Soluble tungsten compounds Determination in workplace air

2021 ◽  
Vol 37 (2) ◽  
pp. 181-200
Author(s):  
Paweł Wasilewski

Tungsten is a transition metal which occurs in the Earth’s crust as minerals which after being mined is extracted. There is no data on chronic effects of contact with tungsten, although fine tungsten powder is flammable and can cause mechanical irritation to skin and eyes. However, there are soluble tungsten compounds, which are classified as toxic, causing damage to the eyes, and being harmful to the aquatic environment. The aim of the study was to amend Standard No. PN-Z-04221-3 determination of soluble tungsten compounds in workplace air using spectrophotometric method with potassium thiocyanate. The amendment was performed because Standard No. PN-Z-04221-3 describes a method in which the quantification is 0.25 mg/m3, according to European Standard No. EN 482 the quantification of method must be in range of 0.1 – 2 mg/m3. The method is based on depositing soluble tungsten compounds on a cellulose esters filter and then dissolving them in water. Then tungsten is reduced with tin chloride, after reaction with potassium thiocyanate, tungsten becomes a complex. Tungsten complex should be extracted with isoamyl alcohol and then absorbance should be measured on a UV-Vis spectrophotometer. The tests were performed with the UV-Vis Heλios spectrophotometer by ThermoSpectronic model Beta. The validation requirements of European Standard No. EN 482 were met. With this method soluble tungsten compounds in air can be determined at concentration of 0.1 – 2 mg/m3. The limit of quantification (LOQ) is 1.875 ng. The overall accuracy of the method is 5.06% and its relative total uncertainty is 22.09%. The method for determining tungsten has been recorded in a form of an analytical procedure (see Appendix). This article discusses problems of occupational safety and health, which are covered by health sciences and environmental engineering.

2021 ◽  
Vol XXXVII (1) ◽  
pp. 49-75
Author(s):  
Anna Jeżewska ◽  
Agnieszka Woźnica

Benzidine is a white, crystalline solid. In the past, it was used mainly for the production of dyes, and nowadays in chemical analysis. Benzidine can cause bladder cancer to humans. The aim of this study was to develop a method for determining benzidine in workplace air, which will makes it possible to determine its concentrations at the lowest possible level. The method is based on the chemisorption of benzidine on a glass fiber filter treated with sulphuric acid(VI), extraction of benzidine disulphate with water and sodium hydroxide solution, and after extraction to the solid phase (SPE), benzidine is eluted from the SPE cartridge using 1 mL of methanol. The obtained solution is analyzed chromatographically. The tests were performed using a liquid chromatograph (HPLC) 1200 series of Agilent Technologies with a fluorescence detector (FLD). Determinations were performed using an Ultra C18 column (25 cm × 4.6 mm, dp = 5 µm). The procedure was validated according to Standard No. EN 482. The method can be used to determine benzidine in workplace air in the concentration range from 0.1 to 2 µg/m3. The limit of quantification (LOQ) is 0.25 ng/m3. The overall accuracy of the method was 5.36% and its relative total uncertainty was 23%. This method makes it possible to selectively determine benzidine in workplace air in the presence of most substances that do not show fluorescence, and in the presence of: biphenyl-4-amine, 1-naphthylamine and 2-naphthylamine, which show fluorescence. The method of determining benzidine has been recorded as an analytical procedure (see Appendix). This article discusses the problems of occupational safety and health, which are covered by health sciences and environmental engineering.


2021 ◽  
Vol XXXVII (1) ◽  
pp. 77-87
Author(s):  
Anna Jeżewska ◽  
Dorota Kondej

