Joint determination of nicrcumomnp in the hottest

2022-08-20
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Combined determination of Ni, Cr, Cu, Mo, Mn and P in high chromium cast iron

3 Ammonium persulfate solution (5%): effective for 15 days

4 Diphenyl hydrazine solution (0.5%) ethanol solution: add 4G of phthalic anhydride per 100ml of hot ethanol to dissolve, add 0.5g of diphenyl hydrazine to dissolve, and store in a brown bottle

5 Alkaline sodium tartrate solution (15%), containing 10% sodium hydroxide

6 Alkaline dimethylglyoxime solution (0.5%), containing 10% sodium hydroxide

7 Sodium hydroxide solution (10%)

8 Sulfuric acid (1+1), (1+10)

9 Ammonia ammonium citrate solution (15%): ammonia water (1+1) preparation

10 B. C.O solution (0.1%) ethanol (1+1) solution

11 Ammonium thiocyanate solution (25%)

12 Ammonium molybdate -- superior quality of experimental machine sodium tartrate solution (9% each, mixed before use) (1+1)

13 Sodium fluoride -- stannous chloride solution (2.4%-0.2%): add 0.2g stannous chloride solution (for the current shift) to every 100ml of sodium fluoride solution (2.4%)

14 Perchloric acid: 70% (commercially available)

15 Ascorbic acid (5%): prepare with ethanol (1+1)

16 Sodium periodate solution (4%): 30ml of phosphoric acid and 20ml of nitric acid are contained in every 100ml of solution, which is dissolved by boiling

17 Hydrofluoric acid

18 Ammonium chloride solution: 10%

II. Analysis operation

weigh 200mg sample into a 100ml conical flask, add 5ml nitric acid (1+1) and add 10 drops of hydrofluoric acid while heating. After dissolution, add 5ml perchloric acid at medium temperature, heat it until white perchloric acid smoke rises to the mouth of the bottle for 30s, remove it, place it and cool it naturally until there is no white smoke at the mouth of the bottle and there is salt precipitation, add 20ml water to shake and dissolve the salt. Dilute to a 100ml volumetric flask

III. determination of various elements

(I) ke Dongjie told the determination of chromium

suck 10ml of mother liquor into a 250ml volumetric flask, dilute the water to the scale, and shake well. Suck 5ml of mother liquor from a 250ml volumetric flask, put 90ml of phosphoric acid (5+95) into a 150ml conical flask, add 5ml of diphenyl hydrazine solution, place for 1 minute (10s), add 10ml of ammonium chloride solution (10%) and shake well

in 1cm cuvette at 530nm wavelength. Water is the reference and measured

(II) the determination of nickel (0.05 ~ 5%) includes polyglycolide, polylactic acid, (glycolide lactide) copolymer, polycaprolactone, poly2 oxane ketone, polyhydroxy fatty acid ester, poly3 methylene carbonate, polyurethane and polyether urethane, etc.

take 5ml mother liquor from 100ml volumetric flask into 150ml conical flask, add 5ml ammonium persulfate solution (5%), 5ml alkaline sodium tartrate solution (15%), and 5ml alkaline dimethylglyoxime solution (0.5%), Place for 10min, add 30ml of water and shake well

at the wavelength of 480nm, 1--2cm cuvette, water as the reference, measurement

(III) determination of molybdenum (0.05 ~ 1%)

take 10ml of mother liquor from 100ml volumetric flask into 100ml conical flask, add 5ml of sulfuric acid (1+1), 10ml of ascorbic acid solution (5%), shake well, add 3ml of ammonium thiocyanate solution (25%), shake well, add 20ml of water, shake well, and place for min

at the wavelength of 460nm, water is the reference, 2cm cuvette, water is the reference, and measurement

(IV) determination of copper (0.%)

take 10ml of mother liquor from 100ml volumetric flask and put it into 150ml conical flask, add 20ml of ammonia ammonium citrate solution (15%), shake well, add 20ml of BCO solution (0.1%), shake well, and place for 2min

at the wavelength of 620nm, CM cuvette, water as the reference, measurement

(V) determination of manganese (0.05 ~ 2%)

take 20ml of mother liquor from 100ml volumetric flask and put it into 150ml conical flask to meet the increasing demand of American manufacturers for closed-loop regeneration and the trend of manufacturing industry returning to shore. Add 10ml of sodium periodate solution (4%), heat and boil for 1min. After taking it down and cooling, add 20ml of water and shake it well

at 530nm wavelength, 2cm cuvette, water as reference, measurement

(VI) determination of phosphorus (0.001 ~ 0.1%)

take 20ml of the test solution into a 100ml conical flask, add 5ml of sulfuric acid (1+10), add 2ml of sodium sulfite (10%), boil for 15s, take it off, immediately add 5ml of ammonium molybdate sodium tartrate solution, shake for 10s, add 20ml of sodium fluoride stannous chloride solution, shake well

measure immediately at the wavelength of 680nm with 2cm cuvette and water as the reference

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