JP3284783B2 - Moisture measurement method - Google Patents
Moisture measurement methodInfo
- Publication number
- JP3284783B2 JP3284783B2 JP23787994A JP23787994A JP3284783B2 JP 3284783 B2 JP3284783 B2 JP 3284783B2 JP 23787994 A JP23787994 A JP 23787994A JP 23787994 A JP23787994 A JP 23787994A JP 3284783 B2 JP3284783 B2 JP 3284783B2
- Authority
- JP
- Japan
- Prior art keywords
- temperature
- heating
- sample
- moisture
- heating temperature
- 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 - Lifetime
Links
- 238000000691 measurement method Methods 0.000 title claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 64
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000005259 measurement Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 12
- 238000004448 titration Methods 0.000 claims description 9
- 239000012159 carrier gas Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 2
- 238000010586 diagram Methods 0.000 description 8
- 229920002292 Nylon 6 Polymers 0.000 description 4
- 238000009834 vaporization Methods 0.000 description 4
- 230000008016 vaporization Effects 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000003869 coulometry Methods 0.000 description 2
- 230000002452 interceptive effect Effects 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 239000006200 vaporizer Substances 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- YWEUIGNSBFLMFL-UHFFFAOYSA-N diphosphonate Chemical compound O=P(=O)OP(=O)=O YWEUIGNSBFLMFL-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- DLYUQMMRRRQYAE-UHFFFAOYSA-N phosphorus pentoxide Inorganic materials O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
Landscapes
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、水分測定方法に関し、
固体試料中の水分を加熱気化法により測定する水分測定
方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for measuring moisture,
The present invention relates to a moisture measurement method for measuring moisture in a solid sample by a heating vaporization method.
【０００２】[0002]
【従来の技術】固体試料中の水分をカールフィッシャー
（ＫＦ）法で測定する場合、直接、滴定セルに試料を投
入する方法もあるが、最近は加熱気化法により行うのが
通常である。加熱気化法では加熱炉の温度を一定に設定
し、その温度において気化した水分を測定しているが、
適切な加熱温度は試料によって異なるので、正確な水分
の測定を行うためには、その加熱温度が適切か否か判断
する必要がある。従来は加熱温度を変えて測定を繰り返
し、どの加熱温度が適切か判断していた。2. Description of the Related Art When measuring the moisture in a solid sample by the Karl Fischer (KF) method, there is a method of directly charging the sample into a titration cell, but recently, it is usually performed by a heating and vaporizing method. In the heating vaporization method, the temperature of the heating furnace is set to a constant value, and the moisture vaporized at that temperature is measured.
Since an appropriate heating temperature varies depending on the sample, it is necessary to determine whether or not the heating temperature is appropriate in order to perform accurate moisture measurement. Conventionally, the measurement was repeated while changing the heating temperature to determine which heating temperature was appropriate.
【０００３】固体試料の水分をＫＦ電量法で測定する場
合、一般には図１に示したような装置で行う。図１は水
分測定装置の一例を示す図であり、気化部２、キャリヤ
ーガス供給部３および滴定部１から構成される。加熱炉
１０の温度がある設定値になった後、滴定セル５内を無
水状態にしておく。試料投入口１５より試料を試料ボー
ト１２に投入する。試料ボート１２はマグネット１９を
用いた移動機構により加熱炉１０の中央部に移動する。
試料中の水分は加熱炉の設定温度で気化する分だけ滴定
セル５にキャリヤーガス１８により運び込まれる。[0003] In the case of measuring the water content of a solid sample by the KF coulometry, it is generally carried out using an apparatus as shown in FIG. FIG. 1 is a diagram showing an example of the moisture measuring apparatus, which comprises a vaporizing section 2, a carrier gas supply section 3 and a titration section 1. After the temperature of the heating furnace 10 reaches a certain set value, the inside of the titration cell 5 is kept anhydrous. A sample is put into the sample boat 12 through the sample inlet 15. The sample boat 12 is moved to the center of the heating furnace 10 by a moving mechanism using a magnet 19.
