MD4488C1 - Method for determining the amount of potassium in pharmaceutical preparations - Google Patents
Method for determining the amount of potassium in pharmaceutical preparations Download PDFInfo
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- MD4488C1 MD4488C1 MDA20160049A MD20160049A MD4488C1 MD 4488 C1 MD4488 C1 MD 4488C1 MD A20160049 A MDA20160049 A MD A20160049A MD 20160049 A MD20160049 A MD 20160049A MD 4488 C1 MD4488 C1 MD 4488C1
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- Prior art keywords
- tetraphenylborate
- potassium
- excess
- amount
- pharmaceutical preparations
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- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 23
- 239000011591 potassium Substances 0.000 title claims abstract description 23
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000000825 pharmaceutical preparation Substances 0.000 title claims abstract description 12
- -1 sodium tetraphenylborate Chemical compound 0.000 claims abstract description 34
- 238000003918 potentiometric titration Methods 0.000 claims abstract description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 25
- 235000011164 potassium chloride Nutrition 0.000 claims description 8
- 239000001103 potassium chloride Substances 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 7
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004800 polyvinyl chloride Substances 0.000 claims description 6
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- CXVOIIMJZFREMM-UHFFFAOYSA-N 1-(2-nitrophenoxy)octane Chemical compound CCCCCCCCOC1=CC=CC=C1[N+]([O-])=O CXVOIIMJZFREMM-UHFFFAOYSA-N 0.000 claims description 2
- 229910001414 potassium ion Inorganic materials 0.000 abstract description 9
- 238000004448 titration Methods 0.000 abstract description 6
- 238000004313 potentiometry Methods 0.000 abstract description 5
- 239000000243 solution Substances 0.000 description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 6
- 239000011734 sodium Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 150000001768 cations Chemical class 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 239000012086 standard solution Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229910021607 Silver chloride Inorganic materials 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 230000002452 interceptive effect Effects 0.000 description 2
- 239000002555 ionophore Substances 0.000 description 2
- 230000000236 ionophoric effect Effects 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 2
- 210000002966 serum Anatomy 0.000 description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 2
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 description 2
- MITDXNUXOAYFGC-UHFFFAOYSA-N 1-prop-2-ynylbenzimidazole Chemical compound C1=CC=C2N(CC#C)C=NC2=C1 MITDXNUXOAYFGC-UHFFFAOYSA-N 0.000 description 1
- BBUPBICWUURTNP-UHFFFAOYSA-N 2,4-dimethyl-1-nitrobenzene Chemical group CC1=CC=C([N+]([O-])=O)C(C)=C1 BBUPBICWUURTNP-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical class [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 208000020131 Acid-base disease Diseases 0.000 description 1
- 101100283604 Caenorhabditis elegans pigk-1 gene Proteins 0.000 description 1
- 208000002682 Hyperkalemia Diseases 0.000 description 1
- 208000019025 Hypokalemia Diseases 0.000 description 1
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 206010003119 arrhythmia Diseases 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- BFGKITSFLPAWGI-UHFFFAOYSA-N chromium(3+) Chemical compound [Cr+3] BFGKITSFLPAWGI-UHFFFAOYSA-N 0.000 description 1
- GOCJWSXBGBQVSO-UHFFFAOYSA-K chromium(3+);2,2-dimethylpropanoate Chemical class [Cr+3].CC(C)(C)C([O-])=O.CC(C)(C)C([O-])=O.CC(C)(C)C([O-])=O GOCJWSXBGBQVSO-UHFFFAOYSA-K 0.000 description 1
- 230000001079 digestive effect Effects 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 208000035475 disorder Diseases 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000003834 intracellular effect Effects 0.000 description 1
- 235000013675 iodine Nutrition 0.000 description 1
- 229920000554 ionomer Polymers 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 208000018360 neuromuscular disease Diseases 0.000 description 1
- 150000002892 organic cations Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical class OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 1
- 125000005547 pivalate group Chemical group 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 208000024896 potassium deficiency disease Diseases 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
Invenţia se referă la o metodă potenţiometrică de determinare a conţinutului de potasiu şi poate fi aplicată pentru controlul calităţii preparatelor farmaceutice. The invention refers to a potentiometric method for determining the potassium content and can be applied to control the quality of pharmaceutical preparations.
