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GB 26754-2011: [GB/T 26754-2011] Sodium azide for industrial use
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Basic data
Standard ID: GB 26754-2011 (GB26754-2011)
Description (Translated English): [GB/T 26754-2011] Sodium azide for industrial use
Sector / Industry: National Standard
Classification of Chinese Standard: G12
Classification of International Standard: 71.060.50
Word Count Estimation: 18,183
Date of Issue: 2011-07-20
Date of Implementation: 2012-05-01
Quoted Standard: GB 190-2009; GB/T 191-2008; GB/T 3049-2006; GB/T 6678; GB/T 6679; GB/T 6682-2008; GB/T 8170; GB 12268-2005; GB 12463-2009; HG/T 3696.1; HG/T 3696.2; HG/T 3696.3; TG/HY 206-2009
Regulation (derived from): Announcement of Newly Approved National Standards No. 10 of 2011
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 Chinese standard specifies the requirements for industrial sodium azide, test methods, inspection rules, marking, packaging, transportation, storage, and security. This standard applies primarily as automotive airbag gas generating agent, primary explosive, photographic agents, synthetic resin foam, the production of pesticides and pharmaceutical intermediates raw materials for industrial sodium azide.
GB 26754-2011: [GB/T 26754-2011] Sodium azide for industrial use
---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.
Sodium azide for industrial use
ICS 71.060.50
G12
National Standards of People's Republic of China
Industrial sodium azide
Published 2011-07-20
2012-05-01 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China issued
Foreword
This standard 7.1,7.2,7.3,7.5,7.6 and Chapter 8 is mandatory, the rest are recommended.
This standard was drafted in accordance with rules GB/T 1.1-2009 given.
This standard and U.S. Military Standard MIL-S-20552B. 1983 (1995) "Industrial sodium azide" (English) and structural differences in technical
Difference see Appendix A and Appendix B.
The standard proposed by China Petroleum and Chemical Industry Federation.
This standard by the National Standardization Technical Committee chemical inorganic chemicals branch (SAC/TC63/SC1).
This standard was drafted. CNOOC Tianjin Chemical Research & Design Institute, Anhui Province Langxi County Branch of the Industrial Co., Ltd., Tianjin Entry-Exit Inspection
Quarantine Bureau, Gong Yi City, Quality and Technical Supervision and Testing Center.
The main drafters. Xia Junling, Jia Yuliang, from Benny Lau, Liu Ruo, Wang Xiaofeng.
Industrial sodium azide
1 Scope
This standard specifies the requirements sodium azide industrial nitride, test methods, inspection rules, marking, packaging, transportation, storage, and security.
This standard applies primarily as automotive airbag gas generating agent, a primary explosive, photographic agents, foaming synthetic resin, production of pesticides and
Pharmaceutical intermediates industrial raw materials such as sodium azide.
2 Normative references
The following documents for the application of this document is essential. For dated references, only applies to the version dated paper
Pieces. For undated references, the latest edition (including any amendments) applies to this document.
GB 190-2009 dangerous goods packaging logo
GB/T 191-2008 Packaging Pictorial signs
General Method GB/T 3049-2006 industrial chemical products as measured by the iron content of 1,10-Phenanthroline Spectrophotometry
GB/T 6678 General Principles for Sampling Chemical Products
GB/T 6679 General sampling of solid chemical products
GB/T 6682-2008 specifications and test methods for water analysis laboratory
GB/T 8170 rounding off means about rules and determining limiting values
GB 12268-2005 of dangerous goods
GB 12463-2009 transport of dangerous goods packaging technology
Preparation HG/T 3696.1 Inorganic chemicals for chemical analysis of standard titration solution
Preparation HG/T 3696.2 Inorganic chemicals solution used for chemical analysis of standard impurities
Preparations with HG/T 3696.3 Inorganic chemicals Chemical Analysis
TG/HY206-2009 Railway of Dangerous Goods
Molecular formula and molecular weight 3
Molecular formula. NaN3
Molecular weight. 65.01 (according to 2007 international relative atomic mass)
4 Requirements
4.1 Appearance. white crystalline mixture doped with microstrip or pale yellow powder, there should be no visual evidence of impurities.
Sodium azide 4.2 industrial specifications should meet the requirements of Table 1.