The moisture in the sample is carried by the carrier gas 18 into the titration cell 5 by an amount that evaporates at the set temperature of the heating furnace.
【０００４】図５は、従来より水分測定に用いられた、
一般の試料の加熱温度と測定される水分率の関係を示す
図である。実際、試料の水分を測定するときは図５のＢ
領域の温度、すなわち水分が全て気化し且つ加熱分解生
成物が生じない温度に設定しなければならない。Ａ領域
では加熱温度が低すぎ、分析時間は長くかかり、低めの
測定値を与える。Ｃ領域では熱分解によりヨウ素を消費
する生成物、例えば、水、アンモニア等が生成している
ため、高めの測定値を与える。従って、未知の試料の最
適加熱温度を選ぶには、図５に示されるような加熱温度
と測定される水分率のプロットをまず確認する必要があ
った。[0004] FIG. 5 is a diagram showing a conventional structure used for moisture measurement.
It is a figure which shows the relationship between the heating temperature of a general sample, and the moisture content measured. In fact, when measuring the moisture of the sample,
The temperature of the zone must be set at a temperature at which all moisture evaporates and no pyrolysis products are formed. In region A, the heating temperature is too low, the analysis time is long and gives lower measured values. In the region C, a product that consumes iodine by thermal decomposition, for example, water, ammonia, and the like is generated, and thus a higher measured value is given. Therefore, in order to select the optimum heating temperature of the unknown sample, it was necessary to first confirm a plot of the heating temperature and the measured moisture content as shown in FIG.
【０００５】[0005]
【発明が解決しようとする課題】しかし、試料量が少な
い試料の場合は、最適加熱温度を確認するために加熱温
度を変えて何度も測定を繰り返すことはできない。ま
た、試料量が充分にある場合でも、加熱温度を変える度
に試料を秤り直して測定を行うことは時間と労力を要す
る。これまではこのように少量の試料で、且つ、一度の
測定で最適加熱温度を確認することができなかった。本
発明はこのような難点を解決するためになされたもので
ある。However, in the case of a sample having a small sample amount, it is not possible to repeat the measurement many times by changing the heating temperature in order to confirm the optimum heating temperature. Further, even when the amount of the sample is sufficient, it takes time and labor to measure the sample again every time the heating temperature is changed. Until now, it was not possible to confirm the optimum heating temperature with such a small amount of sample and with a single measurement. The present invention has been made to solve such a problem.
【０００６】[0006]
【課題を解決するための手段】本発明は、固体試料中の
水分を加熱気化し、キャリヤーガスで水分計滴定セル内
に送り込み、水分量を測定する方法において、加熱温度
を段階的に上昇させて各温度で気化した水分量を測定
し、該水分量がほぼ０となる温度を求め、これを測定時
の加熱温度とすることを特徴とする水分測定方法であ
る。According to the present invention, there is provided a method for measuring the amount of water by heating and evaporating the water in a solid sample, sending it into a titration cell with a carrier gas using a carrier gas, and increasing the heating temperature stepwise. The method is characterized in that the amount of water vaporized at each temperature is measured at each temperature, a temperature at which the amount of water is substantially zero is obtained, and this is set as a heating temperature at the time of measurement.
【０００７】加熱炉の加熱温度を予め設定して段階的に
昇温し、各設定温度になった時点で試料を加熱炉に移動
させ、前記設定温度で試料の水分の測定を行い、好まし
くは、加熱炉の昇温中は、試料を加熱されていない場所
に移動し、加熱炉の前記設定温度到達後に試料を加熱炉
に移動させて測定を行うことによって各加熱温度におい
て気化される水分量が分かり、一度の測定で最適加熱温
度を決めることができる。また、加熱温度が何度以上に
なれば試料が分解し妨害反応が起きているかということ
も明確になる。[0007] The heating temperature of the heating furnace is set in advance and the temperature is raised stepwise. When the temperature reaches each of the set temperatures, the sample is moved to the heating furnace, and the water content of the sample is measured at the set temperature. During the heating of the heating furnace, the amount of water vaporized at each heating temperature is obtained by moving the sample to a place where the sample is not heated, moving the sample to the heating furnace after reaching the set temperature of the heating furnace, and performing measurement. Thus, the optimum heating temperature can be determined by one measurement. In addition, it becomes clear whether the sample is decomposed and an interfering reaction occurs when the heating temperature is increased more than how many times.