Potasiul este cationul cel mai abundent intracelular, concentraţia normală în ser fiind de 3,5…5,0 mmol/L, iar în celulă de 150 mmol/L. Menţinerea echilibrului ionilor de potasiu în organism este foarte importantă pentru o funcţionare normală. Insuficienţa de K+ (<3,5 mmol/L) în ser se numeşte hipokaliemie, iar excesul de peste 5 mmol/L se numeşte hiperkaliemie, aceste devieri provoacă tulburări neuro-musculare, tulburări digestive, aritmie cardiacă etc. (J. Larry Jameson, Joseph Loscalzo. Harrison's Nephrology and Acid-Base Disorders. McGraw-Hill Medical, 2010, p. 65-72). Preparatele farmaceutice care conţin potasiu au diverse indicaţii terapeutice, controlul calităţii acestora este necesar pentru a nu admite o doză mai mare sau mai mică a acestor ioni. Acest fapt se realizează cu ajutorul metodelor de analiză cantitativă a ionilor de potasiu, inclusiv a metodelor potenţiometrice. Potassium is the most abundant intracellular cation, the normal concentration in the serum being 3.5...5.0 mmol/L, and in the cell 150 mmol/L. Maintaining the balance of potassium ions in the body is very important for normal functioning. Insufficiency of K+ (<3.5 mmol/L) in the serum is called hypokalemia, and excess over 5 mmol/L is called hyperkalemia, these deviations cause neuromuscular disorders, digestive disorders, cardiac arrhythmia, etc. (J. Larry Jameson, Joseph Loscalzo. Harrison's Nephrology and Acid-Base Disorders. McGraw-Hill Medical, 2010, p. 65-72). Pharmaceutical preparations containing potassium have various therapeutic indications, their quality control is necessary in order not to admit a higher or lower dose of these ions. This fact is achieved with the help of quantitative analysis methods of potassium ions, including potentiometric methods.
Se cunoaşte metoda potenţiometrică de determinare a conţinutului de potasiu, care include următoarele etape experimentale: a) la proba ce conţine cationi de K+ se adaugă un exces prestabilit de tetrafenilborat de potasiu; b) excesul de tetrafenilborat interacţionează cu o cantitate exactă de Ag+; c) excesul de Ag+ se titrează potenţiometric cu o soluţie standard de bromură de sodiu utilizând ca indicator un electrod Ag+-selectiv [1]. The potentiometric method for determining the potassium content is known, which includes the following experimental steps: a) a predetermined excess of potassium tetraphenylborate is added to the sample containing K+ cations; b) excess tetraphenylborate interacts with an exact amount of Ag+; c) the excess of Ag+ is titrated potentiometrically with a standard solution of sodium bromide using an Ag+-selective electrode as an indicator [1].
Dezavantajele acestei metode sunt numărul mare de etape experimentale care duc, eventual, la mărirea erorii analizei şi numărul mare de specii genante: toţi anionii care formează precipitate cu Ag+ (doar nitraţii şi acetaţii nu formează precipitate cu ionii de argint) şi cationii care interferează măsurările potenţiometrice. The disadvantages of this method are the large number of experimental steps that lead, possibly, to the increase of the analysis error, and the large number of interfering species: all the anions that form precipitates with Ag+ (only nitrates and acetates do not form precipitates with silver ions) and cations that interfere with the measurements potentiometric.
