JPS5963568A - Rotary sample head for charging preheated sample in quantitative determination device for hydrogen in steel - Google Patents
Rotary sample head for charging preheated sample in quantitative determination device for hydrogen in steelInfo
- Publication number
- JPS5963568A JPS5963568A JP57174195A JP17419582A JPS5963568A JP S5963568 A JPS5963568 A JP S5963568A JP 57174195 A JP57174195 A JP 57174195A JP 17419582 A JP17419582 A JP 17419582A JP S5963568 A JPS5963568 A JP S5963568A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- gas
- tube
- head
- pipe
- 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
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 title claims description 3
- 239000001257 hydrogen Substances 0.000 title claims description 3
- 229910000831 Steel Inorganic materials 0.000 title 1
- 239000010959 steel Substances 0.000 title 1
- 239000010453 quartz Substances 0.000 claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 230000008018 melting Effects 0.000 claims abstract description 14
- 238000002844 melting Methods 0.000 claims abstract description 14
- 238000010926 purge Methods 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims description 23
- 239000011261 inert gas Substances 0.000 claims description 2
- 238000012802 pre-warming Methods 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 10
- 239000010439 graphite Substances 0.000 abstract description 8
- 229910002804 graphite Inorganic materials 0.000 abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- 230000002159 abnormal effect Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract 2
- 238000005096 rolling process Methods 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 230000005856 abnormality Effects 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/20—Metals
- G01N33/202—Constituents thereof
- G01N33/2022—Non-metallic constituents
- G01N33/2025—Gaseous constituents
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は、金属及び鉱物中のガス分析を行う装置に関す
るものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an apparatus for analyzing gases in metals and minerals.
金相及び鉱物中のガス定量を行う場合には、加温、加熱
あるいは融解により分離、発生させた被測定ガスは、通
常不活性ガスにより被測定部へ搬送さイ１．１Ｙｌｌｌ
定され７１゜ ガス発生部へ七ン入されろ試料ζこは大
気中に含：ｌ：れる各秤ガスチ１１あるいは水分がイー
１着、（（・］Ｉ伴してくることは避けられｆｊ（１）
。そこで、これらをトｉ去するためｌこパージを行って
いる。When quantifying gases in gold phases and minerals, the gas to be measured separated and generated by heating, heating, or melting is usually transported to the part to be measured using an inert gas.
71° The sample ζ should be introduced into the gas generating section, so that each weighing gas or moisture contained in the atmosphere should be avoided. (1)
. Therefore, a purge is performed to remove these substances.
これには、パージ１１作な１ちびに徂Ｉｆ ７ｐ Ｒｆ
ｌとのイ色縁を図るために考案された各種ローリングヘ
ッドが多用されてい２）。This includes the 11th Purge series, If 7p Rf
A variety of rolling heads designed to create an A-color edge with the L are widely used2).
また、試料のｌ；ｔ’！！解を行うためには、１０００
℃以上の高温が（■られ、る炭素抵抗加ｔ゛〜あるいは
高周波加熱が用いられ、発熱体、試料容器を兼ねた熱鉛
ルツボが使用されている。Also, l;t'! of the sample. ! In order to solve the problem, 1000
Carbon resistance heating or high-frequency heating is used, and a hot lead crucible that also serves as a heating element and a sample container is used.
分析試月が多孔質あるいはクラックホールのあるような
場合Ｉこは、試料採取、イ〒存、ハ１１製時にこれらに
侵入、残存した水あるいは汀供物が黒り１）ルツボの赤
熱時ｌこ炭素水性化反応ζこより水素が発生するこ乏が
知らイ］ており、これがガス分析時に異常値を生む原因
となっている。If the sample for analysis is porous or has crack holes, the remaining water or sediment that entered the sample during sample collection, preservation, and production may turn black.1) When the crucible is red-hot, It is known that there is a lack of hydrogen generation from the carbon aqueous reaction ζ, and this is the cause of abnormal values during gas analysis.
不発明の目的は、上述しｆこようなＪｊス分析時に異常
（直を生むことのないように＜’：Ｉ １’Ｑ Ｌ／た
ロータリー・サンプルヘッドを提供しようとするにある
。The object of the invention is to provide a rotary sample head that does not cause abnormalities during the above-mentioned Jj analysis.
