COMMERCIAL SODIUM HYDROXIDE

2007- 07

CONTENTS
1 Range .2 2 Requirement2 3 Test methods3 3.1 Prepare the test sample solution...3 3.2 Determination of sodium hydroxide content3 3.3 Determination of sodium carbonate.5 3.4 Determination of sodium chloride ..8 3.5 Iron content determination.10 4 Inspection rules..17 5 Marks.19 6 Packing, transportation, storage.19 7 Safety.20

Commercial Sodium Hydroxide

1. Main contents and applicable range This standard has specified the technical requirement on commercial sodium hydroxide, its test methods, test rules and marking, packing, transportation, storage and safety. This standard applies to the sodium hydroxide to be used for producing chemical linter, and for treating waste water of explosive / propellant. Requirement
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2.

Appearance: Commercial solid sodium hydroxide is mainly of white color, with luster. Allow to have trace of color. Commercial solid sodium hydroxide ( including alkali flake) shall meet the Table 1 requirement: Table 1 Technical requirement on sodium hydroxide
Items Sodium hydroxide, % Sodium carbonate,% Sodium chloride, % Ferric oxide, % Criteria 95.0 1.6 3.2 0.02

3.

Test methods

Prepare the test sample solution Instrument a. Volumetric bottle: 1000 ml b. Porcelain mortar: 500 ml c. Measuring cylinder: 250 ml d. Wash bottle, glass bar, enamel tray, electrician knife, etc. 3.1.2 Method of preparation Take proper amount of solid alkali to be crushed and mixed homogeneously in a mortar by a porcelain bar. First use a beaker to pre-weigh about 36 g uniformly-mixed alkali sample on rough balance. Then on an analytical scale accurately weigh 36 1 g, use carbon dioxide-free distilled water to dissolve and pour into 1000 ml volumetric bottle, dilute to the graduation, stand by. Determination of sodium hydroxide content Method abstract To test sample solution, first add barium chloride to transform sodium carbonate into barium carbonate precipitate, then use phenolphthalein as indicator, use hydrochloric acid standard titration solution to titrate to the termination. Reaction formula as below: Na2CO3 + BaCl2 BaCO3 + 2NaCl NaOH + HCl NaCl + H2O Instrument and equipment a. Triangle bottle: 250 ml with stopper;
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b. Acid burette: 50 ml; c. Pipette: 50 ml; d. Measuring cylinder: 250 ml Reagent and solution a. Hydrochloric acid standard titration solution: c (HCl) = 1.000 mol / L; b. Phenolphthalein indicator: 10 g / L; c. Barium chloride solution: Analytical pure 100g/L. Before the use, use phenolphthalein as indicator, use sodium hydroxide solution to regulate to micro red color. Test procedure Suck ( 3.1) 50 ml test sample solution, inject into 250ml triangle bottle with ground stopper, add 10 ml neutralized 100 g/L barium chloride solution, again add 2 3 drops of 10 g/L phenolphthalein indicator and under non-stopping shaking, use 1 mol / L hydrochloric acid standard solution to titrate till the solution turns micro red as the termination. Calculation of the result X1, the content of sodium hydroxide (NaOH) expressed by mass fraction (% is to be calculated as per formula (1):
X1 = c (V / 1000) 40.00 100% (1) m 50 / 1000

Where: C Actual concentration of hydrochloric acid standard titration solution, mol / L; m Mass of the test sample, g; V The volume of hydrochloric acid standard solution consumed by the titration, ml; 40.00 Mole mass value of sodium hydroxide, g / mol 3.2.6 The allowable error Take the arithmetic average value of parallel determination result to be the determination result. The difference of absolute value of the parallel determination results is not over 0.1%, expressed to the first order of decimal fraction. Determination of sodium carbonate 3.3.1 Method abstract The test sample takes bromine cresol green- methyl red as indicator, use hydrochloric acid standard solution to titrate to the termination. Measure the sum total of the sodium hydroxide and sodium carbonate, then minus the content of the sodium hydroxide to get the content of sodium carbonate.
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NaOH + HCl NaCl + H2O Na2 CO3 + 2 HCl 2NaCl + CO2 + H2O 3.3.2 Reagent and solution a. Hydrochloric acid standard titration solution: c (HCl) = 1.000 mol / L; b. Bromine cresol green methyl red indicator: mix 3 portions of 0.1 g/L ethanol solution of bromine cresol green and 1 portion of ethanol of 0.2g/L ethanol solution of methyl red. 3.3.3 Instrument and equipment a. Triangle bottle: 250 ml with stopper b. Burette: 50 ml; c. Transfer pipette: 50 ml; d. Measuring cylinder: 250 ml. 3.3.4 Measuring procedure Suck ( 3.1 ) 50 ml test sample solution and inject into 250 ml triangle bottle, add 10 drops of bromine cresol green methyl red indicator solution, under non-stopping shaking, use 1 mol / L hydrochloric acid standard titration solution to titrate to the termination of wine-red (claret). Record the volume of the standard titration solution consumed by the titration. 3.3.5 Calculation of the result X2, the content of sodium carbonate (Na2CO3) expressed by mass fraction (% is to be calculated as per formula (2):
X2 = c [ (V
1

