JPS6061649A - Correction of x-ray fluorescence analysis - Google Patents
Correction of x-ray fluorescence analysisInfo
- Publication number
- JPS6061649A JPS6061649A JP16934983A JP16934983A JPS6061649A JP S6061649 A JPS6061649 A JP S6061649A JP 16934983 A JP16934983 A JP 16934983A JP 16934983 A JP16934983 A JP 16934983A JP S6061649 A JPS6061649 A JP S6061649A
- Authority
- JP
- Japan
- Prior art keywords
- temperature
- air
- detector
- ray fluorescence
- ray
- 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
- 238000004458 analytical method Methods 0.000 title claims abstract description 7
- 238000004876 x-ray fluorescence Methods 0.000 title abstract 6
- 238000010521 absorption reaction Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 241001315609 Pittosporum crassifolium Species 0.000 claims 1
- 230000009193 crawling Effects 0.000 claims 1
- 230000008016 vaporization Effects 0.000 claims 1
- 238000009834 vaporization Methods 0.000 claims 1
- 229920006395 saturated elastomer Polymers 0.000 abstract description 2
- 101100491857 Columba livia ASL gene Proteins 0.000 abstract 1
- 230000005540 biological transmission Effects 0.000 abstract 1
- 230000008020 evaporation Effects 0.000 abstract 1
- 238000001704 evaporation Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000000295 fuel oil Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910000976 Electrical steel Inorganic materials 0.000 description 1
- 241000254158 Lampyridae Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 208000014617 hemorrhoid Diseases 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (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)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
Description
【発明の詳細な説明】
例えけ紙（二附着したシリコン（８（）の凪、重油亀二
含まれる硫黄（日）の量、電磁鋼板に含まれるりん（Ｐ
）ノｍ、セメント調合原料中のカルシウム＜ＣＧ＞のｆ
ｆｉ痔を螢光ｘｆｌＡ分析法によって測定する場合に上
述のような元素の螢光ＸＪｌｆｌが大気中を通過すると
、そのときの温度、気圧、並びに湿度等によって大気に
よるＸ線の吸収率が変化するために誤差を生ずる。不発
１ｎはこの誤差を補正して正確な分析を行い得るように
したものである。以下これについてｆ！ｌ”ａ己する。[Detailed description of the invention] For example, the amount of sulfur (day) contained in heavy oil, the amount of phosphorus (P) contained in electrical steel sheets, the amount of sulfur (day) contained in heavy oil,
)nom, f of calcium <CG> in cement preparation raw materials
When fi hemorrhoids are measured by the fluorescence xflA analysis method, when the above-mentioned elemental fluorescence XJlfl passes through the atmosphere, the absorption rate of X-rays by the atmosphere changes depending on the temperature, pressure, humidity, etc. Therefore, errors occur. Misfire 1n is designed to correct this error and enable accurate analysis. About this below f! I'll do it myself.
