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GB 10733-2008 English PDF

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GB 10733-2008: Primary chemical -- Sodium chloride
Status: Valid

GB 10733: Historical versions

Standard IDUSDBUY PDFLead-DaysStandard Title (Description)Status
GB 10733-2008419 Add to Cart 3 days Primary chemical -- Sodium chloride Valid
GB 10733-1989399 Add to Cart 3 days Primary chemical--Sodium chloride Obsolete

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GB/T 9722   HG/T 3489   GB/T 9741   GB 10731   GB 10732   GB 10730   

Basic data

Standard ID: GB 10733-2008 (GB10733-2008)
Description (Translated English): Primary chemical -- Sodium chloride
Sector / Industry: National Standard
Classification of Chinese Standard: G61
Classification of International Standard: 71.040.30
Word Count Estimation: 18,157
Date of Issue: 2008-06-18
Date of Implementation: 2009-06-01
Older Standard (superseded by this standard): GB 10733-1989
Quoted Standard: GB/T 602; GB/T 603; GB/T 609; GB/T 6682; GB/T 9723-2007; GB/T 9724; GB/T 9727; GB/T 9728; GB/T 9735; GB/T 9738; GB/T 9739; GB 15346; HG/T 3484; JJG 99; JJG 116; JJG 153; JJG 1006
Regulation (derived from): Announcement of Newly Approved National Standards No. 10 of 2008 (total 123)
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 characteristics of sodium chloride in the first reference reagent, specifications, testing, inspection and marking and packaging rules. This standard applies to the first reference reagent sodium chloride test.

GB 10733-2008: Primary chemical -- Sodium chloride

---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.
Primary chemical.Sodium chloride ICS 71.040.30 G61 National Standards of People's Republic of China Replacing GB 10733-1989 The first reference reagent sodium chloride Posted 2008-06-18 2009-06-01 implementation Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China Standardization Administration of China released

Foreword

The standard Chapter 4 5.3.3,5.3.4.1 are mandatory, other provisions are recommended. This standard replaces GB 10733-1989 "first reference reagent (capacity) sodium chloride", compared with GB 10733-1989, the major change Of the following. --- Standard name changed to "first reference reagent sodium chloride"; --- Increasing the normative references (1989 edition Chapter 2, Section 2 of this edition); --- Modify the description of the determination of the principles of the (1989 version 4.1.1, this version 5.3.1); --- Modify the constant current coulometric apparatus diagram (1989 version 4.1.3.4, this edition 5.3.2.4); --- Improve titration steps (1989 version 4.1.4.3, this edition 5.3.3.4); --- Modify the inspection rules (1989 edition Chapter 5; Chapter 6 of this edition); --- Increasing the content of the calculation method of Uncertainty (Excerpts Appendix B) was measured; --- Canceled Appendix B, Appendix C (1989 edition Appendix B, Appendix C). This standard appendix A normative appendix, Appendix B is an informative annex. The standard proposed by China Petroleum and Chemical Industry Association. This standard by the Chemicals Branch of the National Chemical Standardization Technical Committee. This standard is drafted by. China Institute of Metrology, Beijing Institute of Chemical reagents. The main drafters of this standard. FEI brother, Wu Bing, Han Baoying, strong Jing Lin. This standard replaces the standards previously issued as follows. --- GB 10733-1989. The first reference reagent sodium chloride Molecular formula. NaCl Molecular Weight. 58.443 (according to 2005 international relative atomic mass).

1 Scope

This standard specifies the characteristics, specifications, testing, inspection rules, and packaging and marking the first reference reagent sodium chloride. This standard applies to the first reference test reagent sodium chloride.

