JPH0457219B2 - - Google Patents
Info
- Publication number
- JPH0457219B2 JPH0457219B2 JP14149085A JP14149085A JPH0457219B2 JP H0457219 B2 JPH0457219 B2 JP H0457219B2 JP 14149085 A JP14149085 A JP 14149085A JP 14149085 A JP14149085 A JP 14149085A JP H0457219 B2 JPH0457219 B2 JP H0457219B2
- Authority
- JP
- Japan
- Prior art keywords
- phosphorus
- container
- sample
- aqueous solution
- solution
- 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.)
- Expired
Links
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 46
- 239000011574 phosphorus Substances 0.000 claims description 46
- 229910052698 phosphorus Inorganic materials 0.000 claims description 46
- 238000000034 method Methods 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000004458 analytical method Methods 0.000 claims description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000002485 combustion reaction Methods 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 5
- 239000000567 combustion gas Substances 0.000 claims description 5
- 238000002798 spectrophotometry method Methods 0.000 claims description 5
- 238000002441 X-ray diffraction Methods 0.000 claims description 4
- 230000005587 bubbling Effects 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims 1
- 239000012670 alkaline solution Substances 0.000 description 8
- 239000007789 gas Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 7
- 238000002835 absorbance Methods 0.000 description 7
- 238000011088 calibration curve Methods 0.000 description 7
- 229910017604 nitric acid Inorganic materials 0.000 description 7
- 239000003921 oil Substances 0.000 description 7
- 238000007796 conventional method Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 4
- 239000005416 organic matter Substances 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000011609 ammonium molybdate Substances 0.000 description 2
- 235000018660 ammonium molybdate Nutrition 0.000 description 2
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 2
- 229940010552 ammonium molybdate Drugs 0.000 description 2
- 239000010727 cylinder oil Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- -1 for example Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002901 radioactive waste Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 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
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Description
（産業上の利用分野）
本発明はリン含有有機物中のリン含有量の測定
方法に関するものであり、特に油中に含まれるリ
ン含有量の測定方法に最適な方法である。
（従来の技術）
従来、有機物中のリン含有量を測定する方法と
しては、JIS K0102に規定されているように試料
を硝酸で加熱分解後、硝酸・過塩素酸でさらに分
解し、リンバナドモリブデン酸アンモニウム法で
リンを比色定量する方法が知られている。
（発明が解決しようとする問題点）
しかしながら上述した方法では、酸により油を
酸化分解する工程に時間がかかるため、１サンプ
ルを分析するのに延べ20時間程度の時間を要する
欠点があつた。そのため、リン含有有機物中のリ
ンの含有量を迅速に知る必要がある場合には適用
できない問題点があつた。
また、酸により油を加熱しながら酸化分解する
ため酸性の蒸気や煙が発生し、そのため作業者が
有害ガスを吸い込んだり試料室内の機器を腐食さ
せたりする欠点もあつた。
本発明は上述した不具合を解消して、有機物特
に油中のリン含有量を迅速に測定できると共に、
人体に有害であり機器を腐食させる酸性の蒸気や
煙を発生することのない有機物中のリン含有量の
測定方法を提供しようとするものである。
（問題点を解決するための手段）
本発明のリンの分析方法は、酸素雰囲気の容器
中でリン含有有機物を燃焼させたのち、燃焼ガス
中のリンをアルカリ水溶液に吸収させ、吸光光度
法又は蛍光Ｘ線分析法により有機物中のリン含有
量を測定することを特徴とするものである。
（作用）
上述した構成において、リン含有有機物の燃焼
はボンベ燃焼器等により短時間で行なうことがで
きるので、実質的は分析所要時間を吸光光度測定
あるいは蛍光Ｘ線分析にかかる時間に短縮するこ
とができる。また、リンを分解するのに容器中で
の燃焼以外の方法は使用していないので、有害な
ガスが発生しても外部に漏れることもない。
第１図は本発明の吸光光度法を実施するのに好
適なボンベ燃焼器の一実施例を示す断面図であ
る。本実施例では、容器本体１の上部テーパ部１
ａと内蓋２の下部テーパ部２ａとは係合して、パ
ツキング４を介して外蓋３を容器本体１にネジ止
めすることにより容器内を密封する構造をとつて
いる。この内蓋２には、ニードルバルブ５、酸素
圧入排出口６および点火端子７を設けている。さ
らに、密封した容器内部には、点火端子７と導通
した電極８、試料ざら９内に設けた試料１０およ
び点火線１１と着火剤１２を設けている。
以下、上述したボンベ燃焼器を使用して実際に
リン含有量の分析を行なう手順を第２図に示すフ
ローチヤートに従つて説明する。まず、油等のリ
ン含有有機物よりなる試料１０を試料ざら９内に
所定量入れると共に、容器内下部にNaOH、
KOH、NaCO3、KCO3等のアルカリ溶液、好ま
しくは0.1〜1.0NのNaOH、KOH等のアルカリ溶
液を満たす。次に、外蓋３により容器を密封して
