JP2019215313A - Discomfort determination method of odor of kerosene oil composition, quality control method of kerosene oil composition, and manufacturing method of kerosene oil composition - Google Patents

Discomfort determination method of odor of kerosene oil composition, quality control method of kerosene oil composition, and manufacturing method of kerosene oil composition Download PDF

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JP2019215313A
JP2019215313A JP2018240571A JP2018240571A JP2019215313A JP 2019215313 A JP2019215313 A JP 2019215313A JP 2018240571 A JP2018240571 A JP 2018240571A JP 2018240571 A JP2018240571 A JP 2018240571A JP 2019215313 A JP2019215313 A JP 2019215313A
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hydrogen sulfide
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史弥 遠藤
Fumiya Endo
史弥 遠藤
靖智 三浦
Yasutomo Miura
靖智 三浦
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Cosmo Oil Co Ltd
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Abstract

To provide a method of appropriately determining the discomfort of the odor of a kerosene oil composition.SOLUTION: The discomfort determination method of the odor of a kerosene oil composition includes: a gas phase hydrogen sulfide concentration measurement process of inputting a kerosene oil composition as a quality evaluation target into a test container to produce a gas-liquid equilibrium state at a predetermined quality evaluation temperature, then collecting a gas phase in the test container, and measuring the hydrogen sulfide concentration in the collected gas phase; and a discomfort determination process of determining the discomfort of the kerosene oil composition as a quality evaluation target on the basis of the hydrogen sulfide concentration in the gas phase.SELECTED DRAWING: Figure 1

Description

本発明は、灯油組成物の臭気の不快度判定方法、灯油組成物の品質管理方法及び灯油組成物の製造方法に関し、詳しくは、灯油組成物から発生する臭気の不快度を判定する方法、不快臭の少ない灯油組成物の品質管理方法及び製造方法に関する。   The present invention relates to a method for determining the degree of discomfort of an odor of a kerosene composition, a method for controlling the quality of a kerosene composition, and a method for producing a kerosene composition, and more particularly, a method for determining the degree of discomfort of an odor generated from a kerosene composition, The present invention relates to a quality control method and a production method for a kerosene composition having a low odor.

灯油は、家庭用の暖房用燃料として広く使われているが、ストーブ、ファンヒーターへの給油等の灯油を取り扱う際に発生する臭気によって使用者が不快に感じる場合がある。   Kerosene is widely used as heating fuel for home use, but a user may feel uncomfortable due to odor generated when handling kerosene such as refueling a stove or a fan heater.

そして、灯油は揮発成分を含んでいるため、従来は、常温で、揮発する灯油中の成分が、不快臭のもとであると考えられていた(特許文献1等)。   Since kerosene contains a volatile component, it has been conventionally considered that a component in kerosene that volatilizes at normal temperature is a source of unpleasant odor (Patent Document 1 and the like).

そのため、従来は、灯油の不快臭を減らすには、揮発成分量をコントロールすることが重要であると考えられていた。   For this reason, conventionally, it has been considered that it is important to control the amount of volatile components in order to reduce the unpleasant odor of kerosene.

特開昭63−150380号公報JP-A-63-150380

ところが、本発明者らが、この灯油から生じる臭気の不快感について、鋭意検討を行ったところ、灯油の性状により、臭気を強く感じるものや、それほど強く臭気を感じないものがあるが、灯油の臭気の強さと、不快感とには、必ずしも相関がないことがわかった。   However, the present inventors have conducted intensive studies on the discomfort of the odor generated from this kerosene.Depending on the properties of the kerosene, some of them have a strong odor and others do not have such a strong odor. It was found that there was not always a correlation between the intensity of the odor and the discomfort.

そのため、灯油から生じる臭気の不快度を適切に判定する方法がなく、灯油から生じる不快臭が少ないという観点での品質管理が難しかった。また、不快臭の原因が不明確であったため、不快臭の少ない灯油を効率よく製造することが困難であった。   Therefore, there is no method for appropriately determining the degree of unpleasantness of the odor generated from kerosene, and it has been difficult to perform quality control from the viewpoint of reducing the unpleasant odor generated from kerosene. In addition, since the cause of the unpleasant odor was unclear, it was difficult to efficiently produce kerosene with less unpleasant odor.

従って、本発明の目的は、灯油組成物の臭気の不快度を適切に判定する方法を提供することにある。また、本発明の目的は、灯油組成物から生じる不快臭が少ないという観点での品質管理を行うことができる灯油組成物の品質管理方法を提供することにある。また、本発明の目的は、不快臭の発生の少ない灯油を効率よく製造することができる灯油組成物の製造方法を提供することにある。   Therefore, an object of the present invention is to provide a method for appropriately determining the degree of odor discomfort of a kerosene composition. It is another object of the present invention to provide a quality control method for a kerosene composition that can perform quality control from the viewpoint of reducing the unpleasant odor generated from the kerosene composition. Another object of the present invention is to provide a method for producing a kerosene composition which can efficiently produce kerosene with less unpleasant odor.

上記課題は、以下の本発明により解決される。
すなわち、本発明(1)は、品質評価対象の灯油組成物を、試験容器内に入れ、所定の品質評価温度で気液平衡状態にし、次いで、該試験容器内の気相を採取し、採取した気相中の硫化水素濃度を測定する気相硫化水素濃度測定工程と、
該気相中の硫化水素濃度により、該品質評価対象の灯油組成物の不快度を判定する不快度判定工程と、
を有することを特徴とする灯油組成物の臭気の不快度判定方法を提供するものである。
The above problem is solved by the present invention described below.
That is, in the present invention (1), the kerosene composition to be quality-evaluated is placed in a test container, brought into a gas-liquid equilibrium state at a predetermined quality evaluation temperature, and then the gas phase in the test container is collected and collected. Gas-phase hydrogen sulfide concentration measuring step of measuring the hydrogen sulfide concentration in the vapor phase,
An unpleasantness determining step of determining the unpleasantness of the kerosene composition of the quality evaluation target by the concentration of hydrogen sulfide in the gas phase,
It is intended to provide a method for judging the degree of discomfort of an odor of a kerosene composition, characterized by having:

また、本発明(2)は、前記気相硫化水素濃度測定工程において、硫化水素ガス検知管を用いて、前記試験容器内の気相を採取すると共に、採取した気相中の硫化水素濃度を測定することを特徴とする(1)の灯油組成物の臭気の不快度判定方法を提供するものである。   Further, in the present invention (2), in the gas-phase hydrogen sulfide concentration measurement step, the gas phase in the test container is sampled using a hydrogen sulfide gas detector tube, and the hydrogen sulfide concentration in the sampled gas phase is measured. It is intended to provide a method for judging the degree of discomfort of the odor of the kerosene composition according to (1), which is characterized by measuring.