2 Normative references

The following documents contain provisions which, through reference in this standard and become the standard terms. For dated references, subsequent Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to the agreement are based on research Whether the latest versions of these documents. For undated reference documents, the latest versions apply to this standard. GB/T 602 Determination of impurities in chemical reagents prepared standard solution (GB/T 602-2002, ISO 6353-1. 1982, NEQ) with GB/T 603 chemical reagent test method Preparations of articles (GB/T 603-2002, ISO 6353-1 with. 1982, NEQ) GB/T 609 chemical reagent - General method for determination of total nitrogen (GB/T 609-2006, ISO 6353-1. 1982, NEQ) GB/T 6682 analytical laboratory use specifications and test methods (GB/T 6682-2008, ISO 3696. 1987, MOD) GB/T 9723-2007 Chemicals flame atomic absorption spectrometry General GB/T 9724 General rule for determination of pH chemical reagent (GB/T 9724-2007, ISO 6353-1. 1982, NEQ) GB/T 9727 General method for the determination of phosphate chemical reagent (GB/T 9727-2007, ISO 6353-1. 1982, NEQ) GB/T 9728 General method for determination of chemical reagents sulfate (GB/T 9728-2007, ISO 6353-1. 1982, NEQ) GB/T 9735 General method for determination of heavy metals Chemicals (GB/T 9735-2008, ISO 6353-1. 1982, NEQ) GB/T 9738 Chemicals water insoluble determination General method (GB/T 9738-2008, ISO 6353-1. 1982, NEQ) GB/T 9739 General method for determination of iron chemical reagents (GB/T 9739-2006, ISO 6353-1. 1982, NEQ) GB 15346 chemical reagent packaging and marking HG/T 3484 standard chemical reagents glass emulsion and clarity standards JJG99 weight JJG116 standard resistor JJG153 standard battery JJG1006 a standard material specification

3 Characters

This reagent is a white crystalline powder, soluble in water, almost insoluble in ethanol.

4 Specification

Sodium chloride as shown in Table 1. Table 1 Name the first reference Content (NaCl), /% 99.98 ~ 100.02 pH value (50g/L, 25 ℃) 5.0 ~ 8.0 Table 1 (continued) Name the first reference Clarity test/number ≤2 Water-insoluble, /% ≤0.003 Iodide (I), /% ≤0.001 Bromide (Br), /% ≤0.005 Sulphate (SO4), /% ≤0.001 Total nitrogen (N), /% ≤0.0005 Phosphate (PO4), /% ≤0.0005 Hexacyanoferrate (Ⅱ) salt (with Fe (CN) 6 meter), /% ≤0.0001 Magnesium (Mg), /% ≤0.001 Potassium (K), /% ≤0.01 Calcium (Ca), /% ≤0.002 Iron (Fe), /% ≤0.0001 Barium (Ba), /% ≤0.001 Heavy metals (Pb), /% ≤0.0005