Se cunoaşte electrodul senzitiv la prezenţa tetrafenilboraţilor confecţionat în varianta membranei lichide în 4-nitro-m-xilen la firma Orion, care a fost testat pentru determinarea volumetrică a unor cationi organici din clasa sărurilor cuaternare de amoniu [2] şi a cationilor de natură organică din preparatele farmaceutice [3]. We know the electrode sensitive to the presence of tetraphenylborates made in the version of the liquid membrane in 4-nitro-m-xylene by the Orion company, which was tested for the volumetric determination of some organic cations from the class of quaternary ammonium salts [2] and cations of an organic nature from pharmaceutical preparations [3].
Cea mai apropiată soluţie de metoda propusă este determinarea potasiului utilizând electrodul terafenilborat senzitiv pe bază de [Cr3O(C5H9O2)6(C10H8N2)1,5][B(C6H5)4] [4]. The closest solution to the proposed method is the determination of potassium using the sensitive teraphenylborate electrode based on [Cr3O(C5H9O2)6(C10H8N2)1.5][B(C6H5)4] [4].
Dezavantajul acestei metode constă în aceea că electrodul propus nu este susceptibil pentru determinarea potasiului în preparatele farmaceutice. The disadvantage of this method is that the proposed electrode is not suitable for the determination of potassium in pharmaceutical preparations.
Problema pe care o rezolvă prezenta invenţie constă în elaborarea unei metode potenţiometrice pe baza unui electrod tetrafenilborat senzitiv de determinare a conţinutului de potasiu în preparatele farmaceutice. The problem that the present invention solves consists in the development of a potentiometric method based on a sensitive tetraphenylborate electrode for determining the potassium content in pharmaceutical preparations.
Esenţa invenţiei constă în faptul că se propune o metodă de determinare a conţinutului de potasiu în preparatele farmaceutice care prevede adăugarea în exces a unei cantităţi prestabilite de tetrafenilborat de sodiu la proba analizată, titrarea potenţiometrică a excesului de tetrafenilborat cu soluţie standard de clorură de potasiu, utilizând un electrod tetrafenilborat-senzitiv cu membrană pe bază de (µ3-oxo)-hexa(pivalato)-triaquatricrom(III) [Cr3O(C5H9O2)6(H2O)3][B(C6H5)4], şi calcularea conţinutului de potasiu în preparat conform diferenţei dintre cantitatea prestabilită şi excesul de tetrafenilborat. The essence of the invention consists in the fact that a method for determining the potassium content in pharmaceutical preparations is proposed which provides for the addition of a predetermined amount of sodium tetraphenylborate in excess to the analyzed sample, the potentiometric titration of the excess of tetraphenylborate with a standard solution of potassium chloride, using a tetraphenylborate-sensitive membrane electrode based on (µ3-oxo)-hexa(pivalato)-triaquatrichromium(III) [Cr3O(C5H9O2)6(H2O)3][B(C6H5)4], and calculating the potassium content in the preparation according to the difference between the predetermined amount and the excess of tetraphenylborate.
Rezultatul tehnic al prezentei invenţii constă în elaborarea unei metode şi a unui electrod corespunzător pentru determinarea ionilor de potasiu în preparatele farmaceutice. The technical result of the present invention consists in the development of a method and an appropriate electrode for the determination of potassium ions in pharmaceutical preparations.
Metoda de determinare a conţinutului de potasiu în preparatele farmaceutice cuprinde adăugarea în exces a unei cantităţi prestabilite de tetrafenilborat de sodiu la proba analizată, titrarea potenţiometrică a excesului de tetrafenilborat cu soluţie standard de clorură de potasiu, utilizând un electrod tetrafenilborat-senzitiv cu membrană care conţine (%, mas.): The method for determining the potassium content in pharmaceutical preparations includes the addition of a predetermined amount of sodium tetraphenylborate in excess to the analyzed sample, the potentiometric titration of the excess tetraphenylborate with a standard solution of potassium chloride, using a tetraphenylborate-sensitive electrode with a membrane containing (%, mass):
(µ3-oxo)-hexa(pivalato)-triaquatricrom(III), [Cr3O(C5H9O2)6(H2O)3][B(C6H5)4] 1,1...1,6 clorură de polivinil 16,4...16,5 eter 2-nitrofeniloctilic 16,4...16,5 nitrobenzen 65,6...65,9 (µ3-oxo)-hexa(pivalato)-triaquatricrom(III), [Cr3O(C5H9O2)6(H2O)3][B(C6H5)4] 1.1...1.6 polyvinyl chloride 16.4. ..16.5 2-nitrophenyloctyl ether 16.4...16.5 nitrobenzene 65.6...65.9
şi calcularea conţinutului de potasiu în preparat conform diferenţei dintre cantitatea prestabilită şi excesul de tetrafenilborat. and calculating the potassium content in the preparation according to the difference between the predetermined amount and the excess of tetraphenylborate.
