JPH09101259A - Method for determining components using spectrophotometer - Google Patents
Method for determining components using spectrophotometerInfo
- Publication number
- JPH09101259A JPH09101259A JP28789195A JP28789195A JPH09101259A JP H09101259 A JPH09101259 A JP H09101259A JP 28789195 A JP28789195 A JP 28789195A JP 28789195 A JP28789195 A JP 28789195A JP H09101259 A JPH09101259 A JP H09101259A
- Authority
- JP
- Japan
- Prior art keywords
- spectrum
- absorption
- components
- spectrophotometer
- measurement sample
- 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.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims description 24
- 238000001228 spectrum Methods 0.000 claims abstract description 45
- 150000001875 compounds Chemical class 0.000 claims abstract description 27
- 238000000862 absorption spectrum Methods 0.000 claims abstract description 18
- 239000011159 matrix material Substances 0.000 claims abstract description 17
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 3
- 238000005259 measurement Methods 0.000 claims description 19
- 238000011002 quantification Methods 0.000 claims description 15
- 238000004364 calculation method Methods 0.000 claims description 12
- 238000002835 absorbance Methods 0.000 claims description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 abstract description 33
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 abstract description 26
- 235000019253 formic acid Nutrition 0.000 abstract description 14
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 abstract description 12
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 5
- 150000001735 carboxylic acids Chemical class 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract 2
- 150000007513 acids Chemical class 0.000 abstract 2
- 238000010521 absorption reaction Methods 0.000 description 12
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 10
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- 239000001294 propane Substances 0.000 description 5
- 230000035945 sensitivity Effects 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 238000004445 quantitative analysis Methods 0.000 description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 150000002894 organic compounds Chemical class 0.000 description 3
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 2
- 238000000513 principal component analysis Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
Landscapes
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】この発明は、測定試料に光を
照射し、そのとき得られる吸収スペクトル中の複数の指
定された波数ポイントにおける吸光度に基づいて測定試
料中に含まれる成分を定量分析する分光光度計を用いた
複数成分の定量方法に関する。TECHNICAL FIELD The present invention irradiates a measurement sample with light, and quantitatively analyzes the components contained in the measurement sample based on the absorbances at a plurality of designated wave number points in the absorption spectrum obtained at that time. The present invention relates to a method for quantifying a plurality of components using a spectrophotometer.
【０００２】[0002]
【従来の技術】上記分光光度計の一つに、フーリエ変換
赤外分光光度計（ＦＴ−ＩＲ）がある。このＦＴ−ＩＲ
は、例えば図１に示すように構成されている。すなわ
ち、この図において、１は分析部、２はこの分析部１の
出力であるインターフェログラムを処理するデータ処理
部である。分析部１は平行な赤外光を発するように構成
された赤外光源３と、ビームスプリッタ４，固定ミラー
５，図外の駆動機構によって例えばＸ−Ｙ方向に平行移
動する可動ミラー６からなる干渉機構７と、測定試料な
どを収容し、干渉機構７を介して赤外光源３からの赤外
光が照射されるセル８と、半導体検出器９などから構成
されている。そして、データ処理部２は、例えばコンピ
ュータよりなり、インターフェログラムを加算平均し、
その加算平均出力を高速でフーリエ変換し、さらに、こ
のフーリエ変換出力に基づいて測定対象成分に関するス
ペクトル演算を行うように構成されている。2. Description of the Related Art One of the above spectrophotometers is a Fourier transform infrared spectrophotometer (FT-IR). This FT-IR
Is configured as shown in FIG. 1, for example. That is, in this figure, 1 is an analysis unit, and 2 is a data processing unit that processes an interferogram output from the analysis unit 1. The analysis unit 1 includes an infrared light source 3 configured to emit parallel infrared light, a beam splitter 4, a fixed mirror 5, and a movable mirror 6 that moves in parallel in, for example, the XY direction by a driving mechanism (not shown). An interference mechanism 7, a cell 8 for accommodating a measurement sample and the like, which is irradiated with infrared light from the infrared light source 3 via the interference mechanism 7, and a semiconductor detector 9 are included. The data processing unit 2 is composed of, for example, a computer, averages the interferograms,
The arithmetic mean output is fast Fourier-transformed, and the spectrum calculation for the measurement object component is performed based on the Fourier-transform output.