酸素を酸素圧入排出口６から圧入する。酸素を圧
入した容器本体１を冷水浴中に入れ酸素の漏れが
ないことを確認したのち、点火用回路に点火端子
７を接続し２〜３秒間回路を閉じて試料を燃焼さ
せる。その後、容器本体１を冷水中に放置したの
ち、１〜５分間程度容器を振とうしてリン分をア
ルカリ溶液中に吸収させる。次に、容器内部の圧
力を一定速度で静かに抜いた後、リンを吸収した
アルカリ溶液を容器に集め、HCl、H2SO4、
HNO3等の酸水溶液で中和する。さらに、モリブ
デン酸アンモニウム等の発色剤を混入して発色さ
せた後、吸光光度計で吸光度を測定し、予め標準
サンプルから求めた検量線に基づきリン含有量を
同定する。
この場合、容器を振とうしてリン分をアルカリ
溶液中に吸収させる代りに、例えば350℃以上の
燃焼ガスをアルカリ溶液中にバブリングしてリン
をアルカリ溶液に吸収させてもよい。また蛍光Ｘ
線分析の場合も吸光光度法の場合とほぼ同様な方
法によりリン含有量を同定する。
（実施例）
ステンレス皿または石英ルツボに試料としてリ
ンを約７％含有するシリンダー油約0.5ｇを精秤
した後、これをボンベの試料台に載せ着火材を点
火線と接続して試料中に挿入した。次に、ボンベ
の容器内に0.1N水酸化ナトリウム溶液10mlを入
れると共に、試料をセツトした内蓋を容器内に入
れゴムパツキングとリングをセツトし外蓋で固く
締めつけて容器内を密封した。その後、酸素圧入
口から酸素ボンベより酸素を30Kg／cm2まで圧入し
た後、ボンベのニードルバルブを締めた。ボンベ
全体を水中に浸してガスもれのないことを確認し
た後、ボンベを水中より取り出し、点火プラグを
点火端子に接続し、点火ボタンを押し試料を燃焼
させた。20分間以上ボンベを放置後、２分間容器
を振とうして析出したP2O5とアルカリ溶液とを
接触させ、リン分をアルカリ溶液中に溶解した。
しかる後ニードルバルブを少し開き容器内のガス
をゆつくりと（１分間以上）放出した後、外蓋を
ゆるめて取りはずした。さらに、内蓋を慎重に取
りはずした後、試料皿及び内蓋の容器内部に露出
した部分を少量の水で洗いビーカー内に入れた。
また、ボンベ容器内のリンを吸収した水酸化ナト
リウム溶液を同じビーカー内へ移し、ボンベの内
側を水で洗浄して同じくビーカー内え移した。吸
収液と洗浄液の合量をビーカー内で40ml程度まで
濃縮し、5Aのろ紙でろ過して固型分を除去した
後、ろ液を100mlメスフラスコに移した。
その後、ろ液にフエノールフタレン１〜２滴を
加えて指示薬とした後0.5NのHNO3でろ液を中
和した。この中和液を二分し、一方の中和液中に
水と濃硝酸の等量よりなる（１＋１）硝酸４mlを
中和したろ液に加え、さらにメタンバナ八ン酸ア
ンモニウム溶液５mlとモリブデン酸アンモニウム
溶液を加えて発色させた後、20分間放置後460n
ｍの波長の光を使用して吸光度を測定した。又、
二分した他方の中和液の10mlを溶液試料セル中に
秤取し、蛍光Ｘ線分析装置を用いて蛍光Ｘ線強度
を測定した。
上述した操作とは別に、吸光度と濃度との関係
を示す検量線および蛍光Ｘ線強度と濃度との関係
を示す検量線をそれぞれ別々に作成するため100
mlメスフラスコ各４個を用意し、そのうちの各１
個はブランク用とし残り３個に各々リン標準液
（１mg／１ml）を１、２、３ml添加した後、少量
の水とフエノールフタレン１〜２滴を加え上述し
た操作と同様に460nｍでのそれぞれの吸光度お
よび蛍光Ｘ線分析装置により蛍光Ｘ線強度をそれ
ぞれ測定した。
上述した試料から求めた吸光度とおよび蛍光Ｘ
線強度とそれぞれの検量線とを使用して、次式に
より試料中のリン含有量（％）を算出した。
Ｐ＝ａ×ｂ×10-2／Ｓ×100
ここでＰ：リンの含有量（％）
ａ：試料の吸光度又は蛍光Ｘ線強度
ｂ：検量線の傾き
Ｓ：採取量（ｇ）
同時に同じ試料すなわちリンを約７％含有する
シリンダー油に対して、従来JIS K0102に規定さ
れる硝酸・過塩素酸分解法でリン含有量を測定し
て比較した。なお、分析結果はそれぞれ３点ずつ
実施した。結果を第１表に示す。
(Industrial Application Field) The present invention relates to a method for measuring phosphorus content in phosphorus-containing organic substances, and is particularly suitable for measuring phosphorus content contained in oil. (Prior art) The conventional method for measuring the phosphorus content in organic substances is to heat decompose a sample with nitric acid and further decompose it with nitric acid/perchloric acid as specified in JIS K0102. A method of colorimetrically determining phosphorus using the acid ammonium method is known. (Problems to be Solved by the Invention) However, the above-mentioned method has the disadvantage that it takes a total of about 20 hours to analyze one sample because the process of oxidatively decomposing the oil with acid takes time. Therefore, there was a problem that this method could not be applied when it was necessary to quickly determine the phosphorus content in phosphorus-containing organic substances. In addition, since the oil is oxidized and decomposed while being heated by the acid, acidic steam and smoke are generated, which has the disadvantage of causing workers to inhale harmful gases and corroding equipment in the sample chamber. The present invention solves the above-mentioned problems and allows rapid measurement of phosphorus content in organic substances, especially oil, and