Exemple de realizare a invenţiei Examples of realization of the invention
Asamblarea electrodului senzitiv la prezenţa ionilor tetrafenilborat Assembling the electrode sensitive to the presence of tetraphenylborate ions
Membrana senzorului se confecţionează în varianta „tip film” pe bază de clorură de polivinil (PVC) (Камман К. Работа с ионселективными электродами, Москва, Мир, 1980, 283 p.). Modul general de preparare a membranelor este: o probă de PVC cu masa de 0,30 g se dizolvă prin agitare în circa 5 mL tetrahidrofuran şi 1 mL nitrobenzen, după dizolvarea totală a polimerului se adaugă 0,30 g de plastifiant (eterul 2-nitrofeniloctilic), se omogenizează, se adaugă 0,02…0,03 g de ionofor ([Cr3O(C5H9O2)6(H2O)3][B(C6H5)4]) şi se amestecă până la omogenizare (sinteza ionoforului a fost efectuată conform: Dîru Mariana. Senzori potenţiometrici pe baza pivalaţilor trinucleari ai cromului(III). Teză de doctor în chimie, 2012, p. 57). Sistemul obţinut se toarnă într-o capsulă Pettri şi se lasă pentru 24 ore, timp suficient pentru evaporarea tetrahidrofuranului. La expirarea acestui termen se formează un film subţire transparent, din care se taie discuri cu diametrul de 12 mm care se încleie cu o soluţie de PVC de 5% în tetrahidrofuran la capătul tubului de PVC pregătit anterior. The membrane of the sensor is manufactured in the "film type" version based on polyvinyl chloride (PVC) (Камман К. Работа с ионселективными елкроддами, Moscow, Мир, 1980, 283 p.). The general way of preparing the membranes is: a sample of PVC with a mass of 0.30 g is dissolved by stirring in about 5 mL of tetrahydrofuran and 1 mL of nitrobenzene, after the complete dissolution of the polymer, 0.30 g of plasticizer is added (ether 2- nitrophenyloctyl), homogenize, add 0.02...0.03 g of ionophore ([Cr3O(C5H9O2)6(H2O)3][B(C6H5)4]) and mix until homogenization (ionophore synthesis was carried out according to: Dîru Mariana. Potentiometric sensors based on trinuclear pivalates of chromium(III). Doctoral thesis in chemistry, 2012, p. 57). The obtained system is poured into a Petri capsule and left for 24 hours, enough time for the evaporation of tetrahydrofuran. When this term expires, a thin transparent film is formed, from which discs with a diameter of 12 mm are cut and glued with a 5% PVC solution in tetrahydrofuran at the end of the previously prepared PVC tube.