また、本発明(3)は、品質評価対象の灯油組成物を、試験容器内に入れ、所定の品質評価温度で気液平衡状態にし、次いで、該試験容器内の気相を採取し、採取した気相中の硫化水素濃度を測定する気相硫化水素濃度測定工程と、
該品質評価対象の灯油組成物の臭気の不快感の有無を該気相中の硫化水素濃度により判断する工程であり、該気相中の硫化水素濃度が所定の合格基準値以下であった場合には、該品質評価対象の灯油組成物を合格品とし、該気相中の硫化水素濃度が所定の合格基準値を超えていた場合には、該品質評価対象の灯油組成物を不合格品とする品質評価工程と、
を有することを特徴とする灯油組成物の品質管理方法を提供するものである。
Further, in the present invention (3), the kerosene composition to be quality-evaluated is placed in a test container, brought into a gas-liquid equilibrium state at a predetermined quality evaluation temperature, and then the gas phase in the test container is collected and collected. Gas-phase hydrogen sulfide concentration measuring step of measuring the hydrogen sulfide concentration in the vapor phase,
This step is a step of judging the presence or absence of odor discomfort of the kerosene composition to be evaluated based on the concentration of hydrogen sulfide in the gas phase, and when the concentration of hydrogen sulfide in the gas phase is equal to or lower than a predetermined acceptable reference value. In the case where the kerosene composition to be evaluated for quality is regarded as a passing product, and if the concentration of hydrogen sulfide in the gas phase exceeds a predetermined passing reference value, the kerosene composition to be evaluated for quality is rejected. Quality evaluation process and
It is intended to provide a quality control method for a kerosene composition characterized by having:

また、本発明(4)は、前記気相硫化水素濃度測定工程において、硫化水素ガス検知管を用いて、前記試験容器内の気相を採取すると共に、採取した気相中の硫化水素濃度を測定することを特徴とする(3)の灯油組成物の品質管理方法を提供するものである。   Further, in the present invention (4), in the gas-phase hydrogen sulfide concentration measuring step, the gas phase in the test container is sampled using a hydrogen sulfide gas detector tube, and the hydrogen sulfide concentration in the sampled gas phase is measured. It is intended to provide a quality control method of the kerosene composition according to (3), wherein the quality is measured.

また、本発明(5)は、前記気相硫化水素濃度測定工程及び前記品質評価工程を行い、気相中の硫化水素濃度が所定の合格基準値以下と判断された灯油組成物と同一ロットの灯油組成物を合格品として出荷することを特徴とする(3)又は(4)いずれかの灯油組成物の品質管理方法を提供するものである。   Further, the present invention (5) performs the gas phase hydrogen sulfide concentration measurement step and the quality evaluation step, and performs the same lot of the kerosene composition in which the hydrogen sulfide concentration in the gas phase is determined to be equal to or less than a predetermined acceptable reference value. The present invention provides a quality control method for a kerosene composition according to any one of (3) and (4), wherein the kerosene composition is shipped as an acceptable product.

また、本発明(6)は、品質評価対象の灯油組成物を、試験容器内に入れ、所定の品質評価温度で気液平衡状態にし、次いで、該試験容器内の気相を採取し、採取した気相中の硫化水素濃度を測定する気相硫化水素濃度測定工程と、
該品質評価対象の灯油組成物の臭気の不快感の有無を該気相中の硫化水素濃度により判断する工程であり、該気相中の硫化水素濃度が所定の合格基準値以下であった場合には、該品質評価対象の灯油組成物を合格品とし、該気相中の硫化水素濃度が所定の合格基準値を超えていた場合には、該品質評価対象の灯油組成物を不合格品とする品質評価工程と、
該品質評価工程で不合格と判断された該品質評価対象の灯油組成物と同一ロットの灯油組成物(A)に、該品質評価工程で不合格と判断された該品質評価対象の灯油組成物とは異なるロットの灯油組成物(B)を混合することにより、合格品を得る混合工程と、
を有することを特徴とする灯油組成物の製造方法を提供するものである。
Further, in the present invention (6), the kerosene composition to be quality-evaluated is placed in a test container, brought into a gas-liquid equilibrium state at a predetermined quality evaluation temperature, and then the gas phase in the test container is collected and collected. Gas-phase hydrogen sulfide concentration measuring step of measuring the hydrogen sulfide concentration in the vapor phase,
This step is a step of judging the presence or absence of odor discomfort of the kerosene composition to be evaluated based on the concentration of hydrogen sulfide in the gas phase, and when the concentration of hydrogen sulfide in the gas phase is equal to or lower than a predetermined acceptable reference value. In the case where the kerosene composition to be evaluated for quality is regarded as a passing product, and if the concentration of hydrogen sulfide in the gas phase exceeds a predetermined passing reference value, the kerosene composition to be evaluated for quality is rejected. Quality evaluation process and
In the kerosene composition of the same lot as the kerosene composition of the quality evaluation object determined to be rejected in the quality evaluation step, the kerosene composition of the quality evaluation object determined to be rejected in the quality evaluation step Mixing a kerosene composition (B) from a different lot to obtain a passable product;
It is intended to provide a method for producing a kerosene composition characterized by having:

また、本発明(7)は、前記気相硫化水素濃度測定工程において、硫化水素ガス検知管を用いて、前記試験容器内の気相を採取すると共に、採取した気相中の硫化水素濃度を測定することを特徴とする(6)の灯油組成物の製造方法を提供するものである。   Further, in the present invention (7), in the gas-phase hydrogen sulfide concentration measuring step, the gas phase in the test container is sampled using a hydrogen sulfide gas detector tube, and the hydrogen sulfide concentration in the sampled gas phase is measured. It is intended to provide a method for producing a kerosene composition according to (6), which is characterized by measuring.

本発明によれば、灯油組成物の臭気の不快度を適切に判定する方法を提供することができる。本発明によれば、灯油組成物から生じる不快臭が少ないという観点での品質管理を行うことができる灯油組成物の品質管理方法を提供することができる。また、本発明によれば、不快臭の発生の少ない灯油を効率よく製造することができる灯油組成物の製造方法を提供することができる。   According to the present invention, it is possible to provide a method for appropriately determining the degree of odor discomfort of a kerosene composition. ADVANTAGE OF THE INVENTION According to this invention, the quality control method of the kerosene composition which can perform quality control from a viewpoint that the unpleasant odor which arises from a kerosene composition is small can be provided. Further, according to the present invention, it is possible to provide a method for producing a kerosene composition capable of efficiently producing kerosene having less unpleasant odor.

実施例の不快度と気相中の硫化水素濃度との関係を示すグラフである。4 is a graph showing the relationship between the degree of discomfort and the concentration of hydrogen sulfide in the gas phase in the example. 実施例の不快度と臭気強度との関係を示すグラフである。It is a graph which shows the relationship between the discomfort degree and the odor intensity | strength of an Example.

本発明の灯油組成物の臭気の不快度判定方法は、品質評価対象の灯油組成物を、試験容器内に入れ、所定の品質評価温度で気液平衡状態にし、次いで、該試験容器内の気相を採取し、採取した気相中の硫化水素濃度を測定する気相硫化水素濃度測定工程と、
該気相中の硫化水素濃度により、該品質評価対象の灯油組成物の不快度を判定する不快度判定工程と、
を有することを特徴とする灯油組成物の臭気の不快度判定方法である。
In the method for judging the degree of discomfort of the odor of the kerosene composition of the present invention, the kerosene composition to be quality-evaluated is placed in a test container, brought into a gas-liquid equilibrium state at a predetermined quality evaluation temperature, and Gas phase hydrogen sulfide concentration measuring step of collecting the phase and measuring the hydrogen sulfide concentration in the collected gas phase,
An unpleasantness determining step of determining the unpleasantness of the kerosene composition of the quality evaluation target by the concentration of hydrogen sulfide in the gas phase,
It is a method for judging the degree of discomfort of an odor of a kerosene composition, characterized by having:

本発明の灯油組成物の臭気の不快度判定方法は、気相硫化水素濃度測定工程と、不快度判定工程と、を有する。   The method for determining the unpleasantness of an odor of a kerosene composition according to the present invention includes a gas-phase hydrogen sulfide concentration measurement step and a discomfort degree determination step.

本発明の灯油組成物の臭気の不快度判定方法に係る気相硫化水素濃度測定工程では、先ず、品質評価対象の灯油組成物を、試験容器内に入れ、試験容器内の品質評価対象の灯油組成物を、所定の品質評価温度で気液平衡状態にする。   In the gas-phase hydrogen sulfide concentration measuring step according to the method for determining the degree of discomfort of the odor of the kerosene composition of the present invention, first, the kerosene composition to be quality-evaluated is placed in a test container, and the kerosene to be quality-evaluated in the test container The composition is brought into a vapor-liquid equilibrium state at a predetermined quality evaluation temperature.