【０００８】本発明は前述の図５のプロットをするため
の測定を、一度の試料で行うものである。具体的に説明
すると、一定量の試料をまず、例えば、１００℃での加
熱温度で測定する。１００℃で一定時間測定し、次は１
２０℃に昇温する。最初の設定温度が低すぎる場合は水
分の気化が遅いため、一定時間、例えば２０分で測定を
強制的に終了し、次の温度に移るのが望ましい。昇温操
作中は試料ボート１２は加熱管４の加熱されていない部
分に移動させる。１２０℃に達したら再び試料ボート１
２を加熱炉１０に移動させる。この加熱温度で気化する
水分を測定する。この操作を例えば、３００℃まで繰り
返す。各温度における気化した水分量をプロットすると
図２のグラフが得られる。In the present invention, the measurement for plotting the above-mentioned FIG. 5 is performed on one sample. Specifically, a certain amount of the sample is first measured at a heating temperature of, for example, 100 ° C. Measure at 100 ° C for a certain period of time.
Raise the temperature to 20 ° C. If the initial set temperature is too low, the vaporization of moisture is slow, so it is desirable to forcibly end the measurement in a certain time, for example, 20 minutes, and move to the next temperature. During the temperature raising operation, the sample boat 12 is moved to an unheated portion of the heating tube 4. When the temperature reaches 120 ° C, sample boat 1 again
2 is moved to the heating furnace 10. The moisture vaporized at this heating temperature is measured. This operation is repeated up to, for example, 300 ° C. When the amount of vaporized water at each temperature is plotted, the graph of FIG. 2 is obtained.
【０００９】図２は、各設定温度で気化した水分量を示
す図である。図２においてＡ領域では加熱温度が低いた
め水分が少しずつ気化してくる。Ｂ領域の加熱温度では
それまでの温度で水分が全て気化しているため水分が出
てこない。この領域が最適加熱温度となる。Ｃ領域では
加熱分解により生成した化合物がヨウ素と反応している
と推測され、従ってＣ領域で測定すると間違った水分値
となる。加熱温度の昇温及び設定温度での温度の維持、
試料ボートの移動はプログラムの設定により、自動で行
わせることも可能である。図２のプロットも自動的に求
めることも可能である。FIG. 2 is a diagram showing the amount of water vaporized at each set temperature. In FIG. 2, in the region A, since the heating temperature is low, moisture evaporates little by little. At the heating temperature in the region B, no water comes out because all the water has been vaporized at the temperature up to that time. This region is the optimum heating temperature. In the region C, it is presumed that the compound generated by the thermal decomposition has reacted with iodine, and therefore, when measured in the region C, an incorrect water value is obtained. Raising the heating temperature and maintaining the temperature at the set temperature,
The movement of the sample boat can be automatically performed by setting a program. The plot of FIG. 2 can also be obtained automatically.
【００１０】水分測定にはＫＦ電量法を用いた場合につ
いて説明したが、ＫＦ容量法や他の測定法、例えば五酸
化燐電解法による水分測定等を適用することも可能であ
る。Although the case of using the KF coulometric method for moisture measurement has been described, it is also possible to apply the KF capacity method and other measuring methods, for example, moisture measurement by a phosphorus pentoxide electrolysis method.