Parametrii funcţionali ai electrodului Functional parameters of the electrode
Datele experimentale au fost colectate folosind ionomerul I-135M1 şi pH-metru milivoltmetrul 3310 JENWAY cu pilele galvanice de tipul: Experimental data were collected using ionomer I-135M1 and pH-meter millivoltmeter 3310 JENWAY with galvanic cells of the type:
Ag,AgCl|NaCl(sat.)|soluţia analizată|membrana|B(C6H5)4 -(0,01M),NaCl(0,005M),AgCl|Ag Ag,AgCl|NaCl(sat.)|analysed solution|membrane|B(C6H5)4 -(0.01M),NaCl(0.005M),AgCl|Ag
Electrodul a fost calibrat în soluţii de tetrafenilborat de sodiu cu concentraţia de 10-1…10-7 mol/L, înregistrându-se respectarea funcţiei Nernst pentru 10-2…10-5 mol/L cu panta de 52 mV/decadă conform figurii din anexă. The electrode was calibrated in sodium tetraphenylborate solutions with a concentration of 10-1...10-7 mol/L, observing the Nernst function for 10-2...10-5 mol/L with a slope of 52 mV/decade according to the figure from the annex.
Pentru a determina domeniul optim al pH-lui de funcţionare a electrodului a fost măsurat potenţialul în soluţii de tetrafenilborat cu concentraţia de 10-3 mol/L, în care varia concentraţia ionilor de hidrogen. S-a stabilit că în domeniul 3…11 răspunsul senzorului practic nu este afectat de valoarea pH-ului. Durata de exploatare a electrodului este de 3 luni, iar cei mai interferenţi anioni sunt percloraţii, iodurile şi nitraţii (Tabelul 1). In order to determine the optimal range of pH for electrode operation, the potential was measured in tetraphenylborate solutions with a concentration of 10-3 mol/L, in which the concentration of hydrogen ions varied. It was established that in the range 3...11 the response of the sensor is practically not affected by the pH value. The operating life of the electrode is 3 months, and the most interfering anions are perchlorates, iodines and nitrates (Table 1).
Tabelul 1. Selectivitatea potenţiometrică pentru senzorul propus în invenţie Table 1. Potentiometric selectivity for the sensor proposed in the invention
X ClO4 - I- NO3 - Br- Cl- CH3COO- HPO4 2- SO4 2- -lgKB(C6H5)4 -/X- 0,15 0,20 0,35 1,28 1,84 2,33 3,18 3,50 X ClO4- I- NO3- Br- Cl- CH3COO- HPO4 2- SO4 2- -lgKB(C6H5)4 -/X- 0.15 0.20 0.35 1.28 1.84 2.33 3.18 3.50
Metoda titrării restului de tetrafenilborat Tetraphenylborate residue titration method
Metoda elaborată are la bază reacţia de precipitare a cationilor de potasiu cu anionul tetrafenilborat: The elaborated method is based on the precipitation reaction of potassium cations with tetraphenylborate anion:
Na[B(C6H5)4]exces + K+ x → K[B(C6H5)4]↓ + Na+ Na[B(C6H5)4]excess + K+ x → K[B(C6H5)4]↓ + Na+
Precipitatul de culoare albă are o solubilitate mică în apă, PS(K[B(C6H5)4]) = 2,43.10-8 mol2/dm6 (Kirgintsev N., Kozitskii V. Solubility of potassium tetraphenylborate in mixture of acetone with water at 0 - 50 ºC and its solubility in water 0 - 97,5 ºC. Russian Chemical Bulletin, 1971, vol. 21(1), p. 1116-1118), dar este solubil în solvenţi organici. Ionul de potasiu nu participă direct la procesul de titrare, se titrează potenţiometric excesul de tetrafenilborat conform ecuaţiei: The white precipitate has a low solubility in water, PS(K[B(C6H5)4]) = 2.43.10-8 mol2/dm6 (Kirgintsev N., Kozitskii V. Solubility of potassium tetraphenylborate in mixture of acetone with water at 0 - 50 ºC and its solubility in water 0 - 97.5 ºC. Russian Chemical Bulletin, 1971, vol. 21(1), p. 1116-1118), but it is soluble in organic solvents. The potassium ion does not directly participate in the titration process, the excess of tetraphenylborate is titrated potentiometrically according to the equation:
Na[B(C6H5)4]rămas + KCl st → K[B(C6H5)4]↓ + Na+ Na[B(C6H5)4]remaining + KCl st → K[B(C6H5)4]↓ + Na+
Concentraţia ionilor de potasiu în proba analizată (K+ x) se calculează după formula: The concentration of potassium ions in the analyzed sample (K+ x) is calculated according to the formula:
C(K+ x) = , C(K+ x) = ,
unde C(Na[B(C6H5)4]) - concentraţia soluţiei de tetrafenilborat de sodiu, V(Na[B(C6H5)4]) - volumul soluţiei de tetrafenilborat de sodiu, C(KCl) - concentraţia soluţiei standard de clorură de potasiu, V(KCl) - volumul soluţiei de clorură de sodiu consumat la titrare, V(K+ x) - volumul alicot de soluţie analizată şi C(K+ x) - concentraţia ionilor de potasiu în probă. where C(Na[B(C6H5)4]) - the concentration of the sodium tetraphenylborate solution, V(Na[B(C6H5)4]) - the volume of the sodium tetraphenylborate solution, C(KCl) - the concentration of the standard sodium chloride solution potassium, V(KCl) - the volume of the sodium chloride solution consumed during the titration, V(K+ x) - the aliquot volume of the analyzed solution and C(K+ x) - the concentration of potassium ions in the sample.
