Selection and preparation of color agents in thin layer analysis.

-related topicsThin Layer Analysis (TLC) Technology TLC Coloring
Reagents
Selection Coloring Reagents Coloring Agents Can be divided into two categories: one is a general color agent for examining general organic compounds, and the other is a special properties color agent designed according to compound classification or special organ groups. There is a wide variety of color agents, listing some commonly used color agents.l. General colorant Sulphate is commonly used in four solutions: sulphuric acid-water (1:1) solution;solution with 0.5% iodine is yellowish brown for many compounds.-neutral 0.05% potassium permanganate solution, the reductive compounds appear yellow on a pale red background.alkaline potassium permanganate reagent reducing compounds appear yellow on a light red background. Solution I: 1% potassium permanganate solution; Solution II.: 5% sodium carbonate solution; Solution I and Solution II. Equivalent mixing applications.acidic potassium permanganate reagent sprayed 1.6% potassium permanganate thick sulfuric acid solution (when dissolved to prevent explosion), after spraying thin layer in 180oC
heating
15 to 20min.acidic potassium chromate reagent spray 5% potassium heavy chromate thick sulfuric acid solution, if necessary, 150oC roasted thin layer.5% phosphate ethanol solution is baked at 120 degrees C after spray, the reducing compound is blue, and then ammonia aromatherapy, then the background becomes colorless.(8) potassium iron cyanide-iron triclosan reagent reducing substances appear blue, and then spray 2mol/L hydrochloric acid solution, then blue deepens. Solution I: 1% potassium iron cyanide solution; Solution II.: 2% iron triclosan solution; Mix solution I and solution II.. 2. Exclusive properties color agents Due to a wide variety of compounds, so the specific properties of color agents are also many, will now be the most commonly used color agents in various types of compounds listed as follows: (1) hydrocarbons(1) silver nitrate / hydrogen peroxide detection: halogenated hydrocarbons. Solution: Silver nitrate O.1g dissolved in water lml, plus 2-benzene-based ethanol lOOml, diluted with acetone to 200ml, plus 30% hydrogen peroxide 1 drop. Methods: The
was
ultraviolet light of the filter, and the result was dark black.(2) luciferin/bromine detection: unsaturated hydrocarbons. Solution: I. Lucifer 0.1g dissolved in ethanol lOOml; II.5% bromine carbon tetrachloride solution. Methods: First spray (I), then placed in a bromine vapor container, luciferin into tybromolyphosin (Twilight), fluorescence disappeared, unsaturated hydrocarbon spots due to the addition of bromine, preventing the generation of dawn red and retain fluorescence, most unsaturated hydrocarbons on a pink background yellow.(3) tetrachlorobenzene xylene was detected: aromatic hydrocarbons. Solution: Acetone and chlorobenzene (10:1) solution of 2% tetrachlorophyl phthalates. Methods: Observation under ultraviolet light after spraying.(4) formaldehyde/sulphuric acid detection: polycyclic
aromatic
. Solution: 37% formaldehyde solution O.2 ml dissolved in l0ml of thick sulfate.(2) alcohols3,512 nitrobenzene chloride detection: alcohols. Solution: I.2% toluene solution; II.0.5% sodium hydroxide solution; III..O.002% rodamin solution. Methods: Spray (I), in the air
driding
overnight, with steam to smoke 2min, paper or thin layer through the test liquid (II.) 30s, spray water wash, while wet through (III.) 15s, air dry, UV lamp observation. ammonium nitrate detected: alcohol. Solution: 0.2mol/L nitrate solution of I.1% ammonium nitrate; II..N, N-dimethyl-diamine hydrochloride 1.5g dissolved in methanol, water and acetic acid (128m1 plus 25m1 plus 1.5m1) mixture, mixed with (I) and (II.) equivalent. After the spray plate, heat 5min at 105oC. (3) vanilla aldehyde/sulphuric acid detection: advanced alcohols, phenols, steroids and essential oils. Solution: Vanilla aldehyde 1g dissolved in lOOml of sulfate. Methods: After spraying, it was heated to the deepest color at 