2 research outputs found
ΠΠΏΡΠΈΠΌΠΈΠ·Π°ΡΠΈΡ ΡΡΠ»ΠΎΠ²ΠΈΠΉ ΠΏΡΠΎΠ±ΠΎΠΏΠΎΠ΄Π³ΠΎΡΠΎΠ²ΠΊΠΈ Π΄Π»Ρ ΠΈΠΎΠ½ΠΎΡ ΡΠΎΠΌΠ°ΡΠΎΠ³ΡΠ°ΡΠΈΡΠ΅ΡΠΊΠΎΠ³ΠΎ ΠΎΠΏΡΠ΅Π΄Π΅Π»Π΅Π½ΠΈΡ Ρ Π»ΠΎΡΠΈΠ΄-ΠΈΠΎΠ½ΠΎΠ², Π²Ρ ΠΎΠ΄ΡΡΠΈΡ Π² ΡΠΎΡΡΠ°Π² Π²ΡΡΠΎΠΊΠΎΠΌΠΎΠ»Π΅ΠΊΡΠ»ΡΡΠ½ΡΡ ΠΎΡΠ³Π°Π½ΠΈΡΠ΅ΡΠΊΠΈΡ ΡΠΎΠ΅Π΄ΠΈΠ½Π΅Π½ΠΈΠΉ Π½Π΅ΡΡΠΈ
A procedure of sample preparation of oil samples for the determination of chloride ions, which are part of high-molecular organic compounds, has been developed. The procedure consists in the extraction of chloride ions from oil into the aqueous phase with a solution of sodium nitrate, followed by ionochromatographic detection. The work was performed on a high-performance LCβ20 Prominence liquid chromatograph with LC Solution software (Shimadzu, Japan), equipped with a conductometric detector (CDDβ10 Avp/10Asp), a 120Γ5 mm KanK-ASt14 ΞΌm separating column (GEOHI RAS, Russia) and a 200Γ6 mm SPS-SAC 50 suppression column ΞΌm (LLC PC Β«AquilonΒ», Russia). A carbonate buffer solution (2.5 mM Na2CO3 + 3.0 mM NaHCO3) was used as an eluent. The volume of the injected sample is 100 ΞΌl. The eluent flow rate was 2.0 ml/min. The temperature of the column thermostat is 33 Β°C. Under these conditions, satisfactory