KR100822454B1 - Manufacturing method of humidity indicator - Google Patents

Manufacturing method of humidity indicator Download PDF

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KR100822454B1
KR100822454B1 KR1020070088412A KR20070088412A KR100822454B1 KR 100822454 B1 KR100822454 B1 KR 100822454B1 KR 1020070088412 A KR1020070088412 A KR 1020070088412A KR 20070088412 A KR20070088412 A KR 20070088412A KR 100822454 B1 KR100822454 B1 KR 100822454B1
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humidity
solution
humidity indicator
silica
manufacturing
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KR1020070088412A
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Korean (ko)
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김철연
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(주) 에버스노
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
    • G01N31/222—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators for investigating moisture content
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00—Coated paper; Coating material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • G01N21/81—Indicating humidity

Abstract

A manufacturing method of a humidity indicator is provided to be adhered on a device like a refrigerant circulation system and to be eco-friendly by not using cobalt compound. A manufacturing method of a humidity indicator includes the steps of: forming gel phase by mixing distilled water and silica or silica base material; forming, drying, and sintering the mixture for manufacturing a carrier; manufacturing a humidity indication solution by adding sulphuric acid to a solution of BTB(BromoThymol Blue) and ethyl alcohol, wherein the humidity indication solution is capable of changing color thereof by humidity; mixing and solving lithium chloride in the humidity indication solution; impregnating the carrier in the humidity indication solution with the lithium chloride; and drying the carrier impregnated humidity indication solution with the lithium chloride.

Description

습도지시제의 제조방법{Manufacturing method of humidity indicator}Manufacturing method of humidity indicator

본 발명은 습도지시제의 제조방법에 관한 것으로, 증류수에 실리카 또는 실리카 기초물질을 혼합하여 겔(gel)상을 형성시킨 다음, 성형, 건조, 소성하여 담지체를 제조하는 제1 공정; 브로모티몰블루를 에틸알코올에 용해한 용액에 황산을 가하여 습도에 따라 변색이 가능한 습도지시용액을 제조하는 제2 공정; 및 제조된 습도지시용액에 염화리튬을 부가하고 교반, 용해한 후, 이 용액에 상기 제1 공정에서 제조한 담지체를 함침한 다음, 건조하는 제3 공정; 으로 이루어진다.The present invention relates to a method of manufacturing a humidity indicator, comprising: a first step of forming a support by mixing silica or silica-based material in distilled water to form a gel, followed by molding, drying, and baking; A second step of adding sulfuric acid to a solution in which bromothymol blue is dissolved in ethyl alcohol to produce a humidity indicating solution that can be discolored according to humidity; And a third step of adding lithium chloride to the prepared humidity indicator solution, stirring and dissolving the same, and impregnating the solution prepared in the first step into the solution, followed by drying; Is done.

상기 본 발명은 습기에 민감한 계(system)를 습기로부터 보호하기 위해 방습 및 제습이 요구되어질 경우 계의 안정성을 판단하기 위해 사용되는 습도지시제의 제조방법으로서, 코발트화합물을 사용하지 않아 환경 친화적이면서 기존의 압지를 이용한 습도지시카드와는 달리 상대습도에 따라 점진적으로 변화되는 양상을 나타냄으로써 시인성이 개선된 습도지시제를 제조할 수 있다.The present invention is a method of manufacturing a humidity indicator used to determine the stability of the system when moisture-proof and dehumidification is required to protect the moisture-sensitive system (system) from moisture, environmentally friendly without using a cobalt compound Unlike the humidity indicator card using a conventional blotting paper, it is possible to manufacture a humidity indicator with improved visibility by showing a gradual change according to relative humidity.

통상 반도체 또는 인쇄회로기판 등과 같이 실내의 습기로 인해 제품에 손상이 발생할 우려가 있는 제품의 포장 시에는 습도지시카드를 포장 내부에 함께 투입하여 피포장된 제품의 손상여부 및 포장상태를 판단하고 있다.In general, when packaging a product that may cause damage to the product due to moisture in a room such as a semiconductor or a printed circuit board, the humidity indication card is put together inside the package to determine whether the packaged product is damaged and the packaging state. .

