GB 19106: Evolution and historical versions
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[GB/T 19106-2013] Sodium hypochlorite
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Solution of sodium hypochlorite
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Basic data | Standard ID | GB 19106-2013 (GB19106-2013) | | Description (Translated English) | [GB/T 19106-2013] Sodium hypochlorite | | Sector / Industry | National Standard | | Classification of Chinese Standard | G12 | | Classification of International Standard | 71.060.50 | | Word Count Estimation | 11,172 | | Older Standard (superseded by this standard) | GB 19106-2003 | | Quoted Standard | GB 190; GB/T 191; GB/T 601; GB/T 602; GB/T 603; GB/T 6678; GB/T 6680; GB/T 6682; GB/T 8170; GB 19107 | | Regulation (derived from) | National Standards Bulletin 2013 No. 23 | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | | Summary | This standard specifies: sodium hypochlorite requirements, sampling, test methods, inspection rules and signs, packaging, transport and storage. This standard applies to: sodium chloride and obtained sodium hypochlorite. |
GB 19106-2013: ---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.
[GB/T 19106-2013] Sodium hypochlorite
ICS 71.060.50
G12
National Standards of People's Republic of China
Replace GB 19106-2003
Sodium hypochlorite
Since March 23,.2017, this standard has become recommended
Standard, the serial number was changed to GB/T 19106-2013.
Released on.2013-11-27
2014-12-01 Implementation
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China
Issued by the National Standardization Administration of China
Foreword
The heavy metals and arsenic indicators in Table 1 of this standard and Chapter 7 are mandatory, and the rest are recommended.
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard replaces GB 19106-2003 "Sodium Hypochlorite Solution". Compared with GB 19106-2003, the main technical changes are as follows.
---Modified some normative reference documents (see Chapter 2, Chapter 2 of the.2003 edition);
---A type has increased the A-I specification (see 3.2, 3.2 in the.2003 edition);
---The mandatory requirements are different (see 3.2 and Chapter 7, the.2003 edition of 3.2, Chapter 7 and Chapter 8);
--- Modified the solution for adjusting the zero point of the spectrophotometer when determining the iron content (see 5.5.4.1.2, 5.3.4.1.2 of the.2003 edition);
---Add "sodium sulfide solution" precipitant (see 5.6.2.5 and 5.6.4.4, 5.4.4.3 of the.2003 edition);
---Improved the analysis steps for the determination of heavy metals (see 5.6.4);
---Modified the inspection rules (see Chapter 6, Chapter 6 of the.2003 edition);
---Added the requirements of "Production License Signs, Safety Labels and the "Upward" Signs specified in GB/T 191" (see 7.1.1,.2003
7.1 of the year edition);
---Added the requirement that "each batch of sodium hypochlorite should be accompanied by a safety technical specification" (see 7.1.2);
---Modified the content of the quality certificate (see 7.1.2, 6.3 of the.2003 edition);
--- Delete the "safety" chapter, put the relevant content in the form of warning words after the standard name (Chapter 8 of the.2003 edition).
This standard was proposed by the China Petroleum and Chemical Industry Federation.
This standard is under the jurisdiction of the Chlor-Alkali Branch of the National Chemical Standardization Technical Committee (SAC/TC63/SC6).
Drafting organizations of this standard. Hangzhou Electrochemical Group Co., Ltd., Fujian Meizhouwan Chlor-Alkali Industry Co., Ltd., Shandong Dadi Salt Chemical Group Co., Ltd.
The company, Binhua Group Co., Ltd., Jinxi Chemical Research Institute.
The main drafters of this standard. Chen Peiyun, Wang Jianying, Jiang Wenfeng, Tian Qixiang, Zhang Zhongzheng, Zhu Changjian, Li Furong, Hu Liming.
The previous editions of the standard replaced by this standard are as follows.
---GB 19106-2003.
Sodium hypochlorite
Warning. Sodium hypochlorite is highly corrosive. The operator should take appropriate safety and health measures.
Protective equipment such as acid-base gloves.
