Offering innovative solutions for dynamically developing industries and markets is a strategic task for KHIMIK. Development and implementation of such solutions is impossible without fundamental research activities, applied research and creation of unique technological processes. These tasks are solved within the enterprise's research and development complex which consists of several specialized units.
Joint work of scientists and developers of the Engineering Center, specialists in the field of applied chemistry of the Testing Laboratory and production technologists, having a unique experience and knowledge, enables to solve the tasks of creating new products and technologies and their continuous improvement.
KHIMIK has been a leading Russian developer and manufacturer of repellent, insecticidal and acaricidal agents over the years. Many products created by the company are innovative and unrivaled. Before new products are brought to the market they go through a long cycle of laboratory and field research.
One of the main types of tests of repellent, insecticidal and acaricidal agents is a test for entomological effectiveness (protection against blood-sucking insects). This research is conducted by KHIMIK in cooperation with the leading Russian and world research companies and institutes in this field. The following is the certain research conducted as part of the development of new products:
Laboratory and experimental study of biological activity and evaluation of target effectiveness of the repellent agents developed within KHIMIK were conducted in 2002–2008 at the Research Center for Household Chemistry of the Research Institute “NICBYTKHIM” and at the Research Institute of Disinfectology (Federal State Institution Research Institute of Disinfectology of Rospotrebnadzor). Based on the research findings the effectiveness of the repellent category and the duration of the repellent effect on blood-sucking insects were determined, when applied to the skin and clothes, the spectrum of repellent action was determined. The research was conducted according to the methods described in the book “Methods for Determining the Effectiveness of Insecticides, Acaricides, Growth Regulators, and Repellents used in Medical Disinsection” (2004), the results were evaluated in accordance with the criteria described in the book “Standard Indicators of Safety and Effectiveness of the Disinfectants Subject to Control under Mandatory Certification” (1997). The activity of the agent against Aedes aeqypti mosquitoes of insectary culture (females aged 8–14 days on a carbohydrate diet) was evaluated under standard conditions: a cage (30 x 30 x 30 cm) with (50 ± 5) female mosquitoes bred in the insectarium. The research was conducted under laboratory conditions at air temperature 23–25 °C and relative humidity 56–60%. The effectiveness of the agent sample was compared with the standard of Category III of the repellent effectiveness. The research was conducted using “on the person” method when applying the agent sample and the standard on the skin of the naked forearm of test volunteers at the rate of consumption of 0.1 g per 100 cm2 of the test volunteer’s forearm. In the performance of the experiments, testers placed both hands with treated forearms in a cage and conducted 3-minute counts of the number of mosquito landings and bites. The experiment started one hour after application, was repeated every 30 minutes, and terminated after three or more mosquito bites per forearm were recorded during the three-minute count. The results of laboratory and experimental study of biological activity and evaluation of the target effectiveness of KHIMIK products are given in the table.
In 2002–2007 the Research Center for Household Chemistry of NICBYTKHIM CJSC conducted research of the following products: DETA Aerosol against Mosquitoes, DETA Lotion, Komaroff Lotion, Komaroff Gel. DETA Aerosol against Mosquitoes, DETA Lotion, Komaroff Lotion are recommended to protect people against attacks of blood-sucking insects (mosquitoes, gnats, midges, sand flies, horse flies and fleas) when applied to the skin and clothing. Komaroff Gel is recommended to protect people against attacks of blood-sucking insects (mosquitoes, midges, sand flies) when applied to the skin.
The research of DETA Sunscreen Milk was conducted in 2006. The product is recommended to protect people against attacks of blood-sucking insects (mosquitoes, gnats, midges, sand flies, horse flies and fleas) when applied to the skin.
The research of BABYDETA Baby Milk and BABYDETA Baby Cream was conducted in 2004. The products are recommended to protect adults and children against attacks of blood-sucking insects (mosquitoes, midges, sand flies) when applied to the skin.
The research of BABYDETA Baby Foam was conducted at the Research Institute of Disinfectology (FSI Research Institute of Disinfectology of Rospotrebnadzor) in 2008. The product is recommended to protect people against flying blood-sucking insects (mosquitoes, midges, sand flies) when applied to exposed parts of the body. The research of DETA Aerosol against Gnats and Ticks and DETA Special Aerosol was conducted in 2007. The conducted research shows that repellent agents DETA Aerosol against Gnats and Ticks and DETA Special Aerosol are highly effective in relation to taiga ticks – carriers of the tick-borne encephalitis pathogens and other dangerous diseases in the territory of the Russian Federation. The product is recommended for use to protect people against ixodic ticks (carriers of the tick-borne encephalitis and Lyme disease pathogens) and blood-sucking insects (mosquitoes, midges, sand flies, gnats, horse flies and fleas) when applied to exposed parts of the body, clothing and other fabric items.