Table 1%
Indicators Project
Index, w
Premium grade First grade Qualified
Sodium azide (NaN3 to count) ≥ 99.0 98.5 98.0
Sodium hydroxide (NaOH) ≤ 0.15 0.3 0.5
Sodium carbonate (Na2CO3) ≤ 0.35 0.5 -
Sodium carbonate (Na2CO3) ≤ 0.35 0.5 -
Water insolubles ≤ 0.1 0.2 -
Chloride (based on Cl) ≤ 0.01 - -
Sulfate (in terms of SO4) ≤ 0.1 - -
Nitrate (NO3 basis) ≤ 0.05 - -
Iron (Fe) ≤ 0.05 - -
≤ 0.15 0.5 1.0 Water
Heavy Metals (as Pb) ≤ 0.001 - -
5 Test methods
5.1 Safety Tips
Reagents used in this test method corrosive or toxic, the operator should be careful as water splashed on the skin immediately
Flushing, severe cases should seek medical care immediately.
This standard indicators measuring all projects should be carried out in a fume hood. The remaining test solution of sodium azide or at should be promptly
Treatment, treatment See Appendix C.
5.2 General Provisions
This standard reagents and water, in the absence of other requirements specified, refer to the specified three analytical reagents and GB/T 6682-2008
Grade water or equivalent water quality. Desired test standard solution, the standard solution impurities, products and preparations, in the absence of other requirements specified, are by
HG/T 3696.1, HG/T 3696.2, preparing a predetermined HG/T 3696.3 is.
5.3 Visual inspection
In natural light, the appearance was visually determined.
5.4 Determination of the content of sodium azide
5.4.1 ammonium ferrous sulfate oxidation-reduction titration (MAL)
5.4.1.1 Method summary
Sodium azide is reacted with ceric ammonium nitrate, the tetravalent cerium is reduced to trivalent cerium; standard ferrous ammonium sulfate titration solution is titrated with an excess of cerium nitrate
Hydroxide solution, a solution in accordance with the consumption of ferrous ammonium sulfate was calculated back to stack the content of sodium azide.
5.4.1.2 Reagents
5.4.1.2.1 standard ferrous ammonium sulfate titration solution. c [(NH4) 2Fe (SO4) 2] ≈0.1mol/L.
5.4.1.2.2 standard titration solution of ammonium cerium nitrate. c [(NH4) 2Ce (NO3) 6] ≈0.1mol/L.
Cerium ammonium nitrate were dissolved in 170g containing 125mL of water and 185mL of concentrated nitric acid solution, stir well. 300mL containing added 12.5mL
Concentrated aqueous nitric acid, with stirring. Under continuous stirring, this solution was diluted to 2500mL. This solution should be stored in a brown bottle.
5.4.1.2.3 phenanthroline indicator solution. 5g/L;
0.5g of ferrous sulfate dissolved in 50mL of water, add 2 drops of concentrated sulfuric acid. Weigh 0.5g phenanthroline were dissolved in this solution, diluted with water
To 100mL.
5.4.1.3 Analysis of step
Weigh about 2.5g sample, accurate to 0.0002g, was placed in a 400mL beaker, dissolved in 200mL water, transferred to a 250mL volume
Volumetric flask, diluted with water to the mark.
Pipette with a pipette 20mL of test solution was placed in a 400mL beaker, with a burette ceric ammonium nitrate was gradually added 40.0mL standard titration
Solution, the reaction should be cooled in water. After completion of the reaction, the solution is adjusted to a volume of about 150 mL of water, 5mL of concentrated sulfuric acid was slowly added, plus
2 drops phenanthroline indicator solution, titration was titrated with standard ferrous ammonium sulfate to the solution from pale green to yellow to red. At the same time a blank test.
Except that no blank test sample addition, and other operations for the same test solution.
5.4.1.4 calculation results
Sodium azide content by mass of sodium azide (of NaN3) fraction w1 meter, according to equation (1).
w1 =
c (V1-V2) × M × 11000
m × 20250
× 100% (1)
Where.