Conţinutul de potasiu (g) se calculează după formula: The potassium content (g) is calculated according to the formula:
m(K+ x) = C(K+ x)*M(K)*Vp, m(K+ x) = C(K+ x)*M(K)*Vp,
unde M(K) - masa atomică relativă a potasiului, iar Vp - volumul total al probei analizate. where M(K) - the relative atomic mass of potassium, and Vp - the total volume of the analyzed sample.
Exemplu de realizare Example of realization
O probă ce conţine ioni de potasiu, cu masa cuprinsă între 0,1…0,3 g, se cântăreşte cu ajutorul balanţei analitice, se trece cantitativ într-un balon cotat de 100 mL, se dizolvă şi se aduce la cotă cu apă distilată. La 5,0 mL soluţie obţinută se adaugă 10,0 mL soluţie standard de tetrafenilborat de sodiu cu concentraţia ≥ 0,03 mol/L. Excesul de tetrafenilborat se titrează cu soluţie standard de clorură de potasiu cu concentraţia ≥ 0,03 mol/L. Din trei titrări paralele se determină volumul titrantului cheltuit pentru a atinge punctul de echivalenţă. A sample containing potassium ions, with a mass between 0.1...0.3 g, is weighed using an analytical balance, transferred quantitatively into a 100 mL volumetric flask, dissolved and brought to volume with distilled water . To 5.0 mL of the obtained solution, add 10.0 mL of standard sodium tetraphenylborate solution with a concentration ≥ 0.03 mol/L. The excess of tetraphenylborate is titrated with a standard solution of potassium chloride with a concentration ≥ 0.03 mol/L. From three parallel titrations, the volume of titrant spent to reach the equivalence point is determined.
Controlul exactităţii cu care se determină cantitatea de potasiu a fost efectuat prin analiza unei soluţii de KCl, preparată din probă cântărită. Rezultatele analizei şi tratarea lor statistică sunt prezentate în tabelul 2. Conform rezultatelor obţinute putem concluziona că valoarea concentraţiei experimentale determinată este apropiată de valoarea reală, totodată în timpul realizării analizelor nu se comite o eroare sistematică. Abaterea standard (S) destul de mică exprimă exactitatea bună a metodei. The control of the accuracy with which the amount of potassium is determined was carried out by analyzing a KCl solution, prepared from the weighed sample. The results of the analysis and their statistical treatment are presented in table 2. According to the obtained results, we can conclude that the value of the determined experimental concentration is close to the real value, at the same time, no systematic error is committed during the analysis. The fairly small standard deviation (S) expresses the good accuracy of the method.