The research conducted in 2008 shows that the repellent agent KOMAROFF Aerosol is recommended for use to protect people against blood-sucking insects (mosquitoes, midges, sand flies, gnats, horse flies and fleas) when applied to exposed parts of the body, clothing and other fabric items.
Time of protective effect against blood-sucking insects: when applied to skin – more than 4 hours, when applied to clothing – up to 20 days. Spectrum of repellent action: mosquitoes, midges, sand flies, gnats, horse flies, fleas.
Research Institute of Disinfectology (FSI Research Institute of Disinfectology of Rospotrebnadzor) conducted the research of acaricidal properties in 2004–2006. The research was conducted according to the methods described in the books “Methods of Testing Disinfectants to Assess their Safety and Effectiveness” (1998) and “Methods for Determining the Effectiveness of Insecticides, Acaricides, Growth Regulators, and Repellents used in Medical Disinsection” (2004). The results were evaluated in accordance with the criteria described in the book “Standard Indicators of Safety and Effectiveness of the Disinfectants Subject to Control under Mandatory Certification” (1997).
The acaricidal activity of the samples was evaluated in an active natural focus of TBE (tick-borne encephalitis) and ITBB (ixodic tick-borne borreliosis) in the Tyumen Region against taiga ticks Ixodes persulcatus P.Sch. under laboratory and field conditions. The number of ticks during the research period according to the standard recording data was 60–89 individuals per 1 accounting flag-kilometer. The experiments were conducted on active uninjured females of the taiga tick Ixodes persulcatus P.Sch. of the natural population. This tick species is the main carrier of tick-borne encephalitis virus and Lyme disease borrelia (ixodic tick-borne borreliosis) in the territory of Russia. The ticks collected from vegetation not more than 1 day before the experiments and stored in wet bandages at temperatures from +10 to +15 °C were used in the laboratory experiments.
The tests of DETA Aerosol against Ticks were conducted by the method of contacting ticks with the fabric treated with consumption rate of 24 s/m2 (or about 20 ml/m2) recommended for aerosol packaged agents. In the wild, taiga ticks, the carriers of pathogens of dangerous human diseases, are found on herbaceous plants, low bushes and cling to passing animals or people. The ticks, due to their inherent negative geotaxis, then crawl up the clothing until they have an opportunity to penetrate the body. The females usually adhere by suction 30–60 minutes after the attack. When studying the agent effectiveness, the testers wearing “pants” over their trousers, which were pre-treated by the aerosol cans with DETA Aerosol against Ticks, were walking through the forest with a large number of ticks and watching those of them which stuck to the “pants” in the ankle area. The tests were conducted 1, 7 and 14 days after treatment.
The agent showed high acaricidal activity while testing fabrics, with an action duration of 14 days. A pronounced knockdown effect was observed, which was a paresis of limbs and, consequently, a fall of ticks from the tested fabric. The conducted research show that acaricidal agent DETA Aerosol against Ticks is highly effective towards taiga ticks, the carriers of pathogens of tick-borne encephalitis and other dangerous diseases in the territory of the Russian Federation. The time of protective action against ticks is up to 15 days. The agent is recommended for use to protect people from ixodic ticks (the carriers of tick-borne encephalitis and Lyme disease pathogens) when treating clothing.
The research conducted in 2007 shows that repellent agent DETA Aerosol from Gnats and Ticks is highly effective towards taiga ticks, the carriers of pathogens of tick-borne encephalitis and other dangerous diseases in the territory of the Russian Federation. The product is recommended for use to protect people against ixodic ticks (carriers of the tick-borne encephalitis and Lyme disease pathogens) and blood-sucking insects (mosquitoes, midges, sand flies, gnats, horse flies and fleas) when applied to exposed parts of the body, clothing and other fabric items.
The research conducted in 2006 show that acaricidal agent KOMAROFF Anti-Tick is recommended for use to protect people against ixodic ticks (carriers of the tick-borne encephalitis and Lyme disease pathogens) under treatment of clothing and other fabric items. The time of protective action against ticks is up to 15 days.
Microbiology
Despite the intense industry development of modern construction technologies, wood remains one of the most widespread and highly-demanded building materials. For all its values wood has a significant disadvantage as a natural material. Untreated wooden structures are subject to weathering effect and biological damage.
By the beginning of 2011, within the framework of development of complex protection systems, KHIMIK Research Laboratories had developed two new products intended for biological protection of wooden surfaces.
KRONA Bio-impregnation is for effective long-term protection of interior and exterior wooden surfaces against biological damage (rot, mold, blueing) in conditions of condensation, periodic moistening and freezing. A distinctive feature of this product is that Bio-impregnation stops the biological damage that has already started.
