JPH02253145A - Standard sample for fluorescent x-ray analysis and production thereof - Google Patents
Standard sample for fluorescent x-ray analysis and production thereofInfo
- Publication number
- JPH02253145A JPH02253145A JP7456489A JP7456489A JPH02253145A JP H02253145 A JPH02253145 A JP H02253145A JP 7456489 A JP7456489 A JP 7456489A JP 7456489 A JP7456489 A JP 7456489A JP H02253145 A JPH02253145 A JP H02253145A
- Authority
- JP
- Japan
- Prior art keywords
- metal
- sample
- standard sample
- rays
- specimen
- 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
- 238000002441 X-ray diffraction Methods 0.000 title claims description 9
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 40
- 239000002184 metal Substances 0.000 claims abstract description 40
- 229920005992 thermoplastic resin Polymers 0.000 claims abstract description 6
- 150000002736 metal compounds Chemical class 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 9
- 150000004706 metal oxides Chemical class 0.000 abstract description 9
- 238000005259 measurement Methods 0.000 abstract description 8
- 238000011088 calibration curve Methods 0.000 abstract description 7
- 150000002739 metals Chemical class 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 229920013716 polyethylene resin Polymers 0.000 abstract description 2
- 230000003252 repetitive effect Effects 0.000 abstract 2
- 230000002238 attenuated effect Effects 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 239000012535 impurity Substances 0.000 description 10
- 239000012528 membrane Substances 0.000 description 5
- 238000005342 ion exchange Methods 0.000 description 4
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 238000009954 braiding Methods 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
Description
【発明の詳細な説明】
［発明の目的］
（産業上の利用分野）
本発明は、メンブレンフィルタ上に捕集された金属量を
蛍光Ｘ線分析装置を用いて定量するための検量線作成に
用いられる標準試料に関する。[Detailed Description of the Invention] [Object of the Invention] (Industrial Application Field) The present invention is directed to the preparation of a calibration curve for quantifying the amount of metal collected on a membrane filter using a fluorescent X-ray analyzer. Regarding the standard sample used.
（従来の技術）
蛍光Ｘ線分析装置は測定対象の検体にＸ線を照射し、検
体中に含まれる金属元素が励起して発生する特性Ｘ線（
蛍光Ｘ線）をフッ化リチウム（Ｌｉｄ）などの分光結晶
によって分光し、シンチレーンヨンカウンタを用いて各
々の金属元素に起因する特性Ｘ線に対応する２θでの計
数値から検体中における金属量を測定しようとするもの
である。(Prior art) A fluorescent X-ray analyzer irradiates a specimen to be measured with X-rays, and generates characteristic X-rays (
Fluorescent X-rays) are separated using a spectroscopic crystal such as lithium fluoride (Lid), and a scintillane counter is used to determine the amount of metal in the sample from the 2θ count value corresponding to the characteristic X-rays caused by each metal element. It is intended to measure the
検出感度は極めて高く、かつ測定の安全性から非常に信
頼性の高い分析機器といえる。そのため、各方面で広く
使用実績があり、近年では原子力発電プラントの各系統
の水質測定にまでその応用分野が広がっている。The detection sensitivity is extremely high, and the measurement safety makes it an extremely reliable analytical instrument. Therefore, it has been widely used in various fields, and in recent years, its field of application has expanded to include water quality measurement in various systems of nuclear power plants.
一般に原子力発電所では、各系統の水質が基準を満足し
ていることを確認するため、および水質管理の目的で常
時金属不純物の濃度が監視されており、この金属不純物
濃度の測定の際に上記蛍光Ｘ線分析装置か用いられてい
る。例えば沸騰水型原子力発電所においては、各系統水
中の金属不純物濃度は極めて低く、直接水中の金属不純
物量を定量することはできないため、系統水を取出して
必要に応じて冷却、減圧し、第２図に示すようなユニッ
ト式サンプラー１内に導入して、高圧ホルダ２内に装着
されている４７ｍｍφのメンブレンフィルタで金属不純
物を捕集し、これを測定することによって水中の金属不
純物濃度を監視している。Generally, at nuclear power plants, the concentration of metal impurities is constantly monitored to confirm that the water quality in each system satisfies standards and for water quality management purposes, and when measuring the concentration of metal impurities, the A fluorescent X-ray analyzer is used. For example, in boiling water nuclear power plants, the concentration of metal impurities in each system water is extremely low, and it is not possible to directly quantify the amount of metal impurities in the water. Therefore, the system water is extracted, cooled and depressurized as necessary, and then The water is introduced into a unit type sampler 1 as shown in Figure 2, and metal impurities are collected with a 47 mm diameter membrane filter installed in a high pressure holder 2, and the metal impurity concentration in water is monitored by measuring this. are doing.
