に影響を与える主な原因は、
一定の原子化条件のもとて硫酸ナトリウムが鉛と反応し
て硫酸鉛や複塩、もしくはそれ以外の安定な化合物とな
り、その条件のもとでは原子化効率を著しく悪化させて
いることによると思われる。The main reason why sodium sulfate affects lead measurements is
This is because sodium sulfate reacts with lead under certain atomization conditions to form lead sulfate, double salts, or other stable compounds, and under those conditions, the atomization efficiency is significantly deteriorated. Seem.
しかし酸素気流中において、硫酸ナトリウムが共存する
鉛の測定を行なうと鉛と酸素が結合して原子化条件およ
び原子化効率の一定した形を生成するため、硫酸ナトリ
ウムの影響を受けなくなり、この効果はＡｕ、Ｓｎ、Ｐ
ｔ等の陽イオンのような他の共存物質に対しても応用出
来ることが確認せられた。However, when measuring lead in the presence of sodium sulfate in an oxygen stream, lead and oxygen combine to form a form with constant atomization conditions and atomization efficiency, so it is no longer affected by sodium sulfate, and this effect are Au, Sn, P
It was confirmed that this method can also be applied to other coexisting substances such as cations such as t.
本発明は１〜４％の酸素を含む雰囲気中において被測定
元素を原子化することにより共存物質による干渉作用を
抑制するもので、以下その一実施例について詳述する。The present invention suppresses interference effects caused by coexisting substances by atomizing the element to be measured in an atmosphere containing 1 to 4% oxygen, and one embodiment thereof will be described in detail below.
発熱体を保持したジャケットを外気からしゃ断するため
に光の通過する位置を石英板を用いたカバーで覆い、そ
の中に１〜１０％の範囲で酸素濃度を可変できる流量調
整器より不活性ガスを通じて行なう。In order to shut off the jacket holding the heating element from the outside air, the position where the light passes is covered with a cover using a quartz plate, and an inert gas is poured into the cover using a flow rate regulator that can vary the oxygen concentration in the range of 1 to 10%. through.
なおりバーにより本装置の原子化部は半密閉されて外部
よりの空気流入を阻止している。The atomization section of this device is semi-sealed by the guide bar to prevent air from entering from the outside.
１は原子化を行なわせるチューブ状のカーボンアトマイ
ザ−で、内径４ｎ程度のチューブからなり、中央部に試
料注入用の小孔２とその両側に不活性ガス通気用の穴３
を有する。1 is a tube-shaped carbon atomizer for atomization, which is made of a tube with an inner diameter of about 4n, and has a small hole 2 in the center for sample injection and holes 3 on both sides for inert gas ventilation.
has.
４は二重円筒状のジャケットで、上部に試料注入用窓６
もしくは不活性ガス注入孔１を有し、内管と外管との間
には冷却水を流す通路５，５′を有する。4 is a double cylindrical jacket with a sample injection window 6 at the top.
Alternatively, it has an inert gas injection hole 1, and passages 5, 5' for flowing cooling water between the inner tube and the outer tube.
このジャケット４は良電導性金属製のアトマイザ−保持
具８と、熱伝導性耐熱性が良い絶縁体９を介してカーボ
ンアトマイザ−１を保持しており、この保持具８に電流
を通ずることによってアトマイザ１が発熱し試料１０を
原子化する。This jacket 4 holds the carbon atomizer 1 via an atomizer holder 8 made of a metal with good conductivity and an insulator 9 with good heat conductivity and heat resistance. The atomizer 1 generates heat and atomizes the sample 10.
またジャケット４内部には不活性ガス注入孔７を介して
不活性ガスが流れる。Further, an inert gas flows inside the jacket 4 through an inert gas injection hole 7.
