JPH0228539A - High-purity gaseous acetylene composition for atomic absorption and atomic emission analysis - Google Patents
High-purity gaseous acetylene composition for atomic absorption and atomic emission analysisInfo
- Publication number
- JPH0228539A JPH0228539A JP17798788A JP17798788A JPH0228539A JP H0228539 A JPH0228539 A JP H0228539A JP 17798788 A JP17798788 A JP 17798788A JP 17798788 A JP17798788 A JP 17798788A JP H0228539 A JPH0228539 A JP H0228539A
- Authority
- JP
- Japan
- Prior art keywords
- acetylene
- acetylene gas
- atomic
- purity
- atomic absorption
- 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
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 title claims abstract description 78
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 20
- 238000004458 analytical method Methods 0.000 title claims abstract description 14
- 239000000203 mixture Substances 0.000 title claims description 9
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 14
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 125000004432 carbon atom Chemical group C* 0.000 claims description 9
- 150000003018 phosphorus compounds Chemical class 0.000 claims description 7
- 150000003568 thioethers Chemical class 0.000 claims description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- 229910021536 Zeolite Inorganic materials 0.000 claims description 5
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 5
- 239000011148 porous material Substances 0.000 claims description 5
- 239000010457 zeolite Substances 0.000 claims description 5
- -1 Phosphorus compound Chemical class 0.000 claims description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 239000011574 phosphorus Substances 0.000 claims description 4
- 239000013042 solid detergent Substances 0.000 claims description 4
- 239000000945 filler Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000004020 luminiscence type Methods 0.000 claims 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 abstract description 8
- 239000012535 impurity Substances 0.000 abstract description 6
- 230000035945 sensitivity Effects 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 230000001629 suppression Effects 0.000 abstract description 5
- 239000004215 Carbon black (E152) Substances 0.000 abstract description 3
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 abstract 2
- 239000007789 gas Substances 0.000 description 45
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 9
- 238000001636 atomic emission spectroscopy Methods 0.000 description 9
- 238000005259 measurement Methods 0.000 description 8
- 229910052712 strontium Inorganic materials 0.000 description 8
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 7
- 239000011575 calcium Substances 0.000 description 7
- 229910052791 calcium Inorganic materials 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 229910052750 molybdenum Inorganic materials 0.000 description 6
- 239000011733 molybdenum Substances 0.000 description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- 229910052744 lithium Inorganic materials 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 4
- 230000004913 activation Effects 0.000 description 4
- 229910052700 potassium Inorganic materials 0.000 description 4
- 239000011591 potassium Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、原子吸光、原子発光分析を、高感度、かつ、
高精度で行うことのできる高純度アセチレンガス組成物
に関するものである。[Detailed Description of the Invention] [Industrial Application Field] The present invention provides atomic absorption and atomic emission spectroscopy with high sensitivity and
The present invention relates to a high-purity acetylene gas composition that can be prepared with high precision.
〔従来の技術及び発明が解決すべき課題〕従来、溶解ア
セチレン（容器に多孔質充填剤を充填し、これに例えば
アセトン等のアセチレンガスの吸収能力の高い溶剤を含
浸させてアセチレンガスを溶解させたもの）は、溶接及
び溶断を主なる目的として製造されており、本発明者ら
の測定によれば、溶解アセチレンより放出されるアセチ
レンガスはその純度が９６，０％以下であり、アセチレ
ンガス中のリン化合物が１０ｐｐｍ以上、硫化物が２５
０ｐｐｍ以上、炭素数３以上の炭化水素が６００ｐｐｍ
以上であり、しかも、これら不純物濃度は、アセチレン
ガスの放出に伴い経時変化することが判明した。又、ア
セトンＧ、１ｍ 関シＴ ハ、「高圧Ｊｆ ス、ＶＯ，
Ｌ、１７． Ｎｏ、１０ 。[Prior art and problems to be solved by the invention] Conventionally, dissolved acetylene (a container is filled with a porous filler and impregnated with a solvent having a high ability to absorb acetylene gas, such as acetone) to dissolve acetylene gas. are manufactured primarily for the purpose of welding and fusing.According to measurements by the present inventors, the purity of the acetylene gas released from dissolved acetylene is 96.0% or less; The phosphorus compounds in it are 10 ppm or more, and the sulfides are 25
0ppm or more, hydrocarbons with carbon number of 3 or more are 600ppm
Moreover, it has been found that the concentration of these impurities changes over time as acetylene gas is released. Also, acetone G, 1m Kanshi T, ``High pressure Jf, VO,
L, 17. No. 10.
