JP2018124272A - Sample weight measurement device and weight measurement method - Google Patents
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Abstract
Description
本発明は、試料の重量測定装置および重量測定方法に属する。 The present invention relates to a sample weight measuring apparatus and a weight measuring method.
工業製品の生産における原料の乾燥工程として真空乾燥が頻繁に行われている。真空乾燥法および真空乾燥機は、試料を乾燥するにあたってその効率の良さから産業上利用される機会が多く、例えば工業製品の生産における原料などの乾燥工程では、工程時間の短縮や操業コストダウンの観点からも非常に重宝されている。 Vacuum drying is frequently performed as a raw material drying process in the production of industrial products. Vacuum drying methods and vacuum dryers are often used industrially due to their high efficiency in drying samples. It is very useful from a viewpoint.
真空乾燥の際に、事前に乾燥する試料の真空乾燥の状況を試験的に調査し、その結果を操業条件に反映することが行われている。その際、扱う原料に関し、温度変化に伴う重量変化についての調査を行い、その調査結果に基づき、試料の適正な乾燥条件を把握することは重要である。 At the time of vacuum drying, the state of vacuum drying of a sample to be dried in advance is examined experimentally, and the result is reflected in the operating conditions. At that time, it is important to conduct an investigation on the weight change accompanying the temperature change with respect to the raw material to be handled, and to grasp an appropriate drying condition of the sample based on the investigation result.
この様な情報を知るための手段として、例えば減圧機能を付与した示差熱天秤（以降、ＴＧ−ＤＴＡ装置と称する。）が考えられる。試料の適正な乾燥条件を把握するためには、原料に応じ、いかなる時間いかなる温度にて加熱すれば乾燥が完了する（すなわち水分量が減少し切る）のかを試験によって把握する必要がある。その試験の際には、雰囲気を減圧または真空とする方が、雰囲気中の水分等の影響を受けにくくなり、正確な結果を得ることができる。
このＴＧ−ＤＴＡ装置については例えば特許文献１に記載のものが例示され、ＴＧ−ＤＴＡ装置を用いた水分量測定方法については例えば特許文献２に記載のものが例示される。
As a means for obtaining such information, for example, a differential thermal balance (hereinafter referred to as a TG-DTA apparatus) provided with a decompression function is conceivable. In order to grasp the proper drying conditions of the sample, it is necessary to know by testing whether the drying is completed (that is, the amount of water is completely reduced) by heating at what temperature for what time according to the raw material. In the test, if the atmosphere is reduced in pressure or vacuum, it is less affected by moisture in the atmosphere, and an accurate result can be obtained.
Examples of this TG-DTA apparatus are those described in Patent Document 1, and examples of the moisture content measuring method using the TG-DTA apparatus are those described in Patent Document 2.
上述の通り、既存のＴＧ−ＤＴＡ装置においては減圧機能を有するものも存在する。その一方で、減圧機能を有するＴＧ−ＤＴＡ装置だと、測定に供することが可能な試料量は、数ｍｇレベルと少量である。試料の重量測定方法において、試料が少量だと、試料間の違いが明確になり難いという知見を本発明者は得た。具体例を挙げると、試料が少量だと、試料内の粒子数が自ずと少なくなる。そうなると、試料が水和物であった場合にたった一つの粒子に多大な水和水が含まれていたとすると、試料全体において水の量を多く見積もってしまうことになる。つまり、粒子一つ一つの状態により測定結果が大きく影響を受けてしまうことになる。また、試料が少量であって粒径が大きい場合、そもそも試料が測定用の容器に入らないという事態も考えられる。それを鑑み、減圧機能を有するＴＧ−ＤＴＡ装置をスケールアップしようとすると、特許文献１に記載のようなＴＧ−ＤＴＡ装置の場合、天秤となる部分も含めて減圧する部分を広げなければならず、大掛かりな装置構成が必要となり、経済性が良好とは言い難い。 As described above, some existing TG-DTA apparatuses have a pressure reducing function. On the other hand, in the case of a TG-DTA apparatus having a decompression function, the amount of sample that can be used for measurement is as small as several mg level. In the method for measuring the weight of a sample, the present inventor has obtained the knowledge that it is difficult to clarify the difference between samples when the amount of the sample is small. As a specific example, when the sample is small, the number of particles in the sample is naturally reduced. In that case, if the sample is a hydrate and a single particle contains a large amount of hydrated water, the amount of water in the entire sample is estimated to be large. That is, the measurement result is greatly influenced by the state of each particle. In addition, when the sample is small and the particle size is large, there may be a situation in which the sample does not enter the measurement container. In view of that, when trying to scale up a TG-DTA device having a decompression function, in the case of a TG-DTA device as described in Patent Document 1, the part to be decompressed must be widened including the part to be a balance. A large-scale apparatus configuration is required, and it is difficult to say that the economy is good.