5 Test

5.1 Warning Reagents used in this test method are toxic or corrosive, some of the testing process can lead to dangerous situations, the operator should take Appropriate safety and health practices. 5.2 General Provisions Unless specified otherwise in this chapter, the use of reagent purity should be more analytical, standard solution, preparations and products, according to GB/T 602, GB/T 603 provisions of preparation, test water should be consistent with GB/T 6682 specifications in two water samples according to precise weighing 0.01g, used Solution "%" are represented by the mass fraction. High purity nitrogen gas should be used. 5.3 Content 5.3.1 Principle of the method Coulomb analysis is performed by measuring a quantitative analysis of material from one electrode reaction, or a substance to be analyzed and the electrode reaction Charge (coulombs) chemical reaction product was quantitatively consumed to quantitative analysis. Coulometry principle is based on the law Where. Molar mass M --- material in units of grams per mole (g/mol); --- Like the number of electron transfer; F --- Faraday constant ampere seconds per mole of (A · s/mol); I --- the current solution by electrolysis, in amperes (A); Constant current precision coulometric titration method is based on a constant current through the electrolytic cell, so that the working electrode electrolysis to produce a titrant with cell The test substance quantitative reaction, electrochemical method to indicate the end of the reaction, the consumption of electricity by electrolysis calculated according to Faraday's law The amount of titrant to calculate the content of the test substance. This method uses more than 99.999% pure silver as the anode, electrolysis silver ion to be measured sodium chloride-containing reaction assay Amount, potentiometric method indicates the end of the reaction. 5.3.2 instruments and devices 5.3.2.1 DVM. accuracy 0.1mV. 5.3.2.2 Weight. meet JJG99 verification requirements. G group, the annual variation of less than 10μg; mg group, the annual variation of less than 4μg. 5.3.2.3 heated fuel tank. temperature control accuracy of ± 0.01 ℃. 5.3.2.4 Coulomb constant current device diagram (see Figure 1). 1 --- high precision timing constant current source; 2 --- 7½-Meter; 3 --- electrolytic cell; 4 --- end indicator (digital voltmeter); 5 --- dummy load resistor; 6 --- Standard resistance; 7 --- galvanometer; 8 --- temperature standard battery pack; . 9 --- step switch; 10 --- heated fuel tank. Figure 1 Schematic diagram of the constant current coulometric a) high-precision timing constant current source. stability is better than one hundred thousandth of the dynamic characteristics of a good steady flow DC power supply, with 1.0186 × 1.0186 × 10mA and 100mA two output current, the current value is determined by the compensation method; the minimum timing resolution 0.1ms, current Timing and synchronization of less than 0.1ms. b) temperature control standard battery pack. should meet the requirements of JJG153. Range 1V, annual variation of less than 5μV. c) Standard resistance. should meet the requirements JJG116 of. Relative uncertainty is generally not more than 3 × 10-6. d) direct radiation galvanometer. resistance < 100Ω, critical external resistance < 1000Ω, dividing the value of < 3 × 10-9A. 5.3.2.5 electrolytic cell apparatus (see Figure 2). An anode compartment (left) and a cathode chamber (right side) is made of quartz glass with a diameter of 50mm, 125mm high cylindrical. With between two chambers Diameter 20mm, glass horizontal length 80mm connections in the tube melting inside back cover sheet respectively No. 2,2,3 glass sand core, thereby forming two Have an intermediate chamber manifold with the piston, and the pressure by pumping nitrogen gas pressurization method the electrolyte solution out of the intermediate chamber. Small room two sand core The distance between the distance 20mm, two large chamber between the sand core is 40mm. The anode chamber mouth tight with a good pre-treated white rubber Plug 1 is inserted through the stopper rods were anode 2 silver, 3 nitrogen inlet, nitrogen outlet pipe 4, double salt bridge calomel electrode 5, silver indicator electrode rod 6, 7 sample dropper. The bottom of the anode compartment has 20mm long was stirred in a sealed Teflon tube about the magnet 9. The anode chamber and the intermediate chamber Both black and red cloth cover with wrap, in order to avoid decomposition of the reaction product to light. Platinum mesh cathode cathode chamber 10, the bottom of a cast silicone gel Plug 11. Electrolytic cell unit on magnetic stirrer workbench. Note. Preparation of silicone gel plug Under stirring, a nitric acid solution to 40mL (2mol/L) was added slowly sodium silicate solution (250g/L) until the solution was slightly acidic when heated to boiling, cooled, Into the electrolytic cell cathode chamber, was added slowly under continued stirring sodium silicate solution (250g/L), until the colloid appears. 