【０００３】上述のように構成されたＦＴ−ＩＲにおい
ては、次のようにして複数の成分を定量分析することが
できる。すなわち、セル８に比較試料または測定試料を
それぞれ収容して赤外光源３からの赤外光をセル８に照
射し、比較試料または測定試料のインターフェログラム
を測定する。これらのインターフェログラムをデータ処
理部２において、それぞれフーリエ変換してパワースペ
クトルを得た後、比較試料のパワースペクトルに対する
測定試料のパワースペクトルの比を求め、これを吸光度
スケールに変換することにより吸収スペクトルを得た
後、この吸収スペクトル中の複数の波数ポイントにおけ
る吸光度に基づいて測定試料中に含まれる複数の成分を
定量分析するのである。In the FT-IR constructed as described above, a plurality of components can be quantitatively analyzed as follows. That is, the comparative sample or the measurement sample is housed in the cell 8, the infrared light from the infrared light source 3 is irradiated to the cell 8, and the interferogram of the comparative sample or the measurement sample is measured. In the data processing unit 2, these interferograms are respectively Fourier-transformed to obtain a power spectrum, then the ratio of the power spectrum of the measurement sample to the power spectrum of the comparative sample is obtained, and this is converted into an absorbance scale to obtain the absorption. After obtaining the spectrum, a plurality of components contained in the measurement sample are quantitatively analyzed based on the absorbances at a plurality of wave number points in the absorption spectrum.
【０００４】上記複数の成分を定量分析する方法とし
て、例えば、この出願の出願人に係る特許出願（特開平
４−６０４２２号）があり、その概要は、吸収スペクト
ル中の複数の波数ポイントにおける局所的ピーク値と局
所的バレー値との差である相対吸光度の和を求め、この
和に基づいて複数の成分の濃度を各別に得るというもの
である。また、ＰＬＳ（部分最小二乗）法、ＰＣＲ（主
成分分析）法なども使用できる。これらの方法はいずれ
も、濃度既知の参照スペクトルに基づいて、予め濃度演
算用のデータ（校正行列）を作成しておき、濃度未知の
試料のスペクトルデータとの演算行列により、複数の成
分の濃度を各別に算出するのである。As a method for quantitatively analyzing the above-mentioned plurality of components, for example, there is a patent application (Japanese Patent Laid-Open No. 4-60422) filed by the applicant of the present application. The sum of relative absorbance, which is the difference between the peak value and the local valley value, is calculated, and the concentrations of a plurality of components are separately obtained based on this sum. Also, PLS (Partial Least Squares) method, PCR (Principal Component Analysis) method, etc. can be used. In each of these methods, data (calibration matrix) for concentration calculation is created in advance based on a reference spectrum of known concentration, and the concentration of multiple components is calculated using the calculation matrix with the spectrum data of a sample of unknown concentration. Is calculated separately for each.
【０００５】[0005]
【発明が解決しようとする課題】上述のように、複数の
成分を同時に定量分析することができるＦＴ−ＩＲを用
いて、測定試料中のある成分を定量したい場合、その成
分の濃度計算に使用している波数領域に他にも吸収をも
つ化合物が存在するときは、濃度計算用の波数ポイント
を選ぶときにそのような化合物の吸収を避けるか、ある
いは、それらの化合物も測定対象成分としておく必要が
ある。何故なら、そうしなければ、濃度計算値に他の化
合物の干渉影響を受けやすくなるからである。なお、こ
の場合、測定試料中に殆ど存在しない化合物については
無視してよい。As described above, when it is desired to quantify a certain component in a measurement sample by using FT-IR capable of quantitatively analyzing a plurality of components simultaneously, it is used for the concentration calculation of the component. If there are other compounds with absorption in the wavenumber region, the absorption of such compounds should be avoided when selecting the wavenumber points for concentration calculation, or those compounds should also be measured. There is a need. This is because otherwise, the calculated concentration will be more susceptible to the interference of other compounds. In this case, compounds that are rarely present in the measurement sample may be ignored.