本発明の灯油組成物の臭気の不快度判定方法に係る気相硫化水素濃度測定工程において、品質評価対象となる灯油組成物は、特に制限されず、通常、石油精製プロセスにて生成する灯油組成物であればよい。品質評価対象の灯油組成物としては、例えば、JIS K2203に規定の1号灯油又は2号灯油に相当する性状のものが挙げられる。品質評価対象の灯油組成物の物性値の例を挙げると、蒸留性状95%流出温度が210〜300℃、引火点が40〜50℃、銅版腐食(50℃、3h)が1以下、煙点が23〜25.5、硫黄分が0.0003〜0.0080質量%、密度が0.7850〜0.7950である。また、灯油組成物が保管される場所の温度は、通常20〜30℃程度である。また、灯油組成物が溶剤や洗浄剤等に使用される場合、使用環境の温度は、通常20〜30℃程度である。   In the gas-phase hydrogen sulfide concentration measuring step according to the method for judging the degree of discomfort of the odor of the kerosene composition of the present invention, the kerosene composition to be subjected to quality evaluation is not particularly limited, and is usually a kerosene composition produced in a petroleum refining process. Anything is good. Examples of the kerosene composition to be evaluated include those having properties equivalent to kerosene No. 1 or kerosene No. 2 specified in JIS K2203. Examples of the physical properties of the kerosene composition to be evaluated include a distillation property of 95%, an outflow temperature of 210 to 300 ° C, a flash point of 40 to 50 ° C, a copper plate corrosion (50 ° C, 3h) of 1 or less, and a smoke point. Is 23 to 25.5, the sulfur content is 0.0003 to 0.0080 mass%, and the density is 0.7850 to 0.7950. The temperature of the place where the kerosene composition is stored is usually about 20 to 30 ° C. When the kerosene composition is used for a solvent, a cleaning agent or the like, the temperature of the use environment is usually about 20 to 30 ° C.

現在、灯油組成物中の硫化水素濃度については規制値がなく、人体に対して十分に無害な範囲まで制限されて市場に出荷されている。そして、硫化水素は、非常に少量であっても、不快臭に対して大きく影響を与えるため、人体に対して十分に安全な硫化水素濃度に管理されていても、不快臭に対して影響を与える濃度との観点からは、市場に出荷されている灯油組成物中の硫化水素濃度のバラツキ範囲は大きい。このようなことから、現在、市場に出荷されている灯油組成物には、不快に感じるものと不快に感じないものが混在する状態となっている。そのため、本発明では、不快臭に対して影響を与える硫化水素濃度との観点から、不快度を判定している。   At present, there is no regulated value for the concentration of hydrogen sulfide in a kerosene composition, and it is shipped to the market with its concentration being harmless to human bodies. Hydrogen sulfide, even in a very small amount, has a significant effect on unpleasant odors. From the viewpoint of the given concentration, the range of the concentration of hydrogen sulfide in the kerosene composition shipped on the market is large. For this reason, kerosene compositions currently being shipped to the market are in a state where some of them feel unpleasant and some do not. For this reason, in the present invention, the degree of discomfort is determined from the viewpoint of the concentration of hydrogen sulfide that affects the unpleasant odor.

品質評価対象となる灯油組成物が入れられる試験容器は、所定の品質評価温度で、灯油組成物の気液平衡状態を維持できるものであれば、特に制限されない。試験容器としては、例えば、灯油保管用のポリタンク、ねじ口瓶等が挙げられる。試験容器には、密閉可能な気相吸引口が設けられていることが好ましい。   The test container in which the kerosene composition to be quality-evaluated is placed is not particularly limited as long as the kerosene composition can maintain a gas-liquid equilibrium state at a predetermined quality evaluation temperature. Examples of the test container include a plastic tank for storing kerosene, a screw-mouth bottle, and the like. The test container is preferably provided with a gas phase suction port that can be sealed.

本発明の灯油組成物の臭気の不快度判定方法に係る気相硫化水素濃度測定工程において、品質評価対象となる灯油組成物を、試験容器内で、気液平衡状態にするときの温度は、灯油組成物が取り扱われる場所の気温等の取り扱い温度に応じて設定される。灯油組成物が取り扱われる場所の取り扱い温度が非常に低い場合には、所定の品質評価温度は、その取り扱い温度に応じて低く設定され、また、灯油組成物が取り扱われる場所の取り扱い温度が比較的高い場合には、所定の品質評価温度は、その取り扱い温度に応じて高く設定される。例えば、灯油組成物の取り扱いが25℃前後で行われる場合には、所定の品質評価温度を25℃と設定する。また、例えば、出荷先での灯油組成物の保管及びストーブやファンヒーターへの給油が行われる場所の平均気温を25℃と見積もる場合には、所定の品質評価温度を20〜30℃の範囲内でいずれかの温度を選択し、所定の品質評価温度と設定する。   In the gas-phase hydrogen sulfide concentration measuring step according to the method for determining the unpleasantness of the odor of the kerosene composition of the present invention, the kerosene composition to be subjected to quality evaluation, in a test container, the temperature at which the vapor-liquid equilibrium state is set, It is set according to the handling temperature such as the temperature of the place where the kerosene composition is handled. When the handling temperature of the place where the kerosene composition is handled is very low, the predetermined quality evaluation temperature is set low according to the handling temperature, and the handling temperature of the place where the kerosene composition is handled is relatively low. If the temperature is high, the predetermined quality evaluation temperature is set high according to the handling temperature. For example, when the kerosene composition is handled at about 25 ° C., the predetermined quality evaluation temperature is set to 25 ° C. Further, for example, when estimating the average temperature of the place where the kerosene composition is stored at the shipping destination and the oil is supplied to the stove or the fan heater to be 25 ° C., the predetermined quality evaluation temperature is in the range of 20 to 30 ° C. To select one of the temperatures and set a predetermined quality evaluation temperature.

そして、本発明の灯油組成物の臭気の不快度判定方法に係る気相硫化水素濃度測定工程では、試験容器に、品質評価対象の灯油組成物を入れ、試験容器内で、品質評価対象の灯油組成物を、所定の品質評価温度において、気液平衡状態にする。試験容器内で品質評価対象の灯油組成物を気液平衡状態にする方法としては、特に制限されず、例えば、試験容器内に品質評価対象の灯油組成物を、所定の気相分の体積が残るような量入れ、密閉後、試験容器を所定の品質評価温度の場所にて放置して、試験容器内で、品質評価対象の灯油組成物を気液平衡状態にする方法や、所定の品質評価温度にされた試験容器に、所定の品質評価温度にされた品質評価対象の灯油組成物を、所定の気相分の体積が残るような量入れ、密閉後、試験容器を所定の品質管理温度に保持されている水浴に入れ、所定時間放置した後、試験容器を振とうさせる方法が挙げられる。所定の気相分の体積は、適宜選択される。なお、品質評価対象の灯油組成物の保存容器から、試験容器内に品質評価対象の灯油組成物を移す場合には、灯油組成物を移す方法としては、灯油組成物を移す際に、灯油組成物中の硫化水素の揮散が少ない方法ほど好ましい。   Then, in the gas-phase hydrogen sulfide concentration measuring step according to the method for judging the degree of discomfort of the odor of the kerosene composition of the present invention, the kerosene composition to be subjected to quality evaluation is put in a test container, and the kerosene to be subjected to quality evaluation is placed in the test container. The composition is brought into a vapor-liquid equilibrium state at a predetermined quality evaluation temperature. The method for bringing the kerosene composition to be subjected to quality evaluation into a gas-liquid equilibrium state in a test container is not particularly limited.For example, the kerosene composition to be subjected to quality evaluation in a test container may have a predetermined gas phase volume. After filling and sealing, the test container is allowed to stand at a predetermined quality evaluation temperature, and the kerosene composition to be subjected to the quality evaluation is set in a gas-liquid equilibrium state in the test container. The kerosene composition to be subjected to the quality evaluation at the predetermined quality evaluation temperature is put into the test container at the evaluation temperature in an amount such that a predetermined gaseous phase volume remains, and after sealing, the test container is subjected to predetermined quality control. A method in which the test container is shaken after being placed in a water bath maintained at a temperature and left for a predetermined time, is used. The volume of the predetermined gas phase is appropriately selected. When transferring the kerosene composition of the quality evaluation target from the storage container of the kerosene composition of the quality evaluation target into the test container, as a method of transferring the kerosene composition, when transferring the kerosene composition, The method in which the volatilization of hydrogen sulfide in the product is smaller is more preferable.