（１９８０） ： ５０１−５０３Ｐ、 Ｊに記載され
ているごとく、アセトン浸潤多孔物質を内蔵する容器に
充填された溶解アセチレンより放出されるアセチレンガ
ス中のアセトン蒸気含有量は、容器の残圧が低くなると
１０％以上にも達することが知られている。(1980): 501-503P, J, the acetone vapor content in the acetylene gas released from dissolved acetylene filled in a container containing an acetone-infiltrated porous material is determined by the amount of acetone vapor contained in the acetylene gas when the residual pressure in the container is low. It is known that it reaches 10% or more.
溶接及び溶断用として使用する場合、従来の溶解アセチ
レンでも使用できたが、原子吸光、原子発光分析に用い
た場合、アセチレンガス中に含まれる不純物の影響によ
り、分析感度及び分析精度が悪化すると同時に分析デー
タの再現性に問題があった。When used for welding and fusing, conventional dissolved acetylene can be used, but when used for atomic absorption and atomic emission spectroscopy, the analytical sensitivity and accuracy deteriorate due to the influence of impurities contained in the acetylene gas. There was a problem with the reproducibility of analytical data.
本発明は、上記事情に鑑みてなされたもので、原子吸光
、原子発光分析における信号の抑制現象のない、高感度
かつ高精度な分析を行うことのできる高純度アセチレン
ガスを提供することを目的とするものである。The present invention was made in view of the above circumstances, and an object of the present invention is to provide a high-purity acetylene gas that does not cause signal suppression in atomic absorption and atomic emission spectroscopy and allows highly sensitive and highly accurate analysis. That is.
本発明者らは、上記の問題を解決する方法について鋭意
検討した結果、リン化合物がｉ ｐｐｍ以下、硫化物が
１０ｐｐｍ以下、炭素数３以上の炭化水素が１００ｐｐ
ｍ以下であり、かつ、アセチレンガス純度が９９．０％
以下であるアセチレンガスを原子吸光、原子発光分析に
使用することにより、被測定物である金属元素の分析感
度及び分析精度を向上できることを見出し、本発明を完
成した。本発明の目的に必要とするアセチレンガスは、
粗アセチレンガスを固体清浄剤、Ａ型ゼオライト、活性
炭で処理し、Ｎ−Ｎ’ジメチルホルムアミド（以下ＤＭ
Ｆと略す）浸潤多孔物質を内蔵する容器に充填した後、
一部放出することにより容易に得られる。As a result of intensive studies on methods to solve the above problems, the inventors of the present invention found that phosphorus compounds are below i ppm, sulfides are below 10 ppm, and hydrocarbons having 3 or more carbon atoms are below 100 ppm.
m or less, and the acetylene gas purity is 99.0%
The present invention was completed based on the discovery that the analytical sensitivity and accuracy of the metal element to be measured can be improved by using the following acetylene gas in atomic absorption and atomic emission spectroscopy. The acetylene gas required for the purpose of the present invention is
Crude acetylene gas is treated with a solid detergent, A-type zeolite, and activated carbon, and then treated with N-N' dimethylformamide (hereinafter DM).
After filling the container containing the infiltrated porous material (abbreviated as F),
Easily obtained by partial release.
以下、本発明の内容について詳細な説明を行う。Hereinafter, the content of the present invention will be explained in detail.