separation of fluoride, chloride, nitrate, and sulfate ions is achieved, and hydrogen sulfide does not have ionic forms and does not manifest ionochromatographically. Using the method of full factorial experiment, the main parameters determining the efficiency of extraction of chloride ions from the organic phase were optimized: extraction of 1 mM with an aqueous solution of NaNO3 at a temperature of 90 Β± 2 Β°C, the volume ratio of oil and extractant 1:10, extraction time 20 min. The developed procedure of sample preparation has been tested on model solutions and real oil samples. In comparison with the known methods, the combination of extraction isolation of organic chlorides with ionochromatographic detection makes it possible to significantly simplify the procedure for determining the analyte due to the high selectivity of the method without loss in sensitivity and measurement accuracyΠ Π°Π·ΡΠ°Π±ΠΎΡΠ°Π½ ΡΠΏΠΎΡΠΎΠ± ΠΏΡΠΎΠ±ΠΎΠΏΠΎΠ΄Π³ΠΎΡΠΎΠ²ΠΊΠΈ ΠΎΠ±ΡΠ°Π·ΡΠΎΠ² Π½Π΅ΡΡΠΈ Π΄Π»Ρ ΠΎΠΏΡΠ΅Π΄Π΅Π»Π΅Π½ΠΈΡ Ρ
Π»ΠΎΡΠΈΠ΄-ΠΈΠΎΠ½ΠΎΠ²,
Π²Ρ
ΠΎΠ΄ΡΡΠΈΡ
Π² ΡΠΎΡΡΠ°Π² Π²ΡΡΠΎΠΊΠΎΠΌΠΎΠ»Π΅ΠΊΡΠ»ΡΡΠ½ΡΡ
ΠΎΡΠ³Π°Π½ΠΈΡΠ΅ΡΠΊΠΈΡ
ΡΠΎΠ΅Π΄ΠΈΠ½Π΅Π½ΠΈΠΉ. Π‘ΠΏΠΎΡΠΎΠ± Π·Π°ΠΊΠ»ΡΡΠ°Π΅ΡΡΡ