【００１１】[0011]
【実施例】以下、本発明を実施例により、さらに具体的
に説明するが、本願発明はその要旨を超えない限り、下
記実施例に限定されるものではない。 実施例１ 微量水分計「ＣＡ−０６」（三菱化成（株）製）と改良
された加熱気化装置「ＶＡ−０６」（三菱化成（株）
製）とを用いてナイロン６の水分測定を行った。予め滴
定セルにはＫＦ電量試薬を満たし、加熱気化装置の加熱
炉も１５０℃に設定した。ナイロン６約０．１ｇを精秤
し、試料投入口より試料ボートに投入する。ナイロン６
の場合は１５０℃の加熱温度は通常低すぎる温度のた
め、なかなか水が気化されない。２０分間で強制的に測
定を終了させ、試料ボートは加熱管の加熱されないゾー
ンに移動させた。加熱温度を１８０℃に上げて試料ボー
トを再び加熱炉に移動させる。この操作を３００℃まで
繰り返した。図３のような結果が得られ、最適加熱温度
は２３０℃から３００℃であることがわかった。水分率
は３．０７％であった。 実施例２ ナイロン６の代わりにコピー用紙を用いた以外は実施例
１と同様に測定した。但し、加熱開始温度は１１０℃か
ら始めた。結果を図４に示した。最適加熱温度は１３０
℃から２３０℃であり、２５０℃以上にすると妨害反応
が起きていることが分かった。２３０℃までで測定した
水分率は８．０７％であった。一方、３００℃までで測
定した見かけの水分率は１５．１７％であった。EXAMPLES Hereinafter, the present invention will be described more specifically with reference to examples, but the present invention is not limited to the following examples unless it exceeds the gist of the present invention. Example 1 Trace moisture meter "CA-06" (manufactured by Mitsubishi Kasei Corporation) and improved heating vaporizer "VA-06" (Mitsubishi Kasei Corporation)
) Was used to measure the moisture content of nylon 6. The titration cell was filled with the KF coulomb reagent in advance, and the heating furnace of the heating vaporizer was also set at 150 ° C. About 0.1 g of nylon 6 is precisely weighed and put into a sample boat from a sample inlet. Nylon 6
In the case of (1), since the heating temperature of 150 ° C. is usually too low, water is not easily vaporized. The measurement was forcibly terminated in 20 minutes, and the sample boat was moved to an unheated zone of the heating tube. The heating temperature is raised to 180 ° C., and the sample boat is moved to the heating furnace again. This operation was repeated up to 300 ° C. The result as shown in FIG. 3 was obtained, and it was found that the optimum heating temperature was from 230 ° C. to 300 ° C. The water content was 3.07%. Example 2 The measurement was performed in the same manner as in Example 1 except that copy paper was used instead of nylon 6. However, the heating start temperature was started from 110 ° C. The results are shown in FIG. The optimal heating temperature is 130
The temperature was from 230 ° C to 230 ° C, and it was found that an interfering reaction occurred at 250 ° C or higher. The water content measured up to 230 ° C. was 8.07%. On the other hand, the apparent moisture content measured up to 300 ° C. was 15.17%.
【００１２】[0012]
【発明の効果】本発明によれば、少量の試料を用いて各
加熱温度での水分値と、その加熱温度までの累積の水分
値を得ることができ、また最適加熱温度を求めることも
できる。従来法では最適加熱温度を精度良く求めること
が困難であった、偏析の大きい試料についても、本発明
によれば前記最適加熱温度を好適に求めることが可能と
なる。さらに、本願発明方法を自動化すると一度の測定
で結果が容易に得られるため、作業者の労力が大幅に軽
減できる。According to the present invention, the moisture value at each heating temperature and the accumulated moisture value up to the heating temperature can be obtained using a small amount of sample, and the optimum heating temperature can be obtained. . According to the present invention, it is possible to suitably obtain the optimum heating temperature even for a sample with large segregation, for which it has been difficult to accurately determine the optimum heating temperature by the conventional method. Further, when the method of the present invention is automated, the result can be easily obtained by one measurement, so that the labor of the operator can be greatly reduced.
【図１】 水分測定装置の一例を示す模式図である。FIG. 1 is a schematic diagram showing an example of a moisture measuring device.