상기 습도지시카드는 명함정도 크기의 압지에 인쇄(printing) 또는 첨착(impregnation)된 습도지시용액이 상대습도의 변화에 따라 변색되는 특성을 이용한 것이다.The humidity indicator card uses a characteristic in which the humidity indicator solution printed or impregnated on a squeezed paper of about the size of a business card is discolored according to the change of relative humidity.

현재 사용되고 있는 습도지시카드의 지시용액은 1984년에 제정된 미국방성 규격인 MIL-I-8835A에 따라 염화코발트(cobalt(Ⅱ) chloride) 수용액을 사용하는데, 이 지시용액은 건조 시에는 청색을 나타내다가 대기 중의 상대습도에 따라 수분을 흡수하게 되면 분홍색으로 변함으로써 해당되는 상대습도를 지시하게 된다.The indicator solution of the humidity indicator card currently used uses a cobalt (II) chloride solution according to the US Department of Defense standard, MIL-I-8835A, which was established in 1984. The indicator solution is blue when dried. When the moisture is absorbed according to the relative humidity in the air, it turns pink to indicate the corresponding relative humidity.

그러나 이러한 습도지시용액은 인체에 매우 유해하면서 환경오염을 유발시키는 염화코발트 수용액을 사용하기 때문에 유럽연합에서는 2000년 7월 1일부터 코발트화합물을 사용한 제품에 대한 판매가 규제되고 있다. However, since the humidity indicator solution uses cobalt chloride solution which is very harmful to the human body and causes environmental pollution, the EU has regulated the sale of products using cobalt compounds since July 1, 2000.

이러한 환경 하에서, 2007년 1월 염화코발트를 전혀 사용하지 않는 환경 친화적인 습도지시용액의 제조방법이 대한민국 특허 제0676777로 등록된 바 있다. Under these circumstances, in January 2007, a method for preparing an environmentally friendly humidity indicator solution using no cobalt chloride was registered in Korean Patent No. 0676777.

상기 특허는 티몰블루, 메틸오렌지, 메틸레드, 뉴트랄레드, 아닐린블루 중에서 한 가지를 선택하여 에틸알코올에 용해한 다음, 상기 용액에 가성소다 용액을 첨가하여 pH에 따라 지시용액의 색이 변화하도록 한 것으로, 상기 지시용액에 금속염화물 및 고분자 유기화합물 용액을 첨가하여 압지에 함침하는 방법으로 습도지시카드를 제조하였다.The patent selects one of thymol blue, methyl orange, methyl red, neutral red, and aniline blue to dissolve in ethyl alcohol, and then add caustic soda solution to the solution to change the color of the indicator solution according to pH. The humidity indicator card was prepared by adding a metal chloride and a polymer organic compound solution to the indicator solution and impregnating the blotter paper.

그러나, 상기한 방법으로 제조된 제품은 압지의 포장 및 흡습에 대한 지시는 가능하나 냉매순환시스템 등과 같은 장치에 부착하기에는 취약한 단점을 갖고 있어 본 발명을 개발하기에 이르렀다.However, the product produced by the above method is capable of instructing the packaging and moisture absorption of the blotter paper, but has a disadvantage in that it is vulnerable to being attached to a device such as a refrigerant circulation system.

본 발명은 코발트화합물을 사용하지 않아 환경 친화적이면서 기존의 압지를 이용한 습도지시카드와는 달리 상대습도에 따라 점진적으로 변화되는 양상을 나타냄으로써 시인성이 개선되고 냉매순환시스템 등과 같은 장치에도 부착 가능한 습도지시제를 제조하는 것을 목적으로 한다.The present invention is environmentally friendly and does not use a cobalt compound, and unlike the conventional humidity indicator card using a conventional blotting paper shows a mode that changes gradually depending on the relative humidity improved visibility and humidity indicator that can be attached to devices such as refrigerant circulation system It aims at manufacturing an agent.