【０００６】ところで、一般に、化合物は、その化学結
合の形に応じて特有の波数領域に吸収を持っている。こ
れは、言い換えれば、化学構造のよく似た化合物は、よ
く似た波数領域に吸収を持つということであり、特に有
機化合物において顕著である。加えて、有機化合物にお
いては、分子量が大きくなるほど吸収がブロードになる
傾向があり、そのため、化学構造のよく似た化合物どう
しは、分子量がある程度大きくなれば吸収の領域だけで
なくその形状も似通ってくる。By the way, in general, a compound has absorption in a specific wave number region depending on the form of its chemical bond. In other words, a compound having a similar chemical structure has absorption in a similar wave number region, which is particularly remarkable in an organic compound. In addition, in organic compounds, absorption tends to become broader as the molecular weight increases, so compounds with similar chemical structures are similar not only in the absorption region but also in their shape as the molecular weight increases to some extent. come.
【０００７】このように、測定試料中に、化学構造のよ
く似た化合物、特に有機化合物が何種類も混在している
と、それらの化合物のうちの一つを定量するために、化
学構造の似た他の多くの化合物をも測定対象としなくて
はならないことが多い。しかし、前述のような吸収の帯
域および形状のよく似た化合物群では、それらの吸収ス
ペクトルを正確に分離して信頼性のある定量分析値を得
ることは困難である。また、干渉計としてきわめて高い
分解能およびＳ／Ｎを有する装置を用いれば分離しやす
くなるが、その場合でも、正確な定量分析値を得るには
測定対象成分として非常に多くの化合物を考慮すること
が必要である。これでは、濃度計算で扱うデータ量が多
くなり過ぎるため、データの処理速度が遅くなり、特に
連続分析時には不都合が生じる。As described above, in the case where many kinds of compounds having similar chemical structures, especially organic compounds, are mixed in the measurement sample, one of the compounds is used to quantify the chemical structure. Many other similar compounds also have to be measured. However, it is difficult to accurately separate the absorption spectra of a group of compounds having similar absorption bands and shapes as described above to obtain a reliable quantitative analysis value. Also, if an interferometer with a device having extremely high resolution and S / N is used, separation will be easy, but even in that case, in order to obtain accurate quantitative analysis values, consider a large number of compounds as measurement components. is required. In this case, since the amount of data handled in the concentration calculation becomes too large, the processing speed of the data becomes slow, which causes inconvenience especially in continuous analysis.
【０００８】このような不都合を解消するものとして、
この出願の出願人に係る特開平４−２６５８４２号公報
に開示された複数成分定量方法がある。この複数成分定
量方法によれば、互いに類似した赤外吸収スペクトル
（例えば、炭素数３以上のアルカンの２８００〜３００
０ｃｍ-1付近の赤外吸収など）を持つ成分を定量する場
合、無理に分離定量しなくても、ある代表成分のスペク
トルを参照スペクトルとして校正行列を作成すること
で、おおよその総量を算出することができる。In order to eliminate such inconvenience,
There is a multi-component quantification method disclosed in Japanese Patent Application Laid-Open No. 4-265842 related to the applicant of this application. According to this multi-component quantification method, infrared absorption spectra similar to each other (for example, 2800 to 300 of an alkane having 3 or more carbon atoms).
In the case of quantifying components having infrared absorption around 0 cm -1, etc., the approximate total amount is calculated by creating a calibration matrix using the spectrum of a certain representative component as the reference spectrum without forcibly separating and quantifying. be able to.
【０００９】しかしながら、上記出願に係る複数成分定
量方法においては、スペクトルの類似性が高いことを前
提としているため、類似性の低い成分をも一括して定量
したい場合、相対的な感度が非常に低くなり、満足でき
る結果が得られないことがあった。However, the multi-component quantification method according to the above application is premised on the fact that the spectra have high similarity, so that when the components with low similarity are to be quantified collectively, the relative sensitivity is very high. There were times when it was too low to obtain satisfactory results.
【００１０】この発明は、上述の事柄に留意してなされ
たもので、その目的は、化学的性質が似ているなど個別
の定量が不要な化合物を、その吸収スペクトル形状の類
似性の大小にかかわらず、簡便に一括して定量すること
ができる分光光度計を用いた複数成分定量方法（以下、
単に複数成分定量方法という）を提供することである。The present invention has been made in view of the above matters, and its object is to reduce the similarity in absorption spectrum shape between compounds which do not require individual quantification due to similar chemical properties. Despite this, a multi-component quantification method using a spectrophotometer (hereinafter,
Simply referred to as a multi-component quantitation method).