図面は本発明の方法を実施するための非分散僅党Ｘ線分
ｔＪ＋装置の侮成を示した区で、Ｘ線管ｌから任意の試
料２（−１次Ｘ線を矢印Ｚのようζ二照射し、試料２か
ら発生した各元素の螢光線を矢印νのように比例副゛数
管のようなＸ線検出器３Ｃ二入射させる。この検出器３
の出力を増幅器４で増幅して波高分析＜ｒｉ ’に加え
ることにより、検出しようとする断部の元素の特性Ｘ線
′ｆｃ選出してスケ〜う６でその強度を検出する。更に
補正回路７を介し°Ｃ上記スケーラ６の出力を表示器８
に加えることにより、検出りようとする元素の特性Ｘ
（ｉｄ強度を測定するもので、試料２の近傍シ；温度？
（’Ｋ）の検出器９と気圧Ｐ（ｙａｍＨｆ／）の検出器
１０および相対湿度デの検出器１１を設け、アナログ、
デシ゛タル変換器１Ｂを介してこれらの検出器の出力を
補正回路りに加えである。すなわち試料２で発生して検
出器３に入射する螢光Ｘ１３はその通路における空気お
よび水蒸気によって吸収を受けるが、この吸収率は温度
、気圧および湿度の夏化による空気並びに水蒸気の密度
によって変化するから１こｔｌらの検出器９ 、１０．
１１の出力に応じて、補正回路７てステープ６の出力に
補正を加えることにより、表示器８で正確な螢光Ｘ線の
強度を表示することができる◎強度工。のＸ線が物質中
を通過すると吸収を受けるから、その強度は工に減少す
るが、この場合エーエ。’”ｐ（（ｐ／ｐ）、ρ・ｔｌ
・山・・（１）但し ｐ／ＰはＸ線が通過する物質の
質量吸収係数
Ｐ は密度
Ｉ は物質のＸ浴！通過距酸
０関係が成立する。また
ｐ４−社（ｐ４）シ・−ｉ 山・自・（２）よＮ・−１
・・・・・・・（３）
Ｌ ′
但し←４）ゼ は−元素の質量段収係哉−−は各元素の
含有亭
であって、Ｘ線の通過する切質を空気とし、その空気に
含まれる水蒸気の分圧を鮨、。ｍ、ｒａＨｇとすると上
記第（２）式は
ｐ４−（／４） 紺 ＋（ｐ／ ）、皺１．・・・・・
（４）１ ａ：
帥 ｌ十、° ぺ（’ ｘ＋、゛”、、、 （１５）但
し）Ｘけ空気ＩＫ７中に含まれる水蒸気のｍｃＫｙ）と
なり、まｒｅ、絶対温度と水蒸気の分圧の関係式但し、
ＯＵ空気および水蒸気の分圧の和（全圧力）ａｆま水蒸
気と空気の分子貝の比で、０．６ｓ’ａＯを用いて１．
２−を水蒸気の分圧ＰＨ，ｏ （屏ｙａＨｙ ）で表わ
すと（５）式は
となる。かつＰ）〜＞０ ” Ｐ／／Ｐ戸” （’／Ｐ
ｋ’であるから前記（４）式は
ｐ４＝＜〜嘔ンン ・・・・・・・ （７ンとなる。更
に水蒸気全台んだ空気の密度を伶、空気のみの密度を’
ａｊｈとすると１
であるから、前記（１）式はこの（８）式およびボイル
シャールの法則から
１０必２，２）
ＴＯはｏ’ａの絶対温度（ｇｖ：ｆ′ｘ）Ｔｌｏ は７
ＱＯｍｍＴ１ｇ
となる。The drawing shows the construction of a non-dispersive marginal X-ray segment tJ+ apparatus for carrying out the method of the present invention, in which an arbitrary sample 2 (-1st order The fluorescent rays of each element generated from the sample 2 are made incident on an X-ray detector 3C2, such as a proportional submultiple tube, as shown by the arrow ν.
By amplifying the output with an amplifier 4 and adding it to the pulse height analysis <ri', a characteristic X-ray 'fc of the element in the section to be detected is selected, and its intensity is detected in a scale 6. Furthermore, the output of the °C scaler 6 is displayed on a display 8 via a correction circuit 7.
By adding the characteristic of the element to be detected
(It measures the id intensity; the temperature in the vicinity of sample 2?
('K) detector 9, atmospheric pressure P (yamHf/) detector 10, and relative humidity detector 11,
The outputs of these detectors are added to a correction circuit via a digital converter 1B. That is, the fluorescent light X13 generated in the sample 2 and incident on the detector 3 is absorbed by the air and water vapor in its path, but this absorption rate changes depending on the density of the air and water vapor due to summerization of temperature, pressure, and humidity. Detectors 9, 10.