1 Scope
This standard specifies the requirements, sampling, test methods, inspection rules and signs, packaging, transportation and storage of sodium hypochlorite.
This standard applies to sodium hypochlorite prepared by chlorination of sodium hydroxide.
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article
Pieces. For undated reference documents, the latest version (including all amendments) is applicable to this document.
GB 190 Dangerous Goods Packaging Mark
GB/T 191 Packaging, Storage and Transportation Graphic Mark (GB/T 191-2009, ISO 780.1997, MOD)
GB/T 601 Preparation of Standard Titration Solution for Chemical Reagents
GB/T 602 Preparation of standard solutions for impurity determination of chemical reagents (GB/T 602-2002, ISO 6353-1.1982, NEQ)
Preparation of preparations and products used in GB/T 603 chemical reagent test method (GB/T 603-2002, ISO 6353-1.1982,
NEQ)
GB/T 6678 General Rules for Sampling of Chemical Products
GB/T 6680 General Rules for Sampling of Liquid Chemical Products
GB/T 6682 Analytical laboratory water specifications and test methods (GB/T 6682-2008, ISO 3696.1987, MOD)
GB/T 8170 Numerical rounding rules and the expression and determination of limit values
GB 19107 Sodium hypochlorite solution packaging requirements
3 requirements
3.1 Appearance. light yellow liquid.
3.2 Sodium hypochlorite should meet the requirements of Table 1.
4 sampling
4.1 Products are inspected in batches. The production enterprise takes the finished tank, the sodium hypochlorite produced in one day or one production cycle as a batch. User
The same batch of sodium hypochlorite arrived is one batch.
4.2 When sodium hypochlorite is shipped in a tanker or storage tank, use the oxidation-resistant sampler specified in GB/T 6680 to start from the upper, middle and lower depths of different depths.
Three places (the upper part is one-tenth of the liquid layer from the liquid surface, and the lower part is one-tenth of the liquid layer from the bottom of the liquid) to take the same amount of samples.
4.3 Sodium hypochlorite was sampled from plastic barrels, plastic cans, and combined packaging consisting of plastic bottle packaging and fiberboard boxes (including corrugated boxes)
At the time, according to the number of sampling units specified in GB/T 6678, samples should be taken with the oxidation-resistant sampler specified in GB/T 6680.
4.4 Mix the sample taken, put it in a clean, dry brown bottle with a ground stopper, and seal it. The sample volume shall not be less than.200mL. Sample
A label should be affixed to the bottle, and the name of the manufacturer, product name, model specification, batch number or production date, sampling amount, sampling date and sampling date should be indicated.
The name of the person, etc.
5 Test method
Safety Tips. Some reagents in this test method are toxic or corrosive, so you should be careful when handling them. If splashed on the skin, use them immediately.
Rinse with water, and treat severe cases immediately.
5.1 General provisions
The reagents and water used in this standard refer to analytical reagents and the tertiary water specified in GB/T 6682 when other requirements are not specified.
The standard titration solutions, impurity standard solutions, preparations and products used in the test, unless other requirements are specified, are in accordance with GB/T 601,
GB/T 602, GB/T 603 regulations are prepared.
5.2 Appearance
Observe visually under natural light.
5.3 Determination of available chlorine
5.3.1 Method summary
In an acidic medium, hypochlorite reacts with potassium iodide to precipitate iodine. Using starch as an indicator solution, use sodium thiosulfate standard titration solution to drop
Set, until the blue disappears as the end point. The reaction formula is as follows.
2H ClO- 2I-=I2 Cl- H2O
I2 2S2O32-=S4O62- 2I-
5.3.2 Reagents
5.3.2.1 Potassium iodide solution. 100g/L. Weigh 100g of potassium iodide, dissolve it in water, dilute to 1000mL, and shake well.
5.3.2.2 Sulfuric acid solution. 3100.Pipette 15mL sulfuric acid, slowly inject 500mL water, cool and shake.
5.3.2.3 Sodium thiosulfate standard titration solution. c(Na2S2O3)=0.1mol/L.
5.3.2.4 Starch indicator solution. 10g/L.
5.3.3 Apparatus
General laboratory equipment and 50mL burette (Grade A, division value. 0.1mL).