【００１１】[0011]
【課題を解決するための手段】上記目的を達成するた
め、この発明は、測定試料に光を照射し、そのとき得ら
れる吸収スペクトル中の複数の指定された波数ポイント
における吸光度に基づいて測定試料中に含まれる成分を
定量分析する分光光度計を用いた複数成分定量方法にお
いて、測定試料に含まれることが予想される複数の化合
物のうち、一部の複数の化合物については、仮想的に単
一成分のスペクトルであるとみなすことができる仮想ス
ペクトルを作成し、この仮想スペクトルを濃度演算用の
校正行列作成時の基準となる参照スペクトルとして用い
ることにより、一つの化合物群としてその総量を一括し
て定量計算するようにしている。In order to achieve the above object, the present invention irradiates a measurement sample with light, and based on the absorbance at a plurality of designated wave number points in the absorption spectrum obtained at that time, the measurement sample is measured. In a multiple-component quantification method using a spectrophotometer that quantitatively analyzes the components contained in some of the compounds expected to be contained in the measurement sample, some of the compounds are virtually Create a virtual spectrum that can be regarded as a spectrum of one component, and use this virtual spectrum as a reference spectrum that serves as a reference when creating a calibration matrix for concentration calculation, so that the total amount is collected as one compound group. I try to calculate quantitatively.
【００１２】この場合、校正行列作成時の基準となる仮
想スペクトルは、計算機上で各成分スペクトルから合成
したところの合成スペクトルを用いたり、また、数成分
を混合した試料の吸収スペクトルを用いることができ
る。In this case, as the virtual spectrum that serves as a reference when creating the calibration matrix, a synthetic spectrum obtained by synthesizing each component spectrum on a computer may be used, or an absorption spectrum of a sample in which several components are mixed may be used. it can.
【００１３】上記複数成分定量方法によれば、吸収スペ
クトル形状の類似性が低い化合物どうしであっても、そ
れらの総量を簡便にしかも従来よりも精度よく定量する
ことができ、したがって、信頼性のある定量分析結果を
得ることができる。そして、合成スペクトルは、濃度の
信頼できる混合ガスを実際に作成するのが難しい成分ど
うしの場合に好適に使用できる。According to the above multi-component quantification method, the total amount of compounds having a low similarity in absorption spectrum shape can be quantified easily and more accurately than in the prior art. A certain quantitative analysis result can be obtained. Then, the synthetic spectrum can be suitably used in the case where it is difficult to actually create a mixed gas having a reliable concentration.
【００１４】[0014]
【発明の実施の形態】以下、この発明の詳細を、図を参
照しながら説明する。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The details of the present invention will be described below with reference to the drawings.
【００１５】この発明の複数成分定量方法が従来のこの
種の複数成分定量方法と大きく異なる点は、測定試料に
含まれることが予想される複数の化合物のうち、一部の
複数の化合物については、仮想的に単一成分のスペクト
ルであるとみなすことができる仮想スペクトルを作成
し、この仮想スペクトルを校正行列作成時の基準となる
参照スペクトルとして用いることにより、一つの化合物
群としてその総量を一括して定量計算するようにした点
である。The point that the multi-component quantification method of the present invention is greatly different from the conventional multi-component quantification method of this kind is that some of the plurality of compounds expected to be contained in the measurement sample are plural compounds. By creating a virtual spectrum that can be virtually regarded as a spectrum of a single component, and using this virtual spectrum as a reference spectrum that serves as a reference when creating the calibration matrix, the total amount is collected as one compound group. The point is that the calculation is made quantitatively.
【００１６】第１の実施の形態として、例えば、同じカ
ルボン酸（Ｒ−ＣＯＯＨ）に属する蟻酸（ＨＣＯＯＨ）
と酢酸（ＣＨ3 ＣＯＯＨ）とを、９００〜１３００ｃｍ
-1付近の赤外吸収に基づいて定量する場合について説明
する。In the first embodiment, for example, formic acid (HCOOH) belonging to the same carboxylic acid (R-COOH) is used.
And acetic acid (CH 3 COOH), 900-1300 cm
A case of quantifying based on infrared absorption near -1 will be described.
【００１７】図２は、図１に示したＦＴ−ＩＲを用いて
測定したほぼ同一濃度〔仮に１００（単位は任意）とす
る〕の蟻酸と酢酸の吸収スペクトルを示すもので、この
図２において、符号１１で示す曲線は、蟻酸の吸収スペ
クトルであり、符号１２で示す曲線は、酢酸の吸収スペ
クトルである。FIG. 2 shows absorption spectra of formic acid and acetic acid at almost the same concentration [probably 100 (unit is arbitrary)] measured using the FT-IR shown in FIG. 1. In FIG. The curve indicated by reference numeral 11 is the absorption spectrum of formic acid, and the curve indicated by the reference numeral 12 is the absorption spectrum of acetic acid.
