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GB 12593-2007Working chemical - Ethylenediaminetetraacetic acid disodium salt (English PDF)

工作基准试剂 乙二胺四乙酸二钠

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Issued by

General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China; Standardization Administration of China

Level / Type

National · Mandatory

Issue date

October 25, 2007

Implementation date

April 1, 2008

Scope

GB 12593-2007 is the English-translated version of 工作基准试剂 乙二胺四乙酸二钠.

China's mandatory national standard for disodium ethylenediaminetetraacetate as a working chemical. EDTA disodium is the reagent of complexometric titration, and the working grade is what laboratories consume in quantity: every water hardness determination, every calcium and magnesium analysis in cement, food and clinical chemistry, and the metal determinations of metallurgical control all run on it. The primary standard grade covered by GB 10734 exists to certify those solutions; this grade exists to make them. What the specification has to control is the hydration state and the free acid, because the disodium salt is normally the dihydrate and a batch that has partly dried or taken up water weighs out to a different molarity than the label implies. The standard specifies the requirements, the impurity limits, the drying conditions and the test methods.

Document preview — GB 12593-2007

National Standard of the People's Republic of China

ICS
71.040.30
Classification
G61

Issued by: General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China; Standardization Administration of China

Contents

  • 1 Scope
  • 2 Normative references
  • 3 Chloride (Cl), /% <=
  • 4 Specification
  • 5 Test
  • 5.0 Network together passing the test Clarity test No. <=
  • 5.3.2 Content
  • 5.5 Test network together
  • 5.5.1 Preparation of test solution and preparation
  • 5.10 Iron
  • 6 Inspection rules
  • 7 Packaging and marking

Foreword

The standard Chapter 4, 5.3.1,

5.3.2 mandatory, other provisions are recommended. This standard replaces GB 12593-1990 "job reference reagent (capacity) disodium edetate," and GB 12593-1990 phase Than the main changes are as follows:

--- Standard name to "work reference reagent disodium edetate";

--- Modify the Content Measurement (before version 4.1, this version 5.3). The standard proposed by China Petroleum and Chemical Industry Association. This standard by the National Standardization Technical Committee Chemistry Chemicals Branch (SAC/TC63/SC3) centralized. This standard is drafted by: Beijing Institute of chemical reagents. Participated in the drafting of this standard. Guangdong Guanghua Chemical Factory Co., Ltd. The main drafters of this standard. Han Baoying, strong Jing Lin, Wang Yuhua, Chenhan Zhao. This standard was first published in 1977, in 1990 the first amendment. Working Standard reagent disodium edetate Molecular formula. C10H14N2O8Na2 · 2H2O Structure. CH2 NaO CH2 HO CH 2 CH 2N CH2 OH CH2 ONa · 2H2O Molecular weight. 372.24 (according to 2003 international relative atomic mass)

1 Scope

China's mandatory national standard for disodium ethylenediaminetetraacetate as a working chemical. EDTA disodium is the reagent of complexometric titration, and the working grade is what laboratories consume in quantity: every water hardness determination, every calcium and magnesium analysis in cement, food and clinical chemistry, and the metal determinations of metallurgical control all run on it. The primary standard grade covered by GB 10734 exists to certify those solutions; this grade exists to make them. What the specification has to control is the hydration state and the free acid, because the disodium salt is normally the dihydrate and a batch that has partly dried or taken up water weighs out to a different molarity than the label implies. The standard specifies the requirements, the impurity limits, the drying conditions and the test methods.

This standard specifies the operating reference reagent

--- disodium edetate traits, specifications, testing, packaging and inspection rules and signs. This standard applies to the reference reagent titration analysis work

--- disodium edetate 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. Preparation of

GB/T 601 chemical reagent standard titration solution

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 6682-1992, neq ISO 3696. 1987)

GB/T 9724 General rule for determination of pH chemical reagent ( GB/T 9724-2007, 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 9729 General method for determination of chloride Chemicals ( GB/T 9729-2007, ISO 6353-1. 1982, NEQ)

GB/T 9735 General method for determination of heavy metals Chemicals ( GB/T 9735-1988, eqv ISO 6353-1. 1982)

GB/T 9739 General method for determination of iron chemical reagents ( GB/T 9739-2006, ISO 6353-1. 1982, NEQ)