5.3.4 Analysis steps
5.3.4.1 Sample solution preparation
Pipette about 20mL laboratory sample, put it in a 100mL beaker filled with about 20mL water and weighed (accurate to 0.01g), weigh
The amount (accurate to 0.01g), then transfer all into a 500mL volumetric flask, dilute to the mark with water, and shake well. This solution is test solution A, use
For the determination of available chlorine content, free alkali content, iron content, heavy metal content, and arsenic content.
5.3.4.2 Determination
Pipette 10.00mL sample solution A, place it in a 250mL iodine measuring flask containing 50mL water, add 10mL potassium iodide solution and
10mL sulfuric acid solution, quickly close the bottle stopper and seal it with water, and let it stand in the dark for 5 minutes. Titrate with sodium thiosulfate standard titration solution to light yellow,
Add 2mL starch indicator solution and continue titration until the blue color disappears as the end point.
5.3.5 Result calculation
Available chlorine is calculated as the mass fraction w1 of chlorine (Cl), and the value is expressed in %, calculated according to formula (1).
w1=
(V/1000)cM
m1×(10/500)×
100=5VcMm1
(1)
Where.
V ---The value of the volume of the sodium thiosulfate standard titration solution, in milliliters (mL);
c --- The accurate value of the concentration of sodium thiosulfate standard titration solution, the unit is moles per liter (mol/L);
m1 --- the value of the mass of the sample, in grams (g);
M ---The value of the molar mass of chlorine (Cl) in grams per mole (g/mol) (M=35.453).
5.3.6 Tolerance
Take the arithmetic mean of the parallel measurement results as the measurement result. The absolute value of the difference between the parallel determination results does not exceed 0.2%.
5.4 Determination of free base
5.4.1 Method summary
Decompose hypochlorite with hydrogen peroxide, use phenolphthalein as indicator solution, and titrate with hydrochloric acid standard titration solution to reddish as the end point. Reaction formula
as follows.
ClO- H2O2=Cl- O2 H2O
OH- H =H2O
5.4.2 Reagents and materials
5.4.2.1 Hydrogen peroxide solution. 15;
5.4.2.2 Hydrochloric acid standard titration solution. c(HCl)=0.1mol/L;
5.4.2.3 Phenolphthalein indicator solution. 10g/L;
5.4.2.4 Starch-potassium iodide test paper.
5.4.3 Apparatus
General laboratory equipment and 25mL burette (A grade, graduation value. 0.1mL).
5.4.4 Analysis steps
Pipette 50.00mL sample solution A, place it in a 250mL conical flask, add hydrogen peroxide solution dropwise until it does not contain hypochlorite (do not use
Starch-potassium iodide test paper turns blue), add (2~3) drops of phenolphthalein indicator solution, titrate with hydrochloric acid standard titration solution to reddish as the end point.
5.4.5 Result calculation
The free alkali is calculated by the mass fraction w2 of sodium hydroxide (NaOH), and the value is expressed in %, which is expressed by formula (2).
w2=
(V/1000)cM
m1×(50/500)×
100=VcMm1
(2)
Where.
c ---The accurate value of the concentration of the hydrochloric acid standard titration solution, the unit is moles per liter (mol/L);
V ---The value of the volume of the hydrochloric acid standard titration solution, in milliliter (mL);
m1---the value of the mass of the sample, in grams (g);
M ---The value of the molar mass of sodium hydroxide (NaOH), in grams per mole (g/mol) (M = 40.00).
5.4.6 Tolerance
Take the arithmetic mean of the parallel measurement results as the measurement result. The absolute value of the difference between the parallel determination results is not more than 0.04%.
5.5 Determination of iron
5.5.1 Method summary
In a medium without hypochlorite, hydroxylamine hydrochloride reduces Fe3 to Fe2.In a pH (4-6) buffer solution system, Fe2 is the same as Fe2.