Dinitrotoluene (DNT) is a yellow, crystalline solid with a characteristic odor. It may consist of 6 isomers, but only two (2,4-DNT and 2,6-DNT) are of industrial importance. DNT can cause cancer. The aim of this study was to develop a method for the determination mixture of DNT isomers in workplace air, which will allow to determine its concentration at the level of 0.033 mg/m3. The method consists in stopping the mixture of dinitrotoluene isomers contained in the air on the glass fiber and the silica gel, extraction with methanol and chromatographic analysis of the obtained solution. The tests were carried out using a liquid chromatograph (HPLC) 1200 series from Agilent Technologies with a diode array detector (DAD). The method was validated in accordance with the requirements of the European Standard No. EN 482. The method allows the determination mixture of DNT isomers in the working environment air in the concentration range: 0.033 ÷ 0.66 mg/m3. The described method enables determination mixture of DNT isomers in the workplace air in the presence of: toluene-2,4-diamine, toluene-2,6-diamine, toluene-2,4-diyl diisocyanate, toluene-2,6-diyl diisocyanate and toluene. The method for determining dinitrotoluene has been recorded in the form of an analytical procedure (see Appendix). This article discusses the problems of occupational safety and health, which are covered by health sciences and environmental engineering.


2019 ◽  
Vol 36 (2(100)) ◽  
pp. 61-72
Author(s):  
Jolanta Surgiewicz

Calcium hydroxide is a white color solid. It is used in construction, chemical industry, water purification and wastewater treatment, flue gas desulphurization. Calcium hydroxide causes serious damage to the eyes, irritates the skin and it can cause after-launch respiratory irritation. Maximum allowable concentration value (MAC) for calcium hydroxide in the work environment in Poland, for the inhalable and respirable fraction is 2 mg/m3 (STEL is 6 mg/m3) and 1 mg/m3 (STEL is 4 mg/m3), respectively. The aim of the study was to develop a method for determining the concentration of calcium hydroxide present in the inhalable and respirable fraction in the workplaces atmosphere, in the range from 1/10 to 2 MAC values in accordance with the requirements of European Standard PN-EN 482. The developed method is based on collecting, stopping calcium hydroxide (contained in the inhalable and the respirable fraction) on membrane filters, mineralizing filters with concentrated nitric acid and determining calcium of the resulted solution by atomic absorption spectrometry with atomization in acetylene-air flame (F-AAS). The described method allows the determination of calcium in workplace air concentrations in the range of 0.50–20.00 µg/ml. The calibration curve characterized by a high value of the correlation coefficient: R2 = 1.0000. The limit of detection (LOD) is 0.1 ng/ml and the limit of quantification (LOQ) is 0.3 ng/ml. The determined coefficient of recovery is 1.00. An analytical method allows the determination of the concentration of the calcium hydroxide present in the workplace air in the inhalable fraction in the concentration range of 0.10–4.11 mg/m3 (sample air volume 720 L) and in the reparable fraction in the concentration range 0.07–2.70 mg/m3 (for a sample air volume of 684 L), which represents 0.05–2.1 MAC value for the inhalable fraction and 0.07–2.7 MAC value for the respirable fraction. The method has good precision and accuracy and meets the requirements of European Standard PN-EN 482 for procedures for determining chemical agents. The method for determining calcium hydroxide has been recorded in the form of an analytical procedure (see Appendix). This article discusses the problems of occupational safety and health, which are covered by health sciences and environmental engineering.


2020 ◽  
Vol 36 (1(103)) ◽  
pp. 113-125
Author(s):  
Anna Jeżewska ◽  
Agnieszka Woźnica

2-Nitroanisole is a colourless or slightly yellowish liquid. This substance is mainly used in the production of o-anisidine (2-methoxyaniline), which is directly or indirectly used for the production of more than 100 azo dyes. 2-Nitroanisole may cause cancer to humans. The aim of this study was to develop a method for determining concentrations of 2-nitroanisole in workplace air in the range from 1/10 to 2 of maximum admissible concentration (MAC) values. The developed method is based on the adsorption of 2-nitroanisole on a silica gel, extraction with methanol and chromatographic analysis of the resulting solution. The tests were performed using a liquid chromatograph (HPLC) 1200 series of Agilent Technologies with a diode array detector (DAD). Determinations were performed using an Ultra C18 column (25 cm × 4.6 mm, dp = 5 µm). The procedure was validated according to Standard No. EN 482. The method can be used to determine 2-nitroanisole in workplace air in the concentration range from 0.16 to 3.2 mg/m3, i.e., from 1/10 to 2 MAC values. In that range, the obtained calibration curve was linear, as evidenced by the regression coefficient of 1. The overall accuracy of the method was about 5.3% and its relative total uncertainty was 23%. This method enables selective determination of 2-nitroanisole in workplace air in the presence of other compounds, such as methanol, o-anisidine, 3-nitroanisole, 4-nitroanisole and 1-chloro-2-nitrobenzene. The method for determining 2-nitroanisole has been recorded in the form of an analytical procedure (see Appendix). This article discusses the problems of occupational safety and health, which are covered by health sciences and environmental engineering.