また、ＴＧ−ＤＴＡ装置ではなく、汎用の真空乾燥機を使用することも考えられる。ただ、その場合、試料の重量測定を行う際に、真空乾燥機内から試料を取り出す作業、すなわち真空を破って常温常圧に戻す作業が必要となる。そうなると、常温常圧に戻す間に試料の重量が変動してしまい、誤差が生じるおそれがある。なお、同一種類の試料を別々に作製し、例えば試料Ａは３０分乾燥を行った結果を示すものとし、試料Ｂは１時間乾燥を行った結果を示すものとする手法もあり得るが、相当な手間がかかる上、厳密に言えば試料Ａと試料Ｂとは別々の試料であり、同一試料における経時的な重量変化を測定しているとは言い難い。 It is also conceivable to use a general-purpose vacuum dryer instead of the TG-DTA apparatus. However, in that case, when measuring the weight of the sample, it is necessary to take out the sample from the inside of the vacuum dryer, that is, to break the vacuum and return to normal temperature and pressure. If so, the weight of the sample fluctuates while returning to room temperature and normal pressure, and an error may occur. There may be a technique in which samples of the same type are prepared separately, for example, sample A indicates the result of drying for 30 minutes, and sample B indicates the result of drying for 1 hour. Strictly speaking, sample A and sample B are separate samples, and it is difficult to say that the change in weight over time in the same sample is measured.
なお、同一試料における経時的な重量変化を測定することが非常に重要であるということは、本発明者の鋭意研究により得られた知見である。詳しく言うと、試料の乾燥条件を把握するうえで、試料の重量と温度との関係のみならず、重量と（所定の温度での）時間との関係についての情報すなわち減圧状態での温度変化に伴う重量の経時変化も、プラント操業工業的に重要な情報であるという知見が得られた。 The fact that it is very important to measure the change in weight over time in the same sample is a finding obtained by earnest research by the present inventors. More specifically, in understanding the drying conditions of a sample, not only the relationship between the weight and temperature of the sample, but also the information about the relationship between the weight and time (at a given temperature), that is, the temperature change in a reduced pressure state. It was found that the accompanying change in weight over time is also important information for the plant operation industry.
ただ、上述の通り、ＴＧ−ＤＴＡ装置を使用するにしても真空乾燥機を使用するにしても、上記情報が正確に得られる状況とは言い難く、ひいては試料の適正な乾燥条件を把握できているとは言い難い。 However, as described above, whether the TG-DTA apparatus or the vacuum dryer is used, it is difficult to say that the above information can be obtained accurately. As a result, the proper drying conditions of the sample can be grasped. It ’s hard to say.
本発明の課題は、試料の重量の制限を受けずに試料の適正な乾燥条件を把握することを可能とする技術を提供することにある。 The subject of this invention is providing the technique which makes it possible to grasp | ascertain the suitable drying conditions of a sample, without receiving the restriction | limiting of the weight of a sample.
上記課題を解決するため検討を行った結果、試料を内部に載置可能な容器に対して減圧機構（例えば真空ポンプ）を連結して容器内を減圧した状態（真空状態を含む）で、試料を該容器ごと秤量するという手法を想到した。それにより、試料の重量の制限を受けずに、減圧環境を維持したまま温度変化に伴う重量の経時変化を測定可能とするという手法を想到した。 As a result of investigations to solve the above-mentioned problems, the sample in a state (including a vacuum state) in which the pressure inside the container is reduced by connecting a pressure reducing mechanism (for example, a vacuum pump) to the container in which the sample can be placed The inventors have come up with a technique of weighing the whole container. As a result, the inventors have come up with a technique that enables measurement of a change in weight over time accompanying a change in temperature while maintaining a reduced pressure environment without being limited by the weight of the sample.