不発明においては、この対策として、試料を黒鉛ルツボ
により高温融解する以前ζこ、３００℃程度で加熱を行
い、発生する水あるいは有機物をカラムで捕捉させ、こ
の後に黒鉛ルツボへ移動させて加熱融解させることによ
り、異常値の発生を防止する。本発明では、３００℃程
度の加熱には石英管中の試料を間接加熱し、被測定ガス
、水、有機物を発生、分離させ、次に石英管を傾動させ
ることにより、金鵬蛇管部を介して高温融解部へ導入さ
せていたものを、金ハ蛇管の屈折疲労による破損ならび
壷こローリングヘッド部分の摩耗によるガス漏れが多発
することから、金再蛇管部およびローリングヘッド部を
まとめてロータリーヘッド試料投入器を完成した。As a countermeasure for this, in the present invention, before the sample is melted at a high temperature in a graphite crucible, it is heated at about 300°C, the generated water or organic matter is captured in a column, and then the sample is transferred to a graphite crucible and heated and melted. This prevents abnormal values from occurring. In the present invention, the sample in the quartz tube is indirectly heated to generate and separate the gas, water, and organic matter to be measured, and then the sample is heated to about 300°C by tilting the quartz tube. The sample was introduced into the high-temperature melting section, but the gold coiled tube and rolling head were often damaged due to bending fatigue and gas leaked due to abrasion of the rolling head, so the gold coiled tube and rolling head were combined into a rotary head sample. Completed the injector.
以下、不発明の鋼中水素定量装置におけるロータリー・
サンプルヘッドを添付図面につき詳絽に説明する。Below, the rotary and
The sample head will be described in detail with reference to the accompanying drawings.
本発明のロータリーヘッドは、互いに気密状態で嵌め合
せることができる固定ヘッド部１および回転ヘッド部２
を具え、両ヘッド部の回転角度に応じて、ガス切換えを
行うｔ！！！’１７９と、試料の方向転換および投下を
・行わ１ｔろｔｒ々措を有する。The rotary head of the present invention has a fixed head part 1 and a rotary head part 2 that can be fitted together in an airtight state.
The gas is switched according to the rotation angle of both heads. ! ! '179, and has a 1 t capacity for redirecting and dropping samples.
固定ヘッド部１の借造をｒＰ、１図１こ示す。固定ヘッ
ド部１には、後述する高温融解部に接して試料投下用バ
イブａが設けられ、側面にはパージガス、低温加熱操作
ガスをカラムへ導くバイブｂが取付けられている。内部
には、パージガスをカラムへ導く開口Ｃおよび低温加熱
発生ガスをカラムへ導く開口ｄが設けられており、両開
■コは結合されてバイブｂに接糾されている。まに、下
部の開口ｅは試料の高温融解部への投入口である。次１
こ述べる回転ヘッド部との接触面は斜面（ｊ： ｌげさ
れ、回転接触部３はＯリング４によるシールが行イ）れ
ている。The fixed head part 1 is shown in FIG. The fixed head section 1 is provided with a sample dropping vibrator a in contact with a high temperature melting section which will be described later, and a vibrator b for guiding purge gas and low temperature heating operation gas to the column is attached to the side surface. Inside, an opening C for guiding purge gas to the column and an opening d for guiding gas generated by low temperature heating to the column are provided, and both the openings 1 and 2 are connected and attached to a vibrator b. The opening e at the bottom is the inlet for introducing the sample into the high-temperature melting section. Next 1
The contact surface with the rotating head portion mentioned above is sloped (j: l), and the rotating contact portion 3 is sealed with an O-ring 4.
第２図に示す回転ヘッド部２は、嵌合取付部５により固
定ヘッド部ｌの接触取付部３に取付けられ、土俯には低
温加熱用石英管ｆおよびこれに続く接続管ｇを有する。The rotating head part 2 shown in FIG. 2 is attached to the contact attachment part 3 of the fixed head part l by a fitting attachment part 5, and has a quartz tube f for low-temperature heating and a connecting tube g following it on the dome.
下端番こは接続管ｇに連なるガスおよび試料の通過口り
が形成されている。A gas and sample passage opening connected to the connecting tube g is formed at the lower end.
上述した固定ヘッド部１および回転ヘッド部２は嵌め合
され、ロータリーヘッドの中心を軸として、石英管ｆが
水平位置より垂直位置まで９０°の回転様能を有する。The fixed head section 1 and the rotary head section 2 described above are fitted together, and the quartz tube f has the ability to rotate through 90 degrees from a horizontal position to a vertical position about the center of the rotary head.