Π² ΡΠΊΡΡΡΠ°ΠΊΡΠΈΠΎΠ½Π½ΠΎΠΌ Π²ΡΠ΄Π΅Π»Π΅Π½ΠΈΠΈ Ρ
Π»ΠΎΡΠΈΠ΄-ΠΈΠΎΠ½ΠΎΠ²
ΠΈΠ· Π½Π΅ΡΡΠΈ Π² Π²ΠΎΠ΄Π½ΡΡ ΡΠ°Π·Ρ ΡΠ°ΡΡΠ²ΠΎΡΠΎΠΌ Π½ΠΈΡΡΠ°ΡΠ° Π½Π°ΡΡΠΈΡ Ρ ΠΈΡ
ΠΏΠΎΡΠ»Π΅Π΄ΡΡΡΠΈΠΌ ΠΈΠΎΠ½ΠΎΡ
ΡΠΎΠΌΠ°ΡΠΎΠ³ΡΠ°ΡΠΈΡΠ΅ΡΠΊΠΈΠΌ Π΄Π΅ΡΠ΅ΠΊΡΠΈΡΠΎΠ²Π°Π½ΠΈΠ΅ΠΌ. Π Π°Π±ΠΎΡΡ Π²ΡΠΏΠΎΠ»Π½ΡΠ»ΠΈ Π½Π° Π²ΡΡΠΎΠΊΠΎΡΡΡΠ΅ΠΊΡΠΈΠ²Π½ΠΎΠΌ
ΠΆΠΈΠ΄ΠΊΠΎΡΡΠ½ΠΎΠΌ Ρ
ΡΠΎΠΌΠ°ΡΠΎΠ³ΡΠ°ΡΠ΅ LCβ20 Prominence Ρ ΠΏΡΠΎΠ³ΡΠ°ΠΌΠΌΠ½ΡΠΌ ΠΎΠ±Π΅ΡΠΏΠ΅ΡΠ΅Π½ΠΈΠ΅ΠΌ LC Solution (Shimadzu,
Π―ΠΏΠΎΠ½ΠΈΡ), ΡΠΊΠΎΠΌΠΏΠ»Π΅ΠΊΡΠΎΠ²Π°Π½Π½ΡΠΌ ΠΊΠΎΠ½Π΄ΡΠΊΡΠΎΠΌΠ΅ΡΡΠΈΡΠ΅ΡΠΊΠΈΠΌ Π΄Π΅ΡΠ΅ΠΊΡΠΎΡΠΎΠΌ (CDDβ10 Avp/10Asp), ΡΠ°Π·Π΄Π΅Π»ΡΡΡΠ΅ΠΉ
ΠΊΠΎΠ»ΠΎΠ½ΠΊΠΎΠΉ 120Γ5 ΠΌΠΌ ΠΠ°Π½Π-ΠΠ‘Ρ14 ΠΌΠΊΠΌ (ΠΠΠΠ₯Π Π ΠΠ, Π ΠΎΡΡΠΈΡ) ΠΈ ΠΏΠΎΠ΄Π°Π²ΠΈΡΠ΅Π»ΡΠ½ΠΎΠΉ ΠΊΠΎΠ»ΠΎΠ½ΠΊΠΎΠΉ 200Γ6 ΠΌΠΌ
Π‘ΠΠ‘-SAC 50 ΠΌΠΊΠΌ (ΠΠΠ ΠΠ Β«ΠΠΊΠ²ΠΈΠ»ΠΎΠ½Β», Π ΠΎΡΡΠΈΡ). Π ΠΊΠ°ΡΠ΅ΡΡΠ²Π΅ ΡΠ»ΡΠ΅Π½ΡΠ° ΠΏΡΠΈΠΌΠ΅Π½ΡΠ»ΠΈ ΠΊΠ°ΡΠ±ΠΎΠ½Π°ΡΠ½ΡΠΉ
Π±ΡΡΠ΅ΡΠ½ΡΠΉ ΡΠ°ΡΡΠ²ΠΎΡ (2,5 ΠΌΠ Na2CO3 + 3,0 ΠΌΠ NaHCO3). ΠΠ±ΡΠ΅ΠΌ Π²Π²ΠΎΠ΄ΠΈΠΌΠΎΠΉ ΠΏΡΠΎΠ±Ρ 100 ΠΌΠΊΠ». Π‘ΠΊΠΎΡΠΎΡΡΡ
ΠΏΠΎΡΠΎΠΊΠ° ΡΠ»ΡΠ΅Π½ΡΠ° ΡΠΎΡΡΠ°Π²Π»ΡΠ»Π° 2,0 ΠΌΠ»/ΠΌΠΈΠ½. Π’Π΅ΠΌΠΏΠ΅ΡΠ°ΡΡΡΠ° ΡΠ΅ΡΠΌΠΎΡΡΠ°ΡΠ° ΠΊΠΎΠ»ΠΎΠ½ΠΊΠΈ 33 Β°C. Π Π΄Π°Π½Π½ΡΡ
ΡΡΠ»ΠΎΠ²ΠΈΡΡ
Π΄ΠΎΡΡΠΈΠ³Π°Π΅ΡΡΡ ΡΠ΄ΠΎΠ²Π»Π΅ΡΠ²ΠΎΡΠΈΡΠ΅Π»ΡΠ½ΠΎΠ΅ ΡΠ°Π·Π΄Π΅Π»Π΅Π½ΠΈΠ΅ ΡΡΠΎΡΠΈΠ΄-, Ρ
Π»ΠΎΡΠΈΠ΄-, Π½ΠΈΡΡΠ°Ρ-, ΡΡΠ»ΡΡΠ°Ρ- ΠΈΠΎΠ½ΠΎΠ², Π° ΡΠ΅ΡΠΎΠ²ΠΎΠ΄ΠΎΡΠΎΠ΄