上記の知見に基づいて成された本発明の態様は、以下の通りである。
本発明の第１の態様は、
試料を内部に載置可能な容器と、
前記容器に連結されて前記容器の内部を減圧可能な減圧機構と、
試料を前記容器ごと秤量可能な秤量機構と、
を備えた、試料の重量測定装置である。
The embodiments of the present invention made based on the above findings are as follows.
The first aspect of the present invention is:
A container in which a sample can be placed;
A decompression mechanism connected to the container and capable of decompressing the interior of the container;
A weighing mechanism capable of weighing the sample together with the container;
Is a sample weight measuring apparatus.
本発明の第２の態様は、第１の態様に記載の発明において、
前記容器の周囲に設けられた加熱炉を更に備える。
According to a second aspect of the present invention, in the invention according to the first aspect,
A heating furnace provided around the container is further provided.
本発明の第３の態様は、第１または第２の態様に記載の発明において、
前記減圧機構は真空ポンプおよびガス排出導管を備える。
According to a third aspect of the present invention, in the invention according to the first or second aspect,
The decompression mechanism includes a vacuum pump and a gas discharge conduit.
本発明の第４の態様は、第１〜第３のいずれかの態様に記載の発明において、
前記秤量機構は天秤であり、天秤のてこの一方には前記容器を把持する把持機構および前記容器が取り付けられ、もう一方には重りが取り付けられており、前記重りの重量は、室温での前記把持機構、前記容器および試料の合計重量と等しい。
According to a fourth aspect of the present invention, in the invention according to any one of the first to third aspects,
The weighing mechanism is a balance, a holding mechanism for holding the container and the container are attached to one of the levers of the balance, and a weight is attached to the other, and the weight of the weight is the same as that at room temperature. Equal to the total weight of the gripping mechanism, the container and the sample.
本発明の第５の態様は、第１〜第３のいずれかの態様に記載の発明において、
前記秤量機構は台秤である。
According to a fifth aspect of the present invention, in the invention according to any one of the first to third aspects,
The weighing mechanism is a platform scale.
本発明の第６の態様は、第１〜第５のいずれかに記載の試料の重量測定装置を使用して、試料を内部に載置した前記容器の内部を減圧したまま試料を前記容器ごと秤量することにより、温度変化に伴う試料の重量の経時変化を測定する、試料の重量測定方法である。 A sixth aspect of the present invention is the sample weight measuring apparatus according to any one of the first to fifth aspects, wherein the sample is put together with the container while the inside of the container on which the sample is placed is decompressed. This is a method for measuring the weight of a sample, in which a change over time in the weight of the sample accompanying a change in temperature is measured by weighing.
本発明によれば、試料の重量の制限を受けずに試料の適正な乾燥条件を把握することが可能となる。 According to the present invention, it is possible to grasp the proper drying conditions of a sample without being restricted by the weight of the sample.
以下、本発明の実施の形態について図１を用いて説明する。図１は、本実施形態における試料の重量測定装置の概略断面図である。 Hereinafter, an embodiment of the present invention will be described with reference to FIG. FIG. 1 is a schematic cross-sectional view of a sample weight measuring apparatus according to the present embodiment.
本実施形態の試料の重量測定装置は主として以下の構成を備える。
・試料を内部に載置可能な容器
・容器に連結されて前記容器の内部を減圧可能な減圧機構
・容器の周囲に設けられた加熱炉
・試料を前記容器ごと秤量可能な秤量機構
The sample weight measuring apparatus of the present embodiment mainly has the following configuration.