V ) / 1000 ] 105.99 2 m 50 / 1000

100% (2)

Where: C Actual concentration of hydrochloric acid standard titration solution, mol / L; V The volume of the hydrochloric acid standard solution consumed by the titration, with phenolphthalein as indicator, ml; V1 The volume of the hydrochloric acid standard solution consumed by the titration, with bromine cresol green methyl red as indicator, ml; m Mass of the test sample, g; 105.99 Mol mass value of sodium carbonate, g / mol. 3.3.6 The allowable error Take the arithmetic average value of parallel determination result to be the determination result. The difference of absolute value of the parallel determination results not over 0.05%, expressed to the first order of decimal fraction.
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Measurement of sodium chloride In pH 2 3 solution, mercury nitrate standard solution of strong ionization turns chlorine ion into mercury chloride of weak ionization, use diphenyl azocarbohydrazide as indicator, with relatively excessive bivalent mercury ion, to form a complex of purple-red. This is the termination. 3.4.2 Instrument and equipment
3.4 3.4.1 a.

Triangle bottle: 250 ml with stopper

b. c. d. e. 3.4.3

Micro burette: 2 ml, 5 ml ; Transfer pipette: 50 ml; Measuring cylinder: 250 ml; Volumetric bottle: 500 ml. Reagent and solution a. Mercury nitrate standard titration solution: c [ 1/ 2 Hg (NO3)2]=0.05 mol/L; b. Diphenyl azocarbohydrazide: 5 g /L ethanol solution; c. Bromophenol blue indicator: 1 g/L ethanol solution; d. Sodium hydroxide solution: 2 mol / L; e. Nitric acid solution: 2 mol / L; f. Nitric acid solution: 1+1; Mercury nitrate standard titration solution: c [ 1/ 2 Hg (NO3)2]=0.005 mol/L; Suck 50.00 ml of mercury nitrate standard titration solution of c [ 1/ 2 Hg (NO3)2]=0.05 mol/L, place into 500 ml volumetric bottle, add water to dilute to the graduation, shake to uniform. 3.4.4 Measuring procedure Suck 50 ml ( 3.1) test sample solution, inject into 250 ml triangle bottle, add water 40 ml, slowly add (1+1) nitric acid solution 5 ml, cool down to room temperature, add 3 drops of bromine phenyl blue indicator solution, if the solution turns blue color, again carefully add, drop by drop, nitric acid (1+1) till the solution turns from blue color to yellow color. Drop by drop, add sodium hydroxide solution (2 mol/L) to make the solution from yellow color to blue color. Drop by drop, add nitric acid ( 2 mol /L) to turn the solution from blue color to yellow color. Again with excessive 3 drops, add 1 ml Diphenyl azocarbohydrazide indicator, use mercury nitrate standard solution to titrate till the solution turns from yellow color to purple red color which is the termination. At the same time, use water to do the blank test. 3.4.5 Calculation of the result X3, the content of sodium chloride (NaCl) expressed by mass
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fraction (% is to be calculated as per formula (3):

X3 = c [ (V V0 ) / 1000 ] 58.44 100% 3 m 50 / 1000

Where: C Actual concentration of mercury nitrate standard titration solution, mol / L; V The volume of the mercury nitrate standard solution consumed by the titration, ml; V 0 The volume of the mercury nitrate standard solution consumed by the blank determination, ml; m Mass of the test sample, g; 58.44 Moor mass value of sodium carbonate, g / mol. 3.4.6 The allowable error Take the arithmetic average of parallel determination result to be the determination result. The absolute difference value of the parallel determination results not over 0.02%, expressed to the first order of decimal fraction. 3.5 Iron content determination 3.5.1 Spectrophotometry 3.5.1.1 Method abstract Use ascorbic acid to reduce the trivalent iron into bivalent iron. In buffer solution system of pH 4 4.5, the bivalent iron, with ophenanthroline, forms complex of orange-red color. Use spectrophotometry to determine. Its reaction: 2 Fe 3+ +C 6 H 8O 6 = 2 Fe 2+ + C6H 6O 6 + 2H+ Fe 2+ + 3 C12 H8N2 = [ Fe (C12 H8N2) 3]2+ 3.5.1.2 Instrument and equipment Common lab instrument and spectrophotometer 3.5.1.3 Reagent and solution a. Hydrochloric acid: 6 mol /L; b. Ammonia; c. Sulfuric acid; d. Para nitro phenol : 0.25% ( m/v) solution; e. Acetic acid sodium acetate buffer solution: pH value 4.5; f. Ascorbic acid: 2% ( m/V) solution, weigh 2 g ascorbic acid to dissolve into 100 ml water; g. O-phenanthroline: 0.2% ( m/Vsolution;
h.