図中、サンプラー１内においてサンプル水の流れる配管
はバイパスライン３とサンプリングライン４に分岐され
ており、バイパスライン３には流量調整用のニードル弁
５と流量計６が、サンプリングライン４にはニードル弁
７、メンブレンフィルタを装着した高圧ホルダ２、流量
計８および積算流量計９などが設置されている。サンプ
リングライン４においてはメンブレンフィルタの性能に
よって流量が設定される。このメンブレンフィルタとし
て、粒子状の金属不純物を捕集するための、例えばフィ
ルタ孔径が０．４５μｍのセルロース系のフィルタ、お
よびイオン状の金属不純物を捕集するためのアクロボア
イオン交換フィルタ（フィルタ両面にイオン交換樹脂を
付、与したもの）またはイオン交換ろ紙（イオン交換繊
維を編みこんでフィルタ状に加工したもの）等が高圧ホ
ルダ２内に装着されている。これらの各フィルタは所定
量の系統水を通過させた後に取出され、乾燥後に蛍光Ｘ
線分析装置にかけられる。このとき、フィルタの通水量
は積算流量計によって正確に７１１１１定される。In the figure, the piping through which the sample water flows in the sampler 1 is branched into a bypass line 3 and a sampling line 4.The bypass line 3 is equipped with a needle valve 5 for adjusting the flow rate and a flow meter 6, and the sampling line 4 is equipped with a needle valve 5 and a flow meter 6. A valve 7, a high pressure holder 2 equipped with a membrane filter, a flow meter 8, an integrated flow meter 9, and the like are installed. In the sampling line 4, the flow rate is set depending on the performance of the membrane filter. These membrane filters include, for example, a cellulose-based filter with a filter pore diameter of 0.45 μm to collect particulate metal impurities, and an acrobore ion exchange filter (filter double-sided) to collect ionic metal impurities. The high-pressure holder 2 is equipped with an ion-exchange filter paper (with an ion-exchange resin applied thereto) or an ion-exchange filter paper (a filter-like filter made by braiding ion-exchange fibers). Each of these filters is taken out after passing a predetermined amount of system water, and after drying, fluorescent
It is subjected to a line analyzer. At this time, the amount of water flowing through the filter is accurately determined by the integrated flow meter.
ところで、シンチレーションカウンタの計数値から金属
量を求めるには、通常既知量の金属を含有する標準試料
を各濃度で測定することによってで得られる検量線を用
いて換算される。従来用いられてきた標準試料は、既知
量の金属もしくは金属酸化物を口過操作によってフィル
タ上に固着させたもので、例えば次のような方法で製造
される。By the way, in order to obtain the amount of metal from the count value of a scintillation counter, conversion is usually performed using a calibration curve obtained by measuring a standard sample containing a known amount of metal at each concentration. A conventionally used standard sample is one in which a known amount of metal or metal oxide is fixed on a filter by a filtering operation, and is manufactured, for example, by the following method.
ます、測定対象とする金属もしくは金属酸化物を微粉砕
し、これを秤量して一定の純水中に入れ、超音波にて均
一に分散させた標準液を調製した後、この標準液から目
標濃度に応じてピペット等を用いて所定量の溶液を分取
して口過器にセットしたフィルタ上に捕集させ乾燥し、
これを標準試料とするものである。またこの上に、金属
もしくは金属酸化物のフィルタからの剥離防止を目的に
高分子膜スプレーを塗布する場合もある。このような標
準試料を金属濃度を違えて数種類作成し、蛍光Ｘ線分析
装置によって計数して計数値から金属量に換算する検量
線を作成してきた。First, a standard solution is prepared by finely pulverizing the metal or metal oxide to be measured, weighing it, placing it in a certain amount of pure water, and uniformly dispersing it using ultrasonic waves. Depending on the concentration, a predetermined amount of solution is taken out using a pipette, etc., collected on a filter set in a mouth filter, and dried.
This will be used as a standard sample. Moreover, a polymer film spray may be applied thereon for the purpose of preventing the metal or metal oxide from peeling off from the filter. Several types of such standard samples with different metal concentrations have been prepared, counted using a fluorescent X-ray analyzer, and a calibration curve for converting the counted values into metal amounts has been created.
（発明が解決しようとする課題）
しかしながら、上記検量線は定期的にチエツクし作成し
直さなければならないが、従来の標準試料は時間ととも
に固着させた金属もしくは金属酸化物の剥離を生じ、標
準試料の機能を果たせなくなることが多く、そのたびに
標準試料を製造し直さなければならなかった。(Problem to be Solved by the Invention) However, the above-mentioned calibration curve must be periodically checked and re-created, but with conventional standard samples, fixed metals or metal oxides peel off over time. The standard sample often failed to perform its function, and the standard sample had to be remanufactured each time.