Tabelul 2. Determinarea concetraţiei unei soluţii de KCl prin metoda titrimetrică cu determinarea potenţiometrică a punctului de echivalenţă utilizând electrodul propus în invenţie Table 2. Determination of the concentration of a KCl solution by the titrimetric method with the potentiometric determination of the equivalence point using the electrode proposed in the invention
V(Na[B(C6H5)4]), mL V(KCl), mL C(KCl)exp, mol/L S Sr δ 5,00 9,57 0,01051 1,49.10-4 0,0145 0,000156 5,00 9,23 0,01089 5,00 9,27 0,01085 10,00 18,43 0,01091 Cexp = (0,01079 ± 0,0002) mol/L 10,00 18,67 0,01077 10,00 18,57 0,01083 V(Na[B(C6H5)4]), mL V(KCl), mL C(KCl)exp, mol/L S Sr δ 5.00 9.57 0.01051 1.49.10-4 0.0145 0.000156 5.00 9.23 0.01089 5.00 9.27 0.01085 10.00 18.43 0.01091 Cexp = (0.01079 ± 0.0002) mol/L 10.00 18.67 0.01077 10.00 18.57 0.01083
probabilitatea de siguranţă P este egală cu 0,95 the safety probability P is equal to 0.95
Exact după acelaşi principiu a fost determinat conţinutul de potasiu în preparatul farmaceutic REHYDRON. Prospectul preparatului indică următoarea compoziţie: Natrii chloridum 3,5 g, Kalii chloridum 2,5 g, natrii citras 2,9 g, glucosum 10,0 g. Rezultatele obţinute indică o valoare experimentală apropiată de cea indicată în prospectul medicamentului (2,5 g de KCl). The potassium content in the pharmaceutical preparation REHYDRON was determined exactly according to the same principle. The leaflet of the preparation indicates the following composition: Natrii chloridum 3.5 g, Kalii chloridum 2.5 g, natrii citras 2.9 g, glucosum 10.0 g. The results obtained indicate an experimental value close to that indicated in the medicine leaflet (2.5 g of KCl).
Tabelul 3. Rezultatele analizei conţinutului de potasiu în preparatul Table 3. Results of the potassium content analysis in the preparation
REHYDRON utilizând electrodul propus în invenţie REHYDRON using the electrode proposed in the invention
Vp, mL V(TFB-), mL V(KCl)st, mL C(KCl)an, M m(KCl), g Limite de siguranţă, g 5,0 10,0 5,2 0,0336 2,5020 10,0 15,0 8,7 0,0337 2,5106 2,49±0,09 15,0 20,0 12,1 0,0331 2,4660 Vp, mL V(TFB-), mL V(KCl)st, mL C(KCl)an, M m(KCl), g Safety limits, g 5.0 10.0 5.2 0.0336 2.5020 10.0 15.0 8.7 0.0337 2.5106 2.49±0.09 15.0 20.0 12.1 0.0331 2.4660
C(TFB-) = 0,0324 M; C(KCl)st = 0,0946 M; P= 0,95 C(TFB-) = 0.0324 M; C(KCl) st = 0.0946 M; P = 0.95
Rezultatele sunt foarte apropiate, fapt care se reflectă în valorile mici ale dispersiei şi abaterii standard. Prin urmare, metoda de determinare a potasiului prin titrarea restului utilizând electrodul revendicat are parametrii statistici acceptabili pentru a fi recunoscută valabilă. The results are very close, a fact that is reflected in the small values of dispersion and standard deviation. Therefore, the method for determining potassium by titration of the residue using the claimed electrode has acceptable statistical parameters to be recognized as valid.