KRONA Antizhuk Impregnation is intended for the long-term protection of interior and exterior wooden surfaces against wood-infesting insects. It destroys wood-infesting insects at all stages of their development. An additional function of this product is effective protection of wooden constructions against mold and blueing.
The development of these products, in addition to the creation of formulations and technologies, included a long and science-intensive stage of testing the functional properties of the compositions and confirming their protective effect. These works were carried out in cooperation with the leading Russian research institute in this field – Nizhny Novgorod State University named after N. I. Lobachevsky (NIIKh NNGU).
The final stage of testing was carried out in January 2011 in the Department of Biological Research of NIIKh NNGU. The main purpose of the tests was to check the fungicidal and fungus-resistant properties of the compositions.
The fungicidal property of a polymer composition is the ability of this material to cause the death of fungi-destructors. A composition with fungicidal properties is capable of not being subjected to the process of biodegradation by micromycetes even in the presence of external contaminants. The fungicidal property of a polymer composition is the ability of the said material not to serve as a food source for fungi-destructors, i.e., not to be subjected to biodegradation. However, in the presence of external contaminants that support the growth of fungi-destructors, the waste products of micromycetes can have a negative, destructive effect on the material.
The tests were carried out according to GOST 9.050-75 Paint and Varnish Coatings. The essence of the method is the application of compositions on a substrate of wood (pine) and incubation of coatings in the conditions optimal for the development of fungi with subsequent assessment of fungus resistance.
Methods of fungus resistance assessment according to GOST 9.050-75.
Sample preparation
10 samples of size 50*50 or 60*40 mm are prepared for testing. The paint and varnish coating is applied on both sides and on the edges in accordance with the recommendations for use specified in the regulatory documentation.
Fungal species:
- Aspergillus niger van Tieghem
- Aspergillus terreus Thom
- Alternaria alternate (Fr) Keissler
- Fusarium moniliforme Sheldon
- Penicillium brevicompactum Dierckx
- Penicillium chrysogenum Thom
- Penicillium funiculosum Thom
- Penicillium ochro-chloron Biourge
- Penicillium martensii Biourge
- Trichodema viride Pers ex.Fr
Test preparation:
Media for cultivation and storage of fungal cultures and tests are prepared according to GOST 9.048-89.
The dishes used for testing are prepared according to GOST 9.048-89.
Test performance
Suspension of fungi spores in water is prepared according to GOST 9.048-89.
Samples are cleaned from external contaminants. Cleaning is performed with a calico swab moistened with warm water heated to (50 ± 10) ºC with soap. If it is necessary to evaluate the effect of humidity on the resistance of coatings, the tested samples are sterilized beforehand. The methods that do not change the properties of the tested samples are used for sterilization. The samples are placed in a device providing the angle of inclination of samples 60º ± 15º or in a Petri dish. The distance between the samples in the device should be at least 20 mm. The devices or Petri dishes with samples are transferred to the box, and the sample surface is contaminated with an aqueous suspension of fungal spores by applying it evenly using a sprayer, avoiding the coalescence of drops. The contaminated samples are kept in the box at temperature (25 ± 10) ºC and relative humidity up to 80% until drops drying, but not more than 60 min. Samples and control Petri dishes are placed in a chamber or an exicator with water at the bottom. The chamber (desiccator) shall be closed. If it is necessary to assess the influence of air humidity, sterile samples are placed in sterile containers (Petri dishes, medical boxes, etc.) and sprayed with sterile distilled water using a sprayer. All containers are covered with lids. The tests are carried out at temperature (29 ± 2) ºC and relative humidity of more than 90%. Condensation of moisture, forced ventilation and exposure to direct natural or artificial light are not allowed in the chamber (exicator). Duration of tests after regime establishment is 28 days. After 5 days, the control Petri dishes are examined. If the fungi development is not observed on the nutrient medium, the fungal spores used for infection are considered non-viable. Tests are repeated on new samples with a newly prepared suspension from a new batch of fungi. In the future, every 7 days the chamber (desiccator) is opened for 3 min for air supply. On completion of the tests the samples are removed from the chamber (desiccator), examined with the naked eye in diffused light at illumination from 2,000 to 3,000 lux and at 56–60* magnification, and the fungus resistance of the coating is assessed on the intensity of fungi development on the samples on a 6-point scale according to GOST 9.048-89.
Processing of results
The maximum score, which is set for at least three samples, shall be taken as the test result. If the maximum score is set on a smaller number of samples, the test is repeated on new samples painted with paintwork material of the same batch.
