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GB 25575-2010: National food safety standards of food additives potassium hydroxide
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National food safety standards of food additives potassium hydroxide
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GB 25575-2010
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Basic data | Standard ID | GB 25575-2010 (GB25575-2010) | | Description (Translated English) | National food safety standards of food additives potassium hydroxide | | Sector / Industry | National Standard | | Classification of Chinese Standard | X42 | | Classification of International Standard | 67.220.20 | | Word Count Estimation | 13,164 | | Date of Issue | 2010-12-21 | | Date of Implementation | 2011-02-21 | | Regulation (derived from) | Ministry of Health Bulletin No. 19 of 2010 | | Issuing agency(ies) | Ministry of Health of the People's Republic of China | | Summary | This Chinese standard applies to potassium chloride solution through the membrane or diaphragm electrolysis from the production of food additives potassium hydroxide. | GB 25575-2010: National food safety standards of food additives potassium hydroxide---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
National food safety standards of food additives potassium hydroxide
National Food Safety Standard
Food additive potassium hydroxide
Issued on. 2010-12-21
2011-02-21 implementation
National Standards of People's Republic of China
People's Republic of China Ministry of Health issued
Foreword
Appendix A of this standard is a normative appendix, Appendix B is an informative annex.
National Food Safety Standard
Food additive potassium hydroxide
1 Scope
This standard applies to potassium chloride solution through the membrane or diaphragm electrolysis production of food additives potassium hydroxide.
2 Normative references
The standard file referenced in the application of this standard is essential. For dated references, only the dated edition of fitness
For this standard. For undated references, the latest edition (including any amendments) applies to this standard.
3 formula and relative molecular mass
Formula 3.1
KOH
3.2 relative molecular mass
56.11 (according to 2007 international relative atomic mass)
4. Technical Requirements
4.1 Sensory requirements. comply with Table 1.
Table 1 Sensory requirements
project
Claim
Testing method
Solid and liquid
Color and odor white or nearly white, no
Colorless, odorless take appropriate solid sample is placed in a plastic beaker 50mL, natural
Light to observe the color and texture. Smell the odor.
Take 50mL liquid sample is placed in 50mL colorimetric tube in natural light
By determining black appearance of the sample perpendicular to the substrate a.
State organization granules, flakes, rods
Or melted solid
Clear or slightly turbid
liquid
After this test a complete wash immediately cuvette.
4.2 Physical indicators. to comply with Table 2.
Table 2. Physical and chemical indicators
Item Index Test Method
Solid and liquid
Potassium hydroxide (KOH), w /% 85.0 ~ 100.5 ≥45.0 Appendix A A.4
Potassium carbonate (K2CO3), w /% ≤ 2.0 2.0 (dry basis) Appendix A A.4
Mercury (Hg)/(mg/kg) ≤ 0.1 0.1 (dry basis) A Appendix A.5
Arsenic (As)/(mg/kg) ≤ 3 3 (dry basis) A.6 in Appendix A
Heavy metals (Pb)/(mg/kg) ≤ 10 10 (dry basis) Appendix A A.7
Lead a (Pb)/(mg/kg) ≤ 5 5 (dry basis) Appendix A A.8
Clarity through test by test A.9 in Appendix A
When a heavy metal when measured result is less than 5mg/kg, the item can be measured free.
Appendix A
(Normative)
Testing method
A.1 Warning
The standard test methods and some reagents used toxic or corrosive, highly corrosive sample obtained shall be handled with care
cautious! As splashed on the skin should immediately wash with water, severe cases should be treated immediately.
A.2 General Provisions
The standard test methods used in the reagents and water, did not indicate when the other requirements, refer to analytically pure reagents and GB/T 6682-2008 in
Three water regulations. Used in the test standard titration solution, impurity standard solution, preparations and products, did not indicate when the other requirements, according to HG/T
3696.1, HG/T 3696.2, HG/T 3696.3 regulations of preparation.
A.3 Identification Test
A.3.1 Identification of hydroxyl ions
A small sample, dissolved in water, can make red litmus paper blue; dropping 2 drops of phenolphthalein indicator solution the solution was purple.
A.3.2 Identification of potassium ions
Take about 0.1g sample was dissolved in 2mL water and access to clean platinum wire with hydrochloric acid to a colorless wet combustion in the flame; dipped into the sample solution, in the absence of
Color flame combustion, flame observed through cobalt glass that is purple.