C --- accurate value of the concentration of the solution of ferrous ammonium sulfate titration standard, in units of moles per liter (mol/L);
Numerical volume standard titration solution of ammonium ferrous sulfate Vl --- blank consumption in milliliters (mL);
--- value V2 standard titration solution of ammonium ferrous sulfate in the sample solution volume consumed in milliliters (mL);
--- numerical molar mass M sodium azide (NaN3), in units of grams per mole (g/mol) (M = 65.01);
The mass values m --- sample in grams (g).
Parallel to the arithmetic average of the measurement results of the measurement result, the absolute difference determination results parallel to not more than 0.3%.
5.4.2 Iodimetry
5.4.2.1 Method summary
Under acidic conditions, the reaction of the sample with a potassium permanganate solution, adding an excess of potassium iodide and potassium permanganate reaction, iodine precipitated thiosulphate
Standard Solution sulfate titration, using starch indicator indicating the end point.
5.4.2.2 Reagents
5.4.2.2.1 sulfuric acid. 15.
5.4.2.2.2 manganese sulfate solution. 151g/L.
5.4.2.2.3 potassium permanganate solution. 3.5g/L.
5.4.2.2.4 potassium iodide solution. 300g/L (protected from light).
5.4.2.2.5 sodium thiosulfate standard titration solution. c (Na2S2O3) ≈0.1mol/L.
5.4.2.2.6 starch indicator. 10g/L.
5.4.2.3 Analysis of step
5.4.2.3.1 Weigh about 0.65g sample, accurate to 0.0002g, in 100mL volumetric flask, add about 70mL of water, shaking the sample
It was dissolved, diluted with water to the mark, the standby.
5.4.2.3.2 To a 250mL flask iodine, were added to 5mL manganese sulfate solution, 10 mL sulfuric acid solution was added 25mL pipette
Potassium permanganate solution was then pipetted into 20mL sample solution, gently shake 10min, capped, 5H left stand at room temperature (or
45 ℃ placed about 2.5h ~ 3h), during which need more shaken to facilitate reaction.
After completion of the reaction 5.4.2.3.3 bubbling was added 10mL potassium iodide solution, capped, gently shaken, seal, placed in the dark
At 20min, standard titration with sodium thiosulfate titration, when the iodine flask yellowish color of the solution was added 1mL starch indicator,
Shake until the color changes to dark gray, continue dropping, the color slowly faded, washed with water bottle and the bottle wall, shaking, carefully titrated to a final solution Yen
Discoloration clear colorless end point, the volume of sodium thiosulfate standard solution consumed in a note.
While the same treatment blank test solution, blank test solution without addition of sample addition, other types of addition of reagents and the same amount of the test solution.
5.4.2.4 calculation results
Sodium azide content by mass of sodium azide (of NaN3) fraction w1 meter, according to equation (2).
w1 =
c (V2-V1) × M × 11000
m × 20100
× 100% (2)
Where.
C accurate value of the concentration of the solution of sodium thiosulfate standard titration ---, units of moles per liter (mol/L);
V2 --- blank solution of sodium thiosulfate standard titration solution consumed volume value in milliliters (mL);
Vl --- consumption value standard titration sample solution volume of sodium thiosulfate solution, in milliliters (mL);
--- numerical molar mass M sodium azide (NaN3), in units of grams per mole (g/mol) (M = 65.01);
The mass values m --- sample in grams (g).
Parallel to the arithmetic average of the measurement results of the measurement result, the absolute difference determination results parallel to no more than 0.5%.
5.5 Determination of the content of sodium hydroxide and sodium carbonate
5.5.1 Method summary
Phenolphthalein as an indicator solution, sodium azide solution was titrated with hydrochloric acid standard solution titration, according to the consumption of hydrochloric acid, to determine hydroxide solution
The combined amount of sodium and sodium carbonate. An excess of sodium hydroxide and barium chloride standard titration solution in the test solution, measured by back titration carbonate
Sodium content. The binding amount obtained by subtracting the content of sodium carbonate content.
5.5.2 Reagents
5.5.2.1 barium chloride solution. 100g/L.
Before using phenolphthalein (5.5.2.4) as an indicator, titration reddish solution was adjusted with sodium hydroxide standard.
5.5.2.2 HCl Standard Solution. c (HCl) ≈0.1mol/L.
5.5.2.3 sodium hydroxide standard titration solution. c (NaOH) ≈0.1mol/L.