【００１８】上記蟻酸と酢酸は、ともにカルボキシル基
（ＣＯＯＨ）を有し、よく似た化学構造をもつにもかか
わらず、図２に示すような波数領域では、スペクトルは
ほとんど重なることはない。そのため、ＰＬＳ法やＰＣ
Ｒ法などを用いて、これらの成分を総量として定量しよ
うとしても、蟻酸を参照スペクトルとして作成した校正
行列では酢酸に対してほとんど感度が得られず、また、
酢酸を参照スペクトルとした場合は蟻酸に対してほとん
ど感度が得られない。Although both the formic acid and acetic acid have a carboxyl group (COOH) and have a similar chemical structure, the spectra hardly overlap in the wave number region as shown in FIG. Therefore, PLS method and PC
Even if an attempt is made to quantify these components as a total amount using the R method or the like, the calibration matrix prepared using formic acid as a reference spectrum shows almost no sensitivity to acetic acid, and
When acetic acid is used as a reference spectrum, almost no sensitivity to formic acid is obtained.
【００１９】そこで、前記両吸収スペクトル１１，１２
を計算機上で合成し、図３に示すような合成スペクトル
１３を仮想的に得る。図４は、その濃度を０，２０，４
０，６０，８０，１００の６段階に変化させた場合を示
し、図中の符号〜の曲線が０〜１００にそれぞれ対
応している。Therefore, both the absorption spectra 11 and 12
Are synthesized on a computer, and a synthesized spectrum 13 as shown in FIG. 3 is virtually obtained. FIG. 4 shows that the concentration is 0, 20, 4
The case where the number is changed in six stages of 0, 60, 80, and 100 is shown, and the curves from 1 to 0 in the figure correspond to 0 to 100, respectively.
【００２０】前記図４に示すスペクトルを参照スペクト
ルとして作成した校正行列によれば、蟻酸と酢酸との総
量を定量することができる。この場合、感度は、例え
ば、蟻酸に対して感度比が約２／３（蟻酸１００に対し
て６７程度）、酢酸に対して感度比が約１／３（酢酸１
００に対して３３程度）というように、やや低くなる。According to the calibration matrix prepared by using the spectrum shown in FIG. 4 as a reference spectrum, the total amount of formic acid and acetic acid can be quantified. In this case, the sensitivity is, for example, about 2/3 for formic acid (about 67 for 100 formic acid) and about 1/3 for acetic acid (1 for acetic acid).
It is slightly lower, such as about 33 compared to 00).
【００２１】そこで、校正行列を作成する際に、合成ス
ペクトルの濃度の情報を、例えば、０，３０，６０，９
０，１２０，１５０というように１．５倍しておけば、
蟻酸に対しては、約１／１倍（＝２／３×３／２）、酢
酸に対しては約１／２（＝１／３×３／２）の感度が得
られる。Therefore, when creating the calibration matrix, information on the concentration of the synthetic spectrum is, for example, 0, 30, 60, 9
If you multiply by 1.5 like 0, 120, 150,
Sensitivity of about 1/1 times (= 2/3 × 3/2) is obtained for formic acid and about 1/2 (= 1/3 × 3/2) for acetic acid.
【００２２】あるいは、校正行列作成時の濃度情報は、
０〜１００のままで、未知スペクトルからの濃度演算結
果に係数を乗ずるようにしてもよい（係数を１．５とす
ると上述した例と同じ結果が得られる）。Alternatively, the concentration information when creating the calibration matrix is
You may make it multiply the coefficient calculation result from an unknown spectrum with a coefficient with 0-100 as it is (if a coefficient is set to 1.5, the same result as the above-mentioned example will be obtained).
【００２３】次に、第２の実施の形態として、アルカン
（メタン・エタン・プロパン・ｎ−ブタン・ｉ−ブタ
ン、……）を２８００〜３０００ｃｍ-1の赤外吸収から
一括定量する場合について説明する。Next, as a second embodiment, a case of collectively quantifying alkanes (methane, ethane, propane, n-butane, i-butane, ...) From infrared absorption at 2800 to 3000 cm -1 will be described. To do.
