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GB 10730-2008 English PDF

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GB 10730-2008: Primary chemical -- Potassium hydrogen phthalate
Status: Valid

GB 10730: Historical versions

Standard IDUSDBUY PDFLead-DaysStandard Title (Description)Status
GB 10730-2008369 Add to Cart 3 days Primary chemical -- Potassium hydrogen phthalate Valid
GB 10730-1989439 Add to Cart 4 days Primary chemical--Potassium hydrogen phthalate Obsolete

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Basic data

Standard ID: GB 10730-2008 (GB10730-2008)
Description (Translated English): Primary chemical -- Potassium hydrogen phthalate
Sector / Industry: National Standard
Classification of Chinese Standard: G61
Classification of International Standard: 71.040.30
Word Count Estimation: 16,190
Date of Issue: 2008-06-18
Date of Implementation: 2009-06-01
Older Standard (superseded by this standard): GB 10730-1989
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 first reference reagent potassium hydrogen phthalate traits, specifications, testing, inspection and marking and packaging rules. This standard applies to the first reference reagent potassium hydrogen phthalate test.

GB 10730-2008: Primary chemical -- Potassium hydrogen phthalate

---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.Potassium hydrogen phthalate ICS 71.040.30 G61 National Standards of People's Republic of China Replacing GB 10730-1989 The first reference reagent potassium hydrogen phthalate 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 10730-1989 "first reference reagent (capacity) of potassium hydrogen phthalate" Compared with GB 10730-1989, Lord To change the following. --- Standard name changed to "first reference reagent potassium hydrogen phthalate"; --- 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); --- Modify the sample pre-treatment conditions (1989 version 4.1.4.1, this edition 5.3.3.2); --- Modified after introducing nitrogen loading conditions (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 10730-1989. The first reference reagent potassium hydrogen phthalate Molecular formula. KHC8H4O4 Molecular Weight. 204.222 (according to 2005 international relative atomic mass).

1 Scope

This standard specifies the first reference reagent potassium hydrogen phthalate traits, specifications, testing, packaging and inspection rules and signs. This standard applies to the first reference reagent potassium hydrogen phthalate test.

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 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 9729 General method for determination of chloride Chemicals (GB/T 9729-2007, 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 JJG119-2005 Laboratory pH (acidity) meter JJG153 standard battery JJG1006 a standard material specification

3 Characters

This reagent is a colorless or white crystalline powder, soluble in water.

