JPH08101145A - Moisture measurement method - Google Patents
Moisture measurement methodInfo
- Publication number
- JPH08101145A JPH08101145A JP23787994A JP23787994A JPH08101145A JP H08101145 A JPH08101145 A JP H08101145A JP 23787994 A JP23787994 A JP 23787994A JP 23787994 A JP23787994 A JP 23787994A JP H08101145 A JPH08101145 A JP H08101145A
- Authority
- JP
- Japan
- Prior art keywords
- temperature
- heating temperature
- heating
- water content
- sample
- 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.)
- Granted
Links
- 238000000691 measurement method Methods 0.000 title claims description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 72
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000005259 measurement Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000004448 titration Methods 0.000 claims abstract description 11
- 239000012159 carrier gas Substances 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- 238000001704 evaporation Methods 0.000 claims abstract 2
- 238000007796 conventional method Methods 0.000 abstract description 3
- 230000001186 cumulative effect Effects 0.000 abstract description 2
- 238000005204 segregation Methods 0.000 abstract description 2
- 238000010586 diagram Methods 0.000 description 7
- 238000009834 vaporization Methods 0.000 description 5
- 229920002292 Nylon 6 Polymers 0.000 description 4
- 238000003869 coulometry Methods 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- 230000008016 vaporization Effects 0.000 description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000002452 interceptive effect Effects 0.000 description 2
- 229910052740 iodine Inorganic materials 0.000 description 2
- 239000011630 iodine Substances 0.000 description 2
- 239000006200 vaporizer Substances 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001514 detection 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
- 238000001125 extrusion Methods 0.000 description 1
- 238000011068 loading method Methods 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
Landscapes
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
(57)【要約】
【構成】 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。
【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。偏析の大きい試料の場合、従来法では最適加熱温度
を精度良く求めることができなかったが、この方法で解
決できる。
(57) [Summary] [Structure] In a method for measuring the water content by heating and evaporating the water content in a solid sample and feeding it into a titration cell with a carrier gas, the heating temperature is raised stepwise at each temperature. A method for measuring water content, characterized in that a vaporized water content is measured, a temperature at which the water content becomes almost 0 is obtained, and this is set as a heating temperature at the time of measurement. According to the present invention, the moisture value at each heating temperature and the cumulative moisture value up to the heating temperature can be obtained using a small amount of sample, and the optimum heating temperature can also be obtained. In the case of a sample with a large segregation, the optimum heating temperature could not be obtained with high accuracy by the conventional method, but this method can solve the problem.
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。FIELD OF THE INVENTION The present invention relates to a method for measuring water content,
The present invention relates to a water content measuring method for measuring water content 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 In the case of measuring the water content in a solid sample by the Karl Fischer (KF) method, there is a method in which the sample is directly put into a titration cell, but recently, it is usually performed by a heating vaporization method. In the heating vaporization method, the temperature of the heating furnace is set constant, and the moisture vaporized at that temperature is measured.
Since the appropriate heating temperature differs depending on the sample, it is necessary to judge whether or not the heating temperature is appropriate in order to accurately measure the water content. Conventionally, the heating temperature was changed and the measurement was repeated 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。When the water content of a solid sample is measured by the KF coulometric method, it is generally carried out by an apparatus as shown in FIG. FIG. 1 is a diagram showing an example of a water content measuring device, which is composed of a vaporization unit 2, a carrier gas supply unit 3, and a titration unit 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 loaded into the sample boat 12 through the sample loading port 15. The sample boat 12 is moved to the central portion of the heating furnace 10 by the moving mechanism using the magnet 19.
Moisture in the sample is carried into the titration cell 5 by the carrier gas 18 by the amount that is vaporized 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。FIG. 5 shows a conventional method 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. Actually, when measuring the water content of the sample, B of FIG.
The temperature of the region must be set, that is, the temperature at which all moisture is vaporized and no thermal decomposition products are generated. In region A, the heating temperature is too low and the analysis time is long, giving lower readings. In the C region, a product that consumes iodine due to thermal decomposition, such as water or ammonia, is generated, and therefore 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 the plot of the heating temperature and the measured water 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 amount of sample, the heating temperature cannot be changed and the measurement cannot be repeated many times in order to confirm the optimum heating temperature. Further, even when the amount of the sample is sufficient, it takes time and labor to re-measure the sample each time the heating temperature is changed and perform the measurement. Until now, it was not possible to confirm the optimum heating temperature with such a small amount of sample and one measurement. The present invention has been made to solve such a difficulty.