A.4 Determination of potassium hydroxide and potassium carbonate
A.4.1 Determination of potassium hydroxide - sodium tetraphenylborate gravimetric method (Arbitration Act)
A.4.1.1 Method summary
Under weakly acidic conditions, potassium and sodium tetraphenylborate generate potassium tetraphenylborate precipitate. Filtration, drying and weighing.
A.4.1.2 Reagents and materials
A.4.1.2.1 ethanol.
A.4.1.2.2 glacial acetic acid. 19.
A.4.1.2.3 ethanol solution of sodium tetraphenylborate. 0.1mol/L.
Weigh 3.4g sodium tetraphenylborate, dissolved in 100mL anhydrous ethanol, placed 24h. Before using glass sand crucible filtration.
A.4.1.2.4 ethanol - saturated solution of potassium tetraphenylborate.
1g test before taking the resulting precipitate potassium tetraphenylborate (A.4.1.4.2), plus ethanol 50mL, 950mL of water, and shake to make it saturated, use weighed
filter.
A.4.1.2.5 methyl red indicator solution; 1g/L.
A.4.1.3 instruments and equipment
Glass sand crucible. Aperture 5μm ~ 15 μm.
A.4.1.4 analysis step
A.4.1.4.1 Preparation of test solution
With rapid weighing bottle, weigh about 80g of solid potassium hydroxide (or equivalent liquid sample 80g solid potassium hydroxide), to the nearest 0.001g, set
Filled with the right amount of water in a beaker of 250mL, dissolved placed to room temperature, all moved into 1000mL volumetric flask, diluted with water to the mark.
Immediately placed in a clean, dry plastic bottle 1000mL save this solution as the test solution A, for potassium hydroxide, potassium content determination.
A.4.1.4.2 Determination
Pipette Pipette 20mL test solution A into 500mL volumetric flask, dilute to the mark, shake. If necessary dry filtration. Pipette
Tube Pipette 20mL of this solution was placed in 100mL beaker, add 1 drop of methyl red indicator solution, with glacial acetic acid solution was adjusted to reddish. Heated to 40 ℃ take
Under stirring was added dropwise an ethanol solution of sodium tetraphenylborate 8mL ~ 9mL, about 5min plus complete. Place 10min. With constant quality glass sand has been a crucible
Filtered, washed with 40 mL ~ 50mL ethanol - saturated solution of potassium tetraphenylborate precipitate was washed, each with 5mL, drained every time. Stop filtration with 2mL
Ethanol wash, then dry. Drying at 120 ℃ ± 5 ℃ to constant mass.
NOTE. potassium hydroxide solution configured for glass containers corrosive.
A.4.1.5 Calculation Results
Potassium hydroxide and potassium hydroxide (KOH) mass fraction w1 and its value is expressed in%, according to formula (A.1) Calculated.
() () 8119.0 050 020 100 020
1566.0
1 × - ×××
× = w
mw (A.1)
Where.
Numerical quality m1-- potassium tetraphenylborate precipitate in grams (g) ;.
m-- sample mass value in grams (g);
0.1566-- Tetraphenylboron potassium in terms of potassium hydroxide coefficient;
w2 - A.4.2 measured value of potassium carbonate mass fraction, expressed as a percentage;
0.8119-- potassium carbonate in terms of potassium hydroxide coefficients.
Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.3%.
A.4.2 Determination of potassium - titration
A.4.2.1 Reagents and materials
With GB/T 7698-2003 of Chapter 4.
A.4.2.2 instruments and equipment
With GB/T 7698-2003 of Chapter 5.
A.4.2.3 analysis step
According to GB/T 7698-2003 Chapter 6 of the pre-test. According to GB/T 7698-2003 7.2 blank test.
Weigh about 25g sample (or the equivalent of liquid sample 25g solid potassium hydroxide), accurate to 0.01g, following in GB/T 7698-2003
Section 7.3.
A.4.2.4 Calculation Results
Potassium content of potassium carbonate (K2CO3) mass fraction w2 and its value is expressed in%, according to formula (A.2) calculated as follows. () []
2 × - = m
cMVV
w (A.2)
Where.
Accurate c-- hydrochloric acid standard titration solution concentration value in units of moles per liter (mol/L);
V0-- value hydrochloric acid standard titration solution consumed in the blank test volume, in milliliters (mL);
V1-- measured value hydrochloric acid standard titration solution volume of sample consumed in milliliters (mL);
m-- sample mass value in grams (g);
M-- potassium carbonate (1/2K2CO3) molar mass values, in units of grams per mole (g/mol) (M = 69.10).
Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference is not more than 0.02%.