본 발명에서는 습도지시용액 및 담지체의 제조와 담지체에 대한 습도지시용액의 함침을 포함하고, 습도지시용액은 변색제인 브로모티몰블루와 습도감응능력을 제시하는 황산 및 흡습성을 제공하는 조해성 물질인 염화리튬으로 구성하며, 습도지시제는 습도지시용액을 실리카 또는 실리카 기초물질을 소성하여 제조된 담지체에 함침하고 건조하여 완성하는 것이 특징이다.The present invention includes the preparation of the humidity indicator solution and the carrier and the impregnation of the humidity indicator solution to the carrier, the humidity indicator solution is a bromothymol blue as a colorant and sulfuric acid to provide a humidity sensitive ability and hygroscopic material that provides hygroscopicity Consists of lithium chloride, the humidity indicator is characterized in that the humidity indicator solution is impregnated in the carrier prepared by firing silica or silica base material and dried.

본 발명은 습기에 민감한 계를 습기로부터 보호하기 위해 방습 및 제습이 요구되어질 경우 계의 안정성을 판단하기 위해 사용되는 습도지시제의 제조방법으로서, 코발트화합물을 사용하지 않아 환경 친화적이면서 기존의 압지를 이용한 습도지시카드와는 달리 상대습도에 따라 점진적으로 변화되는 양상을 나타냄으로써 시인성이 개선되고 냉매순환시스템 등과 같은 장치에도 부착 가능한 습도지시제를 제조할 수 있다.The present invention is a manufacturing method of the humidity indicator used to determine the stability of the system when moisture-proof and dehumidification is required to protect the moisture-sensitive system from the moisture, it is environmentally friendly and does not use cobalt compounds Unlike the humidity indicator card used, the humidity indicator is gradually changed according to relative humidity, thereby improving visibility and manufacturing a humidity indicator that can be attached to a device such as a refrigerant circulation system.

본 발명은 습도를 판단하는 습도지시제의 제조방법에 있어서, The present invention provides a method of manufacturing a humidity indicator for determining the humidity,

증류수에 실리카 또는 실리카 기초물질을 혼합하여 겔(gel)상을 형성시킨 다음, 성형, 건조, 소성하여 담지체를 제조하는 제1 공정; Mixing a silica or silica base material with distilled water to form a gel phase, and then molding, drying, and firing to prepare a support;

브로모티몰블루를 에틸알코올에 용해한 용액에 황산을 가하여 습도에 따라 변색이 가능한 습도지시용액을 제조하는 제2 공정; 및 A second step of adding sulfuric acid to a solution in which bromothymol blue is dissolved in ethyl alcohol to produce a humidity indicating solution that can be discolored according to humidity; And

제조된 습도지시용액에 염화리튬을 부가하고 교반, 용해한 후, 이 용액에 기 제1 공정에서 제조한 담지체를 함침한 다음, 건조하는 제3 공정; 으로 이루어진 것이 특징이다.A third step of adding lithium chloride to the prepared humidity indicating solution, stirring and dissolving the same, and then impregnating the solution prepared in the first step into the solution, followed by drying; It is characterized by consisting of.

여기서, 상기 제1 공정에서 증류수에 혼합되는 실리카 또는 실리카 기초물질 10~60wt%로 혼합되는 것이 바람직하다.Here, it is preferable to mix with 10 to 60wt% of silica or silica base material mixed in distilled water in the first step.

그 이유는 실리카 또는 실리카 기초물질이 10wt% 미만이면 혼합물이 졸을 이루어 가공이 용이하지 않고, 실리카 또는 실리카 기초물질이 60wt%를 넘으면 혼합이 용이하지 않기 때문이다.This is because if the silica or silica base material is less than 10wt%, the mixture is sol and processing is not easy, and if the silica or silica base material is more than 60wt%, mixing is not easy.