The present invention aims to provide a method for measuring phosphorus content in organic substances that does not generate acidic vapor or smoke that is harmful to the human body and corrodes equipment. (Means for Solving the Problems) The phosphorus analysis method of the present invention involves burning phosphorus-containing organic matter in a container in an oxygen atmosphere, and then absorbing phosphorus in the combustion gas into an alkaline aqueous solution, using the spectrophotometric method or This method is characterized by measuring the phosphorus content in organic substances using fluorescent X-ray analysis. (Function) In the above-described configuration, the combustion of phosphorus-containing organic matter can be carried out in a short time using a cylinder combustor, etc., so that the time required for analysis can be substantially reduced to the time required for absorbance photometry or fluorescent X-ray analysis. Can be done. Furthermore, since no method other than combustion in the container is used to decompose phosphorus, even if harmful gases are generated, they will not leak outside. FIG. 1 is a sectional view showing an embodiment of a cylinder combustor suitable for carrying out the absorptiometric method of the present invention. In this embodiment, the upper tapered part 1 of the container body 1 is
a is engaged with the lower tapered portion 2a of the inner lid 2, and the outer lid 3 is screwed to the container body 1 via the packing 4, thereby sealing the inside of the container. This inner lid 2 is provided with a needle valve 5, an oxygen pressurization inlet/outlet 6, and an ignition terminal 7. Further, inside the sealed container, there are provided an electrode 8 electrically connected to the ignition terminal 7, a sample 10 provided in a sample basin 9, an ignition wire 11, and an ignition agent 12. Hereinafter, the procedure for actually analyzing the phosphorus content using the above-mentioned cylinder combustor will be explained according to the flowchart shown in FIG. First, a predetermined amount of the sample 10 made of phosphorus-containing organic matter such as oil is placed in the sample bowl 9, and NaOH and
Fill with an alkaline solution such as KOH, NaCO 3 or KCO 3 , preferably 0.1-1.0N NaOH or KOH. Next, the container is sealed with the outer lid 3, and oxygen is pressurized through the oxygen injection/exhaust port 6. After the container body 1 into which oxygen has been pressurized is placed in a cold water bath and it is confirmed that there is no leakage of oxygen, the ignition terminal 7 is connected to the ignition circuit and the circuit is closed for 2 to 3 seconds to burn the sample. Thereafter, the container body 1 is left in cold water, and then shaken for about 1 to 5 minutes to absorb phosphorus into the alkaline solution. Next, after gently releasing the pressure inside the container at a constant rate, the alkaline solution that has absorbed phosphorus is collected in the container, and HCl, H 2 SO 4 ,
Neutralize with an aqueous acid solution such as HNO3 . Furthermore, after mixing a coloring agent such as ammonium molybdate to develop a color, the absorbance is measured using an absorptiometer, and the phosphorus content is identified based on a calibration curve determined in advance from a standard sample. In this case, instead of shaking the container to absorb phosphorus into the alkaline solution, for example, combustion gas at 350° C. or higher may be bubbled into the alkaline solution to absorb phosphorus into the alkaline solution. Also fluorescent X
In the case of line analysis, the phosphorus content is identified using almost the same method as in the case of spectrophotometry. (Example) After accurately weighing about 0.5 g of cylinder oil containing about 7% phosphorus as a sample in a stainless steel dish or quartz crucible, place it on the sample stand of the cylinder, connect the ignition material to the ignition wire, and add it to the sample. Inserted. Next, 10 ml of 0.1N sodium hydroxide solution was put into the container of the cylinder, and the inner lid with the sample set was placed inside the container, the rubber packing and ring were