120oC. (4) Diphenyl-based acrylic ' detected: alcohols, terpenes, carboxyls, esters and ethers. Solution: 15mg of this product is dissolved in chloroform 25ml. Methods: After spraying, 5 to lOmin was heated at 110oC. Result: The purple background was yellow speckled. (3) aldehyde ketones masion/sulphate detection: aldehyde-based compounds. Solution: I.0.01% red solution, into sulfur dioxide until colorless; II.0.05mol/L mercury chloride solution; III..O.05mol/L Sulphate Solution. Methods: Mix I, II. and III. at 1:1:10 and dilute the water to l00ml. neighboring fennel amine detection: aldehyde, ketones. Solution: This product acetic acid saturation solution. 2,4-dinitrobenzene: aldehyde, ketone and ketosaccharides. Solution: 2mol/L hydrochloric acid solution of I.0.4% of this product; II. This product O.1g is dissolved in ethanol l00ml, plus thick hydrochloric acid lml. Methods: 2mol/L hydrochloric acid solution of potassium cyanide was sprayed immediately after injection solution I or II. Results: Saturated ketones were immediately blue, saturated aldehyde was slow and olive green, and unsaturated carboxyl compounds were not colored. around Danning to detect: carotenoid aldehyde. Solution: I.1% to 5% around Danin ethanol solution; II.25% ammonium hydroxide or 27% sodium hydroxide solution. Methods: Spray solution I first, then spray solution II. Dry. (4) organic
acids1 bromophenol green detection: organic acids. Solution: Bromophenol green 0.1g dissolved in ethanol 500ml and 0.1mol/L sodium hydroxide solution 5ml. Method: Dip plate. Result: Yellow spots are produced on a blue background. 2 potassium permanganate/sulphuric acid detection: fatty acid derivatives. Solution: See potassium permanganate, the acidic colorant. 3 Hydrogen peroxide detection: aromatic acid. Solution: 0.3% hydrogen peroxide solution. Methods: Observation under ultraviolet light (365nm) after spraying. Result: Strong blue fluorescence. 4 2,5 6-dechlorophenol-sodium indigophenol: organic acids and ketoic acids. Solution: 0.1% ethanol solution of this product. Methods: Micro-temperature after spraying. Result: The blue background is red. (5) phenols 1 Emerson reagents (4-aminoantebirin/potassium ferride (III)) detected substances: phenols, aromatic amines and volatile oils. Solution: I.4-aminoAntebilin 1g soluble in ethanol 100ml; II. Potassium iron cyanide (III.) 4g dissolved in water 50ml, 2 diluted to 100ml with ethanol. Methods: First spray solution I, 3 dry in hot air 5min, 4 then spray solution II., 5 then dry in hot air 5min, 6 then put the plate containing ammonia vapor (25% ammonia solution) in a closed container. Result: The spots were orange-light red. Volatile oil is red against a bright yellow background. 7 Boute reactions detected: phenols, chlorine, bromine, alkyl dephenols. Methods: 3 to 10min in a container with NO2 vapor (containing thick nitric acid) and 8 NH2 vapor (enriched ammonia) was treated. 9 chloroquine (tetrachloroquine) detection: phenols. Solution: 1% of the toluene solution of this product. 10 DDQ (DDQ) reagents detected: phenols. Solution: 2% of the toluene solution of this product. 11 TCNE (vinyl cyanide) reagents detected: phenols, aromatic hydrocarbons, hemlines, aromatic amines. Solution: 0.5% to 1% of the toluene solution of this product. 12 Gibb's (2,13 6-bibromoquine chloramine) reagent detected: phenols. Solution: 2% methanol solution of this product. (7) Iron chloride detection: phenols, hydroxyamide. Solution: 0.5mol/L hydrochloric acid solution of 1% to 5% iron chloride. Results: The phenols were blue and hydroxyamides were red. (6) Nitrogen-containing compounds (1) FCNP (nitrate sodium/iron cyanide) reagents detected: lipid family containing nitride, such as amino cyanide, niacin, niacin and sulfurine and its derivatives, creatine and creatinine. Solution: 10% sodium hydroxide solution, 10% sodium nitrate solution, 10% potassium iron cyanide solution and water according to 1:1:1:3 mix, at room temperature at least 20min, refrigerator storage for several weeks, before using the mixture and acetone and other volume mixing. (2) Dragendorff (potassium iodide reagent) reagents detected: aromatic nitrogen-containing compounds, such as alkaloids, anti-arrhythmic drugs. Solution: I. alkaline nitrate 0.85g dissolved in 10 ml of ice acetic acid and 40 ml of water; Mix the above solutionS I and II. Equivalent, place in a brown bottle as a reserve liquid, use the pre-reserve liquid lml, ice acetic acid 2 ml and water l0ml mixed. Result: Orange spots. 