【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, in a method of vaporizing water in a solid sample by heating and feeding it into a titration cell of a moisture meter with a carrier gas to measure the amount of water, the heating temperature is raised stepwise. Then, the amount of water vaporized at each temperature is measured, the temperature at which the amount of water becomes approximately 0 is determined, and this is used as the 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。The heating temperature of the heating furnace is set in advance and the temperature is raised stepwise, and when each set temperature is reached, the sample is moved to the heating furnace and the water content of the sample is measured at the set temperature, preferably The amount of water vaporized at each heating temperature by moving the sample to a place where it is not heated during the heating of the heating furnace and moving the sample to the heating furnace after the temperature reaches the set temperature of the heating furnace for measurement. Therefore, the optimum heating temperature can be determined with one measurement. In addition, it becomes clear whether the heating temperature is higher than what time the sample is decomposed and the interfering reaction occurs.
【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 making the plot of FIG. 5 described above is performed with a single sample. Specifically, a certain amount of sample is first measured at a heating temperature of 100 ° C., for example. Measure at 100 ° C for a certain period of time, then 1
Raise the temperature to 20 ° C. If the initial set temperature is too low, the water vaporizes slowly, so it is desirable to forcibly terminate the measurement within 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 the unheated portion of the heating tube 4. Once it reached 120 ℃, sample boat 1 again
2 is moved to the heating furnace 10. Moisture vaporized at this heating temperature is measured. This operation is repeated up to 300 ° C., for example. The graph of FIG. 2 is obtained by plotting the amount of vaporized water at each temperature.
【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, since the heating temperature is low in the area A, the moisture gradually vaporizes. At the heating temperature of the B region, the moisture does not come out because all the moisture has been vaporized at the temperatures up to that point. This region is the optimum heating temperature. It is presumed that the compound produced by thermal decomposition reacts with iodine in the C region, and therefore the measurement of the C region gives an incorrect water content value. Raising the heating temperature and maintaining the temperature at the set temperature,
The movement of the sample boat can be automatically performed by setting the program. The plot of FIG. 2 can also be automatically obtained.
【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 coulometry method has been described for the water content measurement, the KF capacitance method and other measurement methods such as the water content measurement by the phosphorus pentoxide electrolysis method can also be applied.
【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。The present invention will be described in more detail with reference to the following examples, but the present invention is not limited to the following examples unless it exceeds the gist. Example 1 Trace moisture meter "CA-06" (manufactured by Mitsubishi Kasei Co., Ltd.) and improved heating vaporizer "VA-06" (Mitsubishi Kasei Co., Ltd.)
Was used to measure the water content of nylon 6. The titration cell was filled with KF coulometric reagent in advance, and the heating furnace of the heating vaporizer was also set to 150 ° C. About 0.1 g of nylon 6 is precisely weighed and charged into the sample boat through the sample charging port. Nylon 6
In the case of 1, since the heating temperature of 150 ° C. is usually too low, water is hardly vaporized. The measurement was forcibly terminated in 20 minutes, and the sample boat was moved to the 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 results shown in FIG. 3 were obtained, and it was found that the optimum heating temperature was 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. 4. Optimum heating temperature is 130
C. to 230.degree. C., and it was found that an interfering reaction occurred at 250.degree. C. or higher. The water content measured up to 230 ° C. was 8.07%. On the other hand, the apparent water 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 cumulative moisture value up to the heating temperature can be obtained using a small amount of sample, and the optimum heating temperature can also be obtained. . According to the present invention, it is possible to preferably obtain the optimum heating temperature even for a sample having a large segregation, which is difficult to obtain the optimum heating temperature with high accuracy 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 significantly 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 heating temperature and 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 1 Titration Part 2 Vaporization Part 3 Carrier Gas Supply Part 4 Heating Tube 5 Titration Cell 6 Detection Electrode 7 Titration Device 8 Electrolyte 9 Blowing Tube 10 Heating Furnace 11 Temperature Control Device 12 Sample Boat 13 Thermocouple 14 Extrusion Rod 15 Sample Input Port 16 Flow meter 17 Drying cylinder 18 Carrier gas 19 Magnet 20 Screw pig