GB 10738 Job reference reagent titration Determination General Weighing

GB 15346 chemical reagent packaging and marking

3 Chloride (Cl), /% <=

0.004 Sulphate (SO4), /% <=

0.01 Nitrilotriacetic acid (C6H9NO6), /% <=

0.05 Iron (Fe), /% <=0.0005 Copper (Cu), /% <=0.00025 Heavy metals (Pb), /% <=0.001

4 Specification

Disodium edetate specifications shown in Table 1. Table 1 specifications of disodium ethylenediaminetetraacetate Name reference work Content (C10H14N2O8Na2 · 2H2O), /% 99.95 ~ 100.05 pH value (50g/L, 25 °C) 4.0 ~

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 standard titration solution, standard solution, preparations and products, according to GB/T 601, GB/T 602, Regulations preparation, test water should be consistent with GB/T 6682 specifications in three water samples according to precise weighing 0.01g, the use of GB/T 603's Solution "%" are represented by the mass fraction.

5.3 Content Measured according to GB 10738 requirements.

5.3.1 standard titration solution of zinc chloride standard titration substance disodium edetate Weigh 0.5g saturated solution of magnesium nitrate (with excess magnesium nitrate crystals) humidistat placed in standard material 7d after edetate Disodium nearest 0.00001g. Placed in a reaction flask, add 100mL of hot water to dissolve, cooling, 10mL of ammonia - ammonium chloride buffer solution A (PH value of 10), with zinc chloride standard titration solution [Ba (ZnCl2) = 0.05mol/L] titration, add 3 drops of chrome black T indicator solution near the end (5g/L), continue titration until the solution changed from blue to red purple. Weighing disodium EDTA standard titration solution should be accurate to 0.0001g. Determination

5.3.2 Content

5.3.1 Determination of the same, instead of the standard sample material. Disodium edetate mass fraction, the value in the "%" means, according to equation (1). (1) Where. b

--- standard substance disodium ethylene diamine tetra-acetic acid content (mass fraction), the value to "%" means; Determined according to the provisions of GB/T 9724's.

5.5.1 Preparation of test solution and preparation

5.5.1.1 sample solution Weigh 0.327g sample is dissolved in hot water, cooled and transferred to 100mL volumetric flask, dilute to the mark.

5.5.1.2 sodium carbonate solution Weigh 0.100g previously dried at 200 °C 2h calcium carbonate, placed in 100mL flask, add 10mL water and 0.4mL hydrochloric acid Solution (20%), was dissolved with aqueous ammonia solution (10%) and diluted to the mark.

5.5.1.3 copper sulphate solution Weigh 0.250g of copper sulfate (CuSO4 · 5H2O), placed in 100mL volumetric flask, dissolved in water, dilute to the mark.

5.5.2 Determination 5.00mL amount of the sample solution, add 3 drops of ammonia solution (10%) and 2.5mL ammonium oxalate solution (40g/L), shaking continuously, Plus 5.00mL sodium carbonate solution, the solution should be transparent. If, after shaking 1min, the solution is still cloudy, plus 0.2mL sample solution, shake After moving 1min, transparent solution strain. Amount of sample solution 5.00mL, 0.5mL add ammonia solution (1%) and 0.5mL hexacyanoferrate (II) solution of potassium (100g/L), Constantly shaking plus 4.8mL copper sulfate solution, the solution should be bluish green, not a red.

5.6 Clarity test Weigh 5g sample was dissolved in 100mL of water. Turbidity is not greater than HG/T 3484 standard stipulated clarity 3.

5.7 Chloride Weigh 0.5g sample was dissolved in 10mL water, add 2mL solution of nitric acid (25%), and shaken until complete precipitation of the precipitation, filtration, water Washed three times, the combined filtrate and washings were diluted to 20mL, determined according to the provisions of GB/T 9729's. The turbidity of the solution was not greater than the standard ratio Turbid solution. Standard preparation turbid solution is to take the ratio of 0.02mg containing chloride (Cl) standard solution was diluted to 20mL, and at the same time with the same volume of test solution Sample processing.