本発明はかかる点に対処してなされたもので、時間とと
もに剥離等の劣化を生ずることなく、繰返し使用するこ
とかできる蛍光Ｘ線分析用標準試料およびその製造方法
を提供することを目的とする。The present invention has been made in response to these problems, and aims to provide a standard sample for fluorescent X-ray analysis that can be used repeatedly without deterioration such as peeling over time, and a method for producing the same. .
［発明の構成］
（課題を解決するための手段）
すなわち、本発明の蛍光Ｘ線分析用標準試料は、Ｘ線の
吸収が少ない熱可塑性樹脂中に所定量の測定対象となる
金属もしくは金属化合物を均一に分散させ、これを所定
の形状に形成したものである。[Structure of the Invention] (Means for Solving the Problems) That is, the standard sample for fluorescent X-ray analysis of the present invention includes a predetermined amount of the metal or metal compound to be measured in a thermoplastic resin that absorbs little X-rays. is uniformly dispersed and formed into a predetermined shape.
また、その製造方法は、Ｘ線の吸収が少ない熱可塑性樹
脂と所定量の測定対象の金属もしくは金属化合物を加熱
混練し、板状に形成した後、これを加熱圧延して薄いシ
ート状に加工し所定のフィルタ形状に切断するというも
のである。The manufacturing method involves heating and kneading a thermoplastic resin that absorbs little X-rays and a predetermined amount of the metal or metal compound to be measured, forming it into a plate shape, and then hot rolling it into a thin sheet. The filter is then cut into a predetermined filter shape.
本発明においては、熱可塑性樹脂中に金属もしくは金属
化合物が均一に分散されていれば良いわけであるが、通
常は金属酸化物か用いられる。In the present invention, it is sufficient that the metal or metal compound is uniformly dispersed in the thermoplastic resin, but usually a metal oxide is used.
（作 用）
本発明の標準試料は、樹脂シート中に所定の金属か金属
酸化物等の形で均一に分散されているため、剥離なとを
生しることなく常に一定の金属量を示すことができ、繰
返し使用することができる。(Function) Since the standard sample of the present invention is uniformly dispersed in the form of a predetermined metal or metal oxide in the resin sheet, it always shows a constant amount of metal without peeling. and can be used repeatedly.
（実施例） 以下、本発明の実施例について説明する。(Example) Examples of the present invention will be described below.
測定対象とする金属の酸化物を十分に微粉砕し、これを
正確に秤量した後、一定量のポリエチレン系樹脂に添加
し、これを１５０ ℃に加熱しながら金属酸化物が均一
に分散するように十分に混練し板状として取出した。さ
らに、この樹脂板を１７０ ’Ｃの温度で２００ｋｇ／
ｃｔｌの圧力で薄いシート状に圧延加工した後、測定試
料であるフィルタ形状に切出して本発明の蛍光Ｘ線分析
用標準試料が得られた。After thoroughly pulverizing the oxide of the metal to be measured and accurately weighing it, it is added to a certain amount of polyethylene resin and heated to 150 °C so that the metal oxide is uniformly dispersed. The mixture was thoroughly kneaded and taken out as a plate. Furthermore, this resin plate was heated to 200 kg/kg at a temperature of 170'C.
After rolling it into a thin sheet at a pressure of ctl, it was cut into a filter shape as a measurement sample to obtain a standard sample for fluorescent X-ray analysis of the present invention.
このようにして得られた蛍光Ｘ線分析用標準試料を用い
て、第１図に示すような蛍光Ｘ線分析装置により計数値
と金属量との関係をグラフにした検量線を求めたところ
、樹脂シート中に均一に金属酸化物が含まれているため
、常に一定の金属量を示すことができ、繰返しの使用に
耐えることができた。Using the standard sample for fluorescent X-ray analysis obtained in this way, a calibration curve was obtained using a fluorescent X-ray analyzer as shown in Fig. 1, which is a graph of the relationship between the count value and the amount of metal. Since the metal oxide was uniformly contained in the resin sheet, a constant amount of metal was always present, and it was able to withstand repeated use.