5.5.2.4 phenolphthalein indicator solution. 10g/L.
5.5.3 Analysis of step
Class product, first-class product weighed sample of about 10g, about 5g good product weighed sample to the nearest 0.01g, placed in 500mL Erlenmeyer flask,
Dissolved in approximately 100mL of carbon dioxide-free water. Add 2 drops of phenolphthalein indicator solution is quickly titrated to the end standard titration with hydrochloric acid solution. Write down
Milliliters of hydrochloric acid titrated consumption V1. Into 10mL pipetted standard titration solution of sodium hydroxide, barium chloride solution was added to about 10mL.
Stand for about 5min, again titrated with a standard solution of hydrochloric acid titrated to the end point. Note the milliliters of hydrochloric acid consumed V2 standard titration solution.
5.5.4 calculation results
Sodium content by mass sodium hydroxide (NaOH) w2 fraction meter, calculated according to formula (3).
w2 =
[C1V1- (10c2-c1V2)] M11000
m × 100%
(3)
Sodium carbonate content mass of sodium carbonate (of Na2CO3) w3 fraction meter, calculated according to formula (4).
w3 =
(10c2-c1V2) M21000
m × 100%
(4)
Where.
Accurate value of C1 --- hydrochloric acid solution concentration standard titration, in mol per liter (mol/L);
Vl --- first titration of hydrochloric acid consumed standard titration solution volume value in milliliters (mL);
Accurate value of the concentration of the solution of sodium hydroxide C2 --- standard titration, expressed in moles per liter (mol/L);
V2 --- second titration of hydrochloric acid consumed standard titration solution volume value in milliliters (mL);
Numerical molar mass Ml --- sodium hydroxide (NaOH), in units of grams per mole (g/mol) (M1 = 40.00);
--- M2 numerical molar mass of sodium carbonate (Na2CO3), in units of grams per mole (g/mol) (M2 = 105.99);
The mass values m --- sample in grams (g).
Parallel to the arithmetic average of the measurement results of the measurement result, the absolute difference determination results parallel to not more than 0.03%.
Determination of water-insoluble matter content of 5.6
5.6.1 Method summary
After the sample is dissolved in water, filtered, washed, dried and weighed.
5.6.2 Reagents
Ferric chloride solution. 100g/L.
5.6.3 instruments and equipment
5.6.3.1 sintered glass crucible. pore size filtration plate 5μm ~ 15μm.
5.6.3.2 Electric oven. temperature control 105 ℃ ± 2 ℃.
5.6.4 Analysis of step
A sample weighing approximately 50g, accurate to 0.01g, was placed 400mL beaker was added 200mL of water were dissolved at room temperature, in advance
At 105 ℃ ± 2 ℃ dried to constant mass sintered glass crucible by suction filtration, and the precipitate was washed well with hot water at room temperature until the filtrate was added
Ferric chloride solution so far is no longer red. The crucible was placed in a glass sand dried to a constant mass 105 ℃ ± 2 ℃ in the electric oven.
5.6.5 calculation results
Water insoluble matter mass fraction w4 basis, calculated according to formula (5).
w4 = m1-m2m × 100%
(5)
Where.
Numerical M1 --- sintered glass crucible and a water insoluble mass in grams (G);
--- M2 values quality glass crucible crucible sand in grams (G);
The mass values m --- sample in grams (g).
Parallel to the arithmetic average of the measurement results of the measurement result, the absolute difference determination results parallel to 0.02%.
5.7 Determination of chloride content
5.7.1 Method summary
In an acidic medium, was added a solution of silver nitrate and chloride ions of silver chloride to produce a white suspension, and turbidimetry visually simultaneously treated in the same
Comparing standard turbidimetric solution.
5.7.2 Reagents
5.7.2.1 nitric acid solution. 14.
5.7.2.2 silver nitrate solution. 17g/L.
5.7.2.3 chloride standard solution. 1mL solution of chlorine (Cl) 0.1mg.
Pipette with a pipette 10mL chloride standard solution according to HG/T 3696.2 formulated, a 100mL volumetric flask, dilute with water
To the mark. Placed inside the refrigerator, valid for one month.