原子吸光、原子発光分析に使用するアセチレンガスは、
溶解アセチレンから放出されるアセチレンガス中の不純
物濃度が、リン化合物が１ｐｐｍ以下、好ましくは０．
１ｐｐｍ以下、硫化物が１０ｐｐｍ以下、好ましくは”
＋ ｐｐｍ以下、炭素数３以上の炭化水素が１１００ｐ
ｐ以下、好ましくは５０ｐｐｍ以下であり、アセチレン
ガス純度は９９．０％以上、好ましくは９９．５％以上
であることが必要である。Acetylene gas used for atomic absorption and atomic emission spectroscopy is
The impurity concentration of phosphorus compounds in the acetylene gas released from dissolved acetylene is 1 ppm or less, preferably 0.
1 ppm or less, sulfide 10 ppm or less, preferably "
+ ppm or less, hydrocarbons with 3 or more carbon atoms are 1100p
p or less, preferably 50 ppm or less, and the acetylene gas purity needs to be 99.0% or more, preferably 99.5% or more.
このアセチレンガスを原子吸光、原子発光分析に使用す
ることにより、信号の抑制現象が認められず、又、信号
強度の経時変化がなく、全金属元素に対して、高感度か
つ高精度な分析が可能となるが、特にカルシウム、スト
ロンチウム、リチウム、カリウム、ナトリウム、モリブ
デンに対して有効である。アセチレンガス中の不純物が
、上記記載の濃度より多いとリン化合物では原子信号の
抑制現象があり、分析感度が低下し、又、硫化物及び炭
素数３以上の炭化水素では信号ノイズが大きくなり、分
析精度が低下する。アセチレンガス純度に関しては、上
記記載の純度より低いと、原子信号の抑制現象が認めら
れ、又、溶解アセチレンからのアセチレンガス放出に伴
う経時変化が急激であることから、データの再現性が問
題となる。本発明の原子吸光、原子発光分析に使用され
る純度の高い溶解アセチレンは、粗アセチレンガス中の
リン化水素、硫化水素を固体清浄剤を用いて酸化固定除
去した侵、Ａ型ゼオライト、活性炭を用いて、水分、硫
化水素以外の硫化物、炭素数３以上の炭化水素類を吸着
除去する。この処理されたガスをＤＭＦ浸潤多孔物質を
内蔵する容器に充填した後、充填ガス最の５〜２０％、
好ましくは１０〜１５％量を放出することにより、酸素
、窒素及びメタンを低減させることができる。放出ｍが
上記割合より少ないと十分な純度が得られず、又、上記
割合より多いとアセチレンガス中の酸素、窒素及びメタ
ンの含有量の少ない溶解アセチレンが得られるが、充填
アセチレン量の損失が多くなり、経済上好ましくない。By using this acetylene gas for atomic absorption and atomic emission spectroscopy, there is no signal suppression phenomenon, and there is no change in signal intensity over time, allowing highly sensitive and highly accurate analysis of all metal elements. It is particularly effective for calcium, strontium, lithium, potassium, sodium, and molybdenum. If the concentration of impurities in acetylene gas is higher than the above-mentioned concentration, phosphorus compounds will suppress the atomic signal, reducing analytical sensitivity, and sulfides and hydrocarbons with 3 or more carbon atoms will increase signal noise. Analysis accuracy decreases. Regarding acetylene gas purity, if it is lower than the purity stated above, atomic signal suppression phenomenon is observed, and the change over time associated with the release of acetylene gas from dissolved acetylene is rapid, so data reproducibility is a problem. Become. The highly purified dissolved acetylene used in the atomic absorption and atomic emission spectroscopy of the present invention is made by oxidizing and fixing hydrogen phosphide and hydrogen sulfide in crude acetylene gas using a solid detergent, A-type zeolite, and activated carbon. It adsorbs and removes moisture, sulfides other than hydrogen sulfide, and hydrocarbons having 3 or more carbon atoms. After filling this treated gas into a container containing a DMF-infiltrated porous material, 5-20% of the filling gas is
Oxygen, nitrogen and methane can be reduced by releasing preferably 10-15% amounts. If the released m is less than the above ratio, sufficient purity cannot be obtained, and if it is larger than the above ratio, dissolved acetylene with low contents of oxygen, nitrogen and methane in the acetylene gas can be obtained, but the amount of charged acetylene is lost. This is not economically desirable.