A.4.3 Determination of potassium hydroxide and potassium carbonate - base titration
A.4.3.1 Method summary
An aliquot of the test solution, using phenolphthalein as indicator, titrate with hydrochloric acid standard titration solution of potassium hydroxide and potassium carbonate. Then methyl orange as indicator
Titration with hydrochloric acid standard titration solution of potassium bicarbonate. In an amount of two titrations titrant consumed content is calculated content of potassium hydroxide and potassium carbonate.
A.4.3.2 Reagents and materials
A.4.3.2.1 hydrochloric acid standard titration solution. c (HCl) = 1mol/L.
A.4.3.2.2 methyl orange indicator solution. 1g/L.
A.4.3.2.3 phenolphthalein indicator solution. 10g/L.
A.4.3.3 analysis step
Pipette Pipette 25mL test solution A (A.4.1.4.1), placed in 250mL conical flask, add 2 drops to 3 drops of phenolphthalein indicator solution, brine
Acid standard solution titration solution titrated to colorless, consumption volume of hydrochloric acid standard titration solution is V1; 1 drop to 2 drops of methyl orange indicator solution with hydrochloric acid
Standard Solution titration to orange-red, the consumption of hydrochloric acid standard solution of total volume V2.
A.4.3.4 Calculation Results
Main content of potassium hydroxide (KOH) mass fraction w1 and its value is expressed in%, according to formula (A.3) calculated as follows. [] 0
1000 /) 2 (121
1 ××
- =
cMVVw (A.3)
Potassium content of potassium carbonate (K2CO3) mass fraction w2 and its value is expressed in%, according to formula (A.4) Calculated.
1000/--212
2 ×× = m
cMVVw) ((A.4)
Where.
Numerical hydrochloric acid standard titration solution volume V1-- phenolphthalein indicating liquid discoloration when consumed titration, in milliliters (mL);
V2-- value of methyl orange indicator solution change color when the total volume of hydrochloric acid standard titration solution consumed titration, in milliliters (mL);
c - accurate hydrochloric acid standard titration solution concentration value in units of moles per liter (mol/L);
m - A.4.1.4.1 weighed sample mass value in grams (g);
Μ1-- numerical molar mass of potassium hydroxide in grams per mole (g/moL) (Μ1 = 56.11);
Numerical Μ2-- potassium carbonate (K2CO3) molar mass in grams per mole (g/moL) (Μ2 = 128.2).
The arithmetic average of the parallel determination results of the measurement results, the two parallel determination results of absolute difference of potassium hydroxide is not more than 0.3% carbon
Not more than 0.02% of potassium.
A.5 Determination of mercury
A.5.1 Reagents and materials
A.5.1.1 sulfuric acid solution. 11.
A.5.1.2 other agents with GB/T 534-2002 in 5.6.2.2.
A.5.2 Instruments and Equipment
With GB/T 534-2002 in 5.6.2.3.
A.5.3 Analysis step
A.5.3.1 Preparation of test solution
Weighing 2.00g ± 0.01g solid sample or a liquid sample is equivalent to 2.00g ± 0.01g solid potassium hydroxide (measured in liquid potassium hydroxide
Content conversion), placed in 100mL beaker, dissolved in 20mL water, 10mL solution of sulfuric acid solution (A.5.1.1), 0.5 mL of permanganate
Potassium solution, cover the surface of the pan, boil for a few seconds, and then cooled.
A.5.3.2 Preparation of the blank test solution
Blank test solution in the preparation of the test solution at the same time, but without addition of the sample, the other operations and the amount of test reagent was added to the same.
A.5.3.3 draw the curve
According to GB/T 534-2002 5.6.2.4.2 of operation, select the amount of mercury curve 0μg ~ 1μg of.
Determination of sample solution A.5.3.4 and the blank test solution
According to GB/T 534-2002 5.6.2.4.3 and 5.6.2.4.4 of the operation.
Mercury-containing waste See Appendix B for processing.
A.5.4 Calculation Results
According to GB/T 534-2002 in 5.6.2.5 and 5.6.2.6.
A.6 Determination of Arsenic
A.6.1 Gutzeit method (Arbitration Act)
Weigh 10.00g ± 0.01g solid sample or equivalent 10.00g ± 0.01g solid potassium hydroxide liquid sample (measured in liquid potassium hydroxide
Mass fraction converted) into 100mL beaker, add about 20 mL of water two to dissolve or dilute. Dropping 2 drops of phenolphthalein indicator solution, with constant stirring slowly
Slow dropwise hydrochloric acid solution (11) and to colorless. Transferred to 100 mL volumetric flask, dilute with water two GB/T 6682-2008 specified to the mark,
Shake (if necessary dry filter, discard filtrate early 10 mL). Immediately placed in a clean, dry 100mL plastic bottles saved this solution as the test solution
Liquid B, Gutzeit method for the determination of arsenic, heavy metals and measured by atomic absorption spectrophotometry Determination of lead content.