次に、不発明によるロータリーヘラ、ドの動作を第３図
ないしεＢ８図を参照しつつ簡単（こ説明する。Next, the operation of the rotary spatula according to the invention will be briefly explained with reference to FIGS. 3 to εB8.
（１） パージ操作（第３図および第４図参照）石英
管部ｆを水平にして試料をへの位置に挿入し、キャリヤ
ーガスとしてＡｒガスを通し。(1) Purge operation (see Figures 3 and 4) Hold the quartz tube part f horizontally, insert the sample into the position, and pass Ar gas as a carrier gas.
試料および装置内空気のパージを行う。粉状試料につい
てはアルミ箔で包装して訓電に供する。第３図および第
４図に示すように、ガスは石英管ｆ１接続管ｇを通り、
通過口りより開口Ｃ１パイプｂを経てカラム６を通過し
、高ｍ融解部７へ導入され、黒鉛ルツボ８の脱ガスに供
され、大気中へ放散される。Purge the sample and the air inside the device. Powdered samples should be wrapped in aluminum foil and used for training purposes. As shown in FIGS. 3 and 4, the gas passes through the quartz tube f1 connecting tube g,
It passes through the column 6 through the opening C1 pipe b from the passage port, is introduced into the high m melting section 7, is subjected to degassing of the graphite crucible 8, and is dissipated into the atmosphere.
０） 低温加熱操作（第５図および第６図参照）石英管
ｆを約３０°Ｍ動させ、試料をＢの位置へ移動させ、ヒ
ーターｌにより３００℃程度に加熱する。これにより発
生するガスは、第５図および第６図に示すように、石英
管ｆ、接続管ｇを通り、通過口りより開口ｄ、バイブｂ
を経てカラム６に導入され、水、有機物管が吸着除去さ
れ、被測定ガスのみが融解部７を辿り測定部で定量゛さ
れる。0) Low-temperature heating operation (see Figures 5 and 6) Move the quartz tube f by about 30°C, move the sample to position B, and heat it to about 300°C with heater l. As shown in FIGS. 5 and 6, the gas generated by this passes through the quartz tube f and the connecting tube g, and from the passage opening to the opening d and the vibrator b.
The gas is introduced into a column 6 through which water and organic substances are adsorbed and removed, and only the gas to be measured follows the melting section 7 and is quantified in the measuring section.
（３）高＠融解部投入（第７図セよび第８図参照）石英
Ｗｆを垂直位置まで傾動させ、第７図および第８図に示
すように、試料をＢ位置より石英管ｆ、接続管ｇを通り
、逼遇口りおよび投下口ｅよりパイプ＆を通って高温１
４１部７の黒鉛ルツボ８中へ投入し、石英管ｆを水平位
置まで復帰後試料の高温融解を行５つ。キャリヤーガス
Ａ１は石英管ｆ、接続管ｇ、開口Ｃ、パイプｂを通り、
カラム６を通過して高ｍ融解部７に入り、試料の列理融
解により分離、発生した被測定ガスとともに測定部へ至
り、被測定ガスのみが定量される。(3) Insertion into the high melting section (see Figures 7 and 8) Tilt the quartz Wf to the vertical position, and connect the sample to the quartz tube f from position B as shown in Figures 7 and 8. The high temperature 1 passes through the pipe g, passes through the reception opening and the outlet e, and passes through the pipe &.
The sample was placed in the graphite crucible 8 of Section 41, and after returning the quartz tube f to the horizontal position, the sample was melted at a high temperature. The carrier gas A1 passes through the quartz tube f, the connecting tube g, the opening C, and the pipe b.
The sample passes through the column 6 and enters the high m melting section 7, where it is separated by columnar melting of the sample, and reaches the measurement section along with the generated gas to be measured, where only the gas to be measured is quantified.