2019 ◽  
Vol 35 (1(99)) ◽  
pp. 5-18
Author(s):  
Anna Jeżewska ◽  
Agnieszka Woźnica

But-2-enal (crotonaldehyde) is a colourless liquid with an unpleasant suffocating odour. But-2-enal occurs naturally in food. It is mainly used for the production of sorbic acid, a food preservative. But-2-enal is a very toxic, highly irritating and allergenic substance – it is suspected of causing genetic defects. The aim of the study was to develop a method for determination of but-2-enal, which will enable determination of concentrations of this substance in the workplace air in the range from 1/10 to 2 MAC values. The tests were performed using a liquid chromatograph (HPLC) with a diode array detector (DAD), equipped with an Ultra C18 column (250 x 4.6 mm; 5 μm). The method consists in retaining the but-2-enal on a silica gel coated with 2,4-dinitrophenylhydrazine. The sample is extracted with acetonitrile and analyzed by HPLC. Validation of the method was carried out in accordance with the requirements of the European standard EN 482. The measuring range of the method is from 0.1 to 2 mg/m3 for a 12 l sample of air. The following validation parameters were obtained: limit of detection: 1.26 ng/ml (0.21 μg/m3), limit of quantification: 3.77 ng/ml (0.63 μg/m3), the overall accuracy of the method: 5.08%, expanded uncertainty: 22%. The developed analytical method enables selective determination of but-2-enal in workplace air at concentrations ranging from 0.1 mg/m3, i.e. from 1/10 of the MAC value in the presence of co-occurring substances. The method is characterized by good precision and accuracy and meets the requirements of the European standard PN-EN 482 for procedures for determination of chemical agents. The developed method of determining but-2-enal has been recorded as an analytical procedure (see Appendix). This article discusses the problems of occupational safety and health, which are covered by health sciences and environmental engineering.


2019 ◽  
Vol 36 (2(100)) ◽  
pp. 47-59
Author(s):  
Agnieszka Woźnica

Dimethyl phthalate (DMP) is a colourless liquid with a slight aromatic odour. It is used in industry as a plasticizer of plastics, as an ingredient of fragrances in the production of cosmetics and detergents. Occupational exposure to DMP can occur through inhalation, or ingestion. The aim of this study was to validate a method for determining DMP concentration in workplace air in the range from 1/10 to 2 MAC values, in accordance with the requirements of standard PN-EN 482. The study was performed using a gas chromatograph (GC) with a flame ionization detector (FID) equipped with a capillary column HP-INNOWAX (60 m x 0.25 mm, 0.15 µm). This method is based on the sorption of dimethyl phthalate vapours on a glass microfiber filter, desorption with ethanol, and analyzed by GC-FID. The average desorption efficiency of DMP from filter was 98%. Application of HP-INNOWAX column allows selective determination of DMP in the presence of other solvents. The measurement range was 0.5 – 10 mg/m3 for a 120-L air sample. Limit of detection: 0.02 µg/ml and limit of quantification: 0.06 µg/ml. The analytical method described in this paper enables a selective determination of DMP in workplace air in the presence of other solvents at concentrations from 0.5 mg/m3 (1/10 MAC value). The method is characterized by good precision and accuracy and meets the criteria for the performance of procedures for the measurement of chemical agents, listed in EN 482. The method may be used for the assessment of occupational exposure to DMP and the associated risk to workers’ health. The developed method of determining DMP has been recorded as an analytical procedure (see appendix). This article discusses the problems of occupational safety and health, which are covered by health sciences and environmental engineering.