set, and the outer lid was tightly tightened to seal the inside of the container. Thereafter, oxygen was pressurized to 30 kg/cm 2 from the oxygen cylinder through the oxygen pressure inlet, and the cylinder's needle valve was tightened. After immersing the entire cylinder in water and confirming that there was no gas leak, the cylinder was taken out of the water, the spark plug was connected to the ignition terminal, and the ignition button was pressed to burn the sample. After leaving the cylinder for 20 minutes or more, the container was shaken for 2 minutes to bring the precipitated P 2 O 5 into contact with the alkaline solution, thereby dissolving the phosphorus in the alkaline solution.
Thereafter, the needle valve was slightly opened to slowly release the gas inside the container (for 1 minute or more), and then the outer lid was loosened and removed. Furthermore, after carefully removing the inner lid, the sample dish and the portion of the inner lid exposed inside the container were washed with a small amount of water and placed in a beaker.
In addition, the sodium hydroxide solution that had absorbed phosphorus in the bomb container was transferred into the same beaker, and the inside of the bomb was washed with water and transferred into the same beaker. The total amount of the absorption liquid and washing liquid was concentrated to about 40 ml in a beaker, filtered through 5A filter paper to remove solids, and the filtrate was transferred to a 100 ml volumetric flask. Thereafter, 1 to 2 drops of phenolphthalene was added to the filtrate to serve as an indicator, and the filtrate was neutralized with 0.5N HNO3 . This neutralized solution is divided into two parts, and 4 ml of (1+1) nitric acid, which is made up of equal parts of water and concentrated nitric acid, is added to the neutralized filtrate, and then 5 ml of ammonium methanobanaate solution and ammonium molybdate are added to one of the neutralized solutions. After adding the solution and developing color, leave it for 20 minutes and then apply 460n.
Absorbance was measured using light at a wavelength of m. or,
10 ml of the other neutralized solution was weighed out into a solution sample cell, and the fluorescent X-ray intensity was measured using a fluorescent X-ray analyzer. Apart from the above-mentioned operations, in order to separately create a calibration curve showing the relationship between absorbance and concentration and a calibration curve showing the relationship between fluorescent X-ray intensity and concentration,
Prepare 4 ml volumetric flasks, one of each
One piece was used as a blank, and after adding 1, 2, and 3 ml of phosphorus standard solution (1 mg/1 ml) to the remaining three pieces, a small amount of water and 1 to 2 drops of phenolphthalene were added, and the same procedure as described above was carried out at 460 nm. The absorbance and fluorescent X-ray intensity of each sample were measured using a fluorescent X-ray analyzer. Absorbance and fluorescence X determined from the above sample
Using the line intensity and each calibration curve, the phosphorus content (%) in the sample was calculated using the following formula. P=a×b×10 -2 /S×100 where P: Phosphorus content (%) a: Sample absorbance or fluorescent X-ray intensity b: Calibration curve slope S: Sample amount (g) Same sample at the same time That is, the phosphorus content of cylinder oil containing about 7% phosphorus was measured and compared using the nitric acid/perchloric acid decomposition method specified in conventional JIS K0102. In addition, the analysis results were conducted for three points each. The results are shown in Table 1.