【図２】 加熱温度と測定される水分率の関係を示す図
である。FIG. 2 is a diagram showing a relationship between a heating temperature and a measured moisture content.
【図３】 各加熱温度で気化した水分量を示す図であ
る。FIG. 3 is a diagram showing the amount of water vaporized at each heating temperature.
【図４】 実施例１の結果を示す図である。FIG. 4 is a diagram showing the results of Example 1.
【図５】 実施例２の結果を示す図である。FIG. 5 is a diagram showing the results of Example 2.
１ 滴定部 ２ 気化部 ３ キャリヤーガス供給部 ４ 加熱管 ５ 滴定セル ６ 検出電極 ７ 滴定装置 ８ 電解液 ９ 吹き込み管 １０ 加熱炉 １１ 温度制御装置 １２ 試料ボート １３ 熱電対 １４ 押し出し棒 １５ 試料投入口 １６ 流量計 １７ 乾燥筒 １８ キャリヤーガス １９ マグネット ２０ ネジブタ DESCRIPTION OF SYMBOLS 1 Titration part 2 Vaporization part 3 Carrier gas supply part 4 Heating tube 5 Titration cell 6 Detecting electrode 7 Titrator 8 Electrolyte 9 Blow-in tube 10 Heating furnace 11 Temperature controller 12 Sample boat 13 Thermocouple 14 Push rod 15 Sample inlet 16 Flow meter 17 Drying cylinder 18 Carrier gas 19 Magnet 20 Screw pig
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平２−234056（ＪＰ，Ａ) 特開 平５−281170（ＪＰ，Ａ) 特開 平４−34350（ＪＰ，Ａ) 特開 平６−265492（ＪＰ，Ａ) 特開 昭59−32856（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) G01N 25/56 G01N 25/00 ────────────────────────────────────────────────── ─── Continuation of the front page (56) References JP-A-2-234056 (JP, A) JP-A-5-281170 (JP, A) JP-A-4-34350 (JP, A) JP-A-6-340 265492 (JP, A) JP-A-59-32856 (JP, A) (58) Fields investigated (Int. Cl. 7 , DB name) G01N 25/56 G01N 25/00
Claims (2)
ヤーガスで水分計滴定セル内に送り込み、水分量を測定
する方法において、加熱温度を段階的に上昇させて各温
度で気化した水分量を測定し、該水分量がほぼ０となる
温度を求め、これを測定時の加熱温度とすることを特徴
とする水分測定方法。1. A method for measuring the amount of water by heating and evaporating the water in a solid sample and sending it into a titration cell using a carrier gas to measure the amount of water. Is measured, and a temperature at which the water content is substantially zero is determined, and this is set as a heating temperature at the time of measurement.
体試料を非加熱部に移動することを特徴とする請求項１
記載の水分測定方法。2. The method according to claim 1, wherein the solid sample is moved to a non-heating section during the stepwise heating to the heating set temperature.
The moisture measurement method described.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23787994A JP3284783B2 (en) | 1994-09-30 | 1994-09-30 | Moisture measurement method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23787994A JP3284783B2 (en) | 1994-09-30 | 1994-09-30 | Moisture measurement method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH08101145A JPH08101145A (en) | 1996-04-16 |
| JP3284783B2 true JP3284783B2 (en) | 2002-05-20 |
Family
ID=17021781
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP23787994A Expired - Lifetime JP3284783B2 (en) | 1994-09-30 | 1994-09-30 | Moisture measurement method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3284783B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5633158B2 (en) | 2010-03-01 | 2014-12-03 | セントラル硝子株式会社 | Method and apparatus for measuring moisture content in compounds containing hydrogen fluoride |
| CN113126671A (en) * | 2019-12-30 | 2021-07-16 | 奥豪斯仪器（常州）有限公司 | Prediction algorithm for heating temperature of moisture meter |
-
1994
- 1994-09-30 JP JP23787994A patent/JP3284783B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH08101145A (en) | 1996-04-16 |
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