本発明の灯油組成物の臭気の不快度判定方法に係る気相硫化水素濃度測定工程では、次いで、試験容器内の気相を採取し、採取した気相中の硫化水素濃度を測定する。試験容器内の気相を採取し、採取した気相中の硫化水素濃度を測定する方法としては、特に制限されず、例えば、チューブを用いて、ガスサンプリングバッグに試験容器内の気相を採取し、次いで、ガスサンプリングバッグ内の気相を、GS−SCD(ガスクロマトグラフ−化学発光硫黄検出器)等の硫化水素の定量分析が可能な分析装置にて分析し、気相中の硫化水素濃度を測定する方法や、硫化水素ガス検知管を用いて、試験容器内の気相を吸引して採取すると同時に、検知管内の検知剤に気相を接触させて、気相中の硫化水素濃度を測定する方法が挙げられる。これらのうち、試験容器内の気相を採取し、採取した気相中の硫化水素濃度を測定する方法としては、硫化水素ガス検知管を用いて、試験容器内の気相を吸引して採取すると同時に、検知管内の検知剤に気相を接触させて、気相中の硫化水素濃度を測定する方法が、大型の分析装置を使用せず且つ試験容器の存在する場所で硫化水素濃度の測定が可能なので、簡便且つ迅速に気相中の硫化水素濃度を測定できる点で好ましい。硫化水素ガス採取器、検知管としては、特に制限されず、市販のものが適用可能である。硫化水素ガス検知管の規格としては、JIS K 0804が挙げられる。   In the gas-phase hydrogen sulfide concentration measuring step according to the method for judging the degree of discomfort of the odor of the kerosene composition of the present invention, the gas phase in the test container is sampled, and the hydrogen sulfide concentration in the sampled gas phase is measured. The method for collecting the gas phase in the test vessel and measuring the concentration of hydrogen sulfide in the collected gas phase is not particularly limited.For example, using a tube, collecting the gas phase in the test vessel into a gas sampling bag Then, the gas phase in the gas sampling bag is analyzed by an analyzer capable of quantitative analysis of hydrogen sulfide such as GS-SCD (Gas Chromatograph-Sulfur Chemiluminescence Detector), and the concentration of hydrogen sulfide in the gas phase is analyzed. Using a hydrogen sulfide gas detector tube, the gas phase in the test container is suctioned and collected, and at the same time, the gas phase is brought into contact with the detecting agent in the detector tube to reduce the hydrogen sulfide concentration in the gas phase. There is a method of measuring. Of these, the gas phase in the test vessel is sampled, and the concentration of hydrogen sulfide in the sampled gas is measured by using a hydrogen sulfide gas detector tube to aspirate the gas phase in the test vessel. At the same time, the method of measuring the concentration of hydrogen sulfide in the gas phase by contacting the gas phase with the detection agent in the detection tube is a method of measuring the concentration of hydrogen sulfide in a place where a test vessel is present without using a large analyzer. This is preferable because the concentration of hydrogen sulfide in the gas phase can be measured simply and quickly. The hydrogen sulfide gas sampling device and the detection tube are not particularly limited, and commercially available products can be applied. The standard of the hydrogen sulfide gas detector tube is JIS K 0804.

本発明の灯油組成物の臭気の不快度判定方法に係る不快度判定工程は、気相硫化水素濃度測定工程を行い得られる気相中の硫化水素濃度の測定結果により、品質評価対象の灯油組成物の不快度を判定する工程である。   The unpleasantness determination step according to the method for determining the unpleasantness of the odor of the kerosene composition of the present invention, the measurement result of the hydrogen sulfide concentration in the gas phase obtained by performing the gas phase hydrogen sulfide concentration measurement step, the kerosene composition of the quality evaluation target This is a step of determining the degree of discomfort of the object.

本発明の灯油組成物の品質管理方法に係る不快度判定工程では、予め定められている気相中の硫化水素濃度に対応する不快度尺度の値に基づいて、気相硫化水素濃度測定工程を行い得られる気相中の硫化水素濃度に対応する不快度尺度を決定し、品質評価対象の灯油組成物の不快度を判定する。例えば、表1に示すように、予め気相中の硫化水素濃度に対応する不快度尺度の値を定めておき、気相硫化水素濃度測定工程を行い得られる気相中の硫化水素濃度より、それに対応する不快度を決定する。   In the discomfort degree determination step according to the quality control method of the kerosene composition of the present invention, the gas phase hydrogen sulfide concentration measurement step is performed based on a value of a discomfort degree scale corresponding to a predetermined concentration of hydrogen sulfide in the gas phase. An unpleasantness scale corresponding to the obtained hydrogen sulfide concentration in the gas phase is determined, and the unpleasantness of the kerosene composition to be evaluated for quality is determined. For example, as shown in Table 1, the value of the discomfort scale corresponding to the concentration of hydrogen sulfide in the gas phase is determined in advance, and the concentration of hydrogen sulfide in the gas phase obtained by performing the gas-phase hydrogen sulfide concentration measurement step is as follows: Determine the corresponding degree of discomfort.

なお、気相中の硫化水素濃度と不快度尺度との対応関係は、灯油組成物の取り扱われ方等、灯油組成物の用途に応じて設定される。   The correspondence between the concentration of hydrogen sulfide in the gas phase and the degree of discomfort is set according to the use of the kerosene composition, such as how the kerosene composition is handled.

本発明の灯油組成物の品質管理方法は、品質評価対象の灯油組成物を、試験容器内に入れ、所定の品質評価温度で気液平衡状態にし、次いで、該試験容器内の気相を採取し、採取した気相中の硫化水素濃度を測定する気相硫化水素濃度測定工程と、
該品質評価対象の灯油組成物の臭気の不快感の有無を該気相中の硫化水素濃度により判断する工程であって、該気相中の硫化水素濃度が所定の合格基準値以下であった場合には、該品質評価対象の灯油組成物を合格品とし、該気相中の硫化水素濃度が所定の合格基準値を超えていた場合には、該品質評価対象の灯油組成物を不合格品とする品質評価工程と、
を有することを特徴とする灯油組成物の品質管理方法である。
The quality control method of the kerosene composition of the present invention comprises: placing a kerosene composition to be quality-evaluated in a test container, in a gas-liquid equilibrium state at a predetermined quality evaluation temperature, and then collecting a gas phase in the test container. And a gas phase hydrogen sulfide concentration measurement step of measuring the concentration of hydrogen sulfide in the collected gas phase,
A step of judging the presence or absence of odor discomfort of the kerosene composition to be evaluated based on the concentration of hydrogen sulfide in the gas phase, wherein the concentration of hydrogen sulfide in the gas phase is equal to or lower than a predetermined acceptable reference value. In this case, the kerosene composition to be evaluated for quality is regarded as an acceptable product, and if the concentration of hydrogen sulfide in the gas phase exceeds a predetermined acceptable reference value, the kerosene composition to be evaluated for quality is rejected. Quality evaluation process and
It is a quality control method of a kerosene composition characterized by having:

本発明の灯油組成物の品質管理方法は、気相硫化水素濃度測定工程と、品質評価工程とを有する。   The quality control method for a kerosene composition of the present invention includes a gas phase hydrogen sulfide concentration measurement step and a quality evaluation step.