第１ （ａ）図およびＦＰ、１ （ｈ）図はそれぞれ本
発明のロータリーヘッドの固定ヘッド部の正面図および
側面図、第２（〜図および第２（ｂ）図はそれぞれ本発
明のロータリーヘッドの回転ヘッド部の正面図および仰
１面口１、第３図および第４１図は本発明のロークリ−
ヘッドのパージｔ′ψ作時／Ｉ、Ｔ ｉｌＱ與１を示Ｔ
線図、第５図および第６Ｍは本発明のロータリーヘッド
のｆｌけ＾加熱↑：ｆ ｆＥ時の１＾ｐｊ１を示ず両図
、第７図および第８図は本発明のロータリーヘッドの高
温部カイ操作時の状ＶｉＵ ’ｚ２示１−縮図である。
符号の説明
１・・・固定ヘッド部、２・・・トコ１転ヘッド部、３
・・・回転接触部、４・・・０リング、５・・・嵌合部
、６・・・カラム、７・・・高温融解部、８・・・黒鉛
ルツボ、ａ・・・試料投下用パイプ、■）・・・カスパ
イプ、Ｃ・・・パージガス導入口、ｄ・・・発生カス導
入口、ｅ・・・試料投入口、ｆ・・・石英管、ｇ・・・
試料導入パイプ、１１・・・通過１コ、ｉ・・・ヒータ
ー
／Ｉ′ｆ−許出門人 川崎製鉄株式会社第１凹
鴇２図
第３図
第４図Figures 1(a) and FP and 1(h) are respectively a front view and a side view of the fixed head portion of the rotary head of the present invention, and Figures 2(-) and 2(b) are respectively the front view and side view of the fixed head portion of the rotary head of the present invention. The front view of the rotary head portion of the head and the vertical opening 1, FIG. 3, and FIG.
When the head is purged t′ψ/I, TilQ與1 is shown.
The diagrams, FIGS. 5 and 6M, do not show the 1^pj1 at fE of the rotary head of the present invention. Fig. 1 is a miniature diagram showing the state of ViU'z2 during operation. Explanation of symbols 1...Fixed head part, 2...Toko one-turn head part, 3
・・・Rotating contact part, 4...0 ring, 5... Fitting part, 6... Column, 7... High temperature melting part, 8... Graphite crucible, a... For sample dropping Pipe, ■)... Waste pipe, C... Purge gas inlet, d... Generated waste inlet, e... Sample inlet, f... Quartz tube, g...
Sample introduction pipe, 11... 1 passage, i... Heater/I'f-Kawasaki Steel Co., Ltd. 1st hole 2 Fig. 3 Fig. 4
Claims (1)
性ガスおよび試料を送給する管を取り付けるとともに試
料投下口を設けた回転自在な回転ヘッド部と、パージ動
作時および低温加熱時にガスをカラムに導入するガス導
入口および低温加熱後の試４パ１を高温融解部に送給す
る試料＋ｒＴ１過日を有する＋ｉ＜１定ヘッド部とを具
えることを特徴とする鋼中水素定惜装［ｊｌにおける予
備加温試料投入用ロータリー・サンプルヘッド。An inert gas tube has a quartz tube section that temporarily holds the sample and heats it at a low temperature, and a rotatable rotating head section that is equipped with a tube for feeding the sample and a sample drop-in port, and a quartz tube section that supplies gas during purge operations and low-temperature heating. A gas inlet for introducing hydrogen into a column and a head section having a +i < 1 constant temperature for feeding the sample after low-temperature heating to a high-temperature melting section. Rotary sample head for pre-warming sample input in JL equipment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57174195A JPS5963568A (en) | 1982-10-04 | 1982-10-04 | Rotary sample head for charging preheated sample in quantitative determination device for hydrogen in steel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57174195A JPS5963568A (en) | 1982-10-04 | 1982-10-04 | Rotary sample head for charging preheated sample in quantitative determination device for hydrogen in steel |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS5963568A true JPS5963568A (en) | 1984-04-11 |
Family
ID=15974381
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP57174195A Pending JPS5963568A (en) | 1982-10-04 | 1982-10-04 | Rotary sample head for charging preheated sample in quantitative determination device for hydrogen in steel |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5963568A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6282355A (en) * | 1985-10-07 | 1987-04-15 | Kawatetsu Techno Res Kk | Preliminary heater to be used for analyzing hydrogen and carbon in steel |
| WO2025115509A1 (en) * | 2023-11-30 | 2025-06-05 | 株式会社堀場製作所 | Sample carrier and sample analysis system |
-
1982
- 1982-10-04 JP JP57174195A patent/JPS5963568A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6282355A (en) * | 1985-10-07 | 1987-04-15 | Kawatetsu Techno Res Kk | Preliminary heater to be used for analyzing hydrogen and carbon in steel |
| WO2025115509A1 (en) * | 2023-11-30 | 2025-06-05 | 株式会社堀場製作所 | Sample carrier and sample analysis system |
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