【表】
第１表から明らかなように、本発明方法と従来
方法を比較すると、平均値に特に有意差は認めら
れず、変動幅および標準偏差は共に本発明方法の
方が優れていることがわかつた。さらに、測定所
要時間は従来方法が約20時間要するのに対し、本
発明方法は２時間で結果が得られ、測定時間が従
来法の約1/10以下となることがわかつた。
又本発明は吸光光度法および蛍光Ｘ線分析にい
ずれにおいても精度よく測定できることが確認さ
れた。
本発明は上述した実施例にのみ限定されるもの
ではなく、幾多の変形、変更が可能である。例え
ば上述した実施例では、燃焼して得たP2O5を容
器のなかで一旦冷却して容器内面に析出させた後
容器を振とうしてアルカリ水溶液中に吸収させた
が、容器内の燃焼して得たP2O5のガスが約350℃
以上である場合には、容器から燃焼ガスをとりだ
して別の容器中に準備したアルカリ水溶液中でバ
ブリングさせ吸収させることもできる。この場合
温度が350℃以上であるとP2O5はすべて気体とし
て存在するので、本実施例と同様燃焼したP2O5
を完全にアルカリ水溶液中に吸収させることがで
きる。また、リンの標準試料を使用しての検量線
の測定は吸光光度法の場合吸光度計の状態が時間
とともに変化するため測定ごとに行なうことが望
ましいが、連続して分析するような場合は最初に
求めた検量線をすべての分析において使用するこ
とができる。
（発明の効果）
以上詳細に説明したところから明らかなよう
に、本発明のリンの分析方法によれば、従来方法
では時間のかかつていたリン含有有機物からのリ
ンの分離を燃焼により短時間で行なうようにした
ため、分析精度を悪化させることなく分析所要時
間を大幅に短縮することができる。また、この分
離に際し酸等の有害ガス発生元をまつたく使用し
ていないため、人体に有害であると共に測定機器
等を腐食させる有害ガスの発生がまつたくない。
そのため、迅速にリンの含有量を求める必要があ
る油の精製工程や放射性廃棄物特に放射能で汚染
された物質を含む廃油中のリンの測定に有効であ
る。[Table] As is clear from Table 1, when comparing the method of the present invention and the conventional method, there is no significant difference in the average values, and the method of the present invention is superior in both the fluctuation range and standard deviation. I understood. Furthermore, it was found that while the conventional method required about 20 hours for measurement, the method of the present invention could obtain results in 2 hours, making the measurement time less than about 1/10 of the conventional method. It has also been confirmed that the present invention can be used to accurately measure both spectrophotometry and fluorescent X-ray analysis. The present invention is not limited only to the embodiments described above, and numerous modifications and changes are possible. For example, in the above-mentioned example, P 2 O 5 obtained by combustion was once cooled in a container and precipitated on the inner surface of the container, and then the container was shaken to absorb it into the alkaline aqueous solution. The P 2 O 5 gas obtained by combustion is approximately 350℃
In the case above, the combustion gas can be taken out from the container and absorbed by bubbling it in an alkaline aqueous solution prepared in another container. In this case, if the temperature is 350°C or higher, all P 2 O 5 exists as a gas, so as in this example, the burned P 2 O 5
can be completely absorbed into alkaline aqueous solution. In addition, in the case of spectrophotometry, it is desirable to measure the calibration curve using a standard sample of phosphorus for each measurement because the state of the spectrophotometer changes over time, but if continuous analysis is to be performed, The calibration curve obtained can be used in all analyses. (Effects of the Invention) As is clear from the above detailed explanation, according to the phosphorus analysis method of the present invention, phosphorus can be separated from phosphorus-containing organic substances in a short time by combustion, which was time-consuming in conventional methods. As a result, the time required for analysis can be significantly shortened without deteriorating analysis accuracy. In addition, since a source of harmful gas such as acid is not used during this separation, there is no risk of generating harmful gas that is harmful to the human body and corrodes measuring instruments and the like.