本発明の灯油組成物の品質管理方法に係る気相硫化水素濃度測定工程は、本発明の灯油組成物の臭気の不快度判定方法に係る気相硫化水素濃度測定工程と同様である。   The gas-phase hydrogen sulfide concentration measurement step according to the kerosene composition quality control method of the present invention is the same as the gas-phase hydrogen sulfide concentration measurement step according to the odor unpleasantness determination method of the kerosene composition of the present invention.

本発明の灯油組成物の品質管理方法に係る品質評価工程は、品質評価対象の灯油組成物の臭気の不快感の有無を該気相中の硫化水素濃度により判断する工程であり、気相中の硫化水素濃度が所定の合格基準値以下であった場合には、品質評価対象の灯油組成物を合格品とし、気相中の硫化水素濃度が所定の合格基準値を超えていた場合には、品質評価対象の灯油組成物を不合格品とする工程である。   The quality evaluation step according to the kerosene composition quality control method of the present invention is a step of judging the presence or absence of odor discomfort of the kerosene composition to be evaluated based on the concentration of hydrogen sulfide in the gas phase. If the concentration of hydrogen sulfide is less than or equal to a predetermined acceptance criterion, the kerosene composition to be evaluated for quality is regarded as an acceptable product, and if the hydrogen sulfide concentration in the gas phase exceeds the predetermined acceptance criterion, In this step, the kerosene composition to be evaluated for quality is rejected.

本発明の灯油組成物の品質管理方法に係る品質評価工程において、気相中の硫化水素濃度の合格基準値は、灯油組成物の取り扱われ方等、灯油組成物の用途に応じて設定される。例えば、家庭用ヒーターに使用される1号品の場合には、気相中の硫化水素濃度の合格基準値は比較的高めに設定され、また、溶剤や洗浄剤として使用される2号品の場合には、気相中の硫化水素濃度の合格基準値は比較的低めに設定される。   In the quality evaluation step according to the quality control method of the kerosene composition of the present invention, the acceptance criterion value of the concentration of hydrogen sulfide in the gas phase is set according to the use of the kerosene composition, such as how the kerosene composition is handled. . For example, in the case of the first product used for home heaters, the acceptable standard value of the concentration of hydrogen sulfide in the gas phase is set relatively high, and the second product used as a solvent or a cleaning agent is used. In this case, the acceptable reference value for the concentration of hydrogen sulfide in the gas phase is set relatively low.

本発明の灯油組成物の品質管理方法では、品質評価工程において合格品と判断された灯油組成物が、小口の保管容器(例えば、灯油保管用ポリタンク)から採取した灯油組成物であった場合に、品質評価対象とした灯油組成物が充填されていた小口の保管容器内の灯油組成物のみを合格品として出荷することができる。また、本発明の灯油組成物の品質管理方法では、品質評価工程において合格品と判断された灯油組成物が、小口の保管容器から採取した灯油組成物であった場合に、品質評価対象とした灯油組成物と同一ロットの灯油組成物を合格品として出荷することができる。また、本発明の灯油組成物の品質管理方法では、品質評価工程において合格品と判断された灯油組成物が、灯油組成物の貯蔵タンクから採取した灯油組成物であった場合に、品質評価対象とした灯油組成物と同一ロットの灯油組成物を合格品として出荷することができる。なお、品質評価対象の灯油組成物と同一ロットの灯油組成物とは、品質評価対象の灯油組成物が、貯蔵タンクに貯蔵されていたときに、品質評価対象の灯油組成物と一緒に貯蔵されていた貯蔵タンク内の灯油組成物を指す。   In the quality control method of the kerosene composition of the present invention, when the kerosene composition determined to be acceptable in the quality evaluation step is a kerosene composition collected from a small storage container (for example, a kerosene storage plastic tank). In addition, only the kerosene composition in the small-sized storage container filled with the kerosene composition targeted for the quality evaluation can be shipped as an acceptable product. Further, in the quality control method of the kerosene composition of the present invention, when the kerosene composition determined to be acceptable in the quality evaluation step was a kerosene composition collected from a small-sized storage container, it was subjected to quality evaluation. A kerosene composition of the same lot as the kerosene composition can be shipped as an acceptable product. Further, in the kerosene composition quality control method of the present invention, when the kerosene composition determined to be acceptable in the quality evaluation step is a kerosene composition collected from a kerosene composition storage tank, the quality evaluation target The kerosene composition of the same lot as the kerosene composition described above can be shipped as an acceptable product. Note that the kerosene composition of the same lot as the kerosene composition of the quality evaluation target is stored together with the kerosene composition of the quality evaluation target when the kerosene composition of the quality evaluation target is stored in the storage tank. Refers to the kerosene composition in the storage tank that has been running.

従来は、灯油組成物からの不快臭の原因が、灯油組成物の取り扱い時等に発生する揮発成分であると考えられていたので、灯油組成物の不快臭を減らすために、揮発成分量をコントロールして、臭気の強さをコントロールすることが必要であると考えられていた。しかし、本発明者らが、灯油組成物から生じる臭気の不快感について、鋭意検討を行ったところ、灯油組成物の性状により、臭気を強く感じるものや、それほど強く臭気を感じないものがあるが、灯油組成物の臭気の強さ、言い換えると、揮発成分量と、不快感とには、必ずしも相関がなく、気相に揮発する硫化水素の量が、灯油組成物から生じる臭気の不快感と、よく相関することを見出した。つまり、本発明者らは、灯油組成物から生じる揮発成分の大部分を占める揮発性の炭化水素ではなく、灯油組成物から生じる揮発成分に含まれる少量の硫化水素が不快臭の原因となっていることを見出した。   Conventionally, it was thought that the cause of the unpleasant odor from the kerosene composition was a volatile component generated at the time of handling the kerosene composition and the like.In order to reduce the unpleasant odor of the kerosene composition, the volatile component amount was reduced. It was thought that it was necessary to control and control the odor intensity. However, the present inventors have conducted intensive studies on the discomfort of the odor generated from the kerosene composition, and depending on the properties of the kerosene composition, there are those that strongly sense the odor and those that do not strongly sense the odor. However, the intensity of the odor of the kerosene composition, in other words, the amount of volatile components and the discomfort are not necessarily correlated, and the amount of hydrogen sulfide that evaporates in the gas phase is unpleasant with the odor generated from the kerosene composition. And found that they correlated well. In other words, the present inventors have found that a small amount of hydrogen sulfide contained in the volatile components generated from the kerosene composition causes an unpleasant odor, instead of the volatile hydrocarbons that account for most of the volatile components generated from the kerosene composition. I found that.

そして、本発明の灯油組成物の臭気の不快度判定方法及び本発明の灯油組成物の品質管理方法では、不快臭の発生に強く影響を与える気相中の硫化水素濃度に着目しているので、灯油組成物の臭気の不快度の判定及び不快臭が少ない灯油組成物の品質管理を適切に行うことができる。更に、本発明の灯油組成物の品質管理方法では、灯油組成物の取り扱い時の温度に応じて、品質評価温度を設定し、且つ、灯油組成物の用途に応じて、硫化水素濃度の合格基準を設定するので、灯油組成物の取り扱い温度や用途に応じた品質管理を行うことができる。   The method for determining the degree of discomfort of the odor of the kerosene composition of the present invention and the method for controlling the quality of the kerosene composition of the present invention focus on the concentration of hydrogen sulfide in the gas phase, which strongly affects the generation of an unpleasant odor. Thus, it is possible to appropriately determine the degree of unpleasantness of the odor of the kerosene composition and appropriately control the quality of the kerosene composition having less unpleasant odor. Furthermore, in the quality control method of the kerosene composition of the present invention, the quality evaluation temperature is set according to the temperature at the time of handling the kerosene composition, and, according to the use of the kerosene composition, the passing standard of the hydrogen sulfide concentration. Is set, quality control can be performed according to the handling temperature and use of the kerosene composition.