アセチレンガス放出は、特に規定するものではないが、
容器充填後、２４時間以上、好ましくは４８時間以上静
置後行うのが、効率的に酸素、窒素及びメタンを低減さ
せることができるので、経済上の観点から好ましい。Acetylene gas release is not particularly specified, but
From an economical point of view, it is preferable to carry out the reaction after being allowed to stand for 24 hours or more, preferably 48 hours or more after filling the container, since oxygen, nitrogen and methane can be efficiently reduced.
上記処理を施した溶解アセチレンは、アセチレンガス放
出に伴う不純物の経時変化が、従来の溶解アセチレンに
比較して著しく小さく、原子吸光、原子発光分析に使用
しても原子信号の抑制がなく、又、経時変化がないこと
から分析データの再現性が向上する。Dissolved acetylene subjected to the above treatment has a significantly smaller change in impurities over time due to the release of acetylene gas than conventional dissolved acetylene, and does not suppress atomic signals even when used in atomic absorption and atomic emission spectroscopy. , the reproducibility of analytical data is improved because there is no change over time.
使用される清浄剤は各種市販品のいずれを用いても良い
が、使用に当たっては、空気中で十分に賦活処理を施す
ことが必要である。Any of various commercially available detergents may be used, but before use, it is necessary to perform a sufficient activation treatment in the air.
Ａ型ビオライトは３Ａ型、４Ａ型、５Ａ型のいずれを用
いても良いが、吸着力の点から５Ａ型が望ましく、使用
に当たっては、不活性ガス雰囲気、または真空中で２５
０〜４００”Ｃ，好ましくは３００〜３５０℃で賦活処
理を施すことが望ましい。処理温度が上記より低い場合
は十分な吸着力が得られず、又、高い場合は吸着剤の劣
化が起き、好ましくない。Type A biolite may be 3A type, 4A type, or 5A type, but 5A type is preferable from the viewpoint of adsorption power.
It is desirable to carry out the activation treatment at 0 to 400"C, preferably 300 to 350C. If the treatment temperature is lower than the above, sufficient adsorption power will not be obtained, and if it is higher, the adsorbent will deteriorate, Undesirable.
活性炭は、粒状活性炭が圧力損失など操作上好ましい。Granular activated carbon is preferable from the viewpoint of pressure loss and other operational considerations.
使用に当たっては、ゼオライトの場合と同じく、同雰囲
気中２００〜３５０℃、好ましくは２５０〜３００℃で
賦活処理を施すことが望ましい。When using it, it is desirable to perform activation treatment at 200 to 350°C, preferably 250 to 300°C in the same atmosphere as in the case of zeolite.
（実施例）
固体清浄剤１１００９を大気中で４時間毎に１２回撹拌
して賦活処理した俊、直径２インチ、長ざ１ＴｒＬのス
テンレス製管に充填した。(Example) Solid detergent 11009 was filled in a stainless steel tube with a diameter of 2 inches and a length of 1 TrL, which had been activated by stirring 12 times every 4 hours in the atmosphere.
５Ａ型ゼオライトは上記と同仕様の管に１４００９充填
した後、窒素ガスを毎分０．５Ｎ１流しながら、３５０
℃で６時間、又、粒状活性炭は上記と同仕様の管に１０
００ｇ充填し、３００℃で同様に賦活処理を施した。Type 5A zeolite was filled with 14009 into a tube with the same specifications as above, and then heated at 350°C while flowing nitrogen gas at 0.5N1 per minute.
℃ for 6 hours, and granular activated carbon was placed in a tube with the same specifications as above for 10 hours.
00g was filled, and the same activation treatment was performed at 300°C.