Iron standard solution: 1 ml corresponds to 0.1 mg ferric oxide. Weigh 0.6039 g ammonium ferric sulfate, put into 200 ml beaker, add 100 ml water, 10 ml sulfuric acid. All transfer to 1000 ml
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volumetric bottle, dilute to the graduation, shake to uniform; i. Iron standard solution: 1 ml corresponds to 0.01 mg ferric oxide. Take (3.5.1.3 h) solution to dilute to the10 times. This solution is to be prepared just prior to the use. 3.5.1.4 Plot the standard curve 3.5.1.4.1 Preparation of the stand reference solution Take the iron standard solution (3.5.1.3 i) as per the order of 0.0, 2.0, 4.0, 6.0, 8.0, 10.0, 15.0, 20.0, 30.0, 40.0, 50.0 ml, and put into 100 ml volumetric bottle. Then add 2.5 ml ascorbic acid, 10 ml buffer solution, 5 ml o-phenanthroline solution, use water to dilute to the graduation, shake to uniform. 3.1.5.4.2 Determination of the absorbency of the standard reference solution Use the reference solution without addition of standard iron solution, to regulate the instrument absorbency to zero, at wave length 510 mm, according to the Table 3-given ferric oxide content scope, choose the colorimetric dish, to determine the absorbency of the standard reference solution. Table 3 Comparison table for the colorimetric dish used for different content range of ferric oxide Ferric oxide content, % Colorimetric dish, cm Less than 0.005 5 0.005 0.01 2 or 3 0.01 0.015 2 or 1 0.015 0.03 1 Take the mg number of ferric oxide contained in 100 ml standard reference solution as abscissa, its corresponding absorbency as ordinate, plot the standard curve. 3.5.1.5 Determination procedure 3.5.1.5.1 Use weighing bottle to weigh 10 g sample, accurate to 0.1g, place into 400 ml beaker, add water about 100 ml, also add ( 2 3) drops of para-nitrophenol indicator solution, use hydrochloric acid to neutralize till yellow color disappears. Again with excessive 2 ml, heat to boil 5 min., cool down, transfer into 250 ml volumetric bottle, use water to dilute to the graduation, shake to uniform. 3.5.1.5.2 Blank test To 400 ml beaker, add 25 ml water and a quantity of hydrochloric acid equivalent to neutralize the sample (3.5.1.5.1), add ammonia 40 ml, heat to boil 5 min., cool down, transfer into 250 ml volumetric bottle, use water to dilute to the graduation, shake to uniform. Then, according to (3.5.1.5.3) to proceed to the treatment.
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3.5.1.5.3 Color developing Suck 50.0 ml test sample solution (3.5.1.5.1), inject into 100 ml volumetric bottle, then add 2.5 ml ascorbic acid solution, 10 ml buffer solution, 5 ml o-phenanthroline solution, use water to dilute to the graduation, shake to uniform. 3.5.1.5.4 Determination of the test samples absorbency Determine the solutions absorbency as described in (3.5.1.4.2). Before the determination, use blank solution (3.5.1.5.2) to regulate the instrument absorbency to zero. 3.5.1.6 Result calculation From the standard curve, check out the ferric oxide mass (mg) corresponding to the determined absorbency. Ferric oxide ( Fe2O3) mass fraction X4 (%) shall be calculated as per formula 4
1 1000 100 = 0.5 m1 X = 4 4 50 m m 250 m1