By correcting the output of the staple tape 6 using the correction circuit 7 according to the output of the tape 11, the display 8 can display an accurate intensity of the fluorescent X-rays. When X-rays pass through a substance, they are absorbed, so their intensity decreases significantly; '”p((p/p), ρ・tl
・Mountain...(1) However, p/P is the mass absorption coefficient P of the substance through which X-rays pass, and density I is the X-bath of the substance! The passing distance relationship is 0. Also p4-sha (p4) Shi・-i Yama・Se・(2) YoN・−1
・・・・・・・・・(3) L ′ However, ← 4) Ze is the mass balance coefficient of each element. Sushi, the partial pressure of water vapor contained in the air. m, raHg, the above equation (2) is p4-(/4) navy + (p/ ), wrinkle 1.・・・・・・
(4) 1 a: x 10, ° pe('x+,゛'',,, (15) However) However, the relational expression of
OU is the sum of the partial pressures of air and water vapor (total pressure) af, which is the molecular weight ratio of water vapor and air, and is 1.0 using 0.6s'aO.
When 2- is expressed by the partial pressure of water vapor PH,o (屏yaHy), equation (5) becomes as follows. and P) ~>0 ``P//P door''('/P
Since k', the above equation (4) becomes p4 = < ~ 7 n.Furthermore, the density of air containing all the water vapor is 2, and the density of only air is 2.
Since 1 if ajh, the above equation (1) is 10 from this equation (8) and Boyleschard's law.TO is the absolute temperature of o'a (gv:f'x)Tlo is 7
QOmmT1g.
空気と水蒸気との混合気体は、こ！″Ｌを理想気体とみ
なすことができるから、水蒸気の分圧ＰＨ１ｏと相対湿
度ψとの同には
Ｐる０
ル ・・・・・・・（”Ｏ）
ラウジウスの法則から一鵜的に
ムＰ７−−−千−十”Ｃ
Ｔ
オヶゎあＰ −ｅ−灯悌
！ ・・・・・・・（１１）
但し、階はモル黒夕す熱（９，ｌユヮｌ；＜１０カロリ
奉）Ｒは気体定数（１，Ｑ８ワカロリＡ−）Ｃは定数
として定まる。This is a gas mixture of air and water vapor! Since ``L can be regarded as an ideal gas, the partial pressure of water vapor PH1o and the relative humidity ψ are the same as Pru0. P7----1000-10"C T OgawaaP-e-Light! ・・・・・・・・・(11) However, the floor is black and the heat (9,100 calories; <10 calories) ) R is a gas constant (1, Q8 Wakarori A-) C is determined as a constant.
従って（９）式に（１０）（１１１式を代入するとψで
偏分してｘ、俳強度工に対する補正量Δ工をめるど、
ｏＰ
’１−一（ｕ／Ｐシ’−ｉ−” ’ｐ−Ｊ” ｐ ’ム
ｔ −ｘとなる。すなわち基量温度Ｔ、基準気圧Ｐおよ
び基準湿度ｒと測定時（二おける温度、気圧および湿度
の差ＪＴ、ＪＰおよびΔＦ（＝応じてｘ ５強度の７（
１１定値工に上記（１３）式で与えられる補正量ΔＩを
加減することによって試料から放出された真の螢ツｌ（
、Ｘ線強度をめることができるものである。Therefore, by substituting equations (10) and (111) into equation (9), by dividing by ψ and adding the correction amount Δfactor for the force force factor, oP'1-1(u/Pshi'-i- ``'p-J''p'mut-x.In other words, the difference between base temperature T, reference pressure P, reference humidity r, and temperature, pressure, and humidity at the time of measurement (JT, JP, and ΔF (= depending on x 5 strength of 7 (
11 By adjusting the correction amount ΔI given by the above equation (13) to the constant value, the true firefly l released from the sample (
, which can increase the X-ray intensity.