【００２４】前記アルカンのうち、プロパンより炭素数
の多いもの（ｎ−ブタン・ｉ−ブタン・……）について
は、プロパンとよく似た吸収をもつため、プロパンを参
照スペクトルとする校正行列で、おおよその総量として
の定量が可能である。そこで、この場合、残りのメタン
・エタンとプロパンとの合成スペクトルとの合成スペク
トルを参照スペクトルとし、校正行列を作成すればよ
い。Among the alkanes, those having more carbon atoms than propane (n-butane, i-butane, ...) Have absorption similar to that of propane, and therefore, in the calibration matrix using propane as the reference spectrum, Quantification as an approximate total amount is possible. Therefore, in this case, the calibration matrix may be created by using the synthetic spectrum of the residual methane / ethane and the synthetic spectrum of propane as the reference spectrum.
【００２５】上述の実施の形態は、いずれも計算機上で
各成分スペクトルを合成して仮想的なスペクトルでを求
め、この仮想スペクトルを濃度演算用の校正行列作成時
の基準となる参照スペクトルとして用いることにより、
一つの化合物群としてその総量を一括して定量計算する
ようにしていたが、これに代えて、一括定量すべき複数
の成分を混合して混合標準ガスとし、これをＦＴ−ＩＲ
で測定してスペクトル（仮想スペクトル）を得、この仮
想スペクトルを濃度演算用の校正行列作成時の基準とな
る参照スペクトルとして用いるようにしてもよい。In each of the above-described embodiments, each component spectrum is combined on a computer to obtain a virtual spectrum, and this virtual spectrum is used as a reference spectrum that serves as a reference when creating a calibration matrix for concentration calculation. By
Although the total amount was collectively calculated as one compound group, instead of this, a plurality of components to be collectively determined were mixed to form a mixed standard gas, which was used as FT-IR.
It is also possible to obtain the spectrum (virtual spectrum) by measuring in step 1 above and use this virtual spectrum as a reference spectrum that serves as a reference when creating a calibration matrix for concentration calculation.
【００２６】この発明は、ＦＴ−ＩＲによる複数成分の
定量のみならず、広く分光光度計による複数成分の定量
方法に適用することができる。The present invention can be widely applied not only to quantification of a plurality of components by FT-IR but also to a method of quantification of a plurality of components by a spectrophotometer.
【００２７】[0027]
【発明の効果】以上説明したように、この発明によれ
ば、吸収スペクトル形状の類似性が低い化合物どうしで
あっても、それらの総量を簡便にしかも従来よりも精度
よく定量することができ、したがって、信頼性のある定
量分析結果を得ることができる。As described above, according to the present invention, it is possible to easily quantify the total amount of compounds having a low absorption spectrum shape similarity and more accurately than ever before. Therefore, a reliable quantitative analysis result can be obtained.
【００２８】そして、請求項２に記載の発明によれば、
濃度の信頼できる混合ガスを実際に作成するのが難しい
成分どうしの場合にも簡単に定量することができる。According to the invention described in claim 2,
Even if it is difficult to actually create a gas mixture with a reliable concentration, it can be easily quantified.
【図１】この発明方法を実施するための装置の一例を概
略的に示す図である。FIG. 1 is a diagram schematically showing an example of an apparatus for carrying out the method of the present invention.
【図２】代表的なカルボン酸の吸収スペクトルを示す図
である。FIG. 2 is a diagram showing an absorption spectrum of a typical carboxylic acid.
【図３】合成スペクトルの一例を示す図である。FIG. 3 is a diagram showing an example of a synthetic spectrum.
【図４】図３に示した合成スペクトルの濃度を０，２
０，４０，６０，８０，１００の６段階に変化させて示
す図である。FIG. 4 is a graph showing the density of the synthetic spectrum shown in FIG.
It is a figure changed and shown in 6 steps of 0,40,60,80,100.
１３…仮想スペクトル。 13 ... Virtual spectrum.