なお第１図において、符号１１はＸ線源であり、このＸ
線源１１からＸ線が測定試料または標準試料の検体１２
に照射される。通常、検体１２は測定中回転され、金属
不純物を捕集したフィルタ等の測定試料における金属分
布の不均一が補正される。Ｘ線が照射されると、検体１
２に含まれている金属を特徴とする特性Ｘ線（蛍光線）
が放出され、放出された特性Ｘ線は必要に応じてスリッ
ト１３によってその強度か減じられた後、分光結晶１４
によって波長分散され、各波長に対応する２θ間をスキ
ャンするシンチレーションカウンタユ５によって計数さ
れるようになっている。金属量が未知の測定試料では、
この計数値から金属量への換算に予め作成しておいた検
量線が用いられる。In FIG. 1, reference numeral 11 is an X-ray source, and this
X-rays are emitted from the radiation source 11 to the sample 12, which is a measurement sample or a standard sample.
is irradiated. Normally, the specimen 12 is rotated during the measurement, and non-uniformity in metal distribution in the measurement sample, such as a filter that collects metal impurities, is corrected. When X-rays are irradiated, specimen 1
Characteristic X-rays (fluorescent rays) characterized by the metals contained in 2.
is emitted, and the emitted characteristic
The wavelength is dispersed by the scintillation counter 5 which scans the 2θ range corresponding to each wavelength. For measurement samples with unknown metal content,
A calibration curve prepared in advance is used to convert this count value into a metal amount.
［発明の効果コ
以上の説明からも明らかなように、本発明の蛍光Ｘ線分
析用標準試料は、従来の標準試料における剥離等の問題
を生ずることなく、繰返し使用することかできる。その
結果、毎回標準試料を作り直す必要がなく手間が省ける
とともに、標準試料製造時の誤差の発生を防止すること
ができる。また、常に同じ標準試料を使用することがで
きるため、経時変化を監視して装置自体の異常を早期に
発見することができる。[Effects of the Invention] As is clear from the above description, the standard sample for fluorescent X-ray analysis of the present invention can be used repeatedly without causing problems such as peeling that occur in conventional standard samples. As a result, it is not necessary to recreate the standard sample each time, which saves time and effort, and it is possible to prevent errors from occurring during the production of the standard sample. Furthermore, since the same standard sample can always be used, changes over time can be monitored and abnormalities in the device itself can be discovered at an early stage.
第１図は本発明の標準試料を適用する蛍光Ｘ線分析装置
の構成を示す説明図、第２図は沸騰水型原子力発電所の
各系統水中の金属不純物を捕集するためのサンプラーの
配管系統図である。
１１・・・・・・・・・・・・Ｘ線源
１２・・・・・・・・・・・検体
１３・・・・・・・・・・・・スリット１４・・・・・
・・・・・・・分光結晶１５・・・・・・・・・・・・
シンチレーションカウンタ出願人 日本原子
カ事業株式会社出願人 株式会社 東 芝Figure 1 is an explanatory diagram showing the configuration of a fluorescent X-ray analyzer to which the standard sample of the present invention is applied, and Figure 2 is the piping of a sampler for collecting metal impurities in water from each system of a boiling water nuclear power plant. It is a system diagram. 11......X-ray source 12......Specimen 13...Slit 14...
・・・・・・Spectral crystal 15・・・・・・・・・・・・
Scintillation counter applicant: Japan Atomic Energy Corporation Applicant: Toshiba Corporation
Claims (2)
定対象の金属もしくは金属化合物を均一に分散させ所定
の形状に形成してなることを特徴とする蛍光Ｘ線分析用
標準試料。(1) A standard sample for fluorescent X-ray analysis, characterized in that a predetermined amount of a metal or metal compound to be measured is uniformly dispersed in a thermoplastic resin that absorbs little X-rays and formed into a predetermined shape.
対象の金属もしくは金属化合物を加熱混練し板状に形成
した後、これを加熱圧延して薄いシート状に加工し所定
のフィルタ形状に切断することを特徴とする蛍光Ｘ線分
析用標準試料の製造方法。(2) A thermoplastic resin that absorbs little X-rays and a predetermined amount of the metal or metal compound to be measured are heated and kneaded to form a plate, and then heated and rolled to form a thin sheet into a predetermined filter shape. 1. A method for producing a standard sample for fluorescent X-ray analysis, the method comprising cutting a standard sample for fluorescent X-ray analysis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7456489A JPH02253145A (en) | 1989-03-27 | 1989-03-27 | Standard sample for fluorescent x-ray analysis and production thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7456489A JPH02253145A (en) | 1989-03-27 | 1989-03-27 | Standard sample for fluorescent x-ray analysis and production thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02253145A true JPH02253145A (en) | 1990-10-11 |
Family
ID=13550840
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7456489A Pending JPH02253145A (en) | 1989-03-27 | 1989-03-27 | Standard sample for fluorescent x-ray analysis and production thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02253145A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008089441A (en) * | 2006-10-03 | 2008-04-17 | Natl Inst Of Radiological Sciences | Assay standard and method for producing the same |
-
1989
- 1989-03-27 JP JP7456489A patent/JPH02253145A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008089441A (en) * | 2006-10-03 | 2008-04-17 | Natl Inst Of Radiological Sciences | Assay standard and method for producing the same |
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