Pipette pipette 5mL test solution B, placed in a given arsenic bottle, the following press GB/T 5009.76-2003 Gutzeit method was measured.
Limited have formulated standard solution. Pipette 1.50mL arsenic standard solution [1mL solution containing arsenic (As) 1.0μg], the following according to GB/T 5009.76-2003
Gutzeit method was measured.
A.6.2 Plasma Spectrometry
A.6.2.1 Reagents and materials
A.6.2.2.1 arsenic standard solution. 1mL solution containing arsenic (As) 0.010mg.
Pipette Pipette 1.00mL arsenic standard solution according to HG/T 3696.2 formulated into 100mL volumetric flask, dilute to the mark with two water,
Shake well.
A.6.2.2.2 two water. in line with GB/T 6682-2008 requirements.
A.6.2.2.3 Argon. purity of not less than 99.9%.
A.6.2.2 instruments and equipment
Plasma atomic emission spectrometer.
Instrument stability. the stability of short-range RSD instrument is not more than 2.0%; long-term stability is not more than 4.0% RSD.
The detection limit of the instrument. the representative element detection limit no greater than 0.005mg/L.
Calibration curve. linear correlation coefficient of the regression line, linear correlation coefficient of arsenic R≥0.99.
A.6.2.3 analysis step
A.6.2.3.1 Preparation of test solution
Pipette respectively 0.00mL, 1.00mL, 3.00mL, 5.00mL arsenic standard solution, 100mL flask placed four in the back.
Weigh about 80g of solid potassium hydroxide (corresponding to a liquid or solid sample is 80g of potassium hydroxide), to the nearest 0.01g, and the solution was transferred to a 1 000mL
Volumetric flask, dilute to the mark with two water, shake, stored in a clean, dry plastic bottles. This solution is a test solution C, used in plasma
Determination of arsenic and lead.
In the four 100mL flask were added with a pipette 50mL test solution C, diluted with water two to the mark, shake, test.
A.6.2.3.2 Determination
Under optimum measurement conditions, the measurement sample solution is added to the standard configuration of the above-described method of arsenic in spectral intensity, according to the computer input
Related data, automatically calculate the concentration of arsenic.
A.6.2.4 Calculation Results
Arsenic content of arsenic (As) mass fraction w3 and its value in mg/kg according to formula (A.5) Calculated.
() 10005010 3-3 ××
× =
Vcw (A.5)
Where.
c - numerical solution to be measured by the calibration curve obtained arsenic concentration, in milligrams per milliliter (mg/mL);
V-- volume of the sample solution, in milliliters (mL);
m-- sample mass value in grams (g).
Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference of not more than 0.1mg/kg.
A.7 Determination of Heavy Metals
Pipette Pipette 20mL test solution B (A.6.1) placed in 50mL colorimetric tube, with aqueous ammonia solution (11) was adjusted to pink, according to the following
GB/T 5009.74-2003 Determination of Chapter 6.
Pipette and Pipette 5.00mL 10.00mL lead standard solution respectively [1mL solution containing lead (Pb) 1μg] as a standard, the following according to GB/T
Chapter 6 5009.74-2003 Determination.
A.8 Determination of Lead
A.8.1 atomic absorption spectrophotometry (GFAAS for the Arbitration Act)
A.8.1.1 Reagents and materials
A.8.1.1.1 hydrochloric acid solution. 1 + 1.
A.8.1.1.2 Lead standard solution. 1mL solution containing lead (Pb) 0.010mg.
Pipette Pipette 1.00mL lead standard solution according to HG/T 3696.2 formulated into 100mL volumetric flask, dilute to the mark,
Shake well.
A.8.1.1.3 two water. in line with GB/T 6682-2008 requirements.
A.8.1.2 instruments and equipment
Atomic absorption spectrophotometer. with lead hollow cathode lamp.