例えばシリコンのＫａ ＩＮ ＜波長？、１２Ａ）を検
出する場合につき、基準状態の温度Ｔ、気圧Ｐおよび湿
Ｋ ｔ”ｉ： ソ創、 ソｔ１．２ｏ８°Ｋ （２１５
’Ｏ） 、 ７５０ ｙｂｍＦＩｙ Ｊ３ ヨヒ６ｏｓ
トシ・贅７７１．Ｘ線が空気中を通過するｌＬ！Ｐｆｆ
ｌｉｇを１．５Ｃ擲、飽和無気１１２３．７６μ篇■■
９とすると、温度の変化量ＪＴが例えば＋３°の場合の
補正量ｌ工（よ前記（１３）式より１．１憾となる。ま
た気圧の変化量ΔＰを７．６ｍ５Ｈ９とすると、これに
対する補正量は−１，３６憾となり一更にが凹の変化量
Δψを＋３０％とするｔｌこれ（二対する補正量は−０
，４９優となる。For example, Ka IN of silicon <wavelength? , 12A), the reference state temperature T, atmospheric pressure P, and humidity K t"i: Sore, Sot1.2o8°K (215
'O), 750 ybmFIy J3 Yohi 6os
Toshi Wataru 771. X-rays pass through the air! Pff
lig 1.5C, saturated airless 1123.76μ ■■
9, the correction amount when the temperature change JT is, for example, +3° is 1.1 from equation (13). Also, if the atmospheric pressure change ΔP is 7.6m5H9, then The correction amount is -1,36, and the first one makes the concave change amount Δψ +30%.
, 49 wins.
以上詳細に説明したように本発明は、例えば図１ωｇ−
示したような補止回路９を段けて、前記１３式Ｃ二もと
づく補正を行わせることにより、試料から発生して検出
器に入射する螢光Ｘ ＭＡの通路における吸収率の於動
を補償することができるー。従って気温、気圧および湿
度等の変化に関係なく正確な分析を行い得るものである
。As explained in detail above, the present invention can be applied, for example, to FIG.
By setting up the compensation circuit 9 as shown and performing the correction based on Equation 13C2, the fluctuation of the absorption rate in the path of the fluorescent light XMA generated from the sample and incident on the detector can be compensated for. You can. Therefore, accurate analysis can be performed regardless of changes in temperature, atmospheric pressure, humidity, etc.
、４、図面の簡単な説明
図面は本発明の方法を実施する装置の一例（二つきその
’５’ｓ Ｉｊ！’＋を示Ｌ ’ｔｖ ｐ；ｉである。, 4. BRIEF DESCRIPTION OF THE DRAWINGS The drawing shows an example of an apparatus for carrying out the method of the invention (two pieces of '5's Ij!'+L'tv p;i).
４お図（＝おいて、１はＸ経管、２Ｉ−、試料、３はＸ
嗣検出餡１．４ｔま増’ｆＱＩ）ン＋ｊｆｓ５は波高分
析器、６はスナーラ、７ｕ補正回路、８は表示器、９は
温度検出器、工ｏＨ気圧検出器、１１は相対湿度の検出
器である。4 Diagram (=, 1 is the X tube, 2I-, the sample, 3 is the X
5 is a wave height analyzer, 6 is a sunara, 7u correction circuit, 8 is a display, 9 is a temperature detector, an air pressure detector, 11 is a relative humidity detector It is.
Claims (1)
度Ｔ（”Ｋ）と気圧Ｆ （ｍｙ＞Ｔｌ／ ）並び区二相
対う；度ｒの検出器を設けて検出された螢光Ｘ＠の強度
工に対し、 但し、（ｐ／ ）Ａｉｔ−、はｌ気圧の空気の螢光Ｘｉ
に対する質量吸収係数 Ｔ、は＄ａ’Ｊ３ （０°Ｃの絶対温度） −ｐＨは’
１６０ ｒｒｂｍＨ＃ ｎ−Ｉｌ＋ｎＢＣ，１ｅＬＷの２！？仇密度（ｌＪ９３
×ｌｏｇ／、ｒｒＬ３） ４ はＸ線の通過距離 ｐ、Ｈ温度Ｔ（−おける飽和水蒸気圧 ａ は水蒸気と空気との分子景の比（ｏ、６ｇｇｏ）Ｌ
、は水蒸気のモル蒸発熱（９，１１）ｌ×１ｄカロ９Ｒ
は気体定数（１，９８７カロリ／ＱＫ／楚）ＡＴ は温
度Ｔと基準温度との差 ΔＦ はう鼓度ヂと基準湿度との差 ｉＰ は気圧Ｐと基準気圧との差 で与えられる補正を加えることを特徴とする螢光ｘｔ８
分析の補正方法[Claims] A detector with a temperature T (K) and an air pressure F (my>Tl/) and a degree r detector is arranged in the vicinity of a sample that emits fluorescent X-rays when irradiated with X-rays. However, (p/)Ait-, is the fluorescence Xi of air at 1 atm.