5.7.3 Analysis of step
Weigh 1.00g ± 0.001g sample was placed in a 400mL beaker, add 20mL of water to dissolve. Nitric acid solution was slowly added dropwise 6mL, was dissolved
PH value of about 1, boil for about 5min, rinsed the cup wall with a little water, and then boiled for 3min ~ 5min, cooled. Move it to 50mL colorimetric
Tube was added silver nitrate solution 1mL, diluted with water to the mark. Placing 10min, the ratio of the standard turbidimetric solution, the turbidity was
It shall be not larger than the standard turbidimetric solution.
Turbidity standard solution was prepared ratio. standard solution was pipetted 1.0mL chloride in 50mL colorimetric tube, add about 30mL of water and 2mL
Diluted nitric acid solution, 1 mL silver nitrate solution, washed with water to the scale, shake for 10min and the sample for comparison.
Standard processing solution while turbidimetric test solution.
5.8 Determination of the sulfate content
5.8.1 Method summary
In an acidic medium, barium sulfate and barium sulfate to generate precipitate with standard turbidimetric solution comparison, to determine the sulfate content.
5.8.2 Reagents
5.8.2.1 hydrochloric acid solution. 11.
5.8.2.2 barium chloride solution. 20g/L.
5.8.2.3 sulfate standard solution. 1mL solution containing sulfate (SO4) 0.1mg.
Pipette with a pipette 10mL sulfate standard solution according to HG/T 3696.2 formulated, a 100mL volumetric flask, dilute with water
To the mark. This solution just before use.
5.8.2.4 starch indicator solution. 5g/L.
5.8.3 Analysis of step
Weigh 0.10g ± 0.001g sample, a 50mL colorimetric tube, was added 25mL of water, neutralized with hydrochloric acid solution to the blue litmus
Red paper, and an excess of 1mL. Then add starch indicator solution and 5mL 5mL barium chloride solution, shake. After 20min standard turbidimetric solution
Liquid ratio, which is not larger than a standard nephelometric turbidity solution.
Turbidity standard solution was prepared ratio. in 50mL colorimetric tube, adding 20mL water, 1mL pipetted into sulfate standard solution plus
1mL hydrochloric acid solution, 5mL 5mL starch indicator solution and barium chloride solution, shake. After 20min can be used for comparison.
5.9 Determination of nitrate content
5.9.1 Method summary
Sodium azide is decomposed (pH of 1-2) under acidic conditions. And removing the N-3 Trace NO-2, in a concentrated sulfuric acid medium, indigo disulfonate
Sodium is the sample fade oxide NO-3, and for a limited visual colorimetric standard solution.
5.9.2 Reagents
5.9.2.1 sulfuric acid.
5.9.2.2 sulfuric acid. 19.
5.9.2.3 sodium chloride solution. 100g/L.
5.9.2.4 indigo carmine solution. c (C16H8N2Na2O8S2) = 0.001mol/L (for the use of 10d).
5.9.2.5 nitrate standard solution. 1mL containing nitrate (NO3) 0.05mg.
Pipette with a pipette 5mL nitrate solution by standard HG/T 3696.2 formulated, a 100mL volumetric flask, dilute to
Mark and shake.
5.9.3 Analysis of step
5.9.3.1 Analysis
Weigh 0.10g ± 0.001g sample in 100mL beaker, add 20mL water dissolved, 5mL of sulfuric acid was added dropwise, heated to boiling
About 5min, washed with water cup wall, continues evaporated to a volume of about 8mL ~ 10mL, cooled, the solution was added 1mL of sodium chloride, and then adding the pipette
1mL into indigo carmine, with constant shaking at fast (10s ~ 15s) 10mL was added sulfuric acid (5.9.2.1), placed 10min, into
25mL, colorimetric tube was diluted with water to the mark, the alignment standard colorimetric solution, the blue color can not be shallower than the standard solution.
5.9.3.2 Preparation of standard colorimetric solution
Pipette with a pipette nitrate standard solution 1mL in 100mL beaker, add water, about 10mL, according to the operation from step 5.9.3.1 "plus
1mL sodium chloride solution into the "Start, and treated in the same sample simultaneously.
Note. Sample decomposition, and concentrated by boiling to be divisible by N-3 and NO-2, to eliminate the interference, but i......
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