또한, 상기 제1 공정에서의 건조 및 소성은 60~80℃에서 건조하여 400~700℃에서 소성하는 것이 좋다.In addition, the drying and firing in the first step is preferably dried at 60 ~ 80 ℃ and baked at 400 ~ 700 ℃.

상기 제2 공정에서 브로모티몰블루를 에틸알코올에 용해할 때 0.001~3.0wt%가 적당하고, 0.001wt% 보다 적으면 용액의 농도가 연하여 좋지 않다.When dissolving bromothymol blue in ethyl alcohol in the second step, 0.001 ~ 3.0wt% is appropriate, if less than 0.001wt% concentration of the solution is not good soft.

또한, 이 용액에 황산을 가할 때 황산은 브로모티몰블루를 기준으로 0.1~6.0wt%가 바람직하고 0.1wt% 미만이면 습도 지시에 있어서 민감한 반응을 하여 좋지 않고 반대로 6.0wt%를 초과할 경우 습도 지시에 둔하여 좋지 않다.In addition, when sulfuric acid is added to this solution, sulfuric acid is preferably 0.1 to 6.0 wt% based on bromothymol blue, and if it is less than 0.1 wt%, it is not good to react sensitively to humidity indication. It's not good at obeying instructions.

상기 제3 공정에서 습도지시용액에 염화리튬을 부가할 때 염화리튬은 브로모티몰블루를 기준으로 0.1~1wt%가 적당하고 0.1wt% 미만이면 시인성이 부족하여 좋지 않고 반대로 1wt%를 넘을 경우 제조된 지시제의 색상이 상기 범위의 색상보다 확연하지 않고 시인성 또한 부족하여 좋지 않다.When the lithium chloride is added to the humidity indicator solution in the third step, lithium chloride may be 0.1 to 1 wt% based on bromothymol blue, and less than 0.1 wt%. The color of the indicated indicator is not as pronounced as the color in the above range, and the visibility is also poor, which is not good.

상기 본 발명에서는 습도지시용액의 담지체로 실리카 또는 실리카 기초물질을 겔상으로 혼합하여 소성을 거쳐 제조하였다.In the present invention, the silica or silica-based material was mixed in a gel form as a carrier of the humidity indicator solution and then manufactured through firing.

또한, 본 발명의 습도지시용액의 제조에 사용한 브로모티몰블루는 pH에 따라 변색하는 지시약으로 변색범위는 pH 6.0~7.6이며, 산성에서 노란색을 염기성에서 파란색을 지시한다. 또한 염산, 황산, 질산과 함께 짙은 보라색을 나타낸다. 이러한 특성을 이용하여 기존의 가성소다 수용액을 사용한 습도지시용액의 제조와는 달리 황산을 사용하였다. In addition, bromothymol blue used in the preparation of the humidity indicator solution of the present invention is a indicator for discoloration according to pH, the discoloration range is pH 6.0 ~ 7.6, yellow to yellow from basic to blue. It is also dark purple with hydrochloric acid, sulfuric acid and nitric acid. By using these characteristics, sulfuric acid was used, unlike the preparation of the humidity indicator solution using the conventional caustic soda solution.

조해성 물질은 자발적인 흡습성을 지닌 물질을 말한다. 이런 특성은 상온에서 포화 수용액의 증기압이 대기 중의 수증기압보다 낮기 때문에 발생하며, 조해성 물질의 포화 수증기압과 습도의 함수로서 흡습성의 크기를 구분한다. 본 발명에 사용한 조해성 물질은 염화리튬으로 타 조해성 물질에 비하여 흡습성이 상당히 큰 것으로 알려져 있는 물질이다. Deliquescent substances refer to substances with spontaneous hygroscopicity. This property occurs because the vapor pressure of the saturated aqueous solution at room temperature is lower than the water vapor pressure in the atmosphere, and distinguishes the magnitude of hygroscopicity as a function of the saturated vapor pressure of the deliquescent material and the humidity. The deliquescent substance used in the present invention is lithium chloride, which is known to have a significantly higher hygroscopicity than other degradable substances.