１１は絶縁体９に形成した小さな隙間で、原子化の前処
理段階で発生する低温揮発成分、すなわち原子化する前
に５００℃以下で溶媒として使用した酸や塩類を揮散さ
せる時発生するガスおよび粒子が内部にこもって測定に
影響を与えたり、あるいはこれらが内部に沈着して腐食
することを防止するために外気を流入させるようにした
ものである。Reference numeral 11 denotes a small gap formed in the insulator 9, in which low-temperature volatile components generated in the pretreatment stage of atomization, i.e., gases and This allows outside air to flow in to prevent particles from getting stuck inside and affecting measurements, or from depositing inside and causing corrosion.
１２は不活性ガス気流中の酸素濃度を一定に保持する手
段としてすなわちアトマイザ−１中に外気中の酸素を混
入させないために原子化部を外気から遮断する半密閉容
器、１３は光束、１４はカバー１２において光束１３が
通過する位置に嵌め込んだ光の屈折のない石英板である
。Reference numeral 12 denotes a semi-closed container which serves as a means to keep the oxygen concentration in the inert gas stream constant, that is, a semi-closed container which shields the atomization section from the outside air in order to prevent oxygen from the outside air from being mixed into the atomizer 1, 13 a luminous flux, and 14 a semi-closed container. It is a quartz plate that is fitted in the cover 12 at a position through which the light beam 13 passes and does not refract light.
したがってアトマイザ−１は外気から遮断されるので、
アトマイザ−１内の酸素量は不活性ガス中の酸素濃度の
みに支配されることになる。Therefore, since atomizer 1 is isolated from the outside air,
The amount of oxygen in the atomizer 1 is controlled only by the oxygen concentration in the inert gas.
この場合、不活性ガス中に含まれる酸素は大気雰囲気中
に含まれる酸素量に比べて充分に少ないのでアトマイザ
−１の表面が燃焼して測定に悪影響を与える様なことは
ない。In this case, since the amount of oxygen contained in the inert gas is sufficiently smaller than the amount of oxygen contained in the atmospheric atmosphere, the surface of the atomizer 1 will not burn and adversely affect the measurement.
次の条件で硫酸ナトリウムが共存する鉛の測定を行ない
、硫酸ナトリウムの影響と酸素の効果を調べると次の通
りである。Measurement of lead in the presence of sodium sulfate was carried out under the following conditions, and the effects of sodium sulfate and oxygen were investigated as follows.
条件
（ｉ）分析線波長 ２１７．０ｎｍ
（１ｉ）試料注入量 １０μ７／１回
（ｉｉ＋）試料乾燥温度 １００℃で１０秒１■試料灰
化温度 約３００℃で３０秒
Ｍ試料原子化温度 約２０００℃で１０秒Ｍ不活性ガス
とその流量 アルゴン５１／分（ｖｉＤ試料中の鉛濃度
０．Ｏ２ｐｐｍ硫酸ナトリウムが７５ｐｐｍ（曲線Ｉ
）、１５０ｐｐｍ （曲線■）、３００ｐｐｍ（曲線■
）含まれる時の酸素濃度の影響をみると第２図に示す通
りで、酸素濃度がＯのとき、それぞれの吸光度は、硫酸
ナトリウムを含まないときの吸光度０．１６に対して０
．０９ 、０．０５ 、０．０３であった。Conditions (i) Analysis line wavelength: 217.0 nm (1i) Sample injection amount: 10μ7/time (ii+) Sample drying temperature: 10 seconds at 100°C 1■ Sample ashing temperature: 30 seconds at approximately 300°C M Sample atomization temperature: Approximately 2000 °C for 10 seconds M inert gas and its flow rate Argon 51/min (viD Lead concentration in the sample 0.02 ppm Sodium sulfate 75 ppm (Curve I
), 150ppm (curve ■), 300ppm (curve ■
) The influence of oxygen concentration when sodium sulfate is included is as shown in Figure 2. When the oxygen concentration is O, each absorbance is 0.16 compared to the absorbance when sodium sulfate is not included.
．． 09, 0.05, and 0.03.