1,10-phenanthroline forms an orange-red complex, and its absorbance is measured at the maximum absorption wavelength (510nm) of the spectrophotometer. The reaction formula is as follows.
4Fe3 2NH2OH=4Fe2 N2O H2O 4H
Fe2 3C12H8N2=[Fe(C12H8N2)3]2
5.5.2 Reagents and materials
5.5.2.1 Hydrogen peroxide solution. 15.
5.5.2.2 Acetic acid-sodium acetate buffer solution. pH value is about 4.5.
5.5.2.3 Hydroxylamine hydrochloride solution. 10g/L. Weigh 1g of hydroxylamine hydrochloride, dissolve in water, and dilute to 100mL.
5.5.2.4 Iron standard solution. 0.1mg/mL.
5.5.2.5 Iron standard solution. 0.01mg/mL. Pipette 25.00mL standard solution (5.5.2.4) and place it in a 250mL volumetric flask.
Dilute with water to the mark and shake well. Prepare this solution before use.
5.5.2.6 1,10-phenanthroline indicator solution. 2g/L.
5.5.2.7 Starch-potassium iodide test paper.
5.5.3 Apparatus
General laboratory instruments and spectrophotometers.
5.5.4 Analysis steps
5.5.4.1 Standard curve drawing
5.5.4.1.1 Pipette 0.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL iron standard solution (5.5.2.5)
Do not put in 6 100mL volumetric flasks, add 5mL hydroxylamine hydrochloride solution and 10mL acetic acid-sodium acetate buffer to each volumetric flask.
Solution and 5mL 1,10-phenanthroline indicator solution, dilute to the mark with water, shake well, and let stand for 10 min.
5.5.4.1.2 Using water as a reference, adjust the spectrophotometer to zero, select an appropriate cuvette at a wavelength of 510nm, and measure the absorbance.
5.5.4.1.3 The absorbance of the blank solution is subtracted from the absorbance of the standard colorimetric solution, and the mass of iron in the 100mL standard colorimetric solution (mg)
The abscissa is the abscissa, and the corresponding absorbance is the ordinate. The standard curve or regression linear equation is drawn.
5.5.4.2 Blank test
No sample solution is added, and the blank test is carried out using exactly the same analysis steps, reagents and dosage as the test sample solution.
5.5.4.3 Determination
Pipette 50.00mL sample solution A, place it in a 100mL volumetric flask, add hydrogen peroxide solution dropwise until it does not contain hypochlorite (do not use
Starch-potassium iodide test paper turns blue), then add 5mL hydroxylamine hydrochloride solution, 10mL acetic acid-sodium acetate buffer solution and 5mL 1,10-phenanthroline
Indicator solution, dilute to the mark with water, shake well, and let stand for 10 min. The following shall be carried out in accordance with the provisions of 5.5.4.1.2.
5.5.5 Result calculation
The iron content is expressed in the mass fraction w3 of iron (Fe), and the value is expressed in %, calculated according to formula (3).
w3 = m2
/1000
m1×(50/500)×
100=m2m1
(3)
Where.
m1---the value of the mass of the sample, in grams (g);
m2---The value obtained from the standard curve corresponding to the absorbance of the sample solution after subtracting the absorbance of the blank solution, or a one-element linear return
The value of the mass of iron calculated by the normalization equation, in micrograms (mg).
5.5.6 Tolerance
Take the arithmetic mean of the parallel measurement results as the measurement result. The absolute value of the difference between the parallel determination results is not more than 0.001%.
5.6 Determination of heavy metals
5.6.1 Method summary
Under weakly acidic conditions (pH 3~4), the heavy metal ions and sulfide ions in the sample form a brown-black precipitate, which is similar to the lead treated by the same method.
Comparing standard solutions, make a limit test.
5.6.2 Reagents and materials
5.6.2.1 Hydrochloric acid.
5.6.2.2 Hydrogen peroxide solution. 15.
5.6.2.3 Acetic acid-sodium acetate buffer solution. pH value is about 3.
5.6.2.4 Saturated solution of hydrogen sulfide. Pour hydrogen sulfide gas into water without carbon dioxide until it is saturated. Before using this solution
preparation.