Therefore, it is effective in oil refining processes where it is necessary to quickly determine the phosphorus content, and in measuring phosphorus in radioactive waste, especially waste oil containing radioactively contaminated substances.
第１図は本発明を実施するのに好適なボンベ燃
焼器の一実施例を示す断面図、第２図は本発明の
分析手順を説明するためのフローチヤートであ
る。
１……容器本体、１ａ……上部テーパ部、２…
…内蓋、２ａ……下部テーパ部、３……外蓋、４
……パツキング、５……ニードルバルブ、６……
酸素圧入排出口、７……点火端子、８……電極、
９……試料ざら、１０……試料、１１……点火
線、１２……着火材。
FIG. 1 is a sectional view showing an embodiment of a cylinder combustor suitable for implementing the present invention, and FIG. 2 is a flowchart for explaining the analysis procedure of the present invention. 1... Container body, 1a... Upper tapered part, 2...
...Inner lid, 2a...Lower taper part, 3...Outer lid, 4
...Packing, 5...Needle valve, 6...
Oxygen pressure inlet/outlet, 7...Ignition terminal, 8...Electrode,
9... Sample plate, 10... Sample, 11... Ignition wire, 12... Ignition material.
Claims (1)
させたのち、燃焼ガス中のリンをアルカリ水溶液
に吸収させ、吸光光度法又は蛍光Ｘ線分析法によ
り有機物中のリン含有量を測定することを特徴と
するリンの分析方法。 ２ 前記燃焼容器としてボンベ燃焼器を用いる特
許請求の範囲第１項記載のリンの分析方法。 ３ 前記アルカリ水溶液として水酸化ナトリウム
又は水酸化カリウム水溶液を用いる特許請求の範
囲第１項記載のリンの分析方法。 ４ 高温の燃焼ガスをアルカリ水溶液中でバブリ
ングしてリンをアルカリ水溶液中に吸収させる特
許請求の範囲第１項記載のリンの分析方法。[Claims] 1. After burning a phosphorus-containing organic substance in a container in an oxygen atmosphere, the phosphorus in the combustion gas is absorbed into an alkaline aqueous solution, and the phosphorus content in the organic substance is determined by spectrophotometry or fluorescent X-ray analysis. A phosphorus analysis method characterized by measuring phosphorus. 2. The phosphorus analysis method according to claim 1, wherein a cylinder combustor is used as the combustion container. 3. The method for analyzing phosphorus according to claim 1, wherein the aqueous alkali solution is a sodium hydroxide or potassium hydroxide aqueous solution. 4. The phosphorus analysis method according to claim 1, which comprises bubbling hot combustion gas in an alkaline aqueous solution to absorb phosphorus into the alkaline aqueous solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14149085A JPS623643A (en) | 1985-06-29 | 1985-06-29 | Analysis of phosphorus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14149085A JPS623643A (en) | 1985-06-29 | 1985-06-29 | Analysis of phosphorus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS623643A JPS623643A (en) | 1987-01-09 |
| JPH0457219B2 true JPH0457219B2 (en) | 1992-09-10 |
Family
ID=15293126
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14149085A Granted JPS623643A (en) | 1985-06-29 | 1985-06-29 | Analysis of phosphorus |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS623643A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102007004339B4 (en) | 2007-01-29 | 2008-10-02 | Lar Process Analysers Ag | Method and device for determining the phosphorus content of an aqueous sample |
| JP2012021797A (en) * | 2010-07-12 | 2012-02-02 | Mie Chuo Kaihatsu Kk | Method for measuring chlorine content in solid fuel |
| CN108627472A (en) * | 2018-03-20 | 2018-10-09 | 苏州市信测标准技术服务有限公司 | The detection method of total phosphorus content in a kind of phosphate ester flame retardants |
-
1985
- 1985-06-29 JP JP14149085A patent/JPS623643A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS623643A (en) | 1987-01-09 |
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