-Container that can place sample inside-Depressurization mechanism that is connected to the container and can decompress the inside of the container-Heating furnace provided around the container-Weighing mechanism that can weigh the sample together with the container
容器としては、試料を内部に載置可能であって、容器の内部を減圧または真空（以降、代表して「減圧」と称する。）とする減圧機構（後述）を連結可能なものであり、且つ、例えば蓋によって容器の内部を減圧状態に維持可能であり、且つ、試料の温度を変化させる加熱炉（後述）が与える熱に耐えうるものであれば形状、材質等は問わない。 As a container, a sample can be placed inside, and a decompression mechanism (described later) that makes the inside of the container depressurized or vacuum (hereinafter referred to as “depressurized”) can be connected. In addition, the shape, material, and the like are not limited as long as the inside of the container can be maintained in a reduced pressure state with a lid and can withstand the heat given by a heating furnace (described later) that changes the temperature of the sample.
以下、図１に記載の容器について一具体例として詳述する。図１においては、容器３として密閉式試料瓶を使用し、密閉式試料瓶３は天秤１に吊り下げられる。密閉式試料瓶３の開口側上部側面および密閉式試料瓶３の蓋６の内側面にねじ加工を施しておき、両者を締め合わせることにより内部を密閉し、その状態を保持可能とする構成を採用する。なお、密閉度を上げるために必要に応じてＯリングを使用するのもよい。
密閉式試料瓶３の蓋６にはガス排出導管２の一方が接続されており、他の一方は真空ポンプ５に接続されている。真空ポンプ５を作動させて、減圧ホース１３を介し、密閉式試料瓶３の内部を所望とする真空度に調整することができる。密閉式試料瓶３の真空度は圧力計９でモニター可能である。密閉式試料瓶３の内部と連通するガス排出導管２は、天秤１に対してコネクター８によって接続され、鉛直上下方向に可動可能とする。
Hereinafter, the container illustrated in FIG. 1 will be described in detail as a specific example. In FIG. 1, a sealed sample bottle is used as the container 3, and the sealed sample bottle 3 is suspended from the balance 1. The opening side upper side surface of the sealed sample bottle 3 and the inner side surface of the lid 6 of the sealed sample bottle 3 are threaded, and the inside is sealed by fastening them together so that the state can be maintained. adopt. Note that an O-ring may be used as necessary to increase the sealing degree.
One end of the gas discharge conduit 2 is connected to the lid 6 of the sealed sample bottle 3, and the other one is connected to the vacuum pump 5. By operating the vacuum pump 5, the inside of the sealed sample bottle 3 can be adjusted to a desired degree of vacuum via the decompression hose 13. The degree of vacuum of the sealed sample bottle 3 can be monitored with a pressure gauge 9. The gas discharge conduit 2 communicating with the inside of the sealed sample bottle 3 is connected to the balance 1 by a connector 8 so as to be movable in the vertical vertical direction.
また、試料７としては特に制限は無く、例えば水和物を含有する試料を用いてもよい。なお、本発明の課題でも述べたところであるが、本実施形態を適用すれば試料７の重量の制限が無くなる。本実施形態は、従来のＴＧ−ＤＴＡ装置（特許文献１）のように秤量機構を減圧雰囲気下に入れるのではなく、閉鎖されて減圧雰囲気となっている空間を構成する容器３ごと、内部に載置された試料７の重量を、常温常圧下で測定する。そのため、試料７を内部に載置している容器３のみを減圧すれば足りる。その結果、装置の構成を大掛かりにせずとも、単に容器３を大きくすれば試料７を増量することが可能となる。試料７が増量可能になることにより、本発明の課題で述べたような場合すなわちたった一つの粒子に多大な水和水が含まれていた場合であっても試料７が多量であれば粒子一つ一つの状態により測定結果が影響を受けてしまうことを抑制できる。 Moreover, there is no restriction | limiting in particular as the sample 7, For example, you may use the sample containing a hydrate. As described in the subject of the present invention, if the present embodiment is applied, the weight of the sample 7 is not limited. In this embodiment, the weighing mechanism is not placed in a reduced-pressure atmosphere as in the conventional TG-DTA apparatus (Patent Document 1), but inside the container 3 that constitutes a closed and reduced-pressure atmosphere. The weight of the placed sample 7 is measured under normal temperature and normal pressure. Therefore, it is sufficient to decompress only the container 3 in which the sample 7 is placed. As a result, the sample 7 can be increased by simply enlarging the container 3 without increasing the size of the apparatus. Since the amount of the sample 7 can be increased, even in the case described in the subject of the present invention, that is, even when a large amount of hydration water is contained in only one particle, if the amount of the sample 7 is large, It can suppress that a measurement result is influenced by each state.