1 --- white rubber plug; 2 --- silver anode rod; 3 --- nitrogen inlet; 4 --- nitrogen outlet pipe; 5 --- double salt bridge SCE; 6 --- Silver Slugger indicator electrode; 7 --- sample dropper; 8 --- sample port; . 9 --- stirring; 10 --- platinum net cathode; . 11 --- silicon gel plug; 12 --- piston 1; Pistons 13 --- 2. 2 cell apparatus of FIG. 5.3.3 Determination 5.3.3.1 Formulation 7mL amount of nitric acid, diluted to 1000mL. 139mL amount of nitric acid, diluted to 1000mL. 5.3.3.1.3 saturated sodium nitrate solution The sodium nitrate dissolved in nitric acid solution (0.1mol/L), and up to the precipitation of crystals. Weigh 0.85g of silver nitrate, dissolved in water, add a few drops of nitric acid, diluted to 1000mL. Weigh 0.58g of sodium chloride dissolved in water and diluted to 1000mL. 5.3.3.1.6 electrolyte solution Weigh 170g sodium nitrate, plus 114.6mL acetic acid (glacial acetic acid) (excellent pure) and 1300mL "ethanol (95%)" (excellent pure), diluted To 2000mL. 5.3.3.2 said sample The sample was placed in a platinum crucible, calcined at 500 ℃ 6h, cooled to room temperature in a desiccator. Small sample is placed in a polyethylene cup, weighing alternative method to the nearest 0.00001g. Sample mass for buoyancy correction, the correction side See Appendix A. Law 5.3.3.3 Pre-titration Cathode chamber 100mL saturated solution of sodium nitrate, in order to eliminate any traces of halide ions cause an error of measurement, in general Silver nitrate solution was added 1mL previously (0.005mol/L). The anode compartment was added 100mL electrolyte solution. At 5 ℃ passing a high purity nitrogen 1h oxygen. To draw a small amount of electrolyte solution to the anode compartment intermediate chamber (solution depth approximately in the middle of the indoor 2mm). Added to the anode chamber 20 drops of sodium chloride solution (0.01mol/L), the anode chamber and the intermediate chamber with the red and black cloth strict. In 10.186mA current electrolysis 90s, with increasing Method for pre-titration curve. After the pre-titration, with compression and decompression method of washing the intermediate chamber, and washed the cell wall, eventually recording means Shown potential. Pre-draw titration curves (Figure 3). Fig. C is a pre-titration end point, A point represents electrolysis stop time, B indicating the completion point Finally, E-value of the solutions after washing. The amount of charge (amount of charge between the respective BC) consumed more than titration, it should be included in the total charge titration. Figure 3 pre-titration curve 5.3.3.4 titration end point and seek In order to open the piston 1 and the piston 2, so that the anode chamber by vacuum intermediate chamber filled with electrolyte solution, closed piston. Sheng to polyethylene sample Ene cup add a few drops of water, make it most dissolved. When loading with a wash solution dropper dropper to suck, the rubber plug is inserted in a hole in the back. And sample cup into the pre-titration undissolved anode compartment of the electrolytic solution, the solution was stirred to make it dissolved. The anode compartment electrolyte solution Continue through the surface of high purity nitrogen. On the dummy load current is adjusted to 101.86mA, connected to two electrodes, stirring was stopped, start electrolysis. When electrolysis When silver ions produced the desired amount of the sample to reach half of the reaction, with stirring, was added a solution of about half of the dropper, stirring was stopped, and then After 500s ~ 1000s, still under stirring, the dropper was all finished, stirring was stopped when the amount of silver ions produced by electrolysis phase When in the sample required 99.90% to 99.95% per volume, stop electrolysis. First open stirring, 5min after using compression and decompression method of washing Polyester intermediate chamber, and washed the cell wall, draw dropper anode compartment electrolyte solution was washed several times, from the middle-high purity nitrogen 40min after the branch pipe, Remove the polyethylene small cup from the anode chamber. In 10.186mA current, pre-titration with the same cell on the ice, as the end point of the titration curve by incremental method, had to end after It can make some more. Anode compartment electrolyte solution washed sand core, the walls several times, and then washed several times dropper, note reading, drawing Finally, E-value of the solutions after a wash. Figure 4 endpoint titration curve 5.3.4 Calculation 5.3.4.1 sodium chloride mass fraction calculated The mass fraction of sodium chloride and its value is "%" means, according to equation (2). = QPQT × 100 = I (2) Where. --- The QP electrolytic sample charge amount actually consumed by the coulombs (the C); Theoretical amount of charge required for electrolysis of the QT --- sample, in units of coulombs (the C); I --- the current solution by electrolysis, in amperes (A); --- The M NaCl numerical molar mass in grams per mole (g/mol); --- Like the number of electron transfer; F --- Faraday constant ampere seconds per mole of (A · s/mol); E --- standard electromotive force in volts (V); R --- standard resistor in ohms (Ω). (2) In the formula. Where. I1 --- large current electrolysis current value in units of milliamperes (mA); I2 --- pre-titration end point and seek current value, in milliamperes (mA); Uncertainty and assay results of calculation 5.3.4.2 Expanded uncertainty assay results should generally be less than 0.02% (k = 2), the calculation method, see Appendix B. Determined according to the provisions of GB/T 9724's. 5.5 Clarity test Clarity Standard No. 2 Weigh 25g sample was dissolved in 100mL of water, turbidity is not greater than HG/T 3484 stipulated. 5.6 Water insoluble matter Weigh 50g sample was dissolved in 200mL of water in the water bath for 1h after, according to the provisions of GB/T 9738 Determination. 5.7 iodide Weigh 11g sample was dissolved in 50mL of water and transferred to a separatory funnel, add 2mL 5mL hydrochloric acid and ferric chloride solution (100g/L), shake Uniform, placed 5min. Add 10mL of carbon tetrachloride, shaking 1min, standing layer, carbon tetrachloride layer was collected in colorimetric tube, and then each time with 5mL carbon tetrachloride extracted twice, into the colorimetric tube (reservations aqueous sample). The organic layer was purple No deeper than the standard colorimetric solution. Preparation of standard color solution is to take the ratio of 1g sample and containing 0.1mg of iodine (I) and a standard solution containing 0.5mg of bromine (Br) standard solution, The same treatment simultaneously with the sample (standard water retention). 5.8 bromide The aqueous sample 5.7 separating funnel to retain each extracted twice with 5mL carbon tetrachloride, carbon tetrachloride was discarded, added to the solution 35mL sulfuric acid solution (1 + 1) and 10mL chromic acid solution (100g/L), shake for 5min. Add 10mL of carbon tetrachloride, shaking 1min, place stratification. Carbon tetrachloride layer was collected in colorimetric tube, and then 5mL carbon tetrachloride extraction, into a colorimetric tube. The organic layer was Yellow No deeper than the standard colorimetric solution. Preparation of standard color solution is to take the ratio of the standard solution 5.7 with an aqueous solution of 5.8 to retain the specimen while the same treatment. 5.9 sulfate Weigh 1g sample was dissolved in 20mL of water, add 0.5mL hydrochloric acid solution (20%) after acidification, according to the provisions of GB/T 9728 Determination. The turbidity of the solution was not greater than the standard turbidity solution. Standard preparation turbid solution is to take the ratio of 0.01mg containing sulfate (SO4) standard solution, and treated in the same sample at the same time. Total nitrogen content of 5.10 Weigh 2g sample was dissolved in water and diluted to 140mL, determined according to the provisions of GB/T 609's. The yellow solution can not be deeper than the standard ratio Color solution. Preparation of the standard developing solution containing 0.01mg ratio is taken of nitrogen (N) standard solution, the same treatment simultaneously with the sample. 5.11 Phosphate Weigh 1g sample was dissolved in an appropriate amount of water, add 2 drops of saturated 2,4-dinitrophenol indicator solution, a solution of nitric acid solution (13%) just to yellow Disappeared after diluted to 10mL, according to the provisions of GB/T 9727 Determination. The organic layer was blue can not be deeper than the standard colorimetric solution. Preparation of the standard developing solution containing 0.005mg is to take the ratio of phosphate (PO4) standard solution, the same treatment simultaneously with the sample. 5.12 hexacyanoferrate (Ⅱ) salt Weigh 3.5g sample was dissolved in 12mL of water, add 0.2mL sulfuric acid solution (20%), plus 0.2mL iron - ferrous mixture, shake, Place 2min. Add 1mL sodium dihydrogen phosphate solution (200g/L), shake for 30min. The solution was blue No deeper than the standard ratio Color solution. Preparation of standard color solution is to take the ratio of 1g sample containing 0.0025mg and the hexacyanoferrate (Ⅱ) salt [Fe (CN) 6] standard solution, and Sample while the same treatment. 5.13 Magnesium Determined according to the provisions of GB/T 9723-2007 of. 5.13.1 Instrument Conditions Source. magnesium hollow cathode lamp; Wavelength. 285.2nm; Fl......
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