一方、灯油組成物の揮発成分量や蒸気圧の分析、液相の灯油組成物中の硫黄分含有量や硫化水素含有量の測定から、不快の度合を推測する方法では、実際に灯油組成物が取り扱われる状態で、使用者が不快と感じるか否かを判断することが困難である。   On the other hand, in the method of estimating the degree of discomfort from the analysis of the volatile component amount and the vapor pressure of the kerosene composition, and the measurement of the sulfur content and the hydrogen sulfide content in the liquid kerosene composition, the kerosene composition is actually used. It is difficult to judge whether or not the user feels uncomfortable in a state where is handled.

本発明の灯油組成物の製造方法は、品質評価対象の灯油組成物を、試験容器内に入れ、所定の品質評価温度で気液平衡状態にし、次いで、該試験容器内の気相を採取し、採取した気相中の硫化水素濃度を測定する硫化水素濃度測定工程と、
該品質評価対象の灯油組成物の臭気の不快感の有無を該気相中の硫化水素濃度により判断する工程であり、該気相中の硫化水素濃度が所定の合格基準値以下であった場合には、該品質評価対象の灯油組成物を合格品とし、該気相中の硫化水素濃度が所定の合格基準値を超えていた場合には、該品質評価対象の灯油組成物を不合格品とする品質評価工程と、
該品質評価工程で不合格と判断された該品質評価対象の灯油組成物と同一ロットの灯油組成物(A)に、該品質評価工程で不合格と判断された該品質評価対象の灯油組成物とは異なるロットの灯油組成物(B)を混合することにより、合格品を得る混合工程と、
を有することを特徴とする灯油組成物の製造方法である。
In the method for producing a kerosene composition of the present invention, a kerosene composition to be subjected to quality evaluation is placed in a test container, brought into a gas-liquid equilibrium state at a predetermined quality evaluation temperature, and then a gas phase in the test container is collected. A hydrogen sulfide concentration measuring step of measuring the hydrogen sulfide concentration in the collected gas phase,
This step is a step of judging the presence or absence of odor discomfort of the kerosene composition to be evaluated based on the concentration of hydrogen sulfide in the gas phase, and when the concentration of hydrogen sulfide in the gas phase is equal to or lower than a predetermined acceptable reference value. In the case where the kerosene composition to be evaluated for quality is regarded as a passing product, and if the concentration of hydrogen sulfide in the gas phase exceeds a predetermined passing reference value, the kerosene composition to be evaluated for quality is rejected. Quality evaluation process and
In the kerosene composition of the same lot as the kerosene composition of the quality evaluation object judged as rejected in the quality evaluation step, the kerosene composition of the quality evaluation object judged as rejected in the quality evaluation step Mixing a kerosene composition (B) from a different lot to obtain a passable product;
It is a manufacturing method of the kerosene composition characterized by having.

本発明の灯油組成物の製造方法に係る気相硫化水素濃度測定工程及び品質評価工程は、本発明の灯油組成物の品質管理方法に係る気相硫化水素濃度測定工程及び品質評価工程と同様である。   The gas-phase hydrogen sulfide concentration measurement step and the quality evaluation step according to the production method of the kerosene composition of the present invention are the same as the gas-phase hydrogen sulfide concentration measurement step and the quality evaluation step according to the quality control method of the kerosene composition of the present invention. is there.

本発明の灯油組成物の製造方法に係る混合工程では、品質評価工程で不合格と判断された品質評価対象の灯油組成物と同一ロットの灯油組成物(A)に、品質評価工程で不合格と判断された品質評価対象の灯油組成物とは異なるロットの灯油組成物(B)を混合することにより、合格品を得る工程である。   In the mixing step according to the method for producing a kerosene composition of the present invention, the kerosene composition (A) of the same lot as the kerosene composition of the quality evaluation target judged to be rejected in the quality evaluation step is rejected in the quality evaluation step. This is a process of obtaining a good product by mixing a kerosene composition (B) of a lot different from that of the kerosene composition to be evaluated for quality.

混合工程において、品質評価対象とした灯油組成物と同一ロットの灯油組成物(A)とは、品質評価対象の灯油組成物が、貯蔵タンクに貯蔵されていたときに、品質評価対象の灯油組成物と一緒に貯蔵されていた貯蔵タンク内の灯油組成物を指す。また、品質評価対象とした灯油組成物とは異なるロットの灯油組成物(B)とは、(i)品質評価対象の灯油組成物が貯蔵されていた貯蔵タンクとは別の貯蔵タンクに貯蔵されていた灯油組成物、又は(ii)品質評価対象の灯油組成物が貯蔵されていた貯蔵タンクと同一の貯蔵タンクに貯蔵されていたが、品質評価対象の灯油組成物とは一緒には貯蔵されていなかった灯油組成物を指す。   In the mixing step, the kerosene composition of the same lot as the kerosene composition targeted for quality evaluation (A) refers to the kerosene composition targeted for quality evaluation when the kerosene composition targeted for quality evaluation is stored in a storage tank. Refers to the kerosene composition in a storage tank that has been stored with the product. The kerosene composition (B) of a lot different from the kerosene composition targeted for quality evaluation is stored in a storage tank different from the storage tank in which (i) the kerosene composition targeted for quality evaluation is stored. (Ii) the kerosene composition to be quality-evaluated was stored in the same storage tank as the storage tank in which the kerosene composition to be quality-evaluated was stored, but was stored together with the kerosene composition to be quality-evaluated. Refers to the kerosene composition that has not been used.

混合工程では、灯油組成物(A)に灯油組成物(B)を混合することにより、合格品と判断される灯油組成物を得る。そのため、灯油組成物(B)としては、灯油組成物(A)と同一の気相硫化水素濃度測定工程を行い気相中の硫化水素濃度を測定した場合に、気相中の硫化水素濃度が、灯油組成物(A)の気相中の硫化水素濃度より低いものが用いられる。つまり、灯油組成物(B)を、灯油組成物(A)と同一の気相硫化水素濃度測定工程を行い気相中の硫化水素濃度を測定した場合に、灯油組成物(B)の気相中の硫化水素濃度は、灯油組成物(A)の気相中の硫化水素濃度より低い。   In the mixing step, the kerosene composition (A) is mixed with the kerosene composition (B) to obtain a kerosene composition that is determined to be acceptable. Therefore, as the kerosene composition (B), when the same gas phase hydrogen sulfide concentration measurement step as that of the kerosene composition (A) is performed and the hydrogen sulfide concentration in the gas phase is measured, the hydrogen sulfide concentration in the gas phase is reduced. A kerosene composition (A) having a concentration lower than the concentration of hydrogen sulfide in the gas phase is used. That is, when the kerosene composition (B) is subjected to the same gas phase hydrogen sulfide concentration measurement step as that of the kerosene composition (A) to measure the hydrogen sulfide concentration in the gas phase, the gaseous phase of the kerosene composition (B) is The concentration of hydrogen sulfide in the gas is lower than the concentration of hydrogen sulfide in the gas phase of the kerosene composition (A).