減圧機構としては、容器３に連結可能であって容器３の内部を減圧可能なものであれば制限は無い。具体例を挙げると、減圧機構は真空ポンプ５、圧力計９およびガス排出導管２を備えてもよい。 The decompression mechanism is not limited as long as it can be connected to the container 3 and can decompress the inside of the container 3. As a specific example, the pressure reducing mechanism may include a vacuum pump 5, a pressure gauge 9, and a gas discharge conduit 2.
加熱炉１０としては、試料７の温度を変化させられるものであれば制限は無く、熱電対を用いたものや高周波誘導加熱を用いたものでも構わない。図１においては容器３の周囲に汎用の加熱炉１０を設けている。この加熱炉１０は、天地の天の方向（上方、上部）に、ガス排出導管２を通過させるための加熱炉貫通孔１４を設けている。なお、加熱炉貫通孔１４は密閉されていない、すなわち加熱炉１０の内部は大気雰囲気となっている。その一方、容器３の内部は密閉されており、真空ポンプ５およびガス排出導管２により減圧雰囲気となっている。 The heating furnace 10 is not limited as long as the temperature of the sample 7 can be changed, and may be one using a thermocouple or one using high frequency induction heating. In FIG. 1, a general-purpose heating furnace 10 is provided around the container 3. This heating furnace 10 is provided with a heating furnace through-hole 14 for allowing the gas discharge conduit 2 to pass in the top-to-bottom direction (upper and upper). In addition, the heating furnace through-hole 14 is not sealed, that is, the inside of the heating furnace 10 is an air atmosphere. On the other hand, the inside of the container 3 is hermetically sealed and a reduced pressure atmosphere is created by the vacuum pump 5 and the gas discharge conduit 2.
秤量機構としては、試料７を容器３ごと秤量可能な構成であれば制限は無い。図１においては、秤量機構は天秤１としている。
そして、天秤１のてこの一方には容器３を把持する把持機構および容器３が取り付けられている。つまり、図１においては加熱炉１０の内部において蓋６をされた容器３が把持機構さらに言うとガス排出導管２により吊り下げられている。そのため、図１においては容器３を把持する把持機構を構成するものとしては、蓋６に連結されたガス排出導管２、ガス排出導管２を天秤１のてこの一方に連結するコネクター８が挙げられる。
天秤１のてこのもう一方には重り（ここではロードセル４）が取り付けられている。このロードセル４の重量は、室温での把持機構、容器３および試料７の合計重量と等しい。この構成においては、加熱前の状態だと天秤１が釣り合っているが、加熱により水分が蒸発して試料７の重量が変化すると天秤１が傾くことになる。この天秤１の傾き量を読み取ることにより、減圧状態での温度変化に伴う重量の経時変化を測定することが可能となる。
The weighing mechanism is not limited as long as the sample 7 can be weighed together with the container 3. In FIG. 1, the weighing mechanism is a balance 1.
A gripping mechanism for gripping the container 3 and the container 3 are attached to one lever of the balance 1. That is, in FIG. 1, the container 3 with the lid 6 is suspended by the gripping mechanism, that is, the gas discharge conduit 2 inside the heating furnace 10. Therefore, in FIG. 1, what constitutes a gripping mechanism for gripping the container 3 includes a gas discharge conduit 2 connected to the lid 6 and a connector 8 for connecting the gas discharge conduit 2 to one of the levers of the balance 1. .
A weight (here, a load cell 4) is attached to the other side of the balance 1 lever. The weight of the load cell 4 is equal to the total weight of the gripping mechanism, the container 3 and the sample 7 at room temperature. In this configuration, the balance 1 is balanced in a state before heating, but the balance 1 is tilted when the weight of the sample 7 changes due to evaporation of moisture due to heating. By reading the amount of inclination of the balance 1, it is possible to measure a change in weight over time accompanying a temperature change in a reduced pressure state.