이하, 실시예를 통하여 본 발명의 구성을 좀 더 상세히 설명한다.Hereinafter, the configuration of the present invention through the embodiment in more detail.

실시예Example

1. 담지체의 제조(제1 공정)1. Preparation of Carrier (First Step)

증류수 20g에 실리카 또는 실리카 기초물질 5g을 혼합하여 겔상을 형성시킨 다음, 도 1과 같이 본을 뜬다. 이어서, 상기물질을 70℃에서 건조하여 400~700℃에서 소성하여 담지체를 제조한다.20 g of distilled water is mixed with 5 g of silica or a silica base material to form a gel, and then an example is illustrated as shown in FIG. 1. Subsequently, the material is dried at 70 ° C. and calcined at 400 ° C. to 700 ° C. to prepare a carrier.

2. 습도지시용액의 제조(제2 공정)2. Preparation of humidity indicator solution (2nd step)

브로모티몰블루 85mg을 에틸알코올 100mL에 녹인 용액을 만든 다음, 이 용액에 황산을 브로모티몰블루를 기준으로 하여 0.1~6.0wt% 가하고, 습도에 따라 변색이 가능한 습도지시용액을 제조한다. A solution of 85 mg of bromothymol blue dissolved in 100 mL of ethyl alcohol is prepared, and sulfuric acid is added to the solution in an amount of 0.1 to 6.0 wt% based on bromothymol blue.

3. 습도지시용액의 함침(제3 공정)3. Impregnation of humidity indicator solution (3rd step)

상기 제2 공정에서 제조된 습도지시용액에 염화리튬을 브로모티몰블루를 기준으로 0.1~1wt%의 범위로 부가하고 교반하여 용해한 후, 이 용액에 상기 제1 공정에서 제조한 담지체를 3시간 이상 함침한 후 80℃에서 3시간 이상 건조하여 본 발명의 습도지시제를 얻었다. Lithium chloride was added to the humidity indicator solution prepared in the second step in the range of 0.1 to 1wt% based on bromothymol blue, stirred and dissolved, and then the carrier prepared in the first step was added to the solution for 3 hours. After the impregnation was carried out for more than 3 hours at 80 ℃ to obtain a humidity indicator of the present invention.

상기 실시예에서 얻어진 본 발명의 습도지시제는 도 1에 도시된 바와 같이 건조한 상태에서 짙은 보라색이며 수분을 흡수한 상태에서는 노란색으로 변색이 이루어지며, 기존의 압지를 이용한 습도지시카드와는 달리 도 2와 같이 상대습도에 따라 점진적으로 변화되는 양상을 보인다. Humidity indicator of the present invention obtained in the above embodiment is dark purple in the dry state as shown in Figure 1 and the color is changed to yellow in the state of absorbing moisture, unlike the conventional humidity indicator card using a blotting paper As shown in Fig. 2, it gradually changes according to relative humidity.

도 1은 본 발명의 습도지시제의 변색상태를 나타내는 사진1 is a photograph showing a discolored state of the humidity indicator of the present invention

도 2는 본 발명의 습도지시제가 상대습도에 따라 점진적으로 변화되는 양상을 나타내는 사진Figure 2 is a photograph showing the aspect of the humidity indicator gradually changes according to the relative humidity of the present invention

Claims (5)