混合工程において、灯油組成物(A)と灯油組成物(B)の混合割合は、灯油組成物(A)及び灯油組成物(B)の気相硫化水素濃度測定工程における気相中の硫化水素濃度、合格品の合格基準値等により、適宜選択され、混合後の灯油組成物が合格品と判断されるように、灯油組成物(A)と灯油組成物(B)の混合割合が選択される。   In the mixing step, the mixing ratio of the kerosene composition (A) and the kerosene composition (B) is determined by the hydrogen sulfide in the gas phase in the gas phase hydrogen sulfide concentration measurement step of the kerosene composition (A) and the kerosene composition (B). The mixing ratio of the kerosene composition (A) and the kerosene composition (B) is selected as appropriate according to the concentration, the pass standard value of the pass product, and the like so that the mixed kerosene composition is judged to be a pass product. You.

本発明の灯油組成物の製造方法では、灯油組成物の取り扱い時の温度及び灯油組成物の用途に応じて、不快臭が発生するおそれのある灯油組成物のみを的確に選択し、不快臭が発生し難い灯油組成物と混合することにより、不快臭の発生が少ない灯油組成物を得ることができるので、不快臭の発生が少ない灯油を効率よく製造することができる。   In the production method of the kerosene composition of the present invention, depending on the temperature at the time of handling the kerosene composition and the use of the kerosene composition, only the kerosene composition that may cause an unpleasant odor is appropriately selected, and the unpleasant odor is reduced. By mixing with a kerosene composition that does not easily generate, a kerosene composition with less unpleasant odor can be obtained, so that kerosene with less unpleasant odor can be efficiently produced.

以下に実施例を示して本発明を更に具体的に説明するが、本発明はこれに制限されるものではない。   Hereinafter, the present invention will be described more specifically with reference to Examples, but the present invention is not limited thereto.

(実施例)
<試験対象灯油組成物>
試験対象の灯油組成物として、試験対象灯油組成物A〜Gを用意した。
(Example)
<Kerosene composition to be tested>
Test kerosene compositions A to G were prepared as kerosene compositions to be tested.

<気液平衡状態の気相中の硫化水素濃度の測定>
密閉可能な気相吸引口及び通気口が取り付けられている1Lの試験容器に、試験対象灯油組成物Aを、空液比が1:1となるように張り込み、密閉した。次いで、試験容器を25℃±1℃に保たれた水浴中で、少なくとも2時間放置した。
放置後、試験容器を30秒間、激しく振とうさせ、振とうを止めた後、速やかに、気相吸引口に硫化水素ガス検知管を取り付け、試験容器内の気相を硫化水素ガス検知管内に導入し、硫化水素濃度を測定した。その結果を表2に示す。
また、試験対象灯油組成物B〜Gについても、同様に行った。その結果を表2に示す。
<Measurement of the concentration of hydrogen sulfide in the gas phase in a gas-liquid equilibrium state>
The kerosene composition A to be tested was placed in a 1 L test container equipped with a gas-phase suction port and a ventilation port capable of being sealed so that the air-liquid ratio was 1: 1 and sealed. The test vessel was then left in a water bath maintained at 25 ° C. ± 1 ° C. for at least 2 hours.
After standing, shake the test container vigorously for 30 seconds.After stopping the shaking, immediately attach a hydrogen sulfide gas detector tube to the gas phase suction port, and put the gas phase in the test container into the hydrogen sulfide gas detector tube. And the concentration of hydrogen sulfide was measured. The results are shown in Table 2.
Moreover, it carried out similarly about the kerosene composition BG for a test. The results are shown in Table 2.

<試験対象灯油組成物の臭気強度及び不快度の評価>
密閉可能な気相吸引口及び通気口が取り付けられている1Lの試験容器に、試験対象灯油組成物Aを、空液比が1:1となるように張り込み、密閉した。同時に、密閉可能な気相吸引口及び通気口が取り付けられている1Lの試験容器に、表3に示す性状のリファレンス灯油組成物を、空液比が1:1となるように張り込み、密閉した。次いで、両試験容器を25℃±1℃に保たれた水浴中に、少なくとも2時間放置した。
放置後、両試験容器を30秒間、激しく振とうさせ、振とうを止めた後、速やかに、両試験容器の通気口を開け、試験対象灯油組成物Aが入れられた試験容器の通気口に、鼻を近づけ、臭いをかぎ、臭気強度の評価を行った。また、リファレンス灯油組成物が入れられた試験容器の通気口と試験対象灯油組成物Aが入れられた試験容器の通気口に、交互に鼻を近づけ、それぞれの臭いをかぎ、不快度の評価を行った。
上記評価試験を、被験者を変えて、表2に示す被験者人数分行った。その結果を表2に示す。
また、試験対象灯油組成物B〜Gについても、同様に行った。その結果を表2に示す。
<Evaluation of odor intensity and discomfort level of kerosene composition to be tested>
The kerosene composition A to be tested was placed in a 1 L test container equipped with a gas-phase suction port and a ventilation port capable of being sealed so that the air-liquid ratio was 1: 1 and sealed. At the same time, a reference kerosene composition having the properties shown in Table 3 was placed in a 1-L test container equipped with a sealable gas-phase suction port and a vent so that the air-liquid ratio was 1: 1 and the container was sealed. . Both test containers were then left in a water bath maintained at 25 ° C. ± 1 ° C. for at least 2 hours.
After standing, both test containers were vigorously shaken for 30 seconds. After the shaking was stopped, the vents of both test containers were immediately opened, and the test container kerosene composition A was put into the test container vent. The nose was approached, the odor was smelled, and the odor intensity was evaluated. In addition, the nose was alternately approached to the vent of the test container containing the reference kerosene composition and the vent of the test container containing the kerosene composition A to be tested, smelling each odor, and evaluating the degree of discomfort. went.
The above evaluation test was performed for the number of subjects shown in Table 2 while changing the subjects. The results are shown in Table 2.
Moreover, it carried out similarly about the kerosene composition BG for a test. The results are shown in Table 2.

<臭気強度の評価>
「無臭」が「0点」、「やっと感知できる程度」が「1点」、「何の臭いかわかる弱い臭い」が「2点」、「楽に感知できる臭い」が「3点」、「強い臭い」が「4点」、「強烈な臭い」が「5点」との評価基準で行った。
<Evaluation of odor intensity>
“No odor” is “0”, “At last, the perceived odor” is “1”, “Weak smell that tells what odor” is “2”, “Easily detectable odor” is “3”, “Strong” The evaluation criteria were "smell" of "4 points" and "strong smell" of "5 points".

<不快度の評価>
リファレンス灯油組成物の不快度を「0」としたときに、リファレンス灯油組成物と比べ、「非常に不快」が「−3点」、「不快」が「−2点」、「やや不快」が「−1点」、「どちらでもない」が「0点」、「やや快」が「1点」、「快」が「2点」、「非常に快」が「3点」との評価基準で行った。
<Evaluation of degree of discomfort>
When the degree of discomfort of the reference kerosene composition is “0”, “very discomfort” is “−3”, “discomfort” is “−2”, and “slightly discomfort” compared to the reference kerosene composition. Evaluation criteria of "-1 point", "None", "0 point", "Slightly pleasant" is "1 point", "Pleasant" is "2 points", and "Very pleasant" is "3 points". I went in.

上記結果に基づき、不快度と気相中の硫化水素濃度との関係を図1に、不快度と臭気強度との関係を図2に示す。その結果、図1に示すように、不快度と気相中の硫化水素濃度との間には、良い相関見られた。一方、図2に示すように、不快度と臭気強度との間には、相関があるとまでは言えない結果であった。   Based on the above results, the relationship between the degree of discomfort and the concentration of hydrogen sulfide in the gas phase is shown in FIG. 1, and the relationship between the degree of discomfort and the odor intensity is shown in FIG. As a result, as shown in FIG. 1, a good correlation was found between the degree of discomfort and the concentration of hydrogen sulfide in the gas phase. On the other hand, as shown in FIG. 2, the results could not be said to have a correlation between the degree of discomfort and the odor intensity.