4 Specification

Potassium hydrogen phthalate as shown in Table 1. Table 1 Name the first reference Content (KHC8H4O4), /% 99.98 ~ 100.02 pH value (50g/L, 25 ℃) 3.8 ~ 4.2 Clarity test/number ≤2 Table 1 (continued) Name the first reference Water-insoluble, /% ≤0.003 Chloride (Cl), /% ≤0.002 Sulfur compounds (of SO4), /% ≤0.006 Sodium (Na), /% ≤0.005 Iron (Fe), /% ≤0.0005 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. M --- molar mass of the substance in 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 a platinum mesh electrode (surface area 60cm2) as a cathode using the cathode electrode reaction on the determination of potassium hydrogen phthalate containing Amount, with pH meter indicates end of the reaction. 2H ++ 2e = H2 ↑ 5.3.2 instruments and devices 5.3.2.1 pH meter. meet JJG119-2005 Chapter 4 "0.001" requirements. 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 (pH meter); 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). A cathode compartment (left) and an anode compartment (right) is made of quartz glass with a diameter of 50mm, 125mm high cylindrical. With between two chambers Diameter 20mm, length 80mm quartz glass tube level connections in the tube melting inside back cover sheet respectively No. 2,2,3 quartz glass sand core, thereby forming Into two intermediate chambers each with a branch of the piston, and the pressure by pumping nitrogen gas pressurization method the electrolyte solution out of the intermediate chamber. Small room The distance between the two sand core distance 20mm, two large chamber between the sand core is 40mm. Tight with a good pre-treated on the cathode chamber opening A white rubber stopper, a glass electrode is inserted through the stopper 2, respectively, a saturated calomel electrode 3, 4 nitrogen inlet, nitrogen outlet pipe 5, surface area 60cm2 platinum net cathode 6. The bottom of the cathode compartment 20mm long was stirred in a sealed Teflon tube about the magnet 9, polyethylene Platinum net cathode cover 10 is placed on top. An anode chamber having a 60mm × 70mm silver sheet 8, the bottom agar casting a rubber stopper 7. Electrolytic cell unit on magnetic stirrer workbench. Note. Preparation of agar plugs Weigh 3g agar, a potassium chloride solution was added 100mL (1mol/L) agar boil until dissolved, hot molding at the bottom of the anode compartment. 1 --- white rubber plug; 2 --- glass electrode; 3 --- saturated calomel electrode; 4 --- nitrogen inlet; 5 --- nitrogen outlet pipe; 6 --- platinum net cathode; 7 --- agar stopper; 8 --- silver flake anode; . 9 --- stirring; 10 --- polyethylene cover; . 11 --- piston 1; 12 --- piston 2. 2 cell apparatus of FIG. 5.3.3 Determination Weigh 74.55g potassium chloride, dissolved in water and diluted to 1000mL. 5.3.3.2 said sample The sample was placed in an open glass weighing bottle, dried at 110 ℃ 2h, cooled to room temperature in a desiccator. Small sample is placed in a polyethylene cup, weighing alternative method to the nearest 0.00001g. The quality of the sample shall be corrected for buoyancy correction See Appendix A. 5.3.3.3 Pre-titration Was added to the anode compartment 100mL potassium chloride solution, the cathode compartment was added 7.5g recrystallized potassium chloride was dissolved in 100mL non-dioxo Carbon water. With compression and decompression method of washing the cell wall and nitrogen outlet tube several times. The cell is placed in ice water, electrolysis Generating H + pH was adjusted to 5 with stirring from the manifold to the cathode compartment solution through high purity nitrogen 40min, removal of dissolved carbon dioxide, glass insert Electrode and a saturated calomel electrode. Adjust the nitrogen intake pipe into the air, maintaining a small nitrogen stream, the cathode chamber on the electrolyte solution level security Holding high purity nitrogen atmosphere. Open the piston 1 and the piston 2, so that the electrolytic solution to flow into the cathode chamber side tube about 2mm deep, the current 10.186mA Under the pre-titration curve for incremental method. After the pre-titration, with compression and decompression method of washing the intermediate chamber, and washed the cell wall, roof And nitrogen outlet pipe, recording the final pH value of the pre-draw titration curves (Figure 3). FIG point C is the titration end point, A point represents electrolysis stop The only time, B represents the point after the completion of the final pH of the washing solution. Exceeds the amount of charge (BC between the amount of charge corresponding) consumed by titration, The total amount of charge should be included in the titration. Remove the glass electrode and a saturated calomel electrode, with a teflon stopper stuffed respective two holes. 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, the use of reduced pressure so that the cathode compartment electrolyte solution filled in the middle chamber, close the piston 1 and piston 2, said good Together with the small sample cup put together the cathode chamber, the nitrogen is regulated to a smaller flow through the intake manifold to blow above the liquid surface, the cathode chamber Maintain a positive pressure to prevent air from entering. The timer is reset to zero in on the dummy load resistor adjusts the current value 101.86mA, connected to two electrodes, Start electrolysis. During electrolysis, at regular intervals, the sample was stirred with a magnetic stirrer while, and observe the changes in current value, subject to change Adjusted. When the sample is about 99.95% of the titration, cut off the power, note the time of electrolysis. As pre-titration, as with nitrogen pressurization and depressurization of the way, the intermediate chamber washing, sand core, wall, roof, and a nitrogen outlet tube several times. The cell was placed in ice water, stirred and the branch pipes passing a high purity nitrogen 30min, remove possible high current electrolysis into the carbon dioxide. Insert The glass electrode and a saturated calomel electrode wash. After the nitrogen, the same as the pre-titration curve, as in 10.186mA current, incremental pH value, B point represents the completion of the final pH value of the washing solution. Figure 4 endpoint titration curve 5.3.4 Calculation 5.3.4.1 potassium hydrogen phthalate content calculation Potassium hydrogen phthalate mass fraction, the value in the "%" 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); Numerical M --- potassium hydrogen phthalate 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 7.5g sample, add 100mL water dissolved by heating, turbidity shall not exceed HG/T 3484 stipulated. 5.6 Water insoluble matter Weigh 40g sample, add 400mL of water, heated and dissolved in the water bath for 1h, the determination according to the provisions GB/T 9738's. 5.7 Chloride 5g samples were weighed, dissolved in 30mL hot water, cooling, 10mL of nitric acid, filtered and diluted to 50mL. Take 10mL, press The provisions of GB/T 9729 Determination. The turbidity of the solution was not greater than the standard turbidity solution. Standard preparation turbid solution is to take the ratio of 0.02mg containing chloride (Cl) standard solution was diluted to 10mL, and at the same time with the same volume of test solution Sample processing. 5.8 sulfur compounds Weigh 0.5g sample was placed in a platinum crucible, add anhydrous sodium carbonate 0.2g, mixing, add 2mL water wet, evaporated on a water bath heated To completely carbonized, gradually warmed up to 700 ℃ and burning to white. As no white residue, add a small amount of cooling water wet, evaporated on a water bath, then blanch burn. Repeat this operation until the residue was completely white, cool, add water, 5mL dissolved (filtered if necessary) with hydrochloric acid (20%) and, dilute Diluted to 10mL, plus 5mL "ethanol (95%)", 0.5mL hydrochloric acid solution (20%), constantly shaking dropping 3mL barium chloride solution (250g/L), diluted to 25mL, shake, place 10min. The turbidity of the solution was not greater than the standard turbidity solution. Standard preparation turbid solution is to take the ratio of 0.03mg containing sulfate (SO4) standard solution, and treated in the same sample at the same time. 5.9 Sodium Determined according to the provisions of GB/T 9723-2007 of. 5.9.1 Instrument Conditions Source. sodium hollow cathode lamp; Wavelength. 589.0nm; Flame. acetylene - air. 5.9.2 Determination Weigh 4g sample was dissolved in water and diluted to 100mL. Take 10mL, a total of four. According to the provisions of GB/T 9723-2007 in 7.2.2 Measurement results calculated according to the provisions of 7.2.3. 5.10 Iron Weigh 1g sample was dissolved in 15mL of hot water, with hydrochloric acid solution (15%) the pH of the solution was adjusted to 2, according to GB/T 9739 of Determination provisions. The red solution should not be deeper than the standard colorimetric solution. Preparation of the standard solution is to take the colorimetric containing 0.005mg of iron (Fe) standard solution, the same treatment simultaneously with the sample. 5.11 Heavy Metal Weigh 4g sample was dissolved in 40mL of hot water. Take 30mL, add 0.2mL acetic acid solution (30%) and 10mL freshly prepared saturated Hydrogen sulfide water, shake, place 10min. The solution was dark can not be deeper than the standard colorimetric solution. Standard Preparation of color solution ratio is to take the remaining 10mL sample solution and standard solution containing 0.01mg of lead (Pb), diluted to 30mL, simultaneously with the same volume of the same treated sample solution.