A.8.1.3 analysis step
Drawing A.8.1.3.1 calibration curve
Take four 100mL flask, graphite furnace were taken using a pipette 0.00mL, 1.00mL, 2.00mL, 3.00mL lead standard solution
(Flame moved 0.00mL, 5.00mL, 10.00mL, 15.00mL lead standard solution). Add 4mL hydrochloric acid solution, diluted with two water to carve
Degree, shake. Using graphite furnace or acetylene - air flame, at a wavelength of 283.3nm at the atomic absorption spectrophotometer adjusted to the best working conditions to
Two water as a reference, measure the absorbance. To the quality of the lead as the horizontal, the vertical axis corresponding to the absorbance, drawing working curve.
A.8.1.3.2 blank test solution preparation
But without addition of the sample, but added a solution of hydrochloric acid and phenolphthalein and the same amount of time to prepare a test solution B A.6.1, in an electric furnace heated to near boiling dry,
Added two 20mL water and transferred to 100 mL volumetric flask, dilute to the mark. This solution is a blank test solution D.
A.8.1.3.3 Determination
Acetylene - air flame, at a wavelength of 283.3nm at the atomic absorption spectrophotometer to an optimal working condition, with second-degree water as a reference,
Measurement Test solution B (A.6.1) and the blank test solution D absorbance (Pipette 25mL test solution B and the blank test solution D placed 100mL
Volumetric flask, dilute to the mark with two water, shake, absorbance was measured by graphite furnace atomic absorption spectrometry), respectively, from the corresponding check curve
The quality of lead.
A.8.1.4 Calculation Results
Lead content of lead (Pb) mass fraction w4 and its value in mg/kg according to formula (A.6) calculated as follows. ()
3-
4 10 ×
- =
mmw (A.6)
Where.
Numerical test solution quality lead m1-- isolated from the working curve, in milligrams (mg);
m0 - value blank test solution isolated from the working curve lead mass in milligrams (mg);
m --A.6.1 said after dispensing or taken through (25/100) value of the sample mass, in grams (g).
Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference of not more than 0.2mg/kg.
A.8.2 Plasma Spectrometry
A.8.2.1 Reagents and materials
A.8.2.1.1 Lead standard solution. 1mL solution containing lead (Pb) 0.010mg.
Pipette Pipette 1.00mL lead standard solution according to HG/T 3696.2 formulated into 100mL volumetric flask, dilute to the mark with water, shake
uniform.
A.8.2.1.2 two water. in line with GB/T 6682-2008 requirements.
A.8.2.1.3 Argon. purity of not less than 99.9%.
A.8.2.2 instruments and equipment
Plasma atomic emission spectrometer
Instrument stability. the stability of short-range RSD instrument is not more than 2.0%; long-term stability is not more than 4.0% RSD.
The detection limit of the instrument. the representative element detection limit no greater than 0.005mg/L.
Calibration curve. linear correlation coefficient of the regression line, linear correlation coefficient Pb in R≥0.99.
A.8.2.3 analysis step
Pipette respectively 0.00mL, 3.00mL, 5.00mL, 10.00mL lead standard solution, placed in four 100 mL volumetric flask spare.
In the four 100mL flask were added with a pipette 50mL test solution C (A.6.2.3.1), dilute to the mark with two water,
Shake test.
Under optimal assay conditions using the standard addition method for the determination of lead in samples of spectral intensities, computer-related data based on the input from
Automatically calculates the concentration of lead in the test solution.
A.8.2.4 Calculation Results
Lead content of lead (Pb) mass fraction w4 and its value in mg/kg according to formula (A.7) calculated as follows.
() 10005010 34 ××
× = -m
Vcw (A.7)
Where.
c - numerical solution of the sample calibration curve obtained in lead concentration in milligrams per milliliter (mg/mL);
Volume V-- sample solution (ie 100 mL volumetric flask and correction) in milliliters (mL);
m - A.6.2.3.1 weighed sample mass value in grams (g).
Take the arithmetic mean of the parallel determination results of the measurement results, the results of two parallel determination of the absolute difference of not more than 0.2mg/kg.
A.9 Clarity
Weigh 2.50g ± 0.001g sample placed in 50mL of water containing 40mL colorimetric tube was completely dissolved, a black background visually observing this solution,
No mechanical impurities and the solution was completely clear, colorless, through tests.
Appendix B
(Informative)
Mercury-containing waste processing
The mercury-containing waste collected in containers of about 50L, 40L about the time when the waste followed by adding 400g/L sodium hydroxide solution 400mL, 100g vulcanization
Sodium (Na2S · 9H2O), shake. Slowly added 10min 30% hydrogen peroxide solution 400mL, mixed thoroughly, placed an upper supernatant row 24h after
Into the waste water precipitate transferred to another vessel, the mercury were recovered by hand.
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