4-methyl umbrella ketones detected: nitrogen-containing hybrids. Solution: This product 0.02g dissolved in ethanol 35ml, add water to 100ml. Methods: In a container of 25% ammonia vapor behind the spray plate, it was removed and observed under ultraviolet lamp (365nm). of potassium iodide detected: alkaloids and organic nitride. Solution: 10% HCB solution 3 ml mixed with water 97 ml, plus 6% potassium iodide solution, mixed well. Pre-use preparation. sulfate high ammonium/sulfuric acid detection: alkaloids and iodine-containing organic compounds. Solution: Radon sulfate 1g suspended in 4 ml of water, added tricloste 1g, boiling, add thick sulfuric acid one by one until the turbidity disappears. Methods: The thin layer after spraying was heated for several minutes at 110 degrees C. RESULTS: Apu morphine, horse money base, autumn daffodil base, poppy base, toxic lentil base and organic iodide can detect (6) Ehrlich (for metformin formaldehyde/hydrochloric acid) reagents detected: pyridine derivatives and amines. Solution: 1% of this product's thick hydrochloric acid solution is mixed with methanol 1:1. Methods: The spray-back plate was heated by 20min at 50 degrees C. Result: Spots of different colors. (7) amine (1) nitric acid/ethanol detection: adipose family amine. Solution: 50 drops of 65% nitric acid in ethanol 100 ml. Method: 120oC heating is required. (2) 2,6-dichloroquine chloramide detection:
antioxidants
, amide (capsaicin), Burr, mid-fatamine, Zhong, shufangamine, aromatic hydrocarbons, drugs, amphetamine herbicides, etc. Solution: Freshly prepared 0.5% to 2% of the ethanol solution. Methods: After spraying, the thin layer was heated at 110oC for 10min and then treated with ammonia vapor. (3) cissin detected: amines. Solution: O.1% of the ethanol solution of this product. (4) butyl /nickel chloride detection: amines. Solution: I. butyl dylconone 1.2g dissolved in hot water 35 ml, nickel chloride 0.95g, cooled with 2 ml of ammonia water; II. Hydroxyamine hydrochloride 0.12g dissolved in 200ml water. Methods: Mix solution I and II, place for 1 day, filter. (5) Pauly (for aminobenzene) reagents detected: phenols, amines, and hexaling compounds that can be combined. Solution: Sulfonate 4.5g dissolved in a warm 12mol/L hydrochloric acid 45ml, diluted to 500ml with water, cooled in ice with lOml, plus 4.5% sodium nitrite cold solution lOml, placed 15min in OoC. Use the first plus equal volume 10% sodium carbonate solution. , cobalt thiocyanate (II.). Detections: alkaloids, bur, Zhong, schoamines. Solution: Ammonium thiocyanate 3g and cobalt chloride 1g dissolved in water 20 ml. Results: Blue spots on white to pink backgrounds, and the color fades after 2h. Color points can be reproduced if a thin layer is sprayed with water or placed in a saturated water vapor container. 1,2-yuan-4-sodium sulfonate detected: aromatic amines. Solution: This product 0.5g dissolved in 95ml water, added acetic acid 5ml, filter out insoluble. Methods: After spraying, the reaction was 30min color show. glucose/phosphoric acid detection: aromatic amines. Solution: Glucose 2g dissolved in 85% phosphate l0ml mixed with water 40ml, plus ethanol and butanol 30ml each. Methods: After spraying, the l0min was heated at 115 degrees C. (8) Nitro and Nitro compounds (1)α-amine detection: 3,51 dinitrobenzene, dinitrobenzene. Solution: I.O.5% α-amine ethanol solution; II.10% potassium hydroxide methanol solution. Methods: First spray solution I, then spray solution II. Result: Reddish-brown spots. (2) Diaphenylamine/chloride detection: nitrosamines. Solution: 1.5% dephenyl ethanol solution and 0.1g chlorination.