The mass absorption coefficient T, for is $a'J3 (absolute temperature of 0°C) -pH is'
160 rrbmH# n-Il+nBC, 1eLW's 2! ? Enemy Density (lJ93
×log/, rrL3) 4 is the passing distance p of X-rays, H temperature T (- saturated water vapor pressure a) is the molecular landscape ratio of water vapor and air (o, 6ggo)L
, is the molar heat of vaporization of water vapor (9,11) l x 1d Karo 9R
is the gas constant (1,987 calories/QK/Chu) AT is the difference between the temperature T and the reference temperature ΔF The difference between the crawling temperature and the reference humidity iP is the correction given by the difference between the atmospheric pressure P and the reference atmospheric pressure Fluorescent xt8 characterized by adding
How to correct the analysis
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16934983A JPS6061649A (en) | 1983-09-16 | 1983-09-16 | Correction of x-ray fluorescence analysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16934983A JPS6061649A (en) | 1983-09-16 | 1983-09-16 | Correction of x-ray fluorescence analysis |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6061649A true JPS6061649A (en) | 1985-04-09 |
Family
ID=15884916
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16934983A Pending JPS6061649A (en) | 1983-09-16 | 1983-09-16 | Correction of x-ray fluorescence analysis |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6061649A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05119000A (en) * | 1991-10-23 | 1993-05-14 | Horiba Ltd | Fluorescent x-ray analyzing device |
| US5721759A (en) * | 1994-11-14 | 1998-02-24 | Ima Engineering Ltd. Oy | Method and equipment for determining the content of an element |
| US7666490B1 (en) | 1999-02-10 | 2010-02-23 | Toyo Boseki Kabushiki Kaisha | Functional roll film and vacuum evaporation apparatus capable of producing the functional roll film |
| CN102735705A (en) * | 2011-03-16 | 2012-10-17 | 奥林巴斯Ndt公司 | Portable xrf analyzer and xrf analysis method |
| CN103197712A (en) * | 2013-01-30 | 2013-07-10 | 王建刚 | X-fluorescence weather-proof test box detection control system and control method thereof |
| CN104165871A (en) * | 2013-05-15 | 2014-11-26 | 国家***第三海洋研究所 | Calculation method for specific fluorescence intensity of high purity phycoerythrin |
| CN105092624A (en) * | 2014-05-20 | 2015-11-25 | 株式会社堀场制作所 | Analyzing apparatus and calibration method |
| JP2015219199A (en) * | 2014-05-20 | 2015-12-07 | 株式会社堀場製作所 | Analysis device and calibration method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5786030A (en) * | 1980-11-17 | 1982-05-28 | Idemitsu Kosan Co Ltd | Method and apparatus for analysis of fluorescence x-rays |
-
1983
- 1983-09-16 JP JP16934983A patent/JPS6061649A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5786030A (en) * | 1980-11-17 | 1982-05-28 | Idemitsu Kosan Co Ltd | Method and apparatus for analysis of fluorescence x-rays |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05119000A (en) * | 1991-10-23 | 1993-05-14 | Horiba Ltd | Fluorescent x-ray analyzing device |
| US5721759A (en) * | 1994-11-14 | 1998-02-24 | Ima Engineering Ltd. Oy | Method and equipment for determining the content of an element |
| US7666490B1 (en) | 1999-02-10 | 2010-02-23 | Toyo Boseki Kabushiki Kaisha | Functional roll film and vacuum evaporation apparatus capable of producing the functional roll film |
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