Claims (3)
る吸収スペクトル中の複数の指定された波数ポイントに
おける吸光度に基づいて測定試料中に含まれる成分を定
量分析する分光光度計を用いた複数成分定量方法におい
て、測定試料に含まれることが予想される複数の化合物
のうち、一部の複数の化合物については、仮想的に単一
成分のスペクトルであるとみなすことができる仮想スペ
クトルを作成し、この仮想スペクトルを濃度演算用の校
正行列作成時の基準となる参照スペクトルとして用いる
ことにより、一つの化合物群としてその総量を一括して
定量計算するようにしたことを特徴とする分光光度計を
用いた複数成分定量方法。1. A spectrophotometer is used which irradiates a measurement sample with light and quantitatively analyzes the components contained in the measurement sample based on the absorbances at a plurality of designated wave number points in the absorption spectrum obtained at that time. In the multiple component quantification method, a virtual spectrum that can be virtually regarded as a single component spectrum is created for some of the multiple compounds expected to be contained in the measurement sample. The spectrophotometer is characterized in that the total amount of one compound group is collectively calculated by using this virtual spectrum as a reference spectrum that serves as a standard when creating a calibration matrix for concentration calculation. Multiple component quantification method using.
クトルから合成したところの合成スペクトルである請求
項１に記載の分光光度計を用いた複数成分定量方法。2. The multiple component quantification method using a spectrophotometer according to claim 1, wherein the virtual spectrum is a synthetic spectrum obtained by synthesizing each component spectrum on a computer.
の吸収スペクトルである請求項１に記載の分光光度計を
用いた複数成分定量方法。3. The method for quantifying plural components using a spectrophotometer according to claim 1, wherein the virtual spectrum is an absorption spectrum of a sample in which several components are mixed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28789195A JPH09101259A (en) | 1995-10-08 | 1995-10-08 | Method for determining components using spectrophotometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28789195A JPH09101259A (en) | 1995-10-08 | 1995-10-08 | Method for determining components using spectrophotometer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH09101259A true JPH09101259A (en) | 1997-04-15 |
Family
ID=17723062
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP28789195A Pending JPH09101259A (en) | 1995-10-08 | 1995-10-08 | Method for determining components using spectrophotometer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH09101259A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008135416A1 (en) * | 2007-05-02 | 2008-11-13 | Siemens Aktiengesellschaft | Detector arrangement for a nondispersive infrared gas analyser and method for the detection of a measuring gas component in a gas mixture by means of such a gas analyser |
| EP2105726A2 (en) | 2008-03-26 | 2009-09-30 | Jasco Corporation | Automatic and continuous quantitative analysis method and apparatus for multiple components |
| JP2013113664A (en) * | 2011-11-28 | 2013-06-10 | Yokogawa Electric Corp | Laser gas analyzer |
| JP2015129769A (en) * | 2015-03-12 | 2015-07-16 | 横河電機株式会社 | laser gas analyzer |
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-
1995
- 1995-10-08 JP JP28789195A patent/JPH09101259A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008135416A1 (en) * | 2007-05-02 | 2008-11-13 | Siemens Aktiengesellschaft | Detector arrangement for a nondispersive infrared gas analyser and method for the detection of a measuring gas component in a gas mixture by means of such a gas analyser |
| US8158945B2 (en) | 2007-05-02 | 2012-04-17 | Siemens Aktiengesellschaft | Detector arrangement for a nondispersive infrared gas analyzer and method for the detection of a measuring gas component in a gas mixture by means of such a gas analyzer |
| EP2105726A2 (en) | 2008-03-26 | 2009-09-30 | Jasco Corporation | Automatic and continuous quantitative analysis method and apparatus for multiple components |
| JP2013113664A (en) * | 2011-11-28 | 2013-06-10 | Yokogawa Electric Corp | Laser gas analyzer |
| US9347877B2 (en) | 2011-11-28 | 2016-05-24 | Yokogawa Electric Corporation | Laser gas analyzer |
| US9671333B2 (en) | 2011-11-28 | 2017-06-06 | Yokogawa Electric Corporation | Laser gas analyzer |
| JP2015129769A (en) * | 2015-03-12 | 2015-07-16 | 横河電機株式会社 | laser gas analyzer |
| WO2019031331A1 (en) * | 2017-08-07 | 2019-02-14 | 株式会社堀場製作所 | Analyzer, analysis method, analyzer program, and analysis learning device |
| JPWO2019031331A1 (en) * | 2017-08-07 | 2020-06-25 | 株式会社堀場製作所 | Analysis device, analysis method, analysis device program, and analysis learning device |
| US11448588B2 (en) | 2017-08-07 | 2022-09-20 | Horiba, Ltd. | Analyzer, analysis method, analyzer program, and analysis learning device |
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