上記各充填処理管３本を直列に配して、表−１の組成の
粗アセチレンガスを操作温度２０℃で毎分５Ｎ１処理し
た後、ＤＭＦ浸潤多孔物質を内蔵する容器に６００ＯＮ
、ｅ充填した。上記充填容器を４８時間静置し、６０
ＯＮＪｌ放出俊のアセチレンガス・の組成を表−２に示
す。After arranging the above three filling treatment tubes in series and treating the crude acetylene gas with the composition shown in Table 1 at 5N1 per minute at an operating temperature of 20℃, it was placed in a container containing a DMF-infiltrated porous material at 600ON.
, e-filled. The above filled container was left standing for 48 hours, and then
Table 2 shows the composition of acetylene gas released by ONJl.
尚、アセチレンガス純度はガスクロマトグラフ（ＴＣＤ
検出器）で、炭化水素類はガスクロマトグラフ（ＦＩＤ
検出器）で、リン化合物、硫化物はガスクロマトグラフ
（ＦＰＤ検出器）で測定した。In addition, the acetylene gas purity was measured using a gas chromatograph (TCD).
Hydrocarbons are detected using a gas chromatograph (FID detector).
The phosphorus compounds and sulfides were measured using a gas chromatograph (FPD detector).
このようにして得られた高純度溶解アセチレンを用いて
カルシウム、ストロンチウム、モリブデンの原子吸光分
析及びカルシウム、ストロンチウム、リチウム、カリウ
ム、ナトリウムの原子発光分析を行ったところ、純度９
９．９９９９％のアセチレンガス（東邦アセチレン■製
の超高純度アセチレン）を用いて測定したときの各元素
の原子吸光及び原子発光信号強度と何ら相違ない信号強
度を得ることができた。Using the high-purity dissolved acetylene thus obtained, atomic absorption spectrometry for calcium, strontium, and molybdenum and atomic emission spectrometry for calcium, strontium, lithium, potassium, and sodium were conducted, and the purity was found to be 9.
It was possible to obtain signal intensities that were no different from the atomic absorption and atomic emission signal intensities of each element when measured using 9.9999% acetylene gas (ultra-high purity acetylene manufactured by Toho Acetylene ■).
尚、測定は、■日立製作所製偏光ゼーマン原子吸光々度
計を用い、金属元素試料は関東化学Ｉｌ製の原子吸光用
標準溶液（各々１１０００ｐｐ ＞をカルシウムは５
ｐｐｍ−に、ストロンチウムは１０００ｍに、モリブデ
ンは５０ｐｐｍに、リチウムは２ｐｐｍに、カリウム及
びナトリウムは４ｐｐｍに各々希釈して用いて行った。The measurement was carried out using a polarized Zeeman atomic absorption spectrophotometer manufactured by Hitachi, Ltd., and the metal element samples were atomic absorption standard solutions manufactured by Kanto Kagaku Il (11,000 pp each), and calcium was 5
strontium was diluted to 1000 m, molybdenum was diluted to 50 ppm, lithium was diluted to 2 ppm, and potassium and sodium were diluted to 4 ppm.
（比較例１）
原子吸光、原子発光分析に９９．９９９９％のアセチレ
ンガスを用いた時と、放出されるアセチレンガス純度が
９１゜Ｏ〜９８．０％、アセチレンガス中に含まれるリ
ン化合物が０．１ｐｐｍ、硫化物が１０ｐｐｍ 、炭素
数３以上の炭化水素が５０Ｅ）Ｅ）ＩＩＩである溶解ア
セチレンを用いた時の原子信号強度を比較した。測定は
カルシウム、ストロンチウム、（原子吸光、原子発光）
モリブデン（原子吸光）、リチウム、ナトリウム（原子
発光）に対して行い、９９゜９９９９％のアセチレンガ
ス使用時の原子信号強度を１００％として、上記溶解ア
セチレン使用時の信号抑制率を％で表した結果を表−３
に示した。(Comparative Example 1) When 99.9999% acetylene gas was used for atomic absorption and atomic emission analysis, the purity of the acetylene gas released was 91°O to 98.0%, and the phosphorus compounds contained in the acetylene gas were The atomic signal intensities were compared when using dissolved acetylene with 0.1 ppm of sulfide, 10 ppm of sulfide, and 50E)E)III of hydrocarbons having 3 or more carbon atoms. Measurements include calcium, strontium, (atomic absorption, atomic emission)
It was conducted for molybdenum (atomic absorption), lithium, and sodium (atomic emission), and the atomic signal intensity when using 99°9999% acetylene gas was set as 100%, and the signal suppression rate when using the above dissolved acetylene was expressed in %. Table 3 shows the results.