1. Walters S. Potentiometric microdetermination of potassium, rubidium and cesium without separation of precipitate. Microchemical Journal, 1988, vol. 37, p. 141-144 1. Walters S. Potentiometric microdetermination of potassium, rubidium and cesium without separation of precipitate. Microchemical Journal, 1988, vol 37, pp 141-144
2. Christopoulos T., Diamandis E., Hadjiioannou T. Potentiometric titration of organic cations with sodium tetraphenylborate and liquid-membrane tetraphenylborate ion-selective electrode. Analytica Chimica Acta, 1982, vol. 143, p. 143-151 2. Christopoulos T., Diamandis E., Hadjiioannou T. Potentiometric titration of organic cations with sodium tetraphenylborate and liquid-membrane tetraphenylborate ion-selective electrode. Analytica Chimica Acta, 1982, vol. 143, pp. 143-151
3. Christopoulos T., Diamandis E. Potentiometric titration of pharmaceutical compounds in formulations with sodium tetraphenylborate. Analytica Chimica Acta, 1983, vol. 152, p. 281-284 3. Christopoulos T., Diamandis E. Potentiometric titration of pharmaceutical compounds in formulations with sodium tetraphenylborate. Analytica Chimica Acta, 1983, vol. 152, pp. 281-284
4. Dîru Mariana. Senzori potenţiometrici pe baza pivalaţilor trinucleari ai cromului(III). Autoreferatul tezei de doctor în chimie, Chişinău, 2012 4. Still Mariana. Potentiometric sensors based on trinuclear chromium(III) pivalates. Abstract of the doctoral thesis in chemistry, Chisinau, 2012
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4214968A (en) * | 1978-04-05 | 1980-07-29 | Eastman Kodak Company | Ion-selective electrode |
| US4608149A (en) * | 1983-06-20 | 1986-08-26 | Eastman Kodak Company | Potassium ion-selective compositions and electrodes containing same |
| EP0129233B1 (en) * | 1983-06-20 | 1989-05-17 | EASTMAN KODAK COMPANY (a New Jersey corporation) | Potassium ion-selective membranes |
| EP0155638B1 (en) * | 1984-03-15 | 1990-09-05 | EASTMAN KODAK COMPANY (a New Jersey corporation) | Potassium-ion-selective electrode |
| US4973394A (en) * | 1988-09-02 | 1990-11-27 | Sri International | Immobilized valinomycin molecule for K+ sensor |
| MD787F1 (en) * | 1997-02-13 | 1997-07-31 | Univ De Stat Din Moldova | Composition of the ion-selective electrode membrane for dodecylsulfate ions determination |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4214968A (en) * | 1978-04-05 | 1980-07-29 | Eastman Kodak Company | Ion-selective electrode |
| US4608149A (en) * | 1983-06-20 | 1986-08-26 | Eastman Kodak Company | Potassium ion-selective compositions and electrodes containing same |
| EP0129233B1 (en) * | 1983-06-20 | 1989-05-17 | EASTMAN KODAK COMPANY (a New Jersey corporation) | Potassium ion-selective membranes |
| EP0155638B1 (en) * | 1984-03-15 | 1990-09-05 | EASTMAN KODAK COMPANY (a New Jersey corporation) | Potassium-ion-selective electrode |
| US4973394A (en) * | 1988-09-02 | 1990-11-27 | Sri International | Immobilized valinomycin molecule for K+ sensor |
| MD787F1 (en) * | 1997-02-13 | 1997-07-31 | Univ De Stat Din Moldova | Composition of the ion-selective electrode membrane for dodecylsulfate ions determination |
Non-Patent Citations (4)
| Title |
|---|
| Christopoulos T., Diamandis E. Potentiometric titration of pharmaceutical compounds in formulations with sodium tetraphenylborate. Analytica Chimica Acta, 1983, vol. 152, p. 281-284 * |
| Christopoulos T., Diamandis E., Hadjiioannou T. Potentiometric titration of organic cations with sodium tetraphenylborate and liquid-membrane tetraphenylborate ion-selective electrode. Analytica Chimica Acta, 1982, vol. 143, p. 143-151 * |
| Dîru Mariana. Senzori potenţiometrici pe baza pivalaţilor trinucleari ai cromului(III). Autoreferatul tezei de doctor în chimie, Chişinău, 2012 * |
| Walters S. Potentiometric microdetermination of potassium, rubidium and cesium without separation of precipitate. Microchemical Journal, 1988, vol. 37, p. 141-144 * |
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