ちなみに、図１に記載の構造の場合、減圧機構すなわち真空ポンプ５およびガス排出導管２の重量の一部も天秤１のてこの一方に加わる可能性があるが、試験前に予め減圧機構のうちどれだけの重量が加わることになるのかを考慮に入れた上で、てこのもう一方に設けられるロードセル４の重量を設定しておけば特に問題は無い。 Incidentally, in the case of the structure shown in FIG. 1, a part of the weight of the decompression mechanism, that is, the vacuum pump 5 and the gas discharge conduit 2 may be added to one of the levers of the balance 1. There is no particular problem if the weight of the load cell 4 provided on the other side of the lever is set in consideration of how much weight is added.
以下、別の実施態様について図２を用いて説明する。図２に示すように、別の実施態様では、天秤１の代わりに台秤１１を使用する。 Hereinafter, another embodiment will be described with reference to FIG. As shown in FIG. 2, in another embodiment, a platform balance 11 is used instead of the balance 1.
以下、図２に記載の容器について一具体例として詳述する。図２においては、ねじ加工を施した容器３と蓋６により密閉式試料瓶３を使用する。密閉式試料瓶３は、ガス排出導管２と一体構造である容器支持棒１２と接合することができる。容器支持棒３の上部と密閉式試料瓶３の底部に加工してあるねじを締め合わせることにより内部を密閉し、ガス排出導管２を密閉式試料瓶３に挿入することができる構造となっている。なお、密閉度を上げるために必要に応じてＯリングを使用するのもよい。
容器支持棒１２の一方には真空ポンプ５が接続されており、真空ポンプ５を作動させて密閉式試料瓶３の内部を所望とする真空度に調整することができる。密閉式試料瓶３の真空度は圧力計９でモニター可能である。
Hereinafter, the container illustrated in FIG. 2 will be described in detail as a specific example. In FIG. 2, a hermetically sealed sample bottle 3 is used by a container 3 and a lid 6 that have been threaded. The hermetically sealed sample bottle 3 can be joined to a container support bar 12 that is integral with the gas discharge conduit 2. The inside of the container support bar 3 and the bottom of the sealed sample bottle 3 are fastened together to seal the inside, and the gas discharge conduit 2 can be inserted into the sealed sample bottle 3. Yes. Note that an O-ring may be used as necessary to increase the sealing degree.
A vacuum pump 5 is connected to one of the container support rods 12, and the vacuum pump 5 can be operated to adjust the inside of the sealed sample bottle 3 to a desired degree of vacuum. The degree of vacuum of the sealed sample bottle 3 can be monitored with a pressure gauge 9.
この場合の加熱炉１は、天地の地の方向（下方、下部）に、容器支持棒１２及びガス排出導管２を通過させるための加熱炉貫通孔１４を設けている。なお、加熱炉貫通孔１４は密閉されていない、すなわち加熱炉１０の内部は大気雰囲気となっている。その一方、容器３の内部は密閉されており、真空ポンプ５およびガス排出導管２により減圧雰囲気となっている。 The heating furnace 1 in this case is provided with a heating furnace through-hole 14 for allowing the container support rod 12 and the gas discharge conduit 2 to pass in the direction of the top and bottom (downward and lower). In addition, the heating furnace through-hole 14 is not sealed, that is, the inside of the heating furnace 10 is an air atmosphere. On the other hand, the inside of the container 3 is hermetically sealed and a reduced pressure atmosphere is created by the vacuum pump 5 and the gas discharge conduit 2.
ちなみに、図２に記載の構造の場合、減圧機構すなわち真空ポンプ５および容器支持棒１２を接続する減圧ホース１３の重量の一部も台秤４に加わる可能性があるが、試験前に予め減圧機構のうちどれだけの重量が加わることになるのかを考慮に入れた上で台秤４の重量を設定しておけば特に問題は無い。また、加熱炉１０は他の部材によって支持すればよく、例えば台座１５（図２中の点線）に加熱炉１０を載置したうえで、台座１５の内部に台秤１１を配置し、台座１５の上面を容器支持棒１２及びガス排出導管２が貫通する態様を採用しても構わない。 Incidentally, in the case of the structure shown in FIG. 2, a part of the weight of the decompression hose 13 connecting the decompression mechanism, that is, the vacuum pump 5 and the container support rod 12 may be added to the platform scale 4. There is no particular problem if the weight of the platform scale 4 is set in consideration of how much of the weight will be added. The heating furnace 10 may be supported by another member. For example, after placing the heating furnace 10 on the pedestal 15 (dotted line in FIG. 2), the pedestal 11 is disposed inside the pedestal 15, You may employ | adopt the aspect through which the container support rod 12 and the gas exhaust conduit 2 penetrate the upper surface.