It was shown to.
尚、測定礪器及び各金属元素の試料調製は実施例１と同
様にして行った。Note that the measurement vessel and sample preparation of each metal element were performed in the same manner as in Example 1.
表−３
（比較例２）
放出されるアセチレンガス純度が９９．５％、アセチレ
ンガス中に含まれるリン化合物が６．１〜１２．０ｐｐ
ｍ 、硫化物が１０ｐｐｍ 、炭素数３以上の炭化水素
が５０ｐｐｍである溶解アセチレンを使用して、カルシ
ウム（原子吸光）、ストロンチウム（原子吸光、原子発
光）、リチウム、カリウム（原子発光）に対して、比較
例１と同様の測定を行った結果を表−４に示した。Table 3 (Comparative Example 2) The purity of the acetylene gas released is 99.5%, and the phosphorus compound contained in the acetylene gas is 6.1 to 12.0 pp.
m, for calcium (atomic absorption), strontium (atomic absorption, atomic emission), lithium, potassium (atomic emission) using dissolved acetylene with 10 ppm sulfide and 50 ppm hydrocarbons with 3 or more carbon atoms. Table 4 shows the results of the same measurements as in Comparative Example 1.
（比較例３）
放出されるアセチレンガス純度！度が９９．５％、アセ
チレンガス中に含まれるリン化合物が、０．１ｐｐｍ
、硫化物が２００ｐｐｍ、炭素数３以上の炭化水素が５
０ｐｐｍである溶解アセチレンを使用して、ストロンチ
ウム、モリブデン（原子吸光）に対して、比較例１と同
様の測定を行った結果を表−５に示した。(Comparative Example 3) Purity of acetylene gas released! The concentration is 99.5%, and the phosphorus compound contained in the acetylene gas is 0.1 ppm.
, 200 ppm of sulfide, 5 of hydrocarbons with carbon number of 3 or more
Table 5 shows the results of the same measurements as in Comparative Example 1 for strontium and molybdenum (atomic absorption) using 0 ppm dissolved acetylene.
表−５
（比較例４）
放出されるアセチレンガス純度が９４．５％、アセチレ
ンガス中に含まれるリン化合物が０．１ｐｐｍ、硫化物
が１０ｐｐｍ 、炭素数３以上の炭化水素が５０ｐｐＩ
ｌｌ、アセトンが５．４％である溶解アセチレンを使用
して、カルシウム、ストロンチウム、モリブデン（原子
吸光）、ナトリウム（原子発光）に対して比較例１と同
様の測定を行った結果を表−６に示した。Table 5 (Comparative Example 4) The purity of the acetylene gas released is 94.5%, the phosphorus compound contained in the acetylene gas is 0.1 ppm, the sulfide is 10 ppm, and the hydrocarbon having 3 or more carbon atoms is 50 ppI.
Table 6 shows the results of the same measurements as in Comparative Example 1 for calcium, strontium, molybdenum (atomic absorption), and sodium (atomic emission) using dissolved acetylene containing 5.4% acetone. It was shown to.