5.6.2.5 Sodium sulfide solution. Weigh 5g of sodium sulfide, dissolve it in a mixture of 10mL of water and 30mL of glycerol, and store it in a sealed container, protected from light.
It is valid for one month.
5.6.2.6 Lead standard solution. 0.1mg/mL.
5.6.2.7 Lead standard solution. 0.01mg/mL. Take an appropriate amount of lead standard solution (5.6.2.6) and dilute it by 10 times. Before using the solution
Preparation.
5.6.2.8 Phenolphthalein indicator solution. 10g/L.
5.6.2.9 Starch-potassium iodide test paper.
5.6.3 Apparatus
General laboratory equipment and 50mL Nessler colorimetric tube.
5.6.4 Analysis steps
5.6.4.1 Tube A. Pipette 1.00mL lead standard solution (5.6.2.7) into a 50mL Nessler colorimetric tube, add water to 25mL, add
5mL acetic acid-sodium acetate buffer solution, shake well. spare.
5.6.4.2 Tube B. Take a Nessler colorimetric tube matched with tube A, pipette 25.00mL sample solution A, and place it in a 50mL Nessler colorimetric tube
In the middle, add hydrogen peroxide solution dropwise until there is no hypochlorite (do not make the starch-potassium iodide test paper blue). Add 1 drop of phenolphthalein indicator solution, use hydrochloric acid
Adjust to reddish, add 5mL acetic acid-sodium acetate buffer solution, and shake well. spare.
5.6.4.3 Tube C. Take a 50mL Nessler colorimetric tube matched with tubes A and B, add the same sample solution A of the same amount as tube B, and then
Add the same amount of lead standard solution (5.6.2.7) as tube A, add hydrogen peroxide solution dropwise, until it does not contain hypochlorite (do not make starch-potassium iodide
The test paper turns blue). Add 1 drop of phenolphthalein indicator solution, adjust to reddish with hydrochloric acid, then add 5mL acetic acid-sodium acetate buffer solution and shake well.
spare.
5.6.4.4 Add 10 mL of freshly prepared saturated hydrogen sulfide solution or 2 drops of sodium sulfide solution to each tube, add water to the 50 mL mark, and mix
Evenly, place in a dark place for 5 minutes. Observed under a white background, the chromaticity of tube B should not be deeper than that of tube A, and the chromaticity of tube C should be the same as that of tube A.
The chroma is equal to or deeper than that of the A tube.
5.7 Determination of arsenic
5.7.1 Method summary
In the presence of potassium iodide and stannous chloride, high-valent arsenic is reduced to trivalent arsenic. The new ecological hydrogen and trivalent arsenic produced by zinc particles and acid produce
Arsenic hydrogen gas, remove the interference of hydrogen sulfide through lead acetate cotton, and then generate yellow to orange stains with mercury bromide test paper, which is compared with standard arsenic spots
Make a limited test.
5.7.2 Reagents and materials
The reagents and materials used do not contain arsenic.
5.7.2.1 Hydrochloric acid.
5.7.2.2 Hydrogen peroxide solution. 15.
5.7.2.3 Potassium iodide solution. 150g/L.
5.7.2.4 Stannous chloride solution. 400g/L.
5.7.2.5 Arsenic standard solution. 0.1mg/mL.
5.7.2.6 Arsenic standard solution. 0.001mg/mL. Pipette an appropriate amount of arsenic standard solution (5.7.2.5), diluted 100 times. This solution uses
Before preparation.
5.7.2.7 Lead acetate cotton.
5.7.2.8 Mercury bromide test paper.
5.7.2.9 Starch-potassium iodide test paper.
5.7.2.10 Zinc particles.
5.7.3 Apparatus
General laboratory equipment and arsenic analyzer. The schematic diagram of the arsenic determination instrument is shown in Figure 1.
5.7.4 Analysis steps
5.7.4.1 Pipette 1.00mL arsenic standard solution (5.7.2.6) into the conical flask of the arsenic analyzer, add 5mL hydrochloric acid, and add water to about
30mL, then add 5mL potassium iodide solution and 5 drops of stannous chloride, shake well, and let stand for 10min.