6 Inspection rules

For mass-produced products, in accordance with the requirements of uniformity JJG1006 initial inspection. Bulk product inspection can be carried out by the preliminary dispensing, after extracting a sample formal test. Official test sample rule. when the total number of units is less than 200, the number of shape extraction unit less than 11; When the whole is greater than the number of units 200 When less than 500, like less than 12; when the total number of more than 500 units, like no less than 15.

7 Packaging and marking

According to GB 15346 requirements for packaging, storage and transportation, and flags are given, including. Packing unit. Class 3; Inner packaging. NB-4, NB-5, NB-6; Packaging forms. The specifications for the 600g/m2 of box board paper box, outer mounted electro-optical purple paper.

Appendix A

(Normative) Substance was weighed mass air buoyancy correction ρW -1 Where. ρK --- when the density of the air weighing in grams per cubic centimeter (g/cm 3); ρW --- density of the material to be weighed in grams per cubic centimeter (g/cm 3); pf --- weights density in grams per cubic centimeter (g/cm 3). Formula (A.1) in. Air density (ρK), in grams per cubic centimeter (g/cm 3), according to equation (A.2) Calculated. ρK = 0.00129 273.15 Where. P1 --- atmospheric pressure value in units of kilopascals (kPa); P2 --- vapor pressure of water at room temperature value in units of kilopascals (kPa); (A.2) in the formula. The value of water vapor pressure (P2), in units of kilopascals (kPa), according to equation (A.3) Calculated. P2 = W × P3 (A.3) Where. W --- values of relative humidity of air in%; Numerical P3 --- saturated vapor pressure of wate......
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