表−６
＊１ Ａ：原子吸光
Ｅ：原子発光
〔発明の効果〕
以上）ホべた様に、本発明によれば、原子吸光、原子発
光分析に高純度アセチレンガスを使用することにより、
測定信号の抑制現象がなく高感度で、かつ、高精度で再
現性のよい分析を行うことができると同時に、必要とさ
れるアセチレンガスを、容易に得ることができ、工業的
価値大なるものがある。Table 6 *1 A: Atomic absorption E: Atomic emission [Effects of the invention] As mentioned above, according to the present invention, by using high-purity acetylene gas for atomic absorption and atomic emission analysis,
It has great industrial value as it allows for highly sensitive, highly accurate and reproducible analysis without the phenomenon of suppressing the measurement signal, and at the same time allows the necessary acetylene gas to be easily obtained. There is.
Claims (4)
ｍ以下、硫化物が１０ｐｐｍ以下、炭素数３以上の炭化
水素が１００ｐｐｍ以下であり、かつ、アセチレンガス
純度が９９．０％以上であることを特徴とする原子吸光
、原子発光分析用高純度アセチレンガス組成物。(1) Phosphorus compound contained in acetylene gas is 1pp
Highly purified acetylene for atomic absorption and atomic emission analysis, characterized in that the content of sulfides is 10 ppm or less, the amount of hydrocarbons having 3 or more carbon atoms is 100 ppm or less, and the acetylene gas purity is 99.0% or more. Gas composition.
スの吸収能力の高い溶剤を含浸させてアセチレンガスを
溶解させた溶解アセチレンであることを特徴とする請求
項１記載の原子吸光、原子発光分析用高純度アセチレン
ガス組成物。(2) The atomic absorption method according to claim 1, wherein the dissolved acetylene is obtained by dissolving acetylene gas by filling a porous filler in a container and impregnating the porous filler with a solvent having a high absorption capacity for acetylene gas. High purity acetylene gas composition for luminescence analysis.
る粗アセチレンガスを固体清浄剤、Ａ型ゼオライト、活
性炭で逐次処理し、リン化合物、硫化物、炭素数３以上
の炭化水素類、水分を除去した後、Ｎ−Ｎ′ジメチルホ
ルムアミド浸潤多孔物質を内蔵する容器に充填されたも
のであることを特徴とする請求項２記載の原子吸光、原
子発光分析用高純度アセチレンガス組成物。(3) Crude acetylene gas, whose main component is acetylene gas, is sequentially treated with a solid detergent, A-type zeolite, and activated carbon to remove phosphorus compounds, sulfides, hydrocarbons with 3 or more carbon atoms, and moisture. 3. The high-purity acetylene gas composition for atomic absorption and atomic emission analysis according to claim 2, wherein the composition is filled into a container containing a porous material infiltrated with N--N' dimethylformamide.
充填量の５〜２０％を放出することにより得られたもの
であることを特徴とする請求項２記載の原子吸光、原子
発光分析用高純度アセチレンガス組成物。(4) Atomic absorption or atomic emission analysis according to claim 2, which is obtained by charging the dissolved acetylene according to claim 3 and then releasing 5 to 20% of the total amount of the charged acetylene. High purity acetylene gas composition for use.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17798788A JPH0228539A (en) | 1988-07-19 | 1988-07-19 | High-purity gaseous acetylene composition for atomic absorption and atomic emission analysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17798788A JPH0228539A (en) | 1988-07-19 | 1988-07-19 | High-purity gaseous acetylene composition for atomic absorption and atomic emission analysis |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0228539A true JPH0228539A (en) | 1990-01-30 |
Family
ID=16040555
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17798788A Pending JPH0228539A (en) | 1988-07-19 | 1988-07-19 | High-purity gaseous acetylene composition for atomic absorption and atomic emission analysis |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0228539A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2706720C1 (en) * | 2019-04-15 | 2019-11-20 | Федеральное государственное бюджетное учреждение науки Ордена Ленина и Ордена Октябрьской революции Институт геохимии и аналитической химии им. В.И. Вернадского Российской академии наук (ГЕОХИ РАН) | Method of atomic emission analysis of solutions |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6219539A (en) * | 1985-07-18 | 1987-01-28 | Nichigou Asechiren Kk | Purification of acetylene and apparatus used therefor |