そこへ酸素を添加すると硫酸ナトリウムが７５ｐｐｍ含
まれる場合、約１％の酸素濃度にすると硫酸ナトリウム
を含まない時の吸光度と同程度の吸光度が得られた。When oxygen was added thereto, when sodium sulfate was contained at 75 ppm, an absorbance comparable to that obtained when sodium sulfate was not included was obtained when the oxygen concentration was approximately 1%.
１５０ｐｐｍ含まれる場合１．５％、３００ｐｐｍ含ま
れる場合は約２％の酸素濃度にすると完全に抑制できた
。When the oxygen concentration was 150 ppm, the oxygen concentration was 1.5%, and when the oxygen concentration was 300 ppm, it was completely suppressed by setting the oxygen concentration to about 2%.
また酸素濃度を２％に固定した場合、硫酸ナトリウムの
干渉をどの程度まで抑制できるかを見ると第３図に示す
通りで、酸素未添加の場合、１０ｐｐｍ以上で負の干渉
を示すが、酸素濃度を２％にすると硫酸ナトリウム約３
００ ｐｐｍまでの干渉を抑制することができた。In addition, when the oxygen concentration is fixed at 2%, the extent to which the interference of sodium sulfate can be suppressed is shown in Figure 3. When no oxygen is added, negative interference is shown at 10 ppm or more, but oxygen When the concentration is 2%, sodium sulfate is about 3
It was possible to suppress interference up to 0.00 ppm.
よって硫酸ナトリウムが多量に共存する試料でも不活性
ガス中に酸素を添加することによって影響なく鉛の測定
をすることができ、また酸素濃度は一定量以上で同じ効
果を示すが４％以上になるとカーボンアトマイザ−の一
部が燃焼し、その燃焼ガスによって測定値に減少をきた
し、寿命も短くなるので酸素濃度はできるだけ低い方が
望ましく、１〜４％が適当である。Therefore, even in samples where a large amount of sodium sulfate coexists, lead can be measured without any effect by adding oxygen to the inert gas, and the same effect is shown when the oxygen concentration exceeds a certain amount, but when it exceeds 4%. A part of the carbon atomizer burns, and the combustion gas causes a decrease in the measured value and shortens the life. Therefore, it is desirable that the oxygen concentration is as low as possible, and 1 to 4% is suitable.
以上のように、本発明によれば、フレームレス原子吸光
分析法によって硫酸ナトリウムが共存する試料中の鉛を
分析することができる。As described above, according to the present invention, lead in a sample containing sodium sulfate can be analyzed by flameless atomic absorption spectrometry.
第１図は本発明の一実施例を実施する原子化装置の断面
図、第２図および第３図は性能線図である。FIG. 1 is a sectional view of an atomization device implementing an embodiment of the present invention, and FIGS. 2 and 3 are performance diagrams.
Claims (1)
酸ナトリウムを共存する試料を原子化して鉛を分析する
ことを特徴とするフレームレス原子吸光分析法。A flameless atomic absorption spectrometry method characterized by analyzing lead by atomizing a sample containing sodium sulfate in an inert gas atmosphere containing 11 to 4% oxygen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6211776A JPS5851615B2 (en) | 1976-05-27 | 1976-05-27 | Frameless atomic absorption spectrometry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6211776A JPS5851615B2 (en) | 1976-05-27 | 1976-05-27 | Frameless atomic absorption spectrometry |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS52145085A JPS52145085A (en) | 1977-12-02 |
| JPS5851615B2 true JPS5851615B2 (en) | 1983-11-17 |
Family
ID=13190783
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6211776A Expired JPS5851615B2 (en) | 1976-05-27 | 1976-05-27 | Frameless atomic absorption spectrometry |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5851615B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5853858B2 (en) * | 1978-09-20 | 1983-12-01 | 松下電器産業株式会社 | Determination of trace amounts of selenium using flameless atomic absorption spectrometry |
-
1976
- 1976-05-27 JP JP6211776A patent/JPS5851615B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS52145085A (en) | 1977-12-02 |
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