5.8.1 Preparation of test solution I Weigh 3g sample placed in a platinum dish, slowly heating carbonization burning to white at 600 °C. If necessary, add 5mL water, evaporated to dryness, and then at 600 °C burning, iterative process until the residue completely white. Add water 20mL, 6mL solution of nitric acid solution (25%), evaporated on a water bath. Residue Dissolved in hot water, cooled and diluted to 30 mL (filtered if necessary).

5.8.2 Determination Amount of test solution 5mL I (5.8.1), diluted to 20mL, determined according to the provisions of GB/T 9728's. The solution was not greater turbidity Standard turbidity solution. Standard preparation turbid solution is to take the ratio of 0.05mg containing sulfate (SO4) standard solution was diluted to 20mL, at the same time with the same volume of test solution The same treatment.

5.9 nitrilotriacetic acid

5.9.1 Instruments Pulse or oscilloscope pole spectrometer.

5.9.2 Test conditions Working electrode. dropping mercury electrode; Reference electrode. silver - silver chloride or saturated calomel electrode; Electrode. platinum electrode; Sensitivity. properly selected; Way oxygen. nitrogen 5min above; Scanning potential range. -0.6V ~ -1.1V.

5.9.3 Determination Weigh 1g sample plus 30mL dissolved in hot water, cooling, pH of the solution was adjusted with sodium hydroxide solution (100g/L) 10.5 ~ 10.7 (Control with pH meter). Solution of cadmium chloride solution (50g/L) to a solution of trace precipitation [should be maintained during the addition the solution pH value of 10.5 ~ 10.7. If necessary, adjusting with sodium hydroxide solution (100g/L)], was diluted to 50mL with sodium hydroxide solution (0.02g/L). With Polarograph Determination of which polarographic wave height shall not exceed half of the standard wave height. Standard is taken containing 0.5mg nitrilotriacetic acid (C6H9NO6) 1g sample and standard solution, add 30mL dissolved in hot water, cooling, and The same volume of sample solution at the same time the same treatment.

5.10 Iron

5.10.1 Preparation of the test solution II Weigh 3g sample placed in a platinum dish, slowly heating carbonization burning to white at 600 °C. If necessary, add 5mL water, evaporated to dryness, and then at 600 °C burning, iterative process until the residue completely white. Add 10mL of water to dissolve the residue, was added dropwise a solution of hydrochloric acid (20%) and the excess 1mL, For 10min in a water bath, diluted to 30mL.

5.10.2 Determination The amount of 10mL test solution II (5.10.1), with aqueous ammonia solution (10%) 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 developing solution containing 0.005mg is to take the ratio of iron (Fe) standard solution, add 0.2mL hydrochloric acid solution (20%), diluted to 10mL, simultaneously with the same volume of the test solution treated similarly. Copper

5.11 The amount of 10mL of the test solution II (5.10.1), add 5mL ammonium citrate solution (200g/L), the pH was adjusted with aqueous ammonia solution 9, and the excess 1mL, diluted to 25mL. Add 1mL diethyl dithiocarbamate solution (1g/L), shake, add 5mL isoamyl alcohol Extraction, shaking 1min, the yellow organic phase can not be deeper than the standard colorimetric solution. Preparation of standard color solution is to take the ratio of 0.0025mg containing copper (Cu) standard solution was diluted to 10mL, and at the same time with the same volume of test solution Sample processing.

5.12 Heavy Metal Measure 20mL test solution I (5.8.1), with aqueous ammonia solution (10%) of the solution was adjusted to pH 4, according to GB/T 9735 regulations Fixed determination. The solution was dark can not be deeper than the standard colorimetric solution. Preparation of the standard developing solution containing 0.02mg ratio is taken of lead (Pb) standard solution, add 0.2mL hydrochloric acid solution (20%), diluted to 20mL, with the same volume of test solution at the same time the same treatment.

6 Inspection rules

According to the provisions of HG/T 3921 is sampled and acceptance.

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. GB 12593-2007 "job reference reagent disodium edetate" National Standard No. 1 amendments The amendments approved by the National Standardization Management Committee on March 24, 2009, with effect from July 1, 2009 implementation. Modify as follows "Work reference reagent disodium edetate," the national standard GB 12593-2008.

5.3.1 Terms of the fourth line of the "Weighing disodium EDTA standard titration solution should be accurate to 0.0001g." Revised as follows: "Weighing zinc chloride standard titration solution should be accurate to 0.0001g."

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