5.7.4.2 Pipette 25.00mL sample solution A into the Erlenmeyer flask of the arsenic analyzer, and add hydrogen peroxide solution dropwise until it does not contain hypochlorite.
Stop (do not make the starch-potassium iodide test paper blue). Use hydrochloric acid to neutralize the sample solution to neutrality, and add 5 mL of hydrochloric acid to excess, add water to about 30 mL, and then
Add 5mL potassium iodide solution and 5 drops of stannous chloride, shake well, and let stand for 10min.
5.7.4.3 Add 2g of zinc granules to each of the above-mentioned conical flasks, and immediately connect the glass tubes with lead acetate cotton and mercury bromide test paper.
Place it in a dark place at 25°C for 1h.
5.7.4.4 Take out the arsenic spot, the arsenic spot of the sample solution shall not be deeper than the arsenic spot of the arsenic limit standard. Standard arsenic spots should be prepared at the same time for each determination.
6 Inspection rules
6.1 The quality index of sodium hypochlorite in this standard is judged by the "rounding value comparison method" specified in GB/T 8170.
6.2 This standard adopts type inspection and factory inspection.
6.2.1 All index items in this standard are type inspection items. Under normal production conditions, type inspection shall be carried out at least once a month. Have the following
In one of the cases, type inspection should also be carried out.
a) There are changes in key production processes;
b) The main raw materials have changed;
c) Resuming production after stopping production;
d) The result of the type inspection is quite different from the previous type inspection.
6.2.2 The available chlorine and free alkali in the items specified in this standard are ex-factory inspection items and shall be inspected batch by batch.
6.3 Sodium hypochlorite should be inspected by the quality supervision department of the manufacturer in accordance with the requirements of this standard, and the manufacturer should ensure that each batch of production
All products should meet the requirements of this standard.
6.4 If the inspection results have indicators that do not meet the requirements of this standard, a representative sample should be taken from twice the volume of the packaging unit.
Re-inspection, even if there is an index in the re-inspection result that does not meet the requirements of this standard, the entire batch of products is unqualified.
7 Marking, packaging, transportation and storage
7.1 Logo
7.1.1 The packaging of sodium hypochlorite should have a firm and clear mark, including. manufacturer name, address, product name, "hazardous chemicals"
Typeface, net content, batch number or production date, production license number and mark, this standard number, "corrosive substances" and
"Oxidizing substances" logo, safety label. For plastic drums, plastic cans and combined packaging consisting of plastic bottle packaging and fiberboard boxes (including
Corrugated boxes) should also have the "upward" sign specified in GB/T 191 on the container.
7.1.2 Each batch of sodium hypochlorite should be accompanied by safety technical specifications and quality certificates. The content of the quality certificate includes. the name of the manufacturer
Name, address, product name, words "hazardous chemicals", net content, batch number or production date, production license number and logo, product quality symbol
The certificate of conformity with this standard and the number of this standard.
7.2 Packaging
Sodium hypochlorite packaging should be implemented in accordance with GB 19107.
7.3 Transportation
Sodium hypochlorite should be sealed when transported, and the shipping container should be anti-corrosion. Do not mix with reductive items during transportation.
7.4 Storage
Packages containing sodium hypochlorite should be stored in a cool, ventilated warehouse, avoid sunlight, and prohibit other possible occurrences with sodium hypochlorite
Dangerously reacting goods are stored together.
Calculated from the date of manufacture of sodium hypochlorite products, the effective chlorine of type A-Ⅰ and B-Ⅰ shall not be less than 12% within 3 days, and not less than 11% within 7 days; A-Ⅱ
Type and B-II available chlorine is not less than 9% within 3 days and not less than 8% within 7 days; Type A-Ⅲ and B-Ⅲ available chlorine is not less than 4.5% within 20 days.
If the warranty period is exceeded, the supplier shall negotiate with the user to determine it or express it in the product label.
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