A material is considered fungus resistant if it receives 0–2 points according to Method 1. Method 2 establishes the presence of fungicidal properties in the coating and assessment of fungus resistance of the coating in the presence of an additional source of nutrition by the degree of the surface destruction. When determining the fungus resistance of the coating by the degree of surface destruction, parallel tests for exposure to air humidity are conducted.
Sample preparation
Samples of 50*50 or 60*40 mm in size are prepared for testing. Paint and vanish coating is applied on both sides in accordance with the recommendations for use specified in the regulatory documentation. The edges of the samples intended for determination of fungus resistance of the coating by the degree of the surface destruction are protected with dark green enamel of EP-525 grade according to GOST 22438-85, protective enamel of EP-567 grade according to GOST 22369-77, dried at temperature (20 ± 2) ºC within 5 days. There should be at least five samples to determine the fungicidal properties of the coating. When determining the fungus resistance of the coating by the degree of surface destruction, the number of samples should be at least thirty, of which fifteen samples are used to determine the effect of humidity.
Test preparation
- The dishes, media, fungal cultures and control Petri dishes are prepared according to GOST 9.048-89.
- The Czapek-Dox medium and Czapek-Dox medium with agar are prepared according to GOST 9.048-89.
- To determine the fungicidal properties of the coating the Czapek-Dox medium with agar is poured into the Petri dishes in an amount of 20–30 cm3 and let it solidify.
- Samples are cleaned from external contaminants. Cleaning is carried out with a calico swab moistened with warm water heated to (50 ± 10) ºC with soap
If it is necessary to evaluate the effect of humidity on the resistance of coatings, the tested samples are sterilized beforehand. The methods that do not change the properties of the tested samples are used for sterilization.
- The samples are placed one by one in the Petri dishes.
- The samples are placed in a device that provides the angle of sample inclination 60º ± 15º at a distance of at least 20 mm from each other or one by one in the Petri dish.
Test performance
A suspension of fungal spores is prepared in the Czapek-Dox medium diluted with distilled water at a ratio of 1:15, or in the Czapek-Dox medium according to GOST 9.048-89. The devices with samples or Petri dishes are transferred to the box, and the sample surface is infected:
- when determining fungicidal properties – by the suspension of fungal spores in the Czapek-Dox medium, diluted with distilled water at a ratio of 1:15;
- when determining the fungus resistance of the coating by the degree of surface destruction – by the suspension of fungal spores in the Czapek-Dox medium.
Infestation is performed with aqueous suspension of fungal spores by applying it evenly using a sprayer, avoiding the coalescence of drops (similarly to Method 1). The contaminated samples are kept in the box at temperature (25 ± 10) ºC and relative humidity up to 80% until drops drying, but not more than 60 min. Samples and control Petri dishes are placed in a chamber or an exicator with water at the bottom. The chamber (desiccator) shall be closed. If it is necessary to assess the influence of air humidity, sterile samples are placed in sterile containers (Petri dishes, medical boxes, etc.) and sprayed with sterile distilled water using a sprayer. All containers are covered with lids. The tests are carried out at temperature (29 ± 2) ºC and relative humidity of more than 90%. Condensation of moisture, forced ventilation and exposure to direct natural or artificial light are not allowed in the chamber (exicator). Duration of tests as from establishing the regime to determine the fungicidal properties is 14 days.
Duration of tests as from establishing the regime to determine the fungus resistance by the degree of destruction of the coating surface is 84 days with interim assessment of fungus resistance of the coating every 28 days. In this case, 5 (five) samples are removed from the test, cleaned from mold fungi by washing with water, kept for 2 hours in the air and then examined with the naked eye and at 56–60* magnification. The degree of destruction of the coating surface associated with the fungi development is determined based on the evaluation of appearance according to the table and on the basis of comparison with the samples tested for exposure to air humidity. Only the side of the sample that has been sprayed with the fungal spore suspension is subjected to appearance evaluation. The tests are repeated after 7 days in case of absence or weak (without sporulation) development of fungi on the surface of the coating when determining the fungus resistance by the degree of surface destruction.
Processing of results
Paint and varnish coating has fungicidal properties, if an inhibitor zone (zone of absence of the fungi development) is observed around the sample on the nutrient medium, or the fungi development is observed on the sample surface or edges, evaluated by points 0 and 1 on a six-point scale according to GOST 9.048-89. The maximum score, which is set for at least 3 (three) samples at the final inspection, shall be taken as the test result. If the maximum score is set on a smaller number of samples, the test is repeated on new samples painted with paintwork material of the same batch.
The test results showed that KRONA Bio-impregnation and Antizhuk Impregnation fully correspond to the declared properties and can be successfully used to protect wood from damage caused by mold fungi. Since May 2011 the KHIMIK enterprise has been producing new products of the complex wood protection line: KRONA Bio-impregnation and Antizhuk Impregnation.