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 of measuring the water content by heating and evaporating the water content in a solid sample into a titration cell using a carrier gas, and increasing the heating temperature stepwise to evaporate the water content at each temperature. Is measured to obtain a temperature at which the water content becomes almost 0, and this is used 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 solid sample is moved to the non-heating section during the stepwise heating to the preset heating 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 true JPH08101145A (en) | 1996-04-16 |
| JP3284783B2 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) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011108384A1 (en) * | 2010-03-01 | 2011-09-09 | セントラル硝子株式会社 | Method and device for measuring water content in hydrogen fluoride-containing compound |
| 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
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011108384A1 (en) * | 2010-03-01 | 2011-09-09 | セントラル硝子株式会社 | Method and device for measuring water content in hydrogen fluoride-containing compound |
| CN102782491A (en) * | 2010-03-01 | 2012-11-14 | 中央硝子株式会社 | Method and device for measuring water content in hydrogen fluoride-containing compound |
| US9097688B2 (en) | 2010-03-01 | 2015-08-04 | Central Glass Company, Limited | Method and device for measuring water content in hydrogen fluoride-containing fluoride salt compounds |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3284783B2 (en) | 2002-05-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Criss et al. | The thermodynamic properties of high temperature aqueous solutions. I. Standard partial molal heat capacities of sodium chloride and barium chloride from 0 to 100 | |
| US4407959A (en) | Blood sugar analyzing apparatus | |
| JPH08101145A (en) | Moisture measurement method | |
| Takahashi | Measurement of thermophysical properties of metals and ceramics by the laser-flash method | |
| Manning et al. | The determination of manganese by electrothermal atomic absorption spectrometry with a graphite furnace at constant temperature | |
| Rettberg et al. | Vaporization kinetics for solids analysis with electrothermal atomic absorption spectrometry: determination of lead in metal samples | |
| JP2536494B2 (en) | Sample-only heat flux type differential scanning calorimeter | |
| JPH0634532A (en) | Method of measuring moisture of sinteref material | |
| Greenfield et al. | A conductimetric micro method for determining hydrogen in organic compounds | |
| Busfield et al. | Studies in the thermochemistry of sulphones. Part 3.—Fusion and vaporization heats of sulphones of the type RSO 2 CH 3 | |
| Goldberg et al. | Evaluation of heats of transition in scanning calorimetry | |
| JPH063343A (en) | Gas chromatograph | |
| Cortijo et al. | Digital control of a differential scanning microcalorimeter | |
| MarchanteáGayˇn | Determination of cadmium in human urine using electrothermal atomic absorption spectrometry with probe atomization and deuterium background correction | |
| Tomkins et al. | Heats of dilution of lithium perchlorate in anhydrous acetonitrile, propionitrile, and isobutyronitrile at 25. degree. C | |
| JP2793841B2 (en) | Determination method of measurement end point in moisture measurement device | |
| JP3058748B2 (en) | Sulfur moisture determination method | |
| SU621996A2 (en) | Heat capacity determining device | |
| JPH05203594A (en) | Melting point measuring method | |
| Vasil ‘ev et al. | Thermodynamics of protolytic equilibria in aqueous solutions of biologically active ligands | |
| JPH06308011A (en) | Moisture or volatile content meter | |
| JPH05332986A (en) | Method and apparatus for estimating silicon concentration in blast furnace hot metal | |
| Kántor et al. | Investigation of thermal properties of high-temperature (1000–4000 K) systems by an arc spectroscopic method: Decomposition of tricalcium phosphate | |
| JPS5540921A (en) | Method and unit for hydrogen analysis in metal | |
| JPH087142B2 (en) | Frameless atomic absorption spectrometric method for trace metal analysis |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20090308 Year of fee payment: 7 |
|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20090308 Year of fee payment: 7 |
|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20100308 Year of fee payment: 8 |
|
| S531 | Written request for registration of change of domicile |
Free format text: JAPANESE INTERMEDIATE CODE: R313531 |
|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20100308 Year of fee payment: 8 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313113 |
|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20100308 Year of fee payment: 8 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20110308 Year of fee payment: 9 |
|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20120308 Year of fee payment: 10 |
|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20130308 Year of fee payment: 11 |
|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20140308 Year of fee payment: 12 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| EXPY | Cancellation because of completion of term |