증류수에 실리카 또는 실리카 기초물질을 혼합하여 겔(gel)상을 형성시킨 다음, 성형, 건조, 소성하여 담지체를 제조하는 제1 공정;Mixing a silica or silica base material with distilled water to form a gel phase, and then molding, drying, and firing to prepare a support; 브로모티몰블루를 에틸알코올에 용해한 용액에 황산을 가하여 습도에 따라 변색이 가능한 습도지시용액을 제조하는 제2 공정; 및A second step of adding sulfuric acid to a solution in which bromothymol blue is dissolved in ethyl alcohol to produce a humidity indicating solution that can be discolored according to humidity; And 제조된 습도지시용액에 염화리튬을 부가하고 교반, 용해한 후, 이 용액에 상기 제1 공정에서 제조한 담지체를 함침한 다음, 건조하는 제3 공정; 으로 이루어지는 것을 특징으로 하는 습도지시제의 제조방법 A third step of adding lithium chloride to the prepared humidity indicating solution, stirring and dissolving the same, and impregnating the solution prepared in the first step into the solution, followed by drying; Method for producing a humidity indicator, characterized in that consisting of 제1항에 있어서, The method of claim 1, 상기 제1 공정에서 증류수에 혼합되는 실리카 또는 실리카 기초물질은 10~60wt%로 혼합되는 것을 특징으로 하는 습도지시제의 제조방법In the first step, the silica or silica-based material mixed in the distilled water is mixed with 10 ~ 60wt% method of producing a humidity indicator 제1항에 있어서, The method of claim 1, 상기 제2 공정에서의 브로모티몰블루를 에틸알코올에 용해할 때의 브로모티몰블루 함량은 0.001~3.0wt%인 것을 특징으로 하는 습도지시제의 제조방법The method of producing a humidity indicator, characterized in that the bromo thymol blue content when dissolving bromo thymol blue in ethyl alcohol in the second step is 0.001 ~ 3.0wt%. 제1항에 있어서, The method of claim 1, 상기 제2 공정에서의 브로모티몰블루를 에틸알코올에 용해한 용액에 대하여 황산은 브로모티몰블루를 기준으로 0.1~6.0wt% 첨가되는 것을 특징으로 하는 습도지시제의 제조방법Sulfuric acid is a method of producing a humidity indicator, characterized in that the addition of 0.1 ~ 6.0wt% sulfuric acid based on bromothymol blue in the solution of bromothymol blue in the second step in ethyl alcohol 제1항에 있어서, The method of claim 1, 상기 제3 공정에서의 습도지시용액에 염화리튬을 부가할 때 염화리튬은 브로모티몰블루를 기준으로 0.1~1wt% 부가되는 것을 특징으로 하는 습도지시제의 제조방법When lithium chloride is added to the humidity indicator solution in the third step, the lithium chloride is added in an amount of 0.1 to 1 wt% based on bromothymol blue.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101165750B1 (en) 2010-06-15 2012-07-17 조미숙 Moisture indicator of pot
JPWO2021199668A1 (en) * 2020-03-31 2021-10-07

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JPS6480841A (en) * 1987-09-24 1989-03-27 Shirakawa Seisakusho Kk Humidity marker
KR20020022649A (en) * 1999-04-22 2002-03-27 이네오스 실리카스 리미티드 Humidity indicators
JP2002350419A (en) 2001-01-18 2002-12-04 Ooe Kagaku Kogyo Kk Humidity detection material, its manufacturing method and desiccant using humidity detection material
KR20060076124A (en) * 2004-12-29 2006-07-04 (주)지피엔이 The producing method of cobalt-free humidity indicating agent and its application

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Publication number Priority date Publication date Assignee Title
JPS6480841A (en) * 1987-09-24 1989-03-27 Shirakawa Seisakusho Kk Humidity marker
KR20020022649A (en) * 1999-04-22 2002-03-27 이네오스 실리카스 리미티드 Humidity indicators
JP2002350419A (en) 2001-01-18 2002-12-04 Ooe Kagaku Kogyo Kk Humidity detection material, its manufacturing method and desiccant using humidity detection material
KR20060076124A (en) * 2004-12-29 2006-07-04 (주)지피엔이 The producing method of cobalt-free humidity indicating agent and its application

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101165750B1 (en) 2010-06-15 2012-07-17 조미숙 Moisture indicator of pot
JPWO2021199668A1 (en) * 2020-03-31 2021-10-07

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