その他、試料７の重量測定（特に試料７における水分量の測定）に供される公知の構成を適宜採用しても構わない。 In addition, a known configuration used for measuring the weight of the sample 7 (particularly, measuring the moisture content in the sample 7) may be appropriately adopted.
本実施形態の試料７の重量測定方法は、上記の重量測定装置を使用して、試料７を内部に載置した容器３の内部を減圧したまま試料７を容器３ごと秤量することにより、減圧状態での温度変化に伴う試料７の重量の経時変化を測定するものである。具体的には、容器３（密閉式試料瓶３）の内部を真空ポンプ５で減圧しながら加熱炉１０を稼働し、試料７を容器３ごと加熱する。そして、密閉式試料瓶３の内部に載置された試料７を真空乾燥する際に、試料７の重量変化を経時的に追跡する。 The weight measurement method for the sample 7 according to the present embodiment uses the above-described weight measurement apparatus to measure the sample 7 together with the container 3 while reducing the pressure inside the container 3 on which the sample 7 is placed. The change over time of the weight of the sample 7 accompanying the temperature change in the state is measured. Specifically, the heating furnace 10 is operated while the inside of the container 3 (sealed sample bottle 3) is depressurized by the vacuum pump 5, and the sample 7 is heated together with the container 3. Then, when the sample 7 placed in the sealed sample bottle 3 is vacuum-dried, the weight change of the sample 7 is traced over time.
以上の結果、本実施形態によれば、試料７の重量の制限を受けずに、減圧環境を維持したまま温度変化に伴う重量の経時変化が測定可能となり、ひいては、試料７の重量の制限を受けずに試料７の適正な乾燥条件を把握することが可能となる。 As a result of the above, according to the present embodiment, it is possible to measure the change over time of the weight accompanying a temperature change while maintaining the reduced pressure environment without being restricted by the weight of the sample 7, and thus, the weight of the sample 7 is restricted. It is possible to grasp the proper drying conditions of the sample 7 without receiving it.
１………天秤
２………ガス排出導管
３………容器（密閉式試料瓶）
４………ロードセル
５………真空ポンプ
６………（密閉式試料瓶用の）蓋
７………試料
８………コネクター
９………圧力計
１０……加熱炉
１１……台秤
１２……容器支持棒
１３……減圧ホース
１４……加熱炉貫通孔
１５……（加熱炉を支持する）台座
1 ... Balance 2 ... Gas exhaust conduit 3 ... Container (sealed sample bottle)
4 ......... Load cell 5 ......... Vacuum pump 6 ......... Cover 7 (for sealed sample bottle) ......... Sample 8 ......... Connector 9 ......... Pressure gauge 10 ... Heating furnace 11 ... Stage scale 12 ...... Vessel support bar 13 ...... Pressure reduction hose 14 ...... Heat-furnace through-hole 15 ...... (supporting the furnace) pedestal
Claims (6)
前記容器に連結されて前記容器の内部を減圧可能な減圧機構と、
試料を前記容器ごと秤量可能な秤量機構と、
を備えた、試料の重量測定装置。 A container in which a sample can be placed;
A decompression mechanism connected to the container and capable of decompressing the interior of the container;
A weighing mechanism capable of weighing the sample together with the container;
An apparatus for measuring the weight of a sample.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2017014135 | 2017-01-30 | ||
| JP2017014135 | 2017-01-30 |
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| Publication Number | Publication Date |
|---|---|
| JP2018124272A true JP2018124272A (en) | 2018-08-09 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2017241629A Pending JP2018124272A (en) | 2017-01-30 | 2017-12-18 | Sample weight measurement device and weight measurement method |
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| JP (1) | JP2018124272A (en) |
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2017
- 2017-12-18 JP JP2017241629A patent/JP2018124272A/en active Pending
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