Π½Π΅ ΠΈΠΌΠ΅Π΅Ρ ΠΈΠΎΠ½Π½ΡΡ
ΡΠΎΡΠΌ ΠΈ ΠΈΠΎΠ½ΠΎΡ
ΡΠΎΠΌΠ°ΡΠΎΠ³ΡΠ°ΡΠΈΡΠ΅ΡΠΊΠΈ Π½Π΅ ΠΏΡΠΎΡΠ²Π»ΡΠ΅ΡΡΡ. Π‘ ΠΈΡΠΏΠΎΠ»ΡΠ·ΠΎΠ²Π°Π½ΠΈΠ΅ΠΌ ΠΌΠ΅ΡΠΎΠ΄Π° ΠΏΠΎΠ»Π½ΠΎΠ³ΠΎ
ΡΠ°ΠΊΡΠΎΡΠ½ΠΎΠ³ΠΎ ΡΠΊΡΠΏΠ΅ΡΠΈΠΌΠ΅Π½ΡΠ° ΠΎΠΏΡΠΈΠΌΠΈΠ·ΠΈΡΠΎΠ²Π°Π½Ρ ΠΎΡΠ½ΠΎΠ²Π½ΡΠ΅ ΠΏΠ°ΡΠ°ΠΌΠ΅ΡΡΡ, ΠΎΠΏΡΠ΅Π΄Π΅Π»ΡΡΡΠΈΠ΅ ΡΡΡΠ΅ΠΊΡΠΈΠ²Π½ΠΎΡΡΡ
ΠΈΠ·Π²Π»Π΅ΡΠ΅Π½ΠΈΡ Ρ
Π»ΠΎΡΠΈΠ΄-ΠΈΠΎΠ½ΠΎΠ²
ΠΈΠ· ΠΎΡΠ³Π°Π½ΠΈΡΠ΅ΡΠΊΠΎΠΉ ΡΠ°Π·Ρ: ΡΠΊΡΡΡΠ°ΠΊΡΠΈΡ 1ΠΌΠ Π²ΠΎΠ΄Π½ΡΠΌ ΡΠ°ΡΡΠ²ΠΎΡΠΎΠΌ NaNO3 ΠΏΡΠΈ
ΡΠ΅ΠΌΠΏΠ΅ΡΠ°ΡΡΡΠ΅ 90Β±2 Β°C, ΠΎΠ±ΡΠ΅ΠΌΠ½ΠΎΠ΅ ΡΠΎΠΎΡΠ½ΠΎΡΠ΅Π½ΠΈΠ΅ Π½Π΅ΡΡΠΈ ΠΈ ΡΠΊΡΡΡΠ°Π³Π΅Π½ΡΠ° 1:10, Π²ΡΠ΅ΠΌΡ ΡΠΊΡΡΡΠ°Π³ΠΈΡΠΎΠ²Π°Π½ΠΈΡ 20
ΠΌΠΈΠ½. Π Π°Π·ΡΠ°Π±ΠΎΡΠ°Π½Π½ΡΠΉ ΡΠΏΠΎΡΠΎΠ± ΠΏΡΠΎΠ±ΠΎΠΏΠΎΠ΄Π³ΠΎΡΠΎΠ²ΠΊΠΈ Π°ΠΏΡΠΎΠ±ΠΈΡΠΎΠ²Π°Π½ Π½Π° ΠΌΠΎΠ΄Π΅Π»ΡΠ½ΡΡ
ΡΠ°ΡΡΠ²ΠΎΡΠ°Ρ
ΠΈ ΡΠ΅Π°Π»ΡΠ½ΡΡ
ΠΎΠ±ΡΠ°Π·ΡΠ°Ρ
Π½Π΅ΡΡΠΈ. ΠΠΎ ΡΡΠ°Π²Π½Π΅Π½ΠΈΡ Ρ ΠΈΠ·Π²Π΅ΡΡΠ½ΡΠΌΠΈ ΠΌΠ΅ΡΠΎΠ΄Π°ΠΌΠΈ ΡΠΎΡΠ΅ΡΠ°Π½ΠΈΠ΅ ΡΠΊΡΡΡΠ°ΠΊΡΠΈΠΎΠ½Π½ΠΎΠ³ΠΎ Π²ΡΠ΄Π΅Π»Π΅Π½ΠΈΡ
ΠΎΡΠ³Π°Π½ΠΈΡΠ΅ΡΠΊΠΈΡ
Ρ
Π»ΠΎΡΠΈΠ΄ΠΎΠ² Ρ ΠΈΠΎΠ½ΠΎΡ
ΡΠΎΠΌΠ°ΡΠΎΠ³ΡΠ°ΡΠΈΡΠ΅ΡΠΊΠΈΠΌ Π΄Π΅ΡΠ΅ΠΊΡΠΈΡΠΎΠ²Π°Π½ΠΈΠ΅ΠΌ ΠΏΠΎΠ·Π²ΠΎΠ»ΡΠ΅Ρ ΡΡΡΠ΅ΡΡΠ²Π΅Π½Π½ΠΎ
ΡΠΏΡΠΎΡΡΠΈΡΡ ΠΏΡΠΎΡΠ΅Π΄ΡΡΡ ΠΎΠΏΡΠ΅Π΄Π΅Π»Π΅Π½ΠΈΡ Π°Π½Π°Π»ΠΈΡΠ° Π·Π° ΡΡΠ΅Ρ Π²ΡΡΠΎΠΊΠΎΠΉ ΡΠ΅Π»Π΅ΠΊΡΠΈΠ²Π½ΠΎΡΡΠΈ ΠΌΠ΅ΡΠΎΠ΄Π° Π±Π΅Π· ΠΏΠΎΡΠ΅ΡΠΈ
Π² ΡΡΠ²ΡΡΠ²ΠΈΡΠ΅Π»ΡΠ½ΠΎΡΡΠΈ ΠΈ ΡΠΎΡΠ½ΠΎΡΡΠΈ ΠΈΠ·ΠΌΠ΅ΡΠ΅Π½ΠΈ