| JPS6245543A (en) * | 1985-08-22 | 1987-02-27 | Toyo Soda Mfg Co Ltd | Production of lower unsaturated hydrocarbon |
| JPS62285988A (en) * | 1986-06-04 | 1987-12-11 | Nichigou Asechiren Kk | Method of providing high-purity acetylene gas and purifying apparatus for use in said method |
-
1988
- 1988-07-19 JP JP17798788A patent/JPH0228539A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6219539A (en) * | 1985-07-18 | 1987-01-28 | Nichigou Asechiren Kk | Purification of acetylene and apparatus used therefor |
| JPS6245543A (en) * | 1985-08-22 | 1987-02-27 | Toyo Soda Mfg Co Ltd | Production of lower unsaturated hydrocarbon |
| JPS62285988A (en) * | 1986-06-04 | 1987-12-11 | Nichigou Asechiren Kk | Method of providing high-purity acetylene gas and purifying apparatus for use in said method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2706720C1 (en) * | 2019-04-15 | 2019-11-20 | Федеральное государственное бюджетное учреждение науки Ордена Ленина и Ордена Октябрьской революции Институт геохимии и аналитической химии им. В.И. Вернадского Российской академии наук (ГЕОХИ РАН) | Method of atomic emission analysis of solutions |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Farquhar et al. | A rapid on‐line technique for determination of oxygen isotope composition of nitrogen‐containing organic matter and water | |
| Sofer | Preparation of carbon dioxide for stable carbon isotope analysis of petroleum fractions | |
| Coburn et al. | Carbon monoxide in blood: analytical method and sources of error | |
| Ayala et al. | New studies on the surface properties of carbon blacks | |
| Goleb et al. | The use of a discharge tube as an absorption source for the determination of lithium-6 and lithium-7 isotopes by atomic absorption spectrophotometry | |
| Russell et al. | The sampling and determination of halocarbons in ambient air using concentration on porous polymer | |
| JPH0228539A (en) | High-purity gaseous acetylene composition for atomic absorption and atomic emission analysis | |
| JP2019505798A (en) | Elemental analysis method | |
| JP4019152B2 (en) | Trace hydrogen molecule and hydrogen isotope molecular separation analyzer | |
| Starokon et al. | Epoxidation of ethylene by anion radicals of α-oxygen on the surface of FeZSM-5 zeolite | |
| Payne et al. | Selectivity for water isotopologues within metal organic nanotubes | |
| US7422907B2 (en) | Process for measuring mercury concentration within hydrocarbons | |
| Craig et al. | The analysis of inorganic and methyl mercury by derivatisation methods; opportunities and difficulties | |
| JPH01124746A (en) | Analysis of nitrogen-containing compound | |
| Ferroni et al. | The Resolution of Complex Antipodes by Optically Active Solids1 | |
| US20050008543A1 (en) | Method and crucible for liberating oxygen isotopes from oxygen-containing solids | |
| CN106093253B (en) | The assay method of benzo [a] pyrene in sample-pretreating method and cigarette smoke for measuring benzo in cigarette smoke [a] pyrene | |
| Appelblad et al. | Fourier Transform Spectroscopy of the B 2Σ-X 2Σ Transition of BaH | |
| Tan | Microdetermination of nitrate by gas chromatography-mass spectrometry technique with multiple ion detector | |
| RU2143680C1 (en) | Method of quantitatively determining summary sulfur in sulfur- containing petroleum products | |
| Henderson et al. | Study of carbon compounds in Apollo 11 and Apollo 12 returned lunar samples | |
| Kirton et al. | Investigation of adsorbents for sampling compounds found in coke oven emissions | |
| Wardencki | Isolation and determination of volatile organic sulphur compounds in aqueous solutions | |
| Prombo et al. | A spectacular nitrogen isotopic anomaly in Bencubbin | |
| Tunnicliff | Solvents for ultraviolet spectrophotometry |