Where: m 1 Ferric oxide mass corresponding to the absorbency of the test solution, mg; m The mass of the test sample, g. 3.5.1.7 The allowable error Take the arithmetic average value of parallel determination result to be the determination result. The absolute difference value of the parallel determination result is not over 0.001%, expressed to the second order of decimal fraction. 3.5.2 Visual colorimetry 3.5.2.1 Method abstract Trivalent iron ion in the acidic solution combines with the radical of sulfocyanic acid to become a red compound. This red intensity depends on the content of the trivalent iron ion. Use colorimetry to determine iron. Fe3+ +3 CNS Fe (CNS) 3 ( red color) 3.5.2.2 Reagent and solution a. Hydrochloric acid: = 1.19 b. Nitric acid: = 1.12 and = 1.4; c. Sulfuric acid solution: 20% ; d. Ammonium sulfocyanide solution: 150 g/L; e. Iron standard solution 0.1 mg / ml ( 1 ml equal to 0.1 mg ferric oxide) f. Iron standard solution 0.01 mg / ml ( prepare just prior to the use); g. Blue litmus test paper.
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3.5.2.3 Instrument and equipment a. Electric stove; b. Measuring cylinder: 50 ml, 250 ml; c. Transfer pipette: 2 ml, 10 ml; d. Volumetric bottle: 250 ml; e. Burette: 10 ml; f. Colorimetric tube: 50 ml. 3.5.2.4 Determination procedure Weigh 10 g solid alkali, accurate to 0.1g, put into 250 ml beaker, add water about 100 ml to dissolve, use litmus test paper as indicator, use hydrochloric acid ( = 1.19) to neutralize, use titration bottle to add nitric acid ( = 1.4) (5 6) drops to acidify. Then put on the electric stove to boil for 5 min., take down and place into porcelain disc filled with cold water to cool down, then transfer into 250 ml volumetric bottle, add water to dilute to the graduation, shake to uniform. Use straw to suck the prepared solution 10 ml and inject into 50 ml colorimetric pipette, also use straw to add, by the sequence, 0.25 ml nitric acid (= 1.12), 0.25 ml sulfuric acid (20%), use measuring cylinder to add 5 ml ammonium sulfocyanide solution(150 g/L), use water to dilute to the graduation and shake to uniform. To another colorimetric tube, add 10 ml water and the same amount of the a/m solution, also by 10 ml burette, add iron standard solution ( 0.01 mg/ml) till the two colorimetric tubes have the same color. Add water to make the two tubes have the same volume and mix to uniform, compare the colors. 3.5.2.5 Calculation of the result X5, the content of ferric oxide (Fe2O3) expressed by mass fraction (% is to be calculated as per formula (5):
X5 = V 0.00001 250 100% (5) m 10

Where: V The volume of iron standard solution consumed by the determination, ml; m Mass of the test sample, g; 0.00001 Concentration of the iron standard solution, g / ml. 3.5.2.6 The allowable error Take the arithmetic average of parallel determination result to be the determination result. The difference of absolute value of the parallel determination results not over 0.008%, expressed to the second order of decimal fraction.
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4.

Inspection rules

Commercial sodium hydroxide shall be inspected by the quality inspection department in the production unit. Commercial sodium hydroxide of each lot ex-works shall meet this standard requirement, and be attached with quality certificate. Inspection item for inward factory a. For sodium hydroxide applicable for treating acidic waste water, only check the content of sodium hydroxide; b. For sodium hydroxide applicable for producing chemical linter, inspect sodium hydroxide, sodium carbonate, sodium chloride, ferric oxide contents; c. Others, not inspected. Lab sample shall be taken from 5% of the total drum number of commercial sodium hydroxide. When lot amount is small, not less than 3 drums. Along the vertical connection of the drum, cut open the drum sheet, cleave the alkali, from upper / middle / lower 3-position, quickly draw the representative samples. The sample amount not less than 500g, mix to uniform. Put into clean dry wide-neck bottle with rubber stopper. Seal and stick bottle marks, stating name of the production factory, product name, lot number, sampling date and samplers name. Production factory may take from the packing drum the molten alkali as the lab sample for inspection. As per 5% of the total drum number for each lot to draw sample, put the obtained lab samples into clean dry wide-neck bottle with stopper, seal. Sample amount not less than 500 kg. If dispute occurs due to different sampling methods affecting the product quality, still cutting-open the drum to take sample is prevailing. If any item in the inspection result does not meet the technical requirement of this standard, re-sampling from the double number of the drums for lab to repeat the inspection. In the re-inspection result, even one item does not meet the technical requirement of this standard, the whole lot is regarded as unqualified. 5. Marks Packing container for commercial sodium hydroxide must have obvious and firm marks. Its contents cover: name of production factory, product name, trade mark, standard code, grade, production date, lot number and net weight, and the sign of
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CORROSIVE ITEM. 6. Packing, transportation, storage

Commercial solid sodium hydroxide should use iron drum to pack. Drum wall thickness over 0.5mm, pressure-resistance over 0.05 MPa. Drum cover must be sealed and firm. Commercial sodium hydroxide must be deposited in dry store, avoid broken / damaged, polluted, dampened, or contacting acid. Prevent colliding during transportation. Product quality shall not be affected during transportation and storage. 7. Safety Sodium hydroxide is strongly corrosive. During the operation, wear well labor protective gears like eye-glass and rubber hand glove, etc.

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