Claims (7)

品質評価対象の灯油組成物を、試験容器内に入れ、所定の品質評価温度で気液平衡状態にし、次いで、該試験容器内の気相を採取し、採取した気相中の硫化水素濃度を測定する気相硫化水素濃度測定工程と、
該気相中の硫化水素濃度により、該品質評価対象の灯油組成物の不快度を判定する不快度判定工程と、
を有することを特徴とする灯油組成物の臭気の不快度判定方法。
The kerosene composition to be subjected to quality evaluation is placed in a test container, brought into a gas-liquid equilibrium state at a predetermined quality evaluation temperature, and then the gas phase in the test container is collected, and the concentration of hydrogen sulfide in the collected gas phase is determined. A gas-phase hydrogen sulfide concentration measurement step to be measured;
An unpleasantness determining step of determining the unpleasantness of the kerosene composition of the quality evaluation target by the concentration of hydrogen sulfide in the gas phase,
A method for judging the degree of discomfort of an odor of a kerosene composition, comprising:
前記気相硫化水素濃度測定工程において、硫化水素ガス検知管を用いて、前記試験容器内の気相を採取すると共に、採取した気相中の硫化水素濃度を測定することを特徴とする請求項1記載の灯油組成物の臭気の不快度判定方法。   In the gas-phase hydrogen sulfide concentration measuring step, a gas phase in the test container is sampled by using a hydrogen sulfide gas detection tube, and a hydrogen sulfide concentration in the sampled gas phase is measured. 2. A method for judging the degree of discomfort of an odor of the kerosene composition according to 1. 品質評価対象の灯油組成物を、試験容器内に入れ、所定の品質評価温度で気液平衡状態にし、次いで、該試験容器内の気相を採取し、採取した気相中の硫化水素濃度を測定する気相硫化水素濃度測定工程と、
該品質評価対象の灯油組成物の臭気の不快感の有無を該気相中の硫化水素濃度により判断する工程であり、該気相中の硫化水素濃度が所定の合格基準値以下であった場合には、該品質評価対象の灯油組成物を合格品とし、該気相中の硫化水素濃度が所定の合格基準値を超えていた場合には、該品質評価対象の灯油組成物を不合格品とする品質評価工程と、
を有することを特徴とする灯油組成物の品質管理方法。
The kerosene composition to be subjected to quality evaluation is placed in a test container, brought into a gas-liquid equilibrium state at a predetermined quality evaluation temperature, and then the gas phase in the test container is collected, and the concentration of hydrogen sulfide in the collected gas phase is determined. A gas-phase hydrogen sulfide concentration measurement step to be measured;
This step is a step of judging the presence or absence of odor discomfort of the kerosene composition to be evaluated based on the concentration of hydrogen sulfide in the gas phase, and when the concentration of hydrogen sulfide in the gas phase is equal to or lower than a predetermined acceptable reference value. In the case where the kerosene composition to be evaluated for quality is regarded as a passing product, and if the concentration of hydrogen sulfide in the gas phase exceeds a predetermined passing reference value, the kerosene composition to be evaluated for quality is rejected. Quality evaluation process and
A quality control method for a kerosene composition, comprising:
前記気相硫化水素濃度測定工程において、硫化水素ガス検知管を用いて、前記試験容器内の気相を採取すると共に、採取した気相中の硫化水素濃度を測定することを特徴とする請求項3記載の灯油組成物の品質管理方法。   In the gas-phase hydrogen sulfide concentration measuring step, a gas phase in the test container is sampled by using a hydrogen sulfide gas detection tube, and a hydrogen sulfide concentration in the sampled gas phase is measured. 3. A quality control method for the kerosene composition according to 3. 前記気相硫化水素濃度測定工程及び前記品質評価工程を行い、気相中の硫化水素濃度が所定の合格基準値以下と判断された灯油組成物と同一ロットの灯油組成物を合格品として出荷することを特徴とする請求項3又は4いずれか1項記載の灯油組成物の品質管理方法。   Perform the gas phase hydrogen sulfide concentration measurement step and the quality evaluation step, and ship a kerosene composition of the same lot as the kerosene composition in which the hydrogen sulfide concentration in the gas phase is determined to be equal to or less than a predetermined acceptable reference value as an acceptable product. The quality control method for a kerosene composition according to any one of claims 3 and 4, characterized in that: 品質評価対象の灯油組成物を、試験容器内に入れ、所定の品質評価温度で気液平衡状態にし、次いで、該試験容器内の気相を採取し、採取した気相中の硫化水素濃度を測定する気相硫化水素濃度測定工程と、
該品質評価対象の灯油組成物の臭気の不快感の有無を該気相中の硫化水素濃度により判断する工程であり、該気相中の硫化水素濃度が所定の合格基準値以下であった場合には、該品質評価対象の灯油組成物を合格品とし、該気相中の硫化水素濃度が所定の合格基準値を超えていた場合には、該品質評価対象の灯油組成物を不合格品とする品質評価工程と、
該品質評価工程で不合格と判断された該品質評価対象の灯油組成物と同一ロットの灯油組成物(A)に、該品質評価工程で不合格と判断された該品質評価対象の灯油組成物とは異なるロットの灯油組成物(B)を混合することにより、合格品を得る混合工程と、
を有することを特徴とする灯油組成物の製造方法。
The kerosene composition to be subjected to quality evaluation is placed in a test container, brought into a gas-liquid equilibrium state at a predetermined quality evaluation temperature, and then the gas phase in the test container is collected, and the concentration of hydrogen sulfide in the collected gas phase is determined. A gas-phase hydrogen sulfide concentration measurement step to be measured;
This is a step of judging the presence or absence of odor discomfort of the kerosene composition to be evaluated based on the concentration of hydrogen sulfide in the gas phase, and when the concentration of hydrogen sulfide in the gas phase is equal to or lower than a predetermined acceptance criterion value. In the case where the kerosene composition to be evaluated for quality is regarded as a passing product, and if the concentration of hydrogen sulfide in the gas phase exceeds a predetermined passing reference value, the kerosene composition to be evaluated for quality is rejected. Quality evaluation process and
In the kerosene composition of the same lot as the kerosene composition of the quality evaluation object determined to be rejected in the quality evaluation step, the kerosene composition of the quality evaluation object determined to be rejected in the quality evaluation step Mixing a kerosene composition (B) from a different lot to obtain a passable product;
A method for producing a kerosene composition, comprising:
前記気相硫化水素濃度測定工程において、硫化水素ガス検知管を用いて、前記試験容器内の気相を採取すると共に、採取した気相中の硫化水素濃度を測定することを特徴とする請求項6記載の灯油組成物の製造方法。   In the gas-phase hydrogen sulfide concentration measuring step, a gas phase in the test container is sampled by using a hydrogen sulfide gas detection tube, and a hydrogen sulfide concentration in the sampled gas phase is measured. 7. A method for producing the kerosene composition according to item 6.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007031512A (en) * 2005-07-25 2007-02-08 Cosmo Oil Co Ltd Kerosene composition
JP2008024840A (en) * 2006-07-21 2008-02-07 Cosmo Oil Co Ltd Kerosene composition
US20100307428A1 (en) * 2007-05-11 2010-12-09 Christiane Behrendt Fuel composition

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007031512A (en) * 2005-07-25 2007-02-08 Cosmo Oil Co Ltd Kerosene composition
JP2008024840A (en) * 2006-07-21 2008-02-07 Cosmo Oil Co Ltd Kerosene composition
US20100307428A1 (en) * 2007-05-11 2010-12-09 Christiane Behrendt Fuel composition

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