1967 ◽  
Vol 50 (6) ◽  
pp. 1269-1273
Author(s):  
William L Hoover ◽  
Sonja C Dtjren

Abstract A procedure for determining low levels of molybdenum in fertilizers by atomic absorption is proposed. With potassium thiocyanate as complexing agent, molybdenum is extracted in an isoamyl alcohol fraction to separate the fraction containing molybdenum from the water-soluble fraction containing materials that would interfere in the atomic absorption procedure. However, the procedure cannot be used with samples that have high concentrations of iron. Tests on the recovery of molybdenum in four fertilizers indicate that the procedure is reliable to levels as low as 2.5 ppm of molybdenum


Author(s):  
Anna Jeżewska ◽  
Joanna Kowalska

Triglycidyl isocyanurate (TGIC) is a white solid in powder or granular form. TGIC does not occur naturally in the environment. It is intentionally manufactured and used as a crosslinking agent or hardener to produce polyester powder coatings. TGIC may cause genetic defects. This article presents the method of TGIC determination in workplace air using high-performance liquid chromatography (HPLC) with a diode-array detector (DAD). The method is based on the collection of TGIC present in the air on a polypropylene filter, extraction with acetonitrile, and chromatographic analysis of the solution obtained in this way. The determination was carried out in the reverse-phase system (mobile phase: acetonitrile: water) using an Ultra C18 column. The measurement range is 2 to 40 µg/m3 for a 720 liters air sample. Limit of detection (LOD) is 23 ng/m3 and limit of quantification (LOQ): 70 ng/m3. The method can be used for assessing occupational exposure to TGIC and associated risk to workers’ health.


2019 ◽  
Vol 35 (1(99)) ◽  
pp. 19-28
Author(s):  
Anna Jeżewska ◽  
Agnieszka Woźnica

Chlorobenzene is a colorless, flammable liquid that has an almond-like odor. It is used in industry as a solvent: resins, paints and fats, raw material for the production of plastics, as well as for the production of phenol, aniline and nitrobenzene. Occupational exposure to chlorobenzene vapors can occur through inhalation, absorption through the skin or ingestion. Harmful if inhaled, causes skin irritation. Long-term exposure affects the central nervous system. The aim of this study was an amendment to the PN-Z-04022- 03:2001 withdrawn from the Polish set of standards, and validate method for determination concentrations of chlorobenzene in the workplace air in the range from 1/10 to 2 MAC values, in accordance with the requirements of the standard PN-EN 482. The study was performed using a gas chromatograph (GC) with a flame ionization detector (FID) equipped with a capillary column HP-5 (30 m x 0.32 mm, 0.25 μm). This method is based on the adsorption of chlorobenzene vapors on activated charcoal, desorption with carbon disulfide, and analyzed by GC-FID. Application of HP-5 column allows selective determination of chlorobenzene in a presence of carbon disulfide, aniline, phenol and nitrobenzene. The measurement range was 2.3 ÷ 46 mg/m3 for a 15 l air sample. Limit of detection: 6.75 ng/ml and limit of quantification: 20.25 ng/ml. Analytical method described in this paper enables selective determination of chlorobenzene in workplace atmosphere in presence of other solvents at concentrations from 2.3 mg/m3 (1/10 MAC value). The method is characterized by good precision and accuracy and meets the criteria for the performance of procedures for the measurement of chemical agents, listed in EN 482. The method may be used for the assessment of occupational exposure to chlorobenzene and the associated risk to workers’ health. The developed method of determining chlorobenzene has been recorded as an analytical procedure (see Appendix). This article discusses the problems of occupational safety and health, which are covered by health sciences and environmental engineering.


Author(s):  
Anna Jeżewska

Propane-1,3-sultone (PS) is an alkylating substance used in the production of polymers, fungicides, insecticides, dyes, and detergents. It is absorbed into the human body by inhalation, digestion, and through the skin; it is also a possible carcinogen. Occupational exposure to this substance may occur on industrial or laboratory contact. In Poland, the maximum allowable concentration (MAC) for PS in workplace air is 7 µg/m3. The paper presents a method for determination of PS in workplace air using a gas chromatograph coupled with a mass spectrometer (GC-MS). Air containing PS is passed through a glass tube containing a glass fiber filter and two layers of silica gel. The substance is washed with acetonitrile and the solution obtained analysed using GC-MS. The measuring range for an air sample of 360 L is 0.7 ÷ 14 µg/m3. The limit of detection (LOD) is 13 ng/m